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Timestamp: 2014-12-19 08:44:14
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Matched Legal Cases: ['Application No. 60', 'Application No. 60', 'Application No. 60', 'Application No. 60', 'Application No. 60', 'Application No. 60', 'Application No. 60']

Patent US6962859 - Thin films and method of making them - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inAdvanced Patent SearchPatentsThin, smooth silicon-containing films are prepared by deposition methods that utilize a silicon-containing precursor. In preferred embodiments, the methods result in Si-containing films that are continuous and have a thickness of about 150 Å or less, a surface roughness of about 5 Å rms or less,...http://www.google.com/patents/US6962859?utm_source=gb-gplus-sharePatent US6962859 - Thin films and method of making themAdvanced Patent SearchPublication numberUS6962859 B2Publication typeGrantApplication numberUS 10/074,564Publication dateNov 8, 2005Filing dateFeb 11, 2002Priority dateFeb 12, 2001Fee statusPaidAlso published asDE60223662D1, DE60223662T2, DE60227350D1, EP1374290A2, EP1374290B1, EP1374291A2, EP1374291B1, EP1421607A2, US6716713, US6716751, US6743738, US6821825, US6900115, US6958253, US7186582, US7273799, US7285500, US7547615, US7585752, US7893433, US8067297, US8360001, US20020168868, US20020173113, US20020197831, US20030022528, US20030068851, US20030068869, US20030082300, US20050048745, US20050064684, US20050208740, US20050250302, US20070102790, US20080014725, US20080073645, US20100012030, WO2002064853A2, WO2002064853A3, WO2002065508A2, WO2002065508A3, WO2002065516A2, WO2002065516A3, WO2002065516A8, WO2002065517A2, WO2002065517A3, WO2002080244A2, WO2002080244A3, WO2002080244A9Publication number074564, 10074564, US 6962859 B2, US 6962859B2, US-B2-6962859, US6962859 B2, US6962859B2InventorsMichael A. Todd, Ivo RaaijmakersOriginal AssigneeAsm America, Inc.Export CitationBiBTeX, EndNote, RefManPatent Citations (68), Non-Patent Citations (2), Referenced by (46), Classifications (117), Legal Events (6) External Links: USPTO, USPTO Assignment, EspacenetThin films and method of making themUS 6962859 B2Abstract Thin, smooth silicon-containing films are prepared by deposition methods that utilize a silicon-containing precursor. In preferred embodiments, the methods result in Si-containing films that are continuous and have a thickness of about 150 Å or less, a surface roughness of about 5 Å rms or less, and a thickness non-uniformity of about 20% or less. Preferred silicon-containing films display a high degree of compositional uniformity when doped or alloyed with other elements. Preferred deposition methods provide improved manufacturing efficiency and can be used to make various useful structures such as wetting layers, HSG silicon, quantum dots, dielectric layers, anti-reflective coatings (ARC's), gate electrodes and diffusion sources.
introducing a gas comprising trisilane to a chamber, wherein the chamber contains a substrate having a surface area of about 300 cm2 or greater and a substrate surface roughness; establishing trisilane chemical vapor deposition conditions in the chamber; and depositing an amorphous Si-containing film onto the substrate, the amorphous Si-containing film having a thickness in the range of 10 Å to 150 Å and a film surface roughness that is greater than the substrate surface roughness by an amount of about 5 Å rms or less, over a surface area of about one square micron or greater. 2. The method of claim 1, wherein the amorphous Si-containing film is deposited directly onto a dielectric material.
3. The method of claim 2, wherein the dielectric material is selected from the group consisting of silicon oxide, metal oxide, metal silicate, silicon oxynitride and silicon nitride.
4. The method of claim 2, wherein the film surface roughness is about 3 Å rms or less.
5. The method of claim 1, further comprising depositing an oxide layer directly onto the amorphous Si-containing film.
6. The method of claim 5, further comprising annealing the amorphous Si-containing film to form a plurality of quantum dots.
7. The method of claim 2, further comprising depositing a doped Si-containing layer directly onto the amorphous Si-containing film.
8. The method of claim 7, wherein the doped Si-containing layer further comprises germanium.
9. The method of claim 8, wherein the doped Si-containing layer further comprises carbon.
10. The method of claim 1, wherein the amorphous Si-containing film has a thickness non-uniformity of about 10% or less for a mean film thickness in the range of 100 Å to 150 Å, a thickness non-uniformity of about 15% or less for a mean film thickness in the range of 50 Å to 99 Å, and a thickness non-uniformity of about 20% or less for a mean film thickness of less than 50 Å.
11. The method of claim 1, wherein the substrate comprises a step or trench.
12. The method of claim 11, further comprising annealing the amorphous Si-containing film to form hemispherical grained silicon.
13. The method of claim 1, wherein the gas further comprises a dopant element selected from the group consisting of boron, arsenic, antimony, indium, and phosphorous.
14. The method of claim 13, wherein the amorphous Si-containing film is a diffusion layer.
15. The method of claim 13, wherein the depositing of the amorphous Si-containing film onto the substrate results in uniform incorporation of the dopant element throughout the amorphous Si-containing film.
16. The method of claim 1, wherein establishing trisilane chemical vapor deposition conditions comprises heating the substrate to a temperature in the range of about 400� C. to about 750� C. in the absence of a plasma.
17. The method of claim 1, wