4.c.i). Owing to the strong N≡N bond and its weak surface binding (Rapcewicz et al., 1997; Guo et al., 1998; Lymperakis and Neugebauer, 2009), nitrogen is more readily released in neutral form, whereas the lower evaporation field of Ga enables its ionization under the same conditions (Tsong, 1978b). Consequently, at low-coordination surface sites exposed to higher laser-induced heating, the available thermal energy is sufficient to release both Ga and N₂, while the electric field preferentially ionizes only Ga. Analysis of background counts further confirms that the apparent nitrogen deficit measured at high Eᵢₗs (1 - 10 pJ) originates from the sublimation of neutral N₂ rather than from uncorrelated evaporation of ionic N₂ species. Even when the full background signal is attributed to N₂, the measured nitrogen counts remain insufficient to achieve a 1:1 Ga:N ratio.

**Role of electric field.** A comprehensive investigation of the field-evaporation behaviour of bulk GaN growth along the (0001) direction as a function of the analysis parameters was reported by Mancini et al. (Mancini et al., 2014a) and by Di Russo et al. (2018) (Russo et al., 2018). Measurements were conducted using three complementary protocols: (i) at fixed laser pulse energy *E*<sub>las</sub> while varying the DC bias applied to the tip, *V*<sub>DC</sub>; (ii) at fixed *V*<sub>DC</sub> while varying *E*<sub>las</sub>; and (iii) at a constant detection rate φ, by keeping *E*<sub>las</sub> fixed and automatically increasing *V*<sub>DC</sub> to compensate for the increasing tip radius during field evaporation. Measurements were carried out using two tomographic atom probe instruments, LaWaTAP and FlexTAP, which provided fully consistent results. Both instruments were operated with UV femtosecond laser pulses (λ = 343 nm, 350 fs), focused onto the specimen to a spot diameter of approximately 20 µm. The laser repetition rate was set to 100 kHz for LaWaTAP and 50 kHz for FlexTAP. In both instruments, ion detection was performed using a custom-designed detector comprising a microchannel plate coupled to an advanced delay-line detector (MCP/aDLD), with a detection efficiency η<sub>MCP</sub> ≈ 0.6 (Costa et al., 2012; Da Costa et al., 2005). Both studies indicate that the measured composition varies as a function of the charge-state ratio, CSR(Ga<sup>2+</sup>/Ga<sup>+</sup>), when using protocols (i) and (iii). Specifically, a Ga fraction of 0.8 is measured at CSR ≈ 0.02, stoichiometric composition is obtained at CSR ≈ 0.08, and a Ga fraction of 0.4 is observed at CSR ≥ 0.3 Fig. [18]-(a,b). This CSR range corresponds to an equivalent field *F*<sub>eq</sub> spanning approximately 23–27 V/nm, and the stoichiometric composition is measured at about 24 V/nm. This CSR range corresponds to an equivalent field *F*<sub>eq</sub> of approximately 23–27 V/nm, with stoichiometric composition achieved at *F*<sub>eq</sub> ≈ 24 V/nm. Particularly noteworthy is the field-dependent evolution of the fraction of detected counts in the mass spectrum, as reported by Mancini *et al*. As the measured Ga fraction decreases from ~0.6 to ~0.4, the fraction of Ga<sup>2+</sup> counts increases from ~1% to ~10%, while Ga<sup>+</sup> counts decrease from 71% to 58%. Simultaneously, N<sup>+</sup> counts increase from 18% to 31%, and N<sup>+</sup> (or N<sub>2</sub><sup>2+</sup>) counts rise from ~4.5% to ~9.5%. Of particular interest, given their role in molecular dissociation phenomena, is the decrease in the fraction of GaN<sub>3</sub><sup>2+</sup> counts, which drops from ~1.9% to ~0.7%, providing clear evidence that high fields do not promote the formation of heterogeneous molecular ions. Lastly, protocol (ii) involves increasing *E*<sub>las</sub> while maintaining a constant field by fixing *V*<sub>DC</sub>. Mancini *et al*. found that varying *E*<sub>las</sub> between 0.7 and 2.4 nJ did not affect the measured Ga fraction within the error bars, which averaged ~0.56 (*F*<sub>eq</sub> ≈ 24 V/nm). In addition, *E*<sub>las</sub> > 2.7 nJ led to asymmetric tip emission, causing severe tip shape deformations. The same experiment was repeated by Di Russo *et al*. at a much lower field (*F*<sub>eq</sub> ≈ 22 V/nm), where the average Ga fraction was ~0.77 while varying *E*<sub>las</sub> from 3 to 40 nJ. Two-dimensional histograms of the charge-state ratio and Ga fraction in detector space reveal a clear correlation between the local electric field and the measured composition. The presence of a c-axis pole is associated with a high-field region and a Ga-poor composition. Furthermore, as the number of detected events increases from ~10<sup>5</sup> up to ~10<sup>7</sup>, a sixfold pattern characteristic of the wurtzite hexagonal structure becomes evident (Fig. [18]-(c,d)). The same pattern is observed in field ion microscopy (FIM) micrographs (Russo et al., 2018), which directly image the electric field distribution at the tip surface. Finally, this work examines whether the compositional biases observed in GaN originate from intrinsic detection effects that can be identified through the analysis of multiple-hit events (see section 4.d.iii). Correlation histograms indicate signatures of neutral species formation, notably N<sub>2</sub> molecules, but the inferred yield is too low to explain the compositional bias at low electric fields. In contrast, dissociation occurring near
the tip surface may not appear in these histograms. Correlation tables and detector hit distances at different electric fields indicate that strong ion-pair correlations mainly arise from correlated field evaporation. No evidence was found for dissociation producing multiple charged fragments, although events yielding one charged ion and one neutral nitrogen atom cannot be excluded.

In 2018, the possible causes of nitrogen underestimation in GaN measurements were in-depth investigated by Morris et al. (Morris et al., 2018). Experiments were conducted using a LEAP 5000 XR equipped with a UV laser (λ =355 nm) and a CAMECA LaWaTAP operated with a green laser (λ =515 nm). The measured composition as a function of the electric field was found to be highly reproducible across different instruments, laser wavelengths and excitation conditions. thereby showing a very high level of reproducibility. In contrast to earlier reports, a stoichiometric Ga:N ratio was recovered under high-field conditions, corresponding to CSR values exceeding 0.3. In 2022, the LEAP 5000 XR electrode was modified by adding a grid on its reverse side to manipulate co-evaporated ions (Morris et al., 2022). This modification reduced the detection efficiency from approximately 52% for the standard electrode to about 7.3% for the grid-equipped electrode, effectively equalizing ion pile-up across all species. However, no effect on the apparent field-dependent stoichiometry was observed, supporting the conclusion that N ion pile-up is not the primary origin of the compositional bias measured in GaN.

<figure><img src="image_26.png" /><figcaption>Figure [22]. Correlation between the atomic Ga fraction in GaN and the CSR(Ga²⁺/Ga⁺). (a) Atomic fraction of Ga from several constant potential measurements (black triangles) or two constant laser intensities (red square and pentagon), and comparison with the constant potential measurements contained in the references [a)=(Agrawal et al., 2011b) [b)=(Diercks and Gorman, 2015). Adapted from reference (Mancini et al., 2014b), Copyright 2014 American Chemical Society.</figcaption></figure>

*Mechanisms for neutral N emission.* Nitrogen loss during atom probe analysis of III-nitrides continues to be debated within the community (Gault et al., 2016). Although significant N₂ loss via thermal decomposition has been suggested (Huang et al., 2025), it was considered unlikely in the context of APT experiments. Other processes, particularly the surface diffusion of Ga and N on the tips surface, are also
likely to play a significant role, potentially affecting the quality of the data. In particular, mass spectra indicates that nitrogen predominantly recombines into N₂ molecules on the tip surface prior to emission. If N₂ molecules are desorbed from the tip during the tip evaporation, they are expected to behave similarly to the imaging gas in field ion microscopy (FIM). The applied field eventually drives gaseous species (adsorbed or desorbed) towards the highest electric field region of the tip, where a higher N-fraction is expected to be observed. This behavior could partly account for the lower specific detection efficiency for nitrogen, ηN, observed in Al_yGa₁-yN (Di Russo et al., 2018). However, the first ionization energy of atomic nitrogen is approximately 14.6 eV, whereas that of molecular nitrogen (N₂) is about 15.6 eV (Hierl and Franklin, 1967; Jaroń-Becker et al., 2004). For a specimen with a tip radius of curvature of 50 nm and a surface electric field of 20 V/nm, the field strength remains above ~17 V/nm over a distance of nearly 5 nm from the surface, which is sufficient to ionize both N₂ and atomic N (Gault et al., 2016). These evidence casts significant doubt on the viability of a loss mechanism involving the direct desorption of neutral molecules in the case of nitrides. An alternative hypothesis attributes the observed nitrogen loss to the emission of neutral species generated by the dissociation of molecular ions in the low-field region near the tip surface. In particular, in GaN it has been observed that low evaporation-field conditions promote the emission of molecular ions such as N₃⁺, GaN²⁺ and GaN₃²⁺ (Russo et al., 2018). The latter is of particular interest, as it can undergo the following dissociation reaction, leading to the emission of neutral nitrogen species: GaN₃²⁺ → Ga⁺ + N⁺ + N₂ (Gault et al., 2016). Molecular dissociation thus represents a compelling explanation. N₂-bearing molecular ions may dissociate in-flight in low-field regions, producing neutral fragments that escape from the sample surface but either miss the detector or fall below the detection threshold. Only quite recently, the hypothesis of direct emission by ejection of sufficiently rapid molecules (possibly in an excited state) minimizing the probability of ionization has been given further arguments in the case of O₂ in oxide materials (see section 4.d.ii and (Veret et al., 2025)). This hypothesis seems to be viable for N₂ in nitrides.

### iii. Other III-Nitrides: AlN, InN, AlGaN, InAlN, InGaN, ScAlN

AlN. The mass spectrum of AlN closely resembles that of GaN (Mancini et al., 2014b). Nitrogen-related ions are predominantly detected at 14 and 28 Da, corresponding to N₂²⁺ and N₂⁺ species, respectively. However, the signal at 14 Da may also include contributions from N⁺ ions; if the peak is entirely assigned to this species, the nitrogen fraction would be decreased by approximately 5%. Interestingly, a weak peak attributed to N²⁺ is observed at 7 Da, which appears in GaN only under high evaporation field conditions (Russo et al., 2018). Aluminium-related peaks are observed at 27, 13.5, and 9 Da, corresponding to Al⁺, Al²⁺, and Al³⁺ ions, respectively. It must be noted that the simultaneous presence of these three charged states represents a deviation of from the Kingham statistic, as Al⁺ and Al³⁺ ions cannot be formed simultaneously (Kingham, 1982). Measurements performed at constant detection rate and fixed laser energies (Eᵢ₉₅ = 1.0, 1.2, 4.5 and 5.3 nJ), using a LaWaTAP system (λ = 343 nm) operated at a repetition frequency of 100 kHz, reveal that the measured composition can be expressed as a function of the charge-state ratio CSR(Al²⁺/Al⁺) (Mancini et al., 2014b). At low field (CSR = 1), the measured Ga fraction is approximately 0.55. A near-stoichiometric composition is obtained at CSR = 10, corresponding to an equivalent field Fᵢ₉₅ ≈ 24.4 V/n. Further increasing the CSR beyond this value leads to a slight reduction in the measured Ga fraction, reaching approximately 0.49. Within this CSR interval, the equivalent field Fᵢ₉₅ ranges from approximately 23 to 25 V/nm, comparable to the evaporation field reported for GaN. This contrasts with the simultaneous observation of N²⁺ and Al³⁺ ions in mass spectra, suggesting that the evaporation field of AlN is higher than that of GaN.

