ARL-TR-7783 ● SEP 2016

US Army Research Laboratory

Characterization of Magnetron Sputtered 

Copper-Nickel Thin Films and Alloys

by Eugene Zakar, Andrew Chen, Robert Burke, 

Samuel G Hirsch, Nicholas Strnad, and James Mulcahy

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ARL-TR-7783 ● SEP 2016

US Army Research Laboratory

Characterization of Magnetron Sputtered 

Copper-Nickel Thin Films and Alloys

by Eugene Zakar, Andrew Chen, and Samuel G Hirsh

Sensors and Electron Devices Directorate, ARL

Robert Burke, Nicholas Strnad, and James Mulcahy

General Technical Services, LLC, Columbia, MD

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10/2015 to 7/2016

4. TITLE AND SUBTITLE

Characterization of Magnetron Sputtered Copper-Nickel Thin Film and Alloys

5a. CONTRACT NUMBER

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6. AUTHOR(S)

Eugene Zakar, Andrew Chen, Robert Burke, Samuel G Hirsch, Nicholas Strnad, 

and James Mulcahy

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5e. TASK NUMBER

5f. WORK UNIT NUMBER

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US Army Research Laboratory

ATTN: RDRL-SER-L

2800 Powder Mill Road

Adelphi, MD 20783-1138

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ARL-TR-7783

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13. SUPPLEMENTARY NOTES

14. ABSTRACT

Copper (Cu)-nickel (Ni) thin films are prepared by magnetron sputtering using an AJA International model ATC-2200 system.

The as-deposited films are in the amorphous state during room temperature deposition but transition to a crystalline state at an 

elevated substrate temperature beyond 250 °C. The crystalline films have a mixed (111)- and (200)-oriented texture that becomes

predominantly (111)-orientated after an annealing treatment. Bilayer CuNi deposited films with ratio of 12:1, 6:1, 4:1, and 3:1

produced final alloy concentrations of 90/10, 83/17, 76/24, and 70/30 atomic %, respectively, after annealing, and their average 

surface roughness increased with higher Cu concentration. These results show that the final thin film alloy composition can be 

effectively controlled by varying the ratio of the initial deposited Cu and Ni layers. The morphology of these films were studied 

by atomic force microscope (AFM), X-ray Diffraction (XRD), electrical 4-point probe, and energy-dispersive X-ray 

spectroscopy (EDX). 

15. SUBJECT TERMS

CuNi alloy, deposition, sputter, thin film, LPCVD

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Eugene Zakar

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(301) 394-1628

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Contents

List of Figures iv

List of Tables iv

1. Introduction 1

1.1 Co-sputter Deposition 1

1.2 Experimental Parameters 1

1.2.1 Sample Preparation 1

2. Experimental Results 3

2.1 Sputter deposition rates for Cu and Ni films 3

2.2 Effect of Argon Chamber Pressure During Sputtering 4

2.3 Effect of Substrate Temperature During Sputtering 5

2.4 XRD texture Analysis of As-deposited CuNi Bilayer and Alloyed Films 6

2.5 Composition Analysis of the Alloyed Films 6

2.6 Effect of Composition on Surface Roughness 7

2.7 Uniformity of the Depositions 8

3. Conclusion 9

4. References and Notes 10

List of Symbols, Abbreviations, and Acronyms 11

Distribution List 12
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List of Figures

Fig. 1 Plot of deposition rates for a) Ni and b) Cu sputtered films..................4

Fig. 2 XRD of as-deposited films showing effect of a) sputter pressure on Cu 

at 25 °C and b) substrate temperature on Ni at 5 mT ............................5

Fig. 3 XRD texture of CuNi bilayer and alloyed films....................................6

Fig. 4 AFM image and roughness measurement of a) 220 nm for 12:1, 

b) 86 nm for 6:1, c) 74 nm for 4:1, and d) 66 nm for 3:1 CuNi alloy....8

Fig. 5 Contour map showing measured electrical resistivity values across 25 

points on a 100-mm diameter substrate for 3:1 CuNi alloy...................8

List of Tables

Table 1 Experimental sputtering parameters ......................................................2

Table 2 List of prepared bilayer CuNi samples ..................................................3

Table 3 EDX composition analysis of the CuNi alloyed films...........................7
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1. Introduction

1.1 Co-sputter Deposition

Sputter coating is the process of creating a vapor via physical means and depositing 

the vapor to form a thin film on a substrate. Sputtering uses ions from a gas 

discharge plasma in an electric field. The electric field accelerates the ions towards 

the target material, the cathode. The resulting collision and transfer of kinetic 

energy dislodges atoms from the target, which then impinge on the substrate—the 

anode—forming the desired thin film.

1 Sputtering sources often employ an 

arrangement of permanent magnets, or magnetrons, that use strong electric and 

magnetic fields to confine charged plasma particles near the surface of the sputter 

target. Electrons follow helical paths around magnetic field lines undergoing more 

ionizing collisions with gaseous neutrals near the target surface. The magnetron

configuration allows a higher sputtering rate than targets without the magnetron 

configuration.

The amount of material sputtered, Q, in a unit of time under constant conditions is 

inversely proportional to the gas pressure, p, and anode-cathode distance, d:

Q = k V I / p d (1)

where k is the constant of proportionality, V is the working distance, and I is the 

discharge current. 

Co-sputtering can be performed by using 2 targets, either simultaneously or by 

alternating the 2 targets. Co-sputtering is used to form alloys or deposit composite

materials. The stoichiometry is controlled by optimizing the power density of each 

gun (target) separately. In this report, we describe a modified co-sputtering process

whereby a first layer of nickel (Ni) thin film is deposited on the substrate, followed 

by a second layer of copper (Cu) thin film that forms an alloy after a hightemperature anneal process. 

1.2 Experimental Parameters

1.2.1 Sample Preparation

We used an AJA International Inc. model ATC-2200 sputter system with 75-mmdiameter targets in a Stiletto Series ST30 source configuration. Options on the 

system include the ability to adjust the substrate distance, tilt the target, and heat 

the substrate. 
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Prior to preparation of the CuNi bilayer, it was necessary to determine the 

deposition rates for Cu and Ni in order to precisely control each film thickness.

Initial deposition rate studies of Cu and Ni were carried out on a 100-mm wafer. 

Uniformity should not be an issue, since the sputter system was designed to provide 

good uniformity across a substrate twice the target diameter. Keeping in mind that 

the uniformity of the film improves if the chamber pressure is decreased and/or the 

distance between target and substrate is increased, we decided to set the distance to 

100 mm. For this study, we chose to vary the argon (Ar) pressure and the substrate 

temperature during sputtering. Power, target to substrate distance, target tilt angle, 

and substrate rotation were held constant. A summary of our experimental 

sputtering parameters is found in Table 1. In theoretical terms the amount of 

sputtered material, Q, is inversely proportional to the substrate distance, d, from the 

source target according to Eq. 1. In order to make up for the reduction in Q due to 

the high d, we intentionally increased the power level to a relatively high level of 

500 W d.c. to improve the deposition rate in order to achieve a film thickness of 

1 μm within a reasonable amount of time. Substrate rotation was employed during 

the sputtering to improve the uniformity of the film across the diameter of the 

substrate.

Table 1 Experimental sputtering parameters

Parameter Const/Var Condition (unit)

Power Constant 500 (W d.c.)

Distance Constant 100 (mm)

Target tilt Constant 6 (mm)

Rotation Constant 60 (rot/min)

Ar pressure Variable 5, 10, 15 (mT)

Substrate temp. Variable 25, 250, 400 (°C)

The starting substrate material consisted of a polished silicon (Si) wafer—500 μm 

thick, 100 mm in diameter with (100) orientation, N-doped, and a 280-nm layer of 

thermal oxide grown on top. After loading the sample and evacuating the sputter 

chamber to a base pressure of ~10–7 Torr, the experiments were performed in the 

presence of different Ar gas pressure and temperature settings for each sample with 

a deposition time of 5 min. After a deposition was complete, the substrate was 

coated with photoresist and exposed to a wet etchant to remove the Cu or Ni film 

from a portion of the wafer in order to measure the film thickness. The film 

thickness was measured using a Tencor KLA-15 profilometer. The deposition rate 

was calculated by taking the measured film thickness and dividing by the deposition 

time. A plot of the calculated deposition rates for Cu and Ni was then generated for 

the variable deposition parameters.
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Based on the derived deposition rates, we then proceeded to prepare several bilayer 

thin film samples with different thickness ratios of Cu to Ni (Table 2). Varying 

amounts of Ni (50, 100, 150, and 200 nm) were sputter-deposited on the starting

wafer, followed by a fixed 600-nm layer of Cu on top. The bilayer stacks were then 

annealed for 30 min at 1000 oC in the presence of 40%H2/60%Ar gas mixture at a 

pressure of 15 Torr to form alloys of varying concentrations that were later 

confirmed by the energy-dispersive X-ray spectroscopy (EDX) method.

Table 2 List of prepared bilayer CuNi samples

Sample 

No.

CuNi 

ratio

Layer Thickness 

(nm)

Temp 

(°C)

Pressure 

(mT)

S1 12:1 (600nmCu:50nmNi 25 5

S2 12:1 (600nmCu:50nmNi 25 15

S3 12:1 (600nmCu:50nmNi 400 5

S4 12:1 (600nmCu:50nmNi 400 15

S5 6:1 (600nmCu:100nmNi) 25 5

S6 6:1 (600nmCu:100nmNi) 25 15

S7 6:1 (600nmCu:100nmNi) 400 5

S8 6:1 (600nmCu:100nmNi) 400 15

S9 4:1 (600nmCu:150nmNi) 25 5

S10 4:1 (600nmCu:150nmNi) 25 15

S11 4:1 (600nmCu:150nmNi) 400 5

S12 4:1 (600nmCu:150nmNi) 400 15

S13 3:1 (600nmCu:200nmNi) 25 5

S14 3:1 (600nmCu:200nmNi) 25 15

S15 3:1 (600nmCu:200nmNi) 400 5

S16 3:1 (600nmCu:200nmNi) 400 15

Characterization of the as-deposited bilayer films and post-annealed CuNi alloys 

was accomplished by an X-ray diffraction (XRD) Rigaku system with CuKα 

radiation, λ=0.15405 nm, in the Bragg-Brentano geometry, and the sealed X-ray 

source tube was operating at 40 kV and 44 mA current. Surface morphology was 

investigated by an atomic force microscopy (AFM) Veeco Nanoman system. The 

microstructural and elemental compositions of the final alloyed films were 

analyzed using EDX.

2. Experimental Results

2.1 Sputter Deposition Rates for Cu and Ni Films

The deposition rates for Cu and Ni with respect to Ar pressure are shown in 

Figs. 1a and b. The differences in the sputter deposition rates for Cu and Ni can be 

attributed to the differences in the mass for Cu and Ni atoms. Based on the data, 

pressure had a significant effect on the sputter rates. The sputter rate for Ni 

increased from 198 to 230 Å/min when there was a reduction in pressure from 
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15 to 5 mT at 25 oC. The sputter rate for Cu increased from 336 to 451 Å/min when 

there was a reduction in pressure from 15 to 5 mT. The substrate temperature did 

not appear to greatly influence the sputter rate at 5 mT pressure for either of the 

target materials, as shown in the plots. The sputter rate for Ni only increased by 

6 Å/min when the substrate temperature was increased from 25 to 400 oC. The Cu 

sputter rate increased by 10 Å/min with the same rise in temperature. 

(a) (b) 

Fig. 1 Plot of deposition rates for a) Ni and b) Cu sputtered films

2.2 Effect of Argon Chamber Pressure during Sputtering

Pressure had a significant effect on the sputter rates for both Cu and Ni samples 

according to the results from Fig. 1. The sputter rates for Cu and Ni increased when 

the pressure decreased from 15 to 5 mT at 25 °C. The increase in the sputtering rate 

is due to the decreased pressure in the chamber that leads to fewer collisions 

between Ar atoms in the plasma, allowing more sputtered atoms to reach the surface 

of the substrate. The effect of Ar pressure on the nature of the XRD diffraction 

patterns for as-deposited Cu film is shown in Fig. 2a. There are 2 major intensity 

peaks for Cu—a (111) peak at 2θ position of 44.6° and a (200) peak at 2θ position

of 50.6°. The intensity of the (111) and (200) peaks increased when there was a 

reduction in Ar pressure, while at the same time each of the peaks became narrower

and sharper. The same effect was seen with sputter-deposited Ni film samples (not 

shown). A low Ar pressure setting of 3 mT produced the highest intensity peak and 

sputter rates for the Cu- and Ni-deposited films. However, due to the unsteady 

nature of the plasma occurring at the low 3-mT setting, we discontinued its use and 

maintained a 5-mT setting for the rest of the experiments.
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 (a) (b)

Fig. 2 XRD of as-deposited films showing effect of a) sputter pressure on Cu at 25 °C and 

b) substrate temperature on Ni at 5 mT

2.3 Effect of Substrate Temperature during Sputtering

The substrate temperature had a significant effect on the crystallinity of the 

deposited films. Figure 2b shows the XRD peaks of a non-crystalline Ni film 

deposited at a substrate temperature of 25 °C and 5 mT. Its 2θ peak intensity of 

(111) texture at 44.6° looks approximately equal in proportion to its width. There 

appears to be a little bump at the 2θ position of 52.1°, which is a typical 

characteristic of an amorphous layer. Amorphous, or non-crystalline, film is 

observed when the X-rays are scattered in many directions, leading to a bump-like 

feature across the 2θ position instead of a narrow and high peak.

3 A crystalline film

is typically composed of highly ordered and periodically arranged atoms in a 3-D 

space. The transition from an amorphous film to a crystalline film was clearly 

attained at higher sputter substrate temperatures of 250 and 400 °C for the Ni film,

as evidenced from the XRD peaks becoming sharper and narrower. The same 

results are observed for the sputtered Cu film samples. The additional appearance 

of (220) and (311) peaks became noticeable (not show here) when the sputtering 

pressure was increased above 15 mT.

2

Since only (111) textured grains are desired in this experiment, we decided to 

narrow our choice of samples to S3, S7, S11, and S15, as they fall within the most 

favorable parameters of 400 °C substrate temperature and 5-mT Ar chamber 

pressure according to Table 2.
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2.4 XRD texture Analysis of As-Deposited CuNi Bilayer and 

Alloyed Films

We studied the evolution of film texture from the as-deposited condition of Cu, Ni, 

and CuNi bilayer films to the final alloying stage. The XRD patterns for individual 

as-deposited Cu and Ni films with (111) and (200) peaks, including the 

co-deposited CuNi bilayer and alloyed film for sample S3, are shown in Fig. 3. The 

Cu and Ni films in this figure were deposited at the optimized deposition pressure 

of 5 mT and temperature of 400 °C. The 3:1 Cu:Ni bilayer films have the additive 

characteristics of the individual Cu and Ni peaks. When the co-deposited bilayer 

films were finally annealed at 1000 °C for 30 min, the final 3:1 CuNi alloy 

transformed to a preferred (111) orientation. There is a slight shift in the 2θ position 

of the (111) peak to a higher angle, which indicates the formation of the alloyed 

film, with the Ni substituting the lattice sites of Cu since the ionic radius of Ni (69 

pm) is lower than that of Cu (72 pm). We observed similar behavior in the other 

samples of Cu and Ni with ratios of 4:1, 6:1, and 12:1, with the exception that 

bilayer films 3:1 sputtered at a low temperature of 25 °C, which produced 

undesirable non-crystalline films. 

Fig. 3 XRD texture of CuNi bilayer and alloyed films

2.5 Composition Analysis of the Alloyed Films

EDX spectroscopy is an analytical technique used for the elemental analysis or

chemical characterization of samples. The EDX parameters used here were a 20-

kV accelerating voltage, 104-μA beam current, 10k counts on the Cu k range, and 

2000x magnification on each of the samples. 
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Several samples sputtered at a high substrate temperature of 400 °C and low 

pressure of 5 mT, which previously showed preferred (111) crystalline structures

were alloyed for EDX analysis. The results of the alloy concentration analysis are 

reported in Table 3 in terms of both the atomic % (at.%) and weight %. Bilayer 

films consisting of Cu to Ni ratios of 12:1, 6:1, 4:1, and 3:1 produced alloy 

concentrations of 90/10, 82/18, 76/24, 71/29 at.%, respectively, after annealing. 

Samples with the 6:1 and 4:1 ratios may have deviated from the expected ideal 

80/20 at.% and 75/25 at.% by approximately ±1 at.% due to slight differences in 

the actual deposited layer thickness of the bilayer films. 