In 2022, Morris et al. (Morris et al., 2022) measured the field-dependent composition of AlN and provided a detailed analysis of the role of multi-hits using a LEAP 5000 XR operated in laser mode (λ
= 355 nm) using a pulse frequency of 125 kHz. As the CSR increased from 0.8 to 7, the overall detected Al fraction decreased from approximately 0.64 to 0.58, while the fraction of multi-hits dropped from 18% to 10%. The measurements were then repeated using an electrode modified with an incorporated grid, which reduced the detection efficiency from ~52% to ~7.3%. This reduced the fraction of multi-hits by a factor of ~4. Nevertheless, the measured composition as a function of the field remained largely unchanged.

The composition of AlN thin films was further investigated by Hans et al. in 2023 (Hans et al., 2023) using two local electrode atom probe (LEAP) instruments: a LEAP 4000X HR operating with a UV laser (λ = 355 nm) and a LEAP 3000X HR equipped with a green laser (λ = 532 nm). Constant detection rate experiments were carried out by systematically varying *E*<sub>las</sub>. For the UV laser, the pulse energy was adjusted between 5 and 50 pJ at a repetition rate of 200 kHz, whereas for the green laser it ranged from 0.1 to 2.0 pJ with a pulse frequency of 250 kHz. The data indicate that the detected Al-fraction decreases from approximately 0.64 to 0.51 as the equivalent field, *F*<sub>eq</sub>, calculated from the CSR(Al<sup>2+</sup>/Al<sup>+</sup>), rises from ~25.6 to ~29.2 V/nm, independent of the experimental conditions. This indicates that the accuracy of composition measurements in AlN is strongly dependent on the applied electric field strength.

InN. [0001]-oriented InN was analysed by Di Russo et al. (supporting information to (Di Russo et al., 2019)) using a FlexTAP instrument operated at constant detection rate with green laser pulses (λ ≈ 515 nm). The resulting mass spectrum closely resembles that of GaN, with nitrogen predominantly detected as N<sub>2</sub><sup>+</sup> ions; contributions from N<sup>+</sup> (or N<sub>2</sub><sup>2+</sup>) and N<sub>3</sub><sup>+</sup> ions are also observed. Indium is detected in both singly and doubly charged states, with In<sup>+</sup> peaks at 113 and 115 Da and In<sup>2+</sup> peaks at 56.5 and 57.5 Da. Several heteronuclear molecular ions are identified, including InN<sup>2+</sup>, giving rise to a prominent peak at 64.5 Da, and InN<sub>3</sub><sup>2+</sup>, observed at 78.5 Da. A spatially resolved analysis of the probed surface revealed pronounced local variations in the indium charge-state ratio CSR(In<sup>2+</sup>/In<sup>+</sup>), exhibiting a radial symmetry centred on the [0001] crystallographic pole. These variations reflect changes in the *F*<sub>eq</sub>, which was estimated to range between approximately 21 and 24 V/nm. This field range suggests that the effective evaporation field of InN may be lower than that of GaN and AlN. A strong correlation was observed between the local CSR and the measured In-fraction. At high effective fields (~24 V/nm), the detected composition was In-depleted, with indium fractions as low as ~0.45, whereas decreasing the field led to progressively In-rich compositions, reaching values up to ~0.7 at ~21 V/nm. Stoichiometric InN was recovered only within a narrow field window around ~23 V/nm, spatially confined to a thin annular region surrounding the [0001] pole. These observations were interpreted in terms of competing field-dependent loss mechanisms. Under high-field conditions, preferential evaporation of indium between laser pulses results in indium depletion. Conversely, at lower fields, nitrogen loss (most likely through the formation of neutral N<sub>2</sub> species that escape detection) dominates, leading to indium enrichment. Accurate stoichiometry is achieved only under intermediate field conditions where these two effects are balanced.

AlGaN. The field dependence of the detected AlGaN composition was first examined in a c-axis-
oriented GaN multiple quantum-well structure presenting thick Al<sub>0.25</sub>Ga<sub>0.75</sub>N barriers (Rigutti et al.,
2016a). Constant detection rate experiments were carried out by maintaining a fixed laser energy E<sub>las</sub>,
which resulted in a progressive decrease of the surface electric field during the analysis while
maintaining an inhomogeneity of surface electric field and microscopically measured composition, as
traced in the detector space histograms of Fig. [23](a). As a consequence, each AlGaN barrier was
evaporated under progressively lower electric-field conditions. For each AlGaN barrier, the average
CSR and the corresponding composition were determined. The evolution of the local electric field was
quantified through the charge-state ratio CSR(Ga<sup>2+</sup>/Ga<sup>+</sup>), which provides an estimate of the equivalent
field F<sub>eq</sub>. An increase in the local electric field is associated with a pronounced decrease in the detected
Ga fraction, which drops from approximately 0.4 to 0.3, while the detected Al fraction remains essentially unchanged. In addition, consistently with observations in GaN, increasing the electric field also leads to an enhancement of the detected nitrogen fraction, which rises from about 40% to 50%. The data show that increasing the CSR from approximately 0.03 to 0.1 results in an increase of the measured group-III site fraction y, defined as y = Al/(Al+Ga), from 0.27 to 0.37. Notably, this range systematically exceeds the nominal Al content of the barriers (y = 0.25), indicating that the measured composition consistently overestimates the true Al fraction. This work also proposed a scheme for the correction of the bias based on the statistical properties of the random AlGaN alloy, as shown in Fig. [20]. These findings are consistent with the work of Di Russo et al. (Di Russo et al., 2019), who reported a correlation between the microscopic electric-field distribution and the measured composition in an Al<sub>0.15</sub>Ga<sub>0.85</sub>N electron-blocking layer in a c-axis-oriented LED structure. Measurements were performed at constant detection rate using FlexTAP (λ = 343 nm, pulse repetition rate 50 kHz), fixing the laser energy E<sub>las</sub> at 1.0 nJ. Results indicate that y increases from 0.20 to 0.35 as CSR(Ga<sup>2+</sup>/Ga<sup>+</sup>) rises from 0.2 to 2.0, corresponding to an equivalent electric field F<sub>eq</sub> ranging from approximately 25 to 27 V/nm. Interestingly, these values are again higher compared to the expected composition. Because the mass spectra typically exhibit peaks attributed to Ga<sup>+</sup>, Ga<sup>2+</sup>, Al<sup>+</sup>, Al<sup>2+</sup>, and Al<sup>3+</sup>, the CSR(Al<sup>2+</sup>/Al<sup>+</sup>) was also calculated. A comparison between the two metrics shows that they are nearly equivalent. In particular, CSR(Al<sup>2+</sup>/Al<sup>+</sup>) spans from approximately 3 to 20, which corresponds to a narrower estimated field range of about 24 to 25 V/nm.

In 2018, Morris et al. have investigated bulk Al<sub>y</sub>Ga<sub>1-y</sub>N (x = 0.08, 0.44, 0.75) using both a LEAP 5000XR (λ = 355 nm) and a CAMECA LaWaTAP (λ = 515 nm), performing measurements at a constant detection rate (Morris et al., 2018). The two instruments demonstrate nearly identical measured compositions as a function of the electric field. The evaporation field of Al<sub>y</sub>Ga<sub>1-y</sub>N depends on the Al fraction x. For sample with y = 0.08, the tip field required at fixed laser energy closely matches that of GaN. In contrast, samples with higher Al content (y = 0.44 and 0.75) require substantially stronger tip fields, with CSR values exceeding 5 and remaining comparable between the two compositions. This increase is consistent with the higher evaporation field of Al. Additionally, the expected 1:1 ratio between group-III elements (Al + Ga) and N is never fully achieved in Al<sub>y</sub>Ga<sub>1-y</sub>N samples, with the exception of the sample with y = 0.44, which reaches a composition close to the expected ratio at high field (CSR = 0.3), whereas GaN exhibits a nearly stoichiometric composition at high field (CSR = 0.5). Interestingly, at the same field, the N fraction decreases as the Al content increases, suggesting that the higher E<sub>las</sub> required to evaporate the tip are associated with a higher tip temperature, which in turn enhances N<sub>2</sub> sublimation. No variation in the site fraction y with applied field is observed for y = 0.08 over the CSR range 0.002 – 0.2. The sample with y = 0.44 shows that y decreases as CSR decreases, reaching the expected composition at CSR ≈ 0.04, before slightly decreasing again. Lastly, for y = 0.75, the expected site fraction y is recovered at both low and high electric fields (CSR = 0.05 and 6, respectively), whereas intermediate field conditions yield y values lower than the nominal composition. This deviation originates from an overestimation of the measured Al-fraction and an underestimation of the Ga-fraction relative to the expected stoichiometry.

The accuracy of compositional measurements in c-axis-oriented Al<sub>y</sub>Ga<sub>1-y</sub>N/Ga multilayers was investigated and modeled by Di Russo et al. in 2018, considering a series of samples with III-site fractions y ranging from 0.07 to 0.56 (Di Russo et al., 2018). Analyses were performed with a LaWaTAP operated with a UV laser (λ = 343 nm) and equipped with a custom-designed detector system (Da Costa et al., 2005). Preliminary analysis of the CSR(Ga<sup>2+</sup>/Ga<sup>+</sup>) and CSR(Al<sup>2+</sup>/Al<sup>+</sup>) shows that they are effectively equivalent at low surface fields, whereas deviations from Kingham's theory emerge at higher fields. Despite this limitation, the associated uncertainty in the surface field determination under the experimental conditions considered here is confined to ~1 V/nm (~5%). The measured composition exhibits a strong dependence on the surface electric field: y is accurately reproduced under low-field conditions but increases systematically with increasing surface field. This trend is general and reproducible over the entire composition range investigated. The presence of GaN layers allowed for an
accurate calibration of the 3D reconstructions and for the determination of element-specific detection efficiencies ηᵢ (see section 4.a.iii). The Al detection efficiency, η<sub>Al</sub>, remains essentially constant along the analysis direction but shows a pronounced radial variation, reaching its highest values in low-field regions, where it approaches the detector efficiency limit (η<sub>Al</sub> ≈ η<sub>MCP</sub> ≈ 0.6). In contrast, the Ga detection efficiency, η<sub>Ga</sub>, is strongly correlated with the CSR(Ga<sup>2+</sup>/Ga<sup>+</sup>) in both axial and radial directions, and approaches the detector efficiency only in low-field regions near the end of the analysis. The N detection efficiency, η<sub>N</sub>, exhibits only a weak radial dependence and a slight increase along the analysis direction, following a trend opposite to that of η<sub>Ga</sub>; however, its average value remains well below the detector efficiency limit (η<sub>N</sub> < η<sub>MCP</sub> ≈ 0.6). These data were subsequently used to formulate a semi-quantitative model describing the preferential evaporation of Al and Ga between laser pulses, which accounts for the observed increase in the measured III-site fraction y with increasing surface electric field and a correct value of composition measured at low field only, as visualized in Fig. [23]-(b). The estimated energy barriers are approximately Q<sub>Ga</sub> = 1.0 eV and Q<sub>Al</sub> = 1.1 eV, with corresponding evaporation fields of F<sub>ev,Ga</sub> = 25 V/nm and F<sub>ev,Al</sub> = 27 V/nm. By contrast, nitrogen is proposed to be lost via a distinct mechanism, involving neutral evaporation and the generation of neutrals from molecular dissociation.

<figure><img src="image_27.png" /><figcaption>**Figure [23].** Field-dependent compositional inaccuracies in AlGaN and InGaN. (a) From left to right, detector space histograms showing the distribution of the CSR(Ga²⁺/Ga⁺), CSR(Al²⁺/Al⁺), atomic fraction of III-type elements and Al III-site fraction issued from an analysis of random AlGaN alloy (Adapted with permission from (Rigutti et al., 2016a), AIP). (b) Correlation between the y III-site fraction in AlGaN and the CSR(Ga²⁺/Ga⁺) ratio for 6 samples with four different compositions of AlGaN (Adapted with permission from (Di Russo et al., 2018) ACS). (c) In III-site fraction plotted as the function of the local CSR(Ga²⁺/Ga⁺) from the analysis of quantum well layers of a LED device. The effective field F<sub>eff</sub> is calculated from the CSR(Ga²⁺/Ga⁺) (Reproduced with permission from (Di Russo et al., 2019), AIP).</figcaption></figure>

InAlN. Only a limited number of studies report compositional measurements of Al<sub>y</sub>In<sub>1-y</sub>N. A representative mass spectrum was reported by Dawahre et al. (Dawahre et al., 2013). The spectrum closely resembles that of AlN, with addition peaks attributed to In ions at 115 and 57.5 Da, corresponding to <sup>115</sup>In<sup>+</sup> and <sup>115</sup>In<sup>2+</sup>, ions respectively (<sup>113</sup>In gives rise to a small peak, accounting for only 4.3% of the total element abundance). Nevertheless, no systematic investigation of the composition as
a function of the analysis parameters has been reported. Mancini et al. measured the composition of a Al<sub>y</sub>In<sub>1-y</sub>N grown along the m-axis. Measurements were performed using a LaWaTAP system operated with a UV laser (λ = 343 nm) at *E*<sub>las</sub> = 1 nJ and constant detection rate. The microscopic distributions of both CSR(Al<sup>2+</sup>/Al<sup>+</sup>) and CSR(In<sup>2+</sup>/In<sup>+</sup>) were reported, together with the corresponding spatial distribution of the measured In/(Al+In) fraction. However, the resulting composition maps showed no correlation with the local surface field (Mancini et al., 2014b).

*InGaN*. The correct quantification of the In III-site fraction in InGaN is technologically significant as this alloy constitutes the quantum well layers of LEDs. Riley et al. (2014) systematically investigated the reliability of indium quantification in In<sub>y</sub>Ga<sub>1-y</sub>N (y ≈ 0.25) quantum wells (QWs) grown on wurtzite GaN along non-polar m-axis. APT measurements were performed using a LEAP 4000X Si instrument equipped with a UV laser (λ = 355 nm), operated at a pulse energy of 0.01 pJ and a repetition rate of 200 kHz. The evaporation behavior of In, Ga, and N atoms is strongly influenced by the structure and surface polarity of the tip facets. In particular, variations in the III/N ratio normal to the non-centrosymmetric c-plane reflect a transition from N-polar to Ga-polar surface termination. N-polar surfaces typically exhibit a balanced Ga-to-N ratio, whereas Ga-polar terminations show systematic nitrogen depletion, as previously reported for *a*-axis-oriented GaN nanowires (Riley et al., 2014). This artifact has been attributed to the preferential diffusion of nitrogen, which promotes N<sub>2</sub> formation and desorption over direct evaporation, leading to nitrogen loss either as neutral species or beyond the detection window. When moving into the QWs along the *m*-axis, Ga counts decrease more than the corresponding increase in In counts on both Ga- and N-polar facets, suggesting a reduced overall detection probability for group-III species. By contrast, Ga counts from the nonpolar *m*-plane remain relatively constant along the analysis direction, indicating enhanced detection of group-III species within the QWs, accompanied by a rise in N counts. The resulting increase in the N/III ratio within the QWs can thus be attributed to a reduced Ga detection probability, consistent with the observed elevation in the Ga<sup>2+</sup>/Ga<sup>+</sup> ratio, which signals a locally increased electric field. Although Ga<sup>+</sup> and In<sup>+</sup> ions have different nominal evaporation fields (15 V/nm and 12 V/nm, respectively) (Tsong, 1978b), their field-dependent evaporation rates are sufficiently similar that variations in local field due to polarity, surface faceting, or composition do not induce measurable changes in the In mole fraction. Moreover, the evaporation characteristics of c-plane (0001) and semipolar (202&#x0304;1) QWs exhibit analogous responses to surface polarity and crystallography, supporting the consistency of these conclusions across different orientations.

The composition of In_yGa_{1-y}N quantum wells grown along the m-axis of a In_yGa_{1-y}N/GaN multi-quantum wells system was analyzed by Mancini et al. (Mancini et al., 2014b). Measurements were performed using a LaWaTAP system operated with a UV laser (λ = 343 nm) at constant flux, with E_{las} fixed at 0.3 nJ. Maps of the CSR(Ga^{2+}/Ga^{+}) revealed a high-field region that attributed to the presence of the m-pole. As observed for GaN, the measured group-III fraction deviates from the stoichiometric value of 0.5, being higher than 0.5 in high-field regions and lower in low-field regions. Within the quantum wells, In is found to form high-concentration stripes approximately aligned with the c-axis, whose position varies from well to well independently of the local surface field. Notably, the indium distribution shows no correlation with either the field distribution or the measured group-III fraction. The analysis of the average charge-state ratio and the average group-III fraction measured along the tip reveals oscillations in both quantities, with a periodicity matching the positions of the In_yGa_{1-y}N quantum wells. These oscillations were interpreted as arising from local modulations of the evaporation field, which is slightly higher in the quantum wells than in the surrounding GaN matrix.

In<sub>y</sub>Ga<sub>1-y</sub>N layers within a c-axis-oriented LED structure, with a nominal indium fraction y = 0.08, were investigated by Di Russo et al. (Di Russo et al., 2019). Spatially resolved measurements of both the local field and composition were performed under constant detection flux using a FlexTAP instrument
operated with a UV laser (λ = 343 nm, 50 kHz) and a fixed E<sub>las</sub> = 0.3. The corresponding mass spectra exhibit all the characteristic peaks typically observed in InN and GaN. Three distinct In<sub>y</sub>Ga<sub>1-y</sub>N layers were analyzed, each experiencing a progressive reduction of the surface electric field due to the so-called cone-angle effect experienced during constant detection rate measurements. The local field distribution was estimated using both CSR(In<sup>2+</sup>/In<sup>+</sup>) and CSR(Ga<sup>2+</sup>/Ga<sup>+</sup>); however, the two metrics were found to differ significantly. The indium charge-state ratio decreased from ~0.7 to ~0.1, corresponding to an equivalent field F<sub>eq</sub> ranging from approximately 22.5 to 21 V nm<sup>-1</sup>. In contrast, the Ga charge-state ratio decreased from ~0.7 to ~0.03, indicating higher equivalent fields, spanning roughly 25 to 23 V nm<sup>-1</sup>. Consequently, the Ga-based charge-state ratio was adopted as the reference metric for comparing compositional measurements in In<sub>y</sub>Ga<sub>1-y</sub>N with other III-N semiconductors. Field maps revealed a pronounced high-field region at the center of the tip, attributed to the alignment with the crystallographic c-axis. The local In group-III site fraction was found to be enhanced in the same regions. When plotted (Fig. [23]-(c)) as a function of the Ga-based charge-state ratio, the In fraction decreased from ~0.14 to ~0.07 (this last value approaches the nominal composition) as CSR(Ga<sup>2+</sup>/Ga<sup>+</sup>) decreased from ~0.4 to ~0.03. As previously observed for Al<sub>y</sub>Ga<sub>1-y</sub>N, the nominal composition in In<sub>y</sub>Ga<sub>1-y</sub>N is therefore recovered under lower-field evaporation conditions.

ScAlN. ScAlN has been the object of several studies in APT (Dzuba et al., 2022; Ndiaye et al., 2023b). The work by Ndiaye et al. has focused on its compositional metrology, monitoring the dependence of the Sc III-site fraction on the CSR(Al), indicating that this quantity is rather constant and thus pointing out for an accurate measurement of composition (Ndiaye et al., 2023b). However, these experiments were conducted on thin films and more statistical significance would be welcome for this alloy.

iv. Other Nitrides

TiN. Multiple detection events may represent up to 78% of detection events for TiN. These multiple hits are linked to ion dissociation and correlated evaporation, which lead to under- or over-estimation of nitrogen and titanium in the reconstructed datasets. Schiester and co-authors have studied the problem by comparing results obtained by hardware filtering ((Thuvander et al., 2013), see also section 5.a.vi on carbides) or by software filtering (i.e. by filtering out the multiple detection events). Filtering obviously decreases the global amount of information, but allows for a better measurement accuracy. In voltage-mode APT, without filtering, the composition deviated by ~3.8 at.% from reference. With hardware + software filtering, deviation improved to 2.1 at.%, and software filtering alone achieved ~0.1 at.% error, within uncertainty limits. Low pulse energy (0.1 nJ) yielded ~1.4 at.% error. In La-APT, higher pulse energy (2.0 nJ) increased error up to 8.1 at.%, corresponding with increased formation of complex molecular ions (e.g. Ti<sub>2</sub>N), and weakened electric field (~36 V/nm vs ~40 V/nm). Using laser-assisted APT, the accuracy was significantly increased through software filtering the same value could be observed with 0.6 nJ LPE within the measurement uncertainties of ToF-ERDA/RBS. However, the investigations of the laser-assisted APT measurements indicated that a high proportion of multiple detection events per se is not responsible for high deviations from the reference composition (Schiester et al., 2024).

Compositional metrology of TiN has been recently studied by Schiester and co-authors not only exploring the space of environmental parameters (laser pulse energy, surface field) but also the performances of instruments differing by laser wavelength and detector technology. The results show a measured composition close to the nearly-stoichiometric one assessed by complementary techniques (Fig. [24]-(a)). For all three instruments the underestimation of the N content is reduced as the electric field strength increases. The use of a deep UV laser (λ=257 nm) is also assessed as beneficial with respect to longer wavelengths (λ=355 nm for the UV and λ=515 nm for the green). On the other hand, the impact of the detector technology (reduction of the dead zone and increase of the microchannel open area in the LEAP generations after the 3000) is not found to play a significant role (Schiester et al.,
2025). Interestingly, the trends reported in this work point out a trend in the measurement which is common to the main III-N materials. However, in the case of TiN the surface field is much more intense and should be sufficient to prevent N losses via post-ionization.