Table 3 EDX composition analysis of the CuNi alloyed films

Cu:Ni CuNi layer thickness Alloy concentration

ratio (nm) (at.%) (weight %)

12:1 600Cu/50Ni 90Cu/10Ni 91Cu/09Ni

6:1 600Cu/100Ni 82Cu/18Ni 83Cu/17Ni

4:1 600Cu/150Ni 76Cu/24Ni 77Cu/23Ni

3:1 600Cu/200Ni 70Cu/30Ni 71Cu/29Ni

2.6 Effect of Composition on Surface Roughness

The CuNi bilayer deposited films were annealed for 30 min at 1000 °C in a lowpressure chemical vapor deposition (LPCVD) reactor with a gas mixture of 

40%H2/60%Ar at 15 Torr pressure to form the final alloys. We measured the 

average roughness (Ra) of the annealed films using AFM over an area consisting of 

20 × 20 μm for each of the samples, and the images are shown in Fig. 4. The size 

of the grains increased, and the Ra decreased as the ratio of Cu to Ni decreased from 

12:1 to 3:1 after the annealing treatment, as evidenced by signs of granular features 

on the surface of AFM images shown in Fig. 4. It appears that the annealing 

parameters here are acceptable for alloys rich in Ni but not yet optimized for alloys

rich in Cu due to evaporation effects. The annealing process needs to be optimized 

in order to reduce the film roughness found in Cu rich alloys, such as the 12:1 CuNi 

samples. We are beginning to experiment with higher pressure during annealing to 

reduce the evaporation rate of Cu that we believe is causing the increased 

roughness.
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 (a) (b) (c) (d)

Fig. 4 AFM image and roughness measurement of a) 220 nm for 12:1, b) 86 nm for 6:1, 

c) 74 nm for 4:1, and d) 66 nm for 3:1 CuNi alloy

2.7 Uniformity of the Depositions

In order to verify the uniformity of the deposited films across a 100-mm-diameter 

wafer, we performed a quick and non-destructive test using an electrical 4-point 

probe measurement technique. We measured the electrical sheet resistivity of the 

deposited films across 25 equally separated points in a circular pattern around the 

wafer, from which we generated the contour map shown in Fig. 5 for 3:1 CuNi

(sample S15). We calculated a uniformity of 94% using the equation:

UUUUUUUUUUUUUUUUUUUU = �1 − ssssss

mmmmmmmm � ∗ 100. (2)

The film uniformity for the deposited bilayer sample was excellent across a 

100-mm-diameter substrate with the established sputtering parameters of 5-mT Ar 

pressure and 400 °C substrate temperature. The color bands in Fig. 5 represent sheet 

resistance (Ω/cm2) values. The other film samples, S1–S16, also exhibited very 

similar calculated values for uniformity and reproducibility.

Fig. 5 Contour map showing measured electrical resistivity values across 25 points on a

100-mm-diameter substrate for 3:1 CuNi alloy
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3. Conclusion

The AJA model ATC-2200 sputtering system can deposit films with a uniformity 

of 94% or better at a substrate distance of 100 mm. A substrate temperature of 

250 °C was required to achieve films with a preferred (111) crystalline orientation

after alloying of the samples. We demonstrated a simple and effective way to

produce CuNi film alloy concentrations in the range from 90/10 to 70/30 at.% by

varying the ratio of the initial deposited Cu and Ni layers.
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4. References and Notes

1. Brodie I, Murray JJ. The physics of microfabrication. New York (NY): Plenum 

Press; 1982.

2. Chen A, Zakar E, Burke R. Preparation of copper (Cu)-nickel (Ni) alloy thin 

films for bilayer graphene growth. Adelphi (MD): Army Research Laboratory 

(US); 2016. Report No.: ARL-TR-7593.

3. Cullity BD. Elements of X-ray diffraction. Reading (MA): Addison-Wesley;

1978. p. 101–102.
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List of Symbols, Abbreviations, and Acronyms

AFM Atomic Force Microscopy

Ar argon

at.% atomic percent

C carbon

CH4 methane

Cu copper

EDX Energy-Dispersive X-ray Spectroscopy

H2 hydrogen

LPCVD Low Pressure Chemical Vapor Deposition

Ni nickel

Ra average roughness

vol.% volume percent

XRD X-ray Diffraction
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