<figure><img src="image_28.png" /><figcaption>**Figure [24].** (a) Dependence of the measured atomic fraction of N in TiN as a function of the CSR($Ti^{3+}/Ti^{2+}$) and for instruments with different laser wavelength and detector technology (Reproduced from ref. (Schiester et al., 2025), Elsevier). (b) Dependence of the measured atomic ratio $N/(Ti+Al)$ as a function of the CSR($Al^{2+}/Al^{+}$) (Adapted from ref. (Hans and Schneider, 2020), IOP Publishing).</figcaption></figure>

**TiAlN.** The accuracy of the composition measurement for the alloy TiAlN has also been investigated (Hans and Schneider, 2019, 2020). This compound evaporates at significantly lower field than TiN, as reported in ref. (Hans and Schneider, 2020) (Fig. [24]-(b)), i.e. at field intensities slightly higher than the typical values for GaN and AlN (Mancini et al., 2014a). The authors study in particular the dependence of the $N/(Ti+Al)$ ratio on the laser pulse energy and on the CSR($Al^{2+}/Al^{+}$). The expected ratio $N/(Ti+Al) \sim 1$ is gradually approximated for increasing field but not reached at the highest tested field (28 V/nm). In general, the increase of the electric field strength from ~25 V/nm to ~28 V/nm reduces the error from the independently measured composition (ERDA, RBS) from 11.4 to 4.1 at% for N (Fig. [24]-(b)), from 8.8 to 3.0 at% for Al and from 2.8 to 0.9 at% for Ti. The authors interpret these phenomena as a gradually increasing ionization efficiency for possible neutral N. The authors also notice that the increase of surface field also translates into an increase of multiple detection events from 27% to 53%. They thus tend to exclude a role of the pile-up in the inaccuracies enhanced at low field (Hans and Schneider, 2020). However, this point could show that at low field the pile-up effectively translates into a larger fraction of multiple events erroneously interpreted as singles.

**TiSiN.** TiSiN is a coating material in which the main challenge for APT is the overlap between the $^{28}$Si$^{n+}$ and the $^{14}$N$^{n+}$ peaks (n=1,2). This problem has been circumvented by replacing $^{14}$N with $^{15}$N, so that peaks of interest in the mass spectrum are shifted, enabling the separation of overlapping signals. This technique allowed identification and quantification of atomic fraction in reasonable agreement with other microanalysis techniques such as energy-dispersive X-ray spectroscopy (EDS) and energy elastic recoil detection analysis (ERDA) (David L. J. Engberg et al., 2018; Naghdali et al., 2025).

## v. Oxides

**ZnO and MgO.** As compounds forming covalent to ionic bonds, oxides have a usually complex evaporation behavior. A first difficulty in compositional metrology of oxides is already in the mass spectrum, where the peak at 16 m/z may be attributed to $O^{+}$ or to $O_{2}^{2+}$, which is also a kinetically stable species (Nobes et al., 1991). While oxides such as $WO_{3}$ and NiO display a composition close to stoichiometry (Oberdorfer et al., 2007), other oxides may undergo moderate to severe compositional
biases in APT measurements. Examples of measurement of composition in selected binary oxides is reported in Fig. [25]. The measurement of the atomic fraction of Zn in ZnO as a function of the CSR(Zn) is reported in Fig. [25]-(a). The composition appears to undergo important oxygen losses, which become moderate when the field increases (Mancini et al., 2014a). The main channel of loss for O is thought to be the emission of neutrals, as detailed in the following. At higher field, the composition may become O-rich as more and more Zn is lost via preferential evaporation (Amirifar et al., 2015). A similar picture can be drawn for MgO, as reported in Fig. [25]-(b). Here, however, the composition globally remains Mg-rich, as reported by different authors (Devaraj et al., 2013; Mancini et al., 2014a). In both cases, the composition is rather independent of the laser energy at constant surface field. ZnO and MgO were among the first systems for which the interpretation of experimental data was backed up by theoretical-computational efforts. These efforts developed along two main directions. The first one was the simulation of the evaporation processes from small clusters by density functional theory (DFT) (Karahka and Kreuzer, 2015; Xia et al., 2015, 2024). These calculations have shown that they can account for features such as bandgap reduction at the apex surface and evaporation of molecular ions such as O<sub>2</sub><sup>+</sup> and ZnO<sup>2+</sup>, as reported in Fig. [26]-(a) (Xia et al., 2015). DFT calculations remain challenging and have significant limitations: beyond the problem of the choice of the DFT exchange potential, the simulation of realistic surfaces with a significant set of atoms is extremely demanding in computation time; furthermore, DFT describes ground states and lacks the capability of exploring excited states. In other words, DFT can provide qualitative trends, but quantitative predictions about critical fields, species formation, and compositional changes must be validated against experiment and sometimes require empirical adjustments or more advanced computational treatments (Ashton et al., 2020b). A second type of approach, tackling the shortcomings of DFT as well as the complexity of a surface process and restricting the attention to the specific problem of in-flight dissociation reactions, is based on calculations vie molecular dynamics (MD). This approach has been applied to the study of ZnO, and in particular to the dissociation behavior of the ZnO<sup>2+</sup> molecule within the singly and doubly excited configuration interaction (MR-SDCI) model (David Zanuttini et al., 2017). According to the results of these calculations, the ZnO<sup>2+</sup>molecular ion exhibits more field-dependent dissociation channels. As reported in Fig. [26]-(b), one channel produces a neutral O atom within a given field threshold which also depends on the state in which the molecule is evaporated. The production of neutral O close to the apex surface represents a channel of loss for O at low field, as displayed in Fig. [26]-(c). When the field increases, the O atom can more and more probably be post-ionized and thus be detected. Notice that the Fig. [26]-(c) supposes that all evaporation occurs through the channel producing a ZnO<sup>2+</sup> molecular ion, while the experiment clearly shows that other channels are represented. Thus, this calculation can reproduce qualitatively the O deficit at low field, but cannot account for the Zn deficit at high field (David Zanuttini et al., 2017).

*Gallium and aluminum oxides.* Gallium oxide evaporates at significantly higher CSR(Ga²⁺/Ga⁺)~0.5-2 than GaN and III-N compounds. The composition analysis in Ga₂O₃ presents some common features with ZnO, as the measurement of the atomic fractions is rather independent of the laser energy at constant surface field, but presents an oxygen deficiency at low field which tends to saturate close to stoichiometry for high fields. As a peculiar feature of this compound, around 2% of the detected events are produced by the dissociation reaction GaO²⁺→Ga⁺+O⁺. and are found therefore outside of the peak neighborhoods of the parent and daughter ions in the mass spectrum (Chabanais et al., 2021). In aluminum oxide (Al₂O₃) several authors have pointed out an excess of Al atomic fraction in the explored space of parameters (Mazumder et al., 2014; Garcia et al., 2023). Interestingly, mass spectra of Al₂O₃ contain significant amounts of the three charge states Al¹⁺, Al²⁺, Al³⁺, in disagreement with the post-ionization theory. Although no study has been performed on this system based on the CSR metrics, recent results showed that extreme UV (EUV)-pulsed APT yields more stable compositions and less thermal tailing in spectra compared to NUV, allowing more predictable and sensitive analysis across a wider range of laser intensities (Garcia et al., 2023).
**Iron oxides.** Iron oxides represent a more complex domain as different stoichiometries should be considered (Bachhav et al., 2013, 2011; Kim et al., 2024). Figure [25]-(c) reports the O fraction measured in Fe₂O₃, Fe₃O₄ and FeO as a function of the CSR(Fe). Significantly, here the measured composition is O-poor, and, contrarily to ZnO and MgO, the oxygen loss tends to increase at higher field. The study of iron oxides points out the high degree of complexity of field evaporation in this system. Dissociation reactions appear to play here a very important role. Some of these have been identified in correlation diagrams and studied by DFT. These dissociations, especially those involving neutral molecules, show a dependence on crystallographic orientation. The significant proportion of multiple events, which exhibit considerable correlations, can be considered as the main metrological feature calling for attention for possible compositional biases (Kim et al., 2024).

<figure><img src="image_29.png" /><figcaption>**Figure [25].** Compositional biases in binary oxides. (a) Zn atomic fraction as a function of the CSR(Zn) in ZnO and (b) Mg atomic fraction as a function of the CSR(Mg) in MgO, collected at different experimental conditions (Adapted from (Mancini et al., 2014a)); (c) O atomic fraction as a function of the CSR (Fe) from different iron oxide compounds (Data reproduced from (Kim et al., 2024)).</figcaption></figure>
<figure><img src="image_30.png" /></figure>

Figure [26]. Computational approaches for the explanation of biases in binary oxides. (a) DFT calculation displaying snapshots from the evolution of the surface of a ZnO cell from field-free conditions (left) to field evaporation (middle, right). The calculations can reproduce the evaporation of O₂⁺ and ZnO₂⁺ (Data adapted from (Xia et al., 2015)). (b) Abundances of species resulting from the evaporation of ZnO₂⁺ molecules as a function of the field in proximity of the surface. The increasing field produces a fast dissociation yielding significant amounts of a neutral fragment (ZnO₂⁺→Zn²⁺+O) between 1.5 and 2.4 V/Å. The increase of the field progressively translates into the post-ionization of the neutral O. (c) Calculated effect on the measured composition considering different initial states for the ZnO₂⁺ molecular ion under the hypothesis that all evaporated ions are ZnO₂⁺; experimental data are reported for comparison (Reproduced from (David Zanuttini et al., 2017), American Physical Society).

**Silicon Oxides.** The case of SiO₂ is important due to its use in microelectronics. This system was studied varying base temperature and peak ranging and attribution within an instrument pulsed by extreme-UV laser. The measured O:Si ratios average quite close to stoichiometric SiO₂. Some scatter is also present depending on the experimental conditions, but no clear trend has been assessed. The standard deviation in the measured compositions suggests that each experimental variable (temperature, pulsing mode, field strength, and specimen preparation) plays a significant role (Chiaramonti et al., 2020).

**More complex oxide compounds.** Two cases of pseudobinary oxide compounds are also worth mentioning because they illustrate that the most satisfying experimental conditions can significantly differ from one compound to another. The first is (Mg,Zn)O, which has properties close to those of a random alloy such as AlₓGa₁-ₓN. Its evaporation behavior is also similar to that of AlGaN (see section 5.a.iii) as the measured composition in terms of the II-site fraction is more accurate at low field. The mechanism is most likely similar to that of AlₓGa₁-ₓN (Di Russo et al., 2018). A second case is the
ordered compound ErMnO₃, in which the composition in terms of atomic fractions approaches the nominal values of 20% Er, 20% Mn, and 60% O for higher CSR(ErO²⁺/ErO⁺). The authors observe a substantial preferential retention of Er atoms, which is suppressed at higher CSRs. The high field regime also helps reducing the loss of neutral O₂ by increasing its post-ionization probability (Hunnestad et al., 2023).

The analysis of Barium doped SrTiO (Ba:STO) is interesting as it represents an attempt to explain the observed oxygen deficit (at least 14% of deficit within different samples and under different experimental conditions) by means of the estimation of specific evaporation fields for the main molecular ions on the basis of their binding energies within the matrix. The attempted method of estimating evaporation fields provided some insights but was not sufficient to fully explain the observed phenomena (for instance, it does not explain why certain molecular ions, such as TiO, are preferentially emitted over elemental ions). Nevertheless, the authors sketch some analogy with the main results of the DFT analyses performed on binary oxides, showing the possibility of evaporating molecular ions, and the possible emission of neutral O (Morris et al., 2024).

## vi. Group IV compounds and carbides

The relevance of group IV semiconductors is mainly related to their use in microelectronics. Carbides may have a large number of applications and are found not only in insulating materials, but also in metal micro and nanostructure. Their evaporation behavior is complex, as C is strongly subjected to surface reactions and yields in general a large amount of multiple hits. An early attempt to tackle the difficulties in the measurement of carbide composition have been proposed by Thuvander and co-authors for the analysis of tungsten carbide. The method consists in placing a grid a few millimeters behind the local electrode. The grid acts as a spatial filter, allowing only ions that follow particular trajectories to reach the detector. Ions produced by multiple evaporation events are more likely to be intercepted by the grid, thus reducing the likelihood they are both recorded. Thus, the overall detection efficiency decreased substantially (from around 37% to about 5%) due to the physical blocking of many ion trajectories, but more significantly the fraction of multiple hits (potentially giving rise to pile-up) was significantly reduced, by over 80% in typical analyses. In this way, a correct measurement of the C atomic fraction could be achieved, even if with a global information loss (Thuvander et al., 2013).

**Silicon Carbide.** Among the group IV semiconductors, SiC has a specific interest as a material for electronics (Nava et al., 2008; Pacchioni, 2017; She et al., 2017; Castelletto and Boretti, 2020), as an example of stoichiometric and perfectly ordered compound, and as a model system for the study of compositional metrology of carbides, making this case relevant also in metallurgy. The APT measurement of carbide composition in steels is generally different from the theoretical composition (Sha et al., 1992; Rementeria et al., 2017), while a strong correlation of the carbon measured fraction with the laser pulse energy is obtained during the analyses of pure cementite (Fe₃C) (Kitaguchi et al., 2014). First studies on SiC by APT evidenced a slight Si deficiency (Miller et al., 1989). Later, La-APT studies evidenced a C deficiency and proposed an explanation of the observation through detector losses, based on the statistics of the ¹²C and ¹³C isotopes (Thuvander et al., 2011). The field evaporation of SiC is complex, with the occurrence of molecular ions generally composed of C, sometimes subjected to in-flight molecular dissociation. FIM analysis shows that the surface is significantly perturbed by atom motion. In SiC, the CSR(Si) expectedly decreases during the analysis due to the increase of the field of view (Fig. [27]-(a)). The measurement of composition in SiC exhibits inaccuracies, as it is shown in Fig. [27]-(b) as a function of the reconstructed depth. The exploration of experimental parameters invariably yields a Si-rich composition. This phenomenon can be consistently interpreted as due to the specific tendency of C to correlated evaporation, yielding a higher fraction of multiple evaporation and
detection events for this element, which is consequently more exposed to measurement errors due to the limitations in the detector performances. This observation is corroborated by the evolution of specific quantities during the analysis. Firstly, the fraction of detected multiples decreases with depth (Fig. [27](c)). Secondly, the detector amplitude recorded in single events shows that the detected C has often large amplitudes, related to double or multiple neighboring impacts which could not be discriminated by the detector and which are therefore treated as a single event (detector dazzling, inset of Fig. [27](d), see also section 4.a.ii). The average amplitude of C impacts increases over time (i.e. with the analyzed depth, Fig. [27](d)). This observed trend of increase of C loss with increasing depth of analysis can then be explained by the decrease in geometric magnification, making it more and more likely for correlated evaporated ions to fall within the so-called “dazzled region” of the detector (Ndiaye et al., 2023a) (Fig.[11](f)). The measurement of composition of SiC by APT are thus subject to inaccuracies that stem from the interplay between high field surface chemistry and detector performances. We remind that the amplitude of detection events is usually not accessible in current commercial instruments, but is featured in the LaWATAP instrument used for this study.

*Silicon-Germanium and related alloys.* SiGe is an important alloy in micro and nanoelectronics as it is used for strain engineering of transistors. Compositional inaccuracies in APT analyses of SiGe can be avoided if using a CSR(Si²⁺/Si⁺) in the order of 100 (Koelling et al., 2009, 2011; Dyck et al., 2017). On the other hand, SiGeC alloys display more complex mass spectra, with frequent C-containing molecular ions (occasionally formed with Si but not with Ge) and compositional inaccuracies. These have been characterized by Estivill et al., who showed that the composition is systematically poor in Ge and in C. The atomic fraction of Ge recovers to the nominal value at high CSR(Si²⁺/Si⁺), while the C atomic fraction decreases further with increasing field. The loss of carbon is attributed to several factors: decrease in signal-to-noise ratio and the possibility that certain peaks are not indexed, such as hypothetical C³⁺, which would overlap with the germanium peaks. The mechanism could likely be similar to what has been ascertained in SiC (Ndiaye et al., 2023a). For germanium there is no clear answer to explain the loss at lower electric field, but a role of the laser intensity is suspected (Estivill et al., 2015).
<figure><img src="image_31.png" /></figure>

**Figure [27].** Advanced analysis of compositional biases in 4H-SiC. (a) Surface electric field around the axis [0001] pole as a function of the analysis depth; in the inset, the 3D reconstructed volume. (b) Variation of the atomic fraction of Si and C as a function of the depth coordinate of the reconstructed volume. (c) Percentage of multiple and single events as a function of the depth. (d) Mean amplitude of single detection events traced versus the depth analysis. In the inset, histograms reporting the distributions of signal amplitudes related to the impacts of Si²⁺ and C²⁺ at the beginning (first 5 million atoms) and the end of analysis (last 5 million atoms over 20). (Adapted with permission from (Ndiaye et al., 2023a), *American Chemical Society*)
## b. Impurities

A correct measurement of dopant and impurity densities in non-metallic materials is critical because even ppm-level variations strongly influence electronic, magnetic, and catalytic properties through charge carrier control, defect formation, and strain effects (Koenraad and Flatté, 2011). Some of these species may also be characterized by statistical properties such as pairing or clustering, which can be addressed by APT and by STM only (Di Russo et al., 2025). Furthermore, the correct assessment of isotopic abundances of trace elements is paramount in geochronology (Reddy et al., 2020). APT is, in principle, a technique of choice due to its sub-nm 3D resolution and low limit of detection across all elements (Koelling et al., 2016), enabling quantification of individual atoms or clusters that determine device properties or carry other important information. However, compositional biases have been shown to occur also in this domain of application and should therefore be critically considered.

### i. Dopants in Si and SiGe

Boron in Si. Boron is the most widely used p-type dopant in silicon and plays a central role in modern microelectronics. The accuracy of B quantification in Si by APT has shown differences across studies. Several reports demonstrate good agreement with reference techniques such as SIMS, particularly in terms of concentration profiles (Kelly et al., 2007; Cojocaru-Mirédin et al., 2009b; Kambham et al., 2011; Cojocaru-Mirédin et al., 2009a). Nevertheless, other studies report notable discrepancies, including boron detection losses of 10–50 % (Costa et al., 2012; Kinno et al., 2017; Ngamo et al., 2009; Yeoh et al., 2020)[ref] and deviations in the implanted dopant profile compared to expected distributions (Mangelinck et al., 2014; Martin and Yatzor, 2019; Ngamo et al., 2009; Ronsheim et al., 2008; Thompson et al., 2006). These discrepancies can be largely attributed to the specific behavior of boron during field evaporation. Boron has a high evaporation threshold relative to silicon and exhibits surface migration, often co-evaporating in multi-ion bursts.

During APT, boron can remain temporarily at the specimen surface and then evaporate in these multi-ion events (Menand and Kingham, 1985; Menand et al., 1984; Costa et al., 2012). Detector limitations, such as pile-up effects, may prevent some ions from being correctly recorded, leading to a preferential loss of B and an underestimation of its concentration in the Si matrix. This phenomenon was clearly demonstrated in a heavily B-implanted Si (1 × 10¹⁰ at./cm²) by (Costa et al., 2012). Their study showed that Fourier-domain processing of signals from a delay-line position-sensitive detector significantly improves temporal resolution, enhancing the ability to resolve multi-ion events, an approach implemented in the so-called “advanced delay-line detector” (aDLD) (see section 4.e).

Using a LEAP 3000X Si operated with a green laser (λ=532 nm), Ronsheim et al. (2010) investigate the composition of two Si:B samples presenting B concentration of 2.4 × 10¹⁹ and 2.15 × 10²⁰ at./cm⁻³ (Ronsheim et al., 2010). Increasing the laser pulse repetition rate modestly improves the fractional B yield, whereas changing *E*<sub>las</sub>, evaporation rate and sample base temperature show no consistent change in the measured composition. The study revealed that the B collection efficiency was significantly below 100%, with the loss primarily attributed to detector limitations rather than evaporation physics. Specifically, B atoms were more likely to be lost due to multiple-event generation during evaporation. The authors suggested that enhancing multiple-event detection could mitigate this limitation and improve quantitative accuracy.

In 2015, Meisenkothen et al. (Meisenkothen et al., 2015) investigated the impact of pile-up phenomena on compositional measurement of a ¹⁰B-implanted Si sample (1 × 10¹⁵ at./cm²) using a conventional three anode delay-line detector installed in both LEAP 4000X HR and S instruments operated with UV pulses (λ=355 nm). This detector exhibits a dead time of 5–20 ns (Jagutzki et al., 2002b), which should be compared with the signal pulse duration, typically less than 5 ns (Vallerga and McPhate, 2000).
Comparative analyses with SIMS indicate that APT measurements are affected by signal losses ranging from approximately 23% (Si configuration) to about 36% (HR configuration). In fact, B is preferentially emitted in multi-hit events, with >60% of the detected B ions belonging to multiples, despite multi-hit events accounting for <40% of total detections in pure B and <3% in B-implanted Si. Ion-correlation histograms demonstrate that same-isotope, same-charge-state B ion pairs are largely absent due to detector dead-time (~3 ns, with partial loss extending to ~6 ns), leading to severe undercounting of correlated evaporation events. This effect disproportionately suppresses the major isotope, producing apparent ¹⁰B/¹¹B ratios up to a factor of ~2 higher than natural abundance. Probabilistic estimates indicate that dead-time-induced pile-up alone can account for ~20% B signal loss. Notably, the magnitude of the boron deficit is similar for pure B and dilute B-in-Si, indicating that the bias is largely independent of concentration. These results establish detector dead-time as a dominant, quantifiable source of B composition bias in APT and impose fundamental limits on dopant accuracy.

Further insights into the relationship between analysis parameters and the measured boron fraction in silicon were provided by Tu et al. (2017) (Tu et al., 2017a). The three-dimensional distribution of B atoms in both c-Si:B and poly-Si:B was investigated using a LEAP 4000X HR operated with a UV laser (λ=355 nm) at a repetition rate of 200 kHz. In c-Si:B, the measured B distribution is almost uniform and homogeneous at low $E_{las}$. Instead, increasing the $E_{las}$ at 100 pJ leads to a B-enrichment near the (001) pole at the center of the specimen where the local density of Si atoms was lower. This accumulation was explained by electric field driven surface migration of B atoms toward high field regions prior to evaporation. This effect was observed to be enhanced by laser pulsing with a $E_{las}$ fixed at 100 pJ. A similar phenomenon has been reported by Gault et al. (2012) for a wide range of solutes including P, Si, Mn, B, C, and N (B. Gault et al., 2012). High $E_{las}$ were also observed to lead to a segregation along the grain boundaries in poly-Si:B, which originates from a similar mechanism. In addition, due to multi-hit events for evaporating B atoms, a loss in the total count with increasing laser power was observed for poly-Si:B. In particular, the measured composition from 5 to $2.5 \times 10^{15}$ at./cm² increasing $E_{las}$ from 10 to 100 nJ. High laser power was also found to increase the specimen temperature, leading to a reduction of the evaporation threshold of $Si^+$ ions, this increasing their fraction among all Si ions, leading thus to a decrease of the CSR($Si^{2+}/Si^+$) from ~0.5 to ~2×10² (Shariq et al., 2009). Therefore, for ensuring a high-fidelity APT measurement of the B distribution in Si, high $E_{las}$ is not recommended.

A systematic study of the impact of the surface electric field on the quantification accuracy of B in Si was performed by Guerguis et al. in 2024 (Guerguis et al., 2024). Si was implanted with ¹⁰B ions at a dose of $1.0 \times 10^{15}$ at./cm². APT analyses were performed a LEAP 5000 XS, operated using a UV laser (λ = 355 nm). During the analyses, the applied laser energy, $E_{las}$, was automatically adjusted from 41 to 9 pJ to maintain a constant detection rate, φ, while achieving CSR($Si^{2+}/Si^+$) values of 0.25, 0.5, 10, 30, 60, and 80. At the same time, the laser pulse frequency was decreased from 294 to 454 kHz. Mass spectra exhibit peaks associated to $B^{2+}$ (5 Da), $B^+$ (10 Da), $BH^+$ (11 Da) and $BH_2^+$ (12 Da). The B depth profiles measured by APT were compared with SIMS measurements. Samples analysed under low-field conditions exhibit pronounced tails in the APT concentration profiles, leading to an apparent underestimation of the B concentration when compared with SIMS results (Fig. [28]-(a,c)). This is consistent with B retention at the tip surface, resulting from an insufficient field, as previously reported in other studies (Martin and Yatzor, 2019; Tu et al., 2017b). The B dose measured by APT was found to increase significantly with the tip surface field. At CSR($Si^{2+}/Si^+$) ≈ 0.25 (low field), only about half of the expected dose is detected, while increasing the field up progressively recovers the nominal B content (Fig. [28]-(b,c)). In fact, at the lowest electric field, about 69% of B atoms are detected in multi-hit events, leading to significant B losses due to simultaneous detection of ions with the same isotope and charge state. The fraction of B multi-hit events decreases as the CSR increases, which has been interpreted as a consequence of reduced B mobility at the tip apex. Under higher laser pulse conditions, B atoms migrate (Fig. [10], top) and form clusters, which co-evaporate in bursts, leading to increased detection losses. Under high and more homogeneous field conditions, on the contrary, reduced surface migration on the specimen surface is proposed as the underlying mechanism behind this improvement
(Fig. [10], bottom). With less B mobility, there is a lower likelihood of B atoms coalescing. At CSR($\text{Si}^{2+}/\text{Si}^{+}$) ≈ 80, a slight excess in the measured B dose is observed (104.7 %). This artifact arises from a loss of Si in multi-hit events, which artificially increases the apparent B dose. Under these conditions, the isotope fraction of detected $\text{Si}^{2+}$ was observed to deviate from the natural abundances (Fig. [19]-(d) and section 4.d.iv). Applying the simple double-hit correction scheme proposed by Miyamoto et al. (Miyamoto et al., 2012) the B dose estimate was improved from 104.7 % to 101.8 % (Fig. [28]-(c)).

<figure><img src="image_32.png" /></figure>

Figure [28]. Systematic analysis of B concentration in Si by APT. (a,b) Bulk volume B concentration profiles measured at (a) low and (b) high field conditions compared with the SIMS-acquired profile shape. (c) Uncorrected and corrected B doses. The correction is performed using a factor issued from the analysis of Si multiple hits and deviations of isotopic abundances from natural abundances (Reproduced with permission from (Guerguis et al., 2024)).
*Boron in SiGe*. Boron-doped SiGe alloys were investigated by Martin and Yatzor et al. in 2009 (Martin and Yatzor, 2019). This study focused on two 25 nm-thick SiGe layers grown on (001)-Si. The first layer contained approximately 26 % Ge, with the top half in-situ doped with ~7 × 10¹⁸ at./cm³ B (as measured by SIMS), while the second layer contained ~42.7 % Ge and an in-situ B concentration of ~2 × 10²⁰ at./cm³ (as measured by SIMS). APT measurements were performed using a LEAP 4000X Si equipped with a UV laser (λ=355 nm) operating at a repetition frequency of 125 kHz. Measurements were performed at a constant detection rate by increasing the laser energy from 1 to 21 pJ while progressively decreasing the applied DC voltage. Boron exhibits behavior similar to that observed in Si:B. Under low-field conditions (i.e., CSR(Si²⁺/Si⁺) ≈ 0.8), boron shows resistance to field evaporation, resulting in a concentration tail extending much deeper than expected along the tip axis and in atom migration toward SiGe poles at the tip apex. Increasing the evaporation field mitigates these effects and improves the measured B profile at interfaces by promoting field evaporation of B from its original lattice sites. The measured Ge fraction agrees with SIMS within ~2 % over a CSR(Si²⁺/Si⁺) range from 7 to 165, but decreases at very high fields. This trend suggests that Ge²⁺ has a lower evaporation field than Si²⁺ and is therefore more readily lost to the background. The best agreement between APT and SIMS, in terms of both profile shape and measured concentrations for Ge and B, is obtained at CSR(Si²⁺/Si⁺) ≈ 200. Increasing the evaporation field beyond this value leads to Ge undercounting and consequently biases the measured B concentration.

*Phosphorus in Si*. In 2014, Douglas et al. (Douglas et al., 2016) investigated a 14-keV phosphorus implantation directly performed on a commercial Si micro-post array, resulting in a peak phosphorus concentration of 0.2 at.% at a depth of approximately 20 nm. To analyze the near-surface doped layer, a Ni capping layer was deposited on top of the micro-post array prior to FIB milling, enabling the preparation of needle-shaped specimens for APT analysis. In addition to facilitating specimen preparation, Ni provides good adhesion and offers an evaporation field comparable to that of Si. The specimens were subsequently analyzed using a LEAP 3000X HR equipped with a green laser (λ = 532 nm) operating at a repetition rate of 200 kHz. Measurements indicate that fixing the laser pulse energy at 0.4 nJ produces an approximately equal number of 1+ and 2+ phosphorus ions, while minimizing the tailing in silicon peaks in the mass spectra. Higher laser energies, in contrast, are reported to promote surface migration of mobile species such as phosphorus (B. Gault et al., 2012). However, the presence of Ni introduces mass spectral overlaps between ²Ni²⁺ and ³¹P⁺ ions, as well as between ⁶²Ni⁺ and ³¹P₂⁺ species, which can potentially compromise dopant quantification. Given the very low P concentration, a control sample was analysed to estimate the contribution of ³⁰SiH⁺ at the Si/Ni interface, which can artificially increase the apparent amount of ³¹P⁺. Despite these challenges, the dopant implantation profiles measured by APT showed excellent agreement with predictions from implantation simulations performed using the SRIM software.

## ii. Impurities in Si

*C implant in Si*. Dumas et al. (2022) addressed the quantification of carbon in implanted silicon, including a detailed analysis of the composition of carbon clusters (Dumas et al., 2021). Carbon was implanted into (100)-oriented Si wafers either as ¹²C alone or as a mixture of ¹²C and ¹³C, at the same dose of 1 × 10¹⁵ at./cm², featuring a C-atomic fraction of ~0.2 at.%. Importantly, the use of isotopically mixed carbon implantation provides a robust strategy to resolve mass-spectrum overlaps and to validate peak assignments based on the known isotopic ratio. Following annealing at ~750 °C to induce recrystallization and carbon clustering, APT analyses were performed using a LaWaTAP system, operated with a UV laser (λ=343 nm) at a repetition rate of 100 kHz. Measurements were first carried out under high electric field conditions and subsequently under lower field conditions by increasing the
laser power. In the high-field regime, the charge-state ratio CSR($Si^+/Si^{2+}$) was approximately 50, whereas under lower field conditions it decreased substantially, ranging from ~3.6 to ~20. These results demonstrate that carbon quantification is significantly improved when operating at lower electric fields, particularly when combined with equal proportions of $^{12}$C and $^{13}$C implanted (see section 4.d.vi on isotope substitution). The primary reason for this improvement lies in the strong suppression of thermal tails in the mass spectra at lower fields. Under these conditions, $C^+$ and $C^{2+}$ ions can be directly detected at 6 and 12 Da, respectively, clearly before the onset of the $Si^+$ and $Si^{2+}$ thermal tails, which are markedly attenuated compared to high-field spectra. Lower-field conditions also enable the identification of molecular ion peaks, including $SiC_2^{2+}$, $SiC_3^{2+}$, and $SiC_2^+$. This behavior can be explained by two complementary mechanisms. First, the reduction of thermal tails reveals peaks that are partially obscured at high fields. Second, molecular ion dissociation during flight to the detector is known to be enhanced at high electric fields (Peng et al., 2019, 2018). Consequently, lowering the field reduces dissociation events, increasing the probability of detecting intact molecular ions. A pronounced attenuation of thermal tails is also observed in the mass spectra associated with cluster regions. This effect directly reflects the decrease in the local electric field, as evidenced by the strong reduction of the CSR($Si^{2+}/Si^+$) from ~50 to 0.6. In samples containing a mixture of $^{12}$C and $^{13}$C, the presence of two carbon isotopes further enhances peak assignment by resolving otherwise ambiguous overlaps. For instance, $^{12}C^{12}C^+$ and $^{30}SiH_2O^{2+}$ coincide at 24 Da, while $C_3^+$ and $(H_2O)_2^+$ overlap at 12 Da; isotopic labelling allows these contributions to be unambiguously separated. Finally, operating at high evaporation fields is known to promote trajectory aberrations and defocusing effects, particularly for high-field species. These artefacts lead to an overestimation of interatomic distances and, consequently, to an underestimation of local carbon concentrations (Blavette et al., 2001). Consistently, lowering the electric field results in a substantial increase in the measured carbon content within the cluster core, from approximately 20 at.% (largely independent of the experimental conditions) to 46 at.%, in excellent agreement with the stoichiometric carbon concentration predicted by the SiC phase diagram.

As implant in Si; H, C and P impurities in Si. Ronsheim et al. (2010) investigated the accuracy of APT measurements for quantifying an As implant (nominal dose of $2.5 \times 10^{15}$ at./cm$^2$), as well as H, C, and P impurities in a Si epitaxial layer (Ronsheim et al., 2010). Despite the lack of detailed experimental conditions and results, the APT-derived concentrations were found to be accurate within 10 % of SIMS measurements.

### iii. Point defects in oxides

Hunnestad et al. have recently achieved atomic-scale quantification of oxygen defects in $(LuFe_2O_9)/(LuFe_2O_4)$ superlattices, providing unprecedented insight into their defect structure (Hunnestad et al., 2024). 3D reconstructions show that oxygen vacancies arranging in a layered three-dimensional structure, locally reaching ~$10^{14}$ cm$^{-2}$. However, the average oxygen concentration is found to be lower than the nominal value, a discrepancy attributed to the detection loss of neutral $O_2$ molecules. Since the CSR exhibits no significant variation in electric field strength, the formation of neutral $O_2$ is not expected to vary across the superlattice. Oxygen deficiencies arising from neutral emission were also observed in $SrTiO_3$ by Rybak et al. (Rybak et al., 2025), with the average oxygen content measured at 0.55 at.%, slightly lower than the expected 0.6 at.%. The apparent strontium deficit, with a measured composition of 17.9 at.% compared to the nominal 20.0 at.%, was recovered by extending the mass range to include the thermal tail and background beyond the peak.
#### iv. Dopants and point defects in nitrides

Mg and Ge dopants in GaN. Despite Mg being the most widely studied dopant in GaN, the accuracy of Mg compositional measurements obtained by APT has not yet been conclusively validated. Amichi et al. reported that, in Mg-doped layers exhibiting Mg clustering, Mg concentrations determined by APT are in good agreement with SIMS measurements (Amichi et al., 2020). By contrast, Di Russo et al. recently applied a posteriori correction to APT data using complementary information provided by SIMS for both GaN:Mg and GaN:Ge (E Di Russo et al., 2020). In a different approach, and building on the findings of Rigutti et al. (Rigutti et al., 2016a), Siladie et al. (Siladie et al., 2018) employed high laser energies and low DC field conditions (FlexTAP, $\lambda$ = 343 nm, $E_{las}$ = 2.4 nJ) to ensure accurate determination of the III-site fractional occupancy (i.e., Mg/(Mg+Ga)). Under these conditions, the $Ga^{2+}/Ga^{+}$ ratio map was homogeneous within 0.05, meeting the criterion established by Koelling et al. for low-field regimes enabling reliable III-site occupancy measurements (Koelling et al., 2016).

Vacancies in (Ti,Al)N. In an early APT study of nano-lamellar cubic (Ti$_{1-x}$Al$_x$)N$_y$ thin films, Qiu et al. (Qiu et al., 2021) reported pronounced nitrogen over- and under-stoichiometry in Ti(Al)N and Al(Ti)N lamellae, respectively, which were attributed to metal and nitrogen vacancies. Vacancy concentrations of up to 12% for metals in Ti-rich regions and up to 36% for nitrogen in Al-rich volumes were inferred from APT data. However, a subsequent correlative study of Hans et al. (Hans et al., 2023) combining ion beam analysis and APT demonstrated that vacancy concentrations in nano-lamellar (Ti$_{1-x}$Al$_x$)N$_y$ cannot be reliably quantified from APT alone, as the apparent stoichiometry critically depends on the field evaporation conditions. These findings indicate that the previously reported high vacancy concentrations predominantly arise from field-induced artefacts rather than reflecting the intrinsic defect chemistry of the material.

#### v. Dopants and impurities in GaAs

Du et al. (Du et al., 2013) investigated the spatial distributions of dopants and impurities in GaAs nanowires (NWs) grown on n-type (111)B substrates. APT analyses were performed using a LEAP 3000X Si instrument equipped with a green laser ($\lambda$ = 532 nm), operated at pulse energies between 10 and 100 pJ. The NWs exhibit a composition of approximately 55% Ga and 45% As, indicating a deviation from the expected 1:1 stoichiometry. This deviation is partly due to peak overlap between $As_2^{2+}$ and $As^+$ ions, but is primarily caused by As ions evaporating between laser pulses, generating extended high-mass tails in the As-related peaks of the mass spectrum. These ions are not correctly ranged, contributing instead to the background noise rather than to the resolved mass peaks. In addition to the matrix species, Si dopants and residual contaminants (H, C, O, etc.) were detected. Although such ions are generally expected to accumulate at the NW edges, they were also observed within the core region. To improve the reliability of the dopant analysis, multiple hit events were selectively filtered. Since instrumental noise occurs only sporadically, events involving more than one ion per pulse are rare, and the mass spectrum is therefore largely dominated by single ion detections. Applying this filtering strategy increased the signal-to-noise ratio from 100:17 to 100:2 (Yao et al., 2010). Prior to filtering, single ion events appeared relatively uniformly distributed throughout the NWs, partly reflecting background noise. After excluding multiple hits, however, the spatial distributions became more physically meaningful, with dopants concentrated in the outer regions of the nanowires, consistent with expectations.
# 6. Conclusions and perspectives

As a concluding part of this review, we will summarize some perspective directions in APT research with potential developments or consequences on compositional metrology. These research domains are categorized into two main domains, which are nevertheless strongly entangled, i.e. the implementation of instrumentation and the implementation of methods. As a conclusion, a set of recommendations will be given for present and perspective users.

## a. Instrumental implementations

### i. Detector Technology

Overcoming the current limitations of detection systems is one of the main zones of instrumental development in APT. In the near future, the development of new event encoding readouts will enable to unlock the bottleneck of DLD detectors. Indeed, the progress in microelectronics during recent decades substantially improved characteristics of various optical sensing devices, which could be combined with MCPs. Historically optical detectors were skipped due to the low achievable repetition rate (OTAP for instance was limited to the kHz regime), and the incapacity to achieve timing measurement on pixels, requiring the use of additional timing measurement. Nevertheless, the parallel multi-hit detection capabilities were without comparison to DLDs. Spots much smaller than one millimeter could be resolved (compared to the cm size for a DLD). The development of highly pixelated fast Timepix readout enabled a large number of novel hybrid detectors, where incoming particles are initially converted into a measurable charge (> 1000 e-) by MCPs (Fig. [29]). Low dark currents and low gain make MCP/Timepix hybrid devices very attractive for the high achievable spatial and temporal resolution detection of low energy ions (~200 ps in the last version Timepix4). One of the major advantages of Timepix readout in MCP detectors is the substantial increase of counting rate capability as each pixel in the readout is an independent counter, enabling ~ GHz rates for a 28 × 28 mm² detector operating in event counting mode. At the same time, many simultaneous events can be encoded by the pixelated readout, which was not possible with most of the conventional high resolution MCP detectors. Another major improvement for the MCP detection technology is a substantial reduction of MCP gain, required for the detection of incoming particles. Due to the relatively low noise level in each pixel amplifier (typically 75 e⁻-rms), the output charge value of ~10⁴ electrons is sufficient for the low noise detection of individual particles, a factor of 10–1000 lower compared to charge division or time propagation readouts used in MCP detectors. The reduced gain also leads to a substantial increase of local count rate capabilities and (Llopart et al., 2007; Tremsin et al., 2020; Tremsin and Vallerga, 2020; Mathew et al., 2022) reduction in artefacts such as Ion Feedback emission increasing the noise level.
<figure><img src="image_33.png" /></figure>

Figure [29]. Schematic drawing of a prototype APT using a TimePix encoding anode. (a) An atom probe chamber was equipped with a detector composed of a pair of MCPs and a phosphor screen. The electrical signals are capacitively taken from the MCPs. The image on the screen is recorded through an UHV window by a TimePix detector (ASI Timepix TPX3). TPX3 instrument enables to record simultaneously the time-of flight (1.5 ns precision) and the position (X,Y with precision better than 100 microns) of every ion hit, enabling (b) mass spectrum (here an FeCr alloy) and (c) 3D reconstruction (only Cr in this case). (Unpublished results, courtesy of Gerald Da Costa and Amsterdam Scientific Instruments)

## ii. Terahertz pulsing

Terahertz-assisted atom probe tomography (THz-APT) has recently emerged as a powerful extension of conventional laser-pulsed APT, offering a fundamentally different pathway to trigger field evaporation. Terahertz (THz) radiation occupies the spectral window between microwaves and the infrared ($\lambda \approx 0.1-30$ THz), corresponding to picosecond temporal scales and photon energies of only a few meV. As a consequence, THz fields are intrinsically non-ionizing and deposit negligible thermal energy compared with near-UV or VIS excitation. This unique combination of low photon energy and sub- to few-picosecond duration makes THz transients particularly well matched to the intrinsic timescales of ion evaporation, enabling a regime in which emission can be driven predominantly by transient electric-field enhancement rather than by laser-induced heating. When interacting with atom probe nanotip, single-cycle THz pulses can be strongly amplified by near-field antenna effects, transiently delivering peak fields in the kV/cm range, boosting the apex field above the evaporation threshold while leaving the lattice temperature largely unchanged (Hunsche et al., 1998; Chen et al., 2000; Mair et al., 2004).
Pump-probe experiments on Al tips have recently provided direct evidence for this athermal, field-
driven mechanism, revealing a pronounced asymmetry between optical heating and THz excitation
(Eriksson et al., 2025). In contrast to conventional laser pulsing, which broadens the evaporation window
through thermal diffusion, THz excitation opens a sharply defined, field-limited emission gate that
suppresses thermal tails and improves temporal control over ion emission. These properties position
THz-APT as a compelling route toward higher-fidelity evaporation dynamics and motivate renewed
interest in the role of ultrafast, non-thermal field control in atom probe tomography. However, several
open challenges remain, including the origin of asymmetric time-of-flight and mass spectra and their
connection to ultrafast ion dynamics (Karam et al., 2023), the quantitative accuracy of compositional
measurements, and the limited efficiency of THz-triggered evaporation in wide-band-gap
semiconductors and oxides and low electrical conductive materials.

vi. *Deep and Extreme UV pulsing*

The use of Deep UV (typically, wavelength around 260-270 nm) has proven beneficial for compositional
accuracy of APT measurements of insulators. Reports of this have appeared for different instruments,
namely the commercial LEAP 6000 model on nitrides (Schiester et al., 2025) and the Photonic Atom
Probe on mineral oxides (Veret et al., 2025). Extreme UV (EUV) pulsing in APT, developed primarily
at NIST since ~2019, uses high-harmonic generation (HHG) to produce ultrafast (fs) pulses at 25-45 eV
(50-28 nm), enabling precise field evaporation with minimal heat and photon fluence for semiconductors
and insulators (Chiaramonti et al., 2020). This approach needs particular attention in the design of optical
paths and interfaces (beam propagation occurs in vacuum only), as well as managing interferences with
the detector by photoelectron generation (Caplins et al., 2023). Major achievements include stable
triggering of evaporation from Si, GaN, with tunable spectra and year-long source stability, overcoming
NIR-UV laser limitations like thermal tails and composition bias in III-nitrides. EUV APT yields cleaner
mass spectra with sharp peaks and low background, as shown in GaN, enabling accurate 50:50 Ga:N
stoichiometry without parameter-dependent bias seen in UV LAPT. For Mg-doped p-GaN, EUV clearly
resolves Mg<sup>2+</sup> at m/z 12 amid N<sub>2</sub><sup>2+</sup> at m/z 14, quantifying dopants reliably; similarly, for AlGaN alloys,
it measures variable III-site fractions with minimal variation across charge-state ratios. In InGaN, EUV
pulsing supports controlled evaporation, improving isotopic and alloy composition fidelity over UV
methods prone to Ga or N loss (Miaja-Avila et al., 2021). Encouraging results have also been reported
for oxides such as Al<sub>2</sub>O<sub>3</sub> and MgO (Garcia et al., 2024).

vii. *Hybrid pulsing*

Recent studies showed that combining voltage and laser pulsing in APT may deliver advantages over
traditional single-mode approaches (Zhao et al., 2017; Larson et al., 2023b). By synchronizing a fast
high-voltage pulse with a laser-induced thermal pulse, evaporation is confined to a narrow time window,
drastically cutting background noise and sharpening mass spectra. This temporal gating effect improves
signal-to-noise ratios—sometimes by an order of magnitude—especially for tricky materials like
semiconductors or low-thermal-diffusivity oxides. Hybrid pulsing reduces thermal tails, enhances peak
resolution, and improves the LOD for solute elements. The approach also widens the practical operating
range: it lowers fracture risks compared to pure laser pulsing and avoids the limitations of voltage-only
modes for fragile or poorly conductive materials. Of course, the gains depend on material-specific tuning
of laser and voltage pulse fractions, but the results—sharper peaks, cleaner spectra, and more accurate
compositions—make it an interesting option for perspective instruments.
viii. Correlative experimental setups

Correlative experiments in APT consist in coupling another technique to the atom probe. Beyond
sequential correlation, that can be achieved by analyzing APT samples with other techniques before
APT analysis, it is possible to design and implement in-situ correlation. Examples of these experiments
are the in-situ and operando APT for the study of chemical reactions in close proximity of the APT
chamber or within it (Haley et al., 2019; Lambeets et al., 2020a, 2020b), the photonic atom probe (PAP)
for the study of photoluminescence from evaporating APT samples (Houard et al., 2020), and the
different approaches for coupling APT with (S)TEM as in the TOMO project (Mayer et al., 2023) or in
the SAT-MET instrument (Da Costa et al., 2024). Although demanding in terms of instrumental
development, correlative techniques can provide important information that can be exploited for the
assessment of a compositional error or its correction (as well as for the confirmation of accuracy, of
course). For instance, the measurement of PL can be exploited as an indicator of the bandgap of an alloy
and for its statistical distribution, which depend on the composition of the sample. In situ TEM, on the
other hand, can help achieve optimal reconstructions and thus obtaining accurate quantification of
losses. Scientists involved in correlative experiments know well that the global information achievable
significantly overcomes the sum of the information separately issued by each technique involved (Di
Russo and Rigutti, 2022).

c. Implementation of methods

i. Field contrast imaging of defects

Compositional biases are an issue that sometimes could be turned into an advantage. This occurs in the
case in which certain structures or features contained in a given sample can be revealed just because of
the effect they have on a composition measurement. The use of CSR in the study of precipitates in metals
has been reported in several studies (Gault et al., 2021). In non-metallic systems, an example of this
approach is given by the possibility of imaging stacking faults even in the absence of impurity
segregation in them. A recent study conducted by Shu et al. reported that stacking faults in zincblende
GaN have higher evaporation field than the surrounding matrix, and this translates into an apparent Ga-
depletion within them, as reproduced in Fig. [30]. The position and orientation of the defects is shown
in Fig. [30]-(a), and are visualized by isoconcentration surfaces with the threshold of 80 at.% of Ga. The
profiles shown in parts (b) and (c) indicate that at the defect the field increases and, consequently, the
Ga fraction falls below the threshold. The reconstructed volume also shows that the defect propagates
into the active region of a LED device, containing QWs. Here, it could be shown that the defect can
influence the alloy distribution. Related studies also reported that SFs can influence the distribution of
dopants (Gundimeda et al., 2025; Xu et al., 2025). These studies are quite interesting in perspective as
they show how CSR inhomogeneities can yield important information about features that are not
associated to real compositional inhomogeneities. Density inhomogeneities could also constitute the
basis for field contrast imaging, provided no effects on the CSRs or on the observed composition occur.
(a)

Ga Iso-surface (80.8 at.%)

In Iso-surface (5 at.%)

N

<figure><img src="image_34.png" /></figure>

20 nm

(b)

100
90
80
70
60
50
40
30
20
10
Distance (nm)

Ga

(c)

0.030
0.025
0.020
0.015
0.010
0.005
0.000

19.5
20.5
21.0
21.5
22.0
22.5
23.0
23.5
24.0
24.5
Distance (nm)

SF

SF

Figure [30]. Field contrast imaging in APT revealing presence and orientation of stacking faults in ZB-GaN. (a) APT reconstruction of an InGaN/GaN MQW LED containing SFs. The yellow iso-concentration surfaces on the right indicate the SFs. (b) One-dimensional atomic fraction and (c) CSR(Ga²⁺/Ga⁺) profile of Ga in a volume along the red arrow in (a) (Reproduced with permission from (Shu et al., 2025), Elsevier).

ii. Cryo-APT and organic systems

The analysis of organic systems can be carried out by APT provided adapted preparation methods are applied (Stoffers et al., 2012; Zhou et al., 2023). The development of cryo-preparation methods has further enabled the analysis of softer matter, such as water solutions, biological systems or organic molecules (Gerstl and Wepf, 2015). A review of APT metrology in these domains is not within the scope of this review, but several general points are worth mentioning. Recent works, demonstrate that APT can achieve sub-Dalton mass resolution and ppm-level sensitivity for small-molecule organic compounds (Proudian et al., 2019; Bingham et al., 2021). Under optimized laser conditions, intact molecular ions are preserved, enabling quantitative analysis with minimal fragmentation. This capability is critical for mapping nanoscale chemistry in organic photovoltaics and OLEDs, linking molecular segregation and interfacial reactions to device performance. DFT modeling complements experiments by predicting ion stability and fragmentation pathways (Nickerson et al., 2015; Dietrich et al., 2025).
Significant complexity arises in these systems as mass spectra are dominated by intact or partially
fragmented molecular ions (often multi-charged), rather than monoatomic ions. This increases peak
number, peak density and the likelihood of overlaps, complicating the interpretation. Molecular peaks
and their isotopic envelopes are resolved with m/Δm ~1000, enabling molecular formula identification.
Post-ionization fragmentation of dications into daughter ions generates multiple-hit events and
additional peaks, introducing ambiguity in peak ranging and compositional quantification (Meng et al.,
2022b). The influence of experimental conditions on the composition measurement has been pointed
out. Laser pulse energy, specimen temperature, and surface field—significantly impact the balance
between intact molecular ions, clusters, and fragments.

Some of the implications for compositional metrology are specific to these systems. On one hand, molecular-level analysis is often required: compositional metrology must operate at the molecular-ion level, matching complex isotopic patterns and charge states to candidate molecular formulas rather than atomic fractions. In this sense, a high mass resolving power is essential to separate overlapping molecular/isotopic peaks. On the other hand, fragmentation and multiple events are extremely frequent and require advanced data correction to avoid under- or over-estimation of species, as fragmentation biases compositions and varies with molecular energetics and experimental conditions (Bingham et al., 2021; Meng et al., 2022b).

iv. Automated/enhanced data mining

The development of automated or enhanced data mining and analysis methods for APT, mostly based
on machine learning (ML) approaches, have been recently reviewed by Li et al. and the reader is referred
to this reference for enjoying an exhaustive snapshot (Li et al., 2026). These methods are particularly
adapted to the extended datasets issued from APT experiments, and may thus have a future impact on
common practices. Among the main objectives of these approaches are speeding up the analysis,
increasing its efficiency, reducing user and instrument dependency and enabling discoveries beyond
human capability. Altogether, these methods should comply with the Findable, Accessible,
Interoperable and Reusable (FAIR) principle. Within the domain of compositional metrology, these
methods are expected to efficiently tackle the challenges related to user dependency and data
complexity. An obvious target for their application is in mass spectrometry, with automated peak
identification and decomposition, but more complex statistical analysis is well within the range of PL
methods, in order to investigate short range ordering, clusters, nanoscale structures, relationship between
chemistry and crystal structure, pushing resolution limits further and helping the user in visualizing and
quantifying relevant features in the system. This, in turn, calls for community-driven efforts to provide
open, reproducible software for APT data analysis, with possible interface to commercial solutions.
This, of course, would not eliminate the need for critical attitudes by APT users, as they will still be
responsible for the accuracy of data and results in order to avoid that biases are simply transferred to IA
(as it may have happened in some non-scientific domains).

c. Recommendations for users

As a distillate of this work on compositional metrology we would like to underline the awareness that compositional biases are an extremely important domain of research in the APT community, and that the users should share this awareness and agree for a minimum set of attitudes and practices concerning the occurrence of errors, the communication about them, and their management. We have therefore listed some recommendations concerning experimental practices, data analysis, standardization and research in APT compositional metrology.
i. *Good experimental practices*

Rigor and precision form the foundation of reliable Atom Probe Tomography (APT) analysis. Absolute certainty in mass spectrum interpretation is essential, as ambiguity introduces the risk of misinterpretation and compromises result integrity. Precise terminology in quantifying composition ensures clarity and reproducibility, minimizing the potential for miscommunication in research. Rational and purposeful exploration of experimental parameters is necessary. Educated guesses in mass spectrum attributions, particularly those made to align with expected outcomes, should be avoided due to their deceptive nature and potential to undermine findings. Awareness of instrument limitations is critical, as it enables realistic interpretation of results. Field evaporation, central to APT, is an inherently complex phenomenon. Its intricacies must remain a focal point, as they directly influence observed data and experimental outcomes.

ii. *Data mining and analysis*

Investigation into the origins of biases should extend beyond standard measurement protocols, such as constant detection rates, in order to uncover the experimental parameters responsible. They also should extend into the data mining protocols and methods. Mass spectra should be regularly reported or made available in data repositories. Portable metrics, including CSRs for the determination of the equivalent field F<sub>eq</sub>, enhance the comparability and applicability of findings across different instruments and different studies. While global accuracy perfection may be unattainable, the pursuit of optimal conditions—for reconstruction fidelity, compositional accuracy, or specimen yield—remains a priority. Post-reconstruction corrections require careful application. Adjustments must align with the statistical properties of unbiased reference datasets in order to maintain analytical integrity. Any future application of machine learning or IA-driven analysis should be critically scrutinized — not only by the developers, but also by any user — before it can serve as an automated or enhanced set of methods for producing results.

iii. *Role of standards*

It is important for users and operators of APT that every step of their work is compliant with the results of the work in standardization that has been carried out over the last fifteen years within the field emission and APT community (Ulfig et al., 2009; Prosa et al., 2014). This work concerns not only terminology, which can be found on the ISO website both for general metrology concepts (“ISO/IEC Guide 99:2007(en), International vocabulary of metrology — Basic and general concepts and associated terms (VIM),” n.d.) and for specific APT concepts (“ISO 18115-1:2023(en), Surface chemical analysis — Vocabulary — Part 1: General terms and terms used in spectroscopy,” n.d.), but also the production of standard systems with known chemical characteristics, and good practices in data analysis and presentation.

iv. *Promoting research in APT metrology*

Bias identification in material systems represents not only a setback, but also a significant opportunity. Such discoveries can yield meaningful contributions to the APT community and may define key research outcomes. No universal protocol exists for ideal APT analysis conditions. While prior studies provide useful reference points, tailored approaches are necessary to meet specific objectives, such as reconstruction fidelity, compositional accuracy, or specimen yield optimization. Measurement
objectives must be clearly defined. For example, in materials like AlGaN, a stoichiometric III/V ratio
may not accurately represent the Al III-site fraction. Precise goal-setting ensures meaningful and aligned
measurements: the optimal conditions for the resolution of interfaces, for instance, may not be the same
as those for optimizing compositional accuracy. Exact composition measurement may not always be
achievable. Research should strive for the highest possible accuracy while acknowledging the inherent
limitations of APT, as with any experimental technique. This pragmatic perspective fosters more robust
and reliable research outcomes, which will be surely applied to the perspective work that is already
ongoing. Furthermore, the work on compositional metrology is tightly bound to the efforts towards a
deeper understanding of field evaporation: bond structure, bond breaking, surface reconstruction, all
these aspects play a role in the determination of evaporating species and of spatial and temporal
correlations (Cojocaru-Mirédin et al., 2024). This effort should be pursued in perspective within the two
aforementioned entangled directions, namely the implementation of instruments and of methods.

Acknowledgements

Financial support was provided by the French National Research Agency (ANR) via the ASCESE-3D
project (ANR-21-CE50-0016), via the BE-SAFE project (ANR-24-CE08-6529), via the LABEX EMC3
QUANTIPHY project and under France 2030 investment plan (reference ANR-22-EXOR-0008).
E.D.R. acknowledges the MOST—Sustainable Mobility Center and the European Union Next-
GenerationEU [PIANO NAZIONALE DI RIPRESA E RESILIENZA (PNRR)—MISSIONE 4
COMPONENTE 2, INVESTIMENTO 1.4 – D.D. 1033 17/06/2022, CN000000023]. This manuscript
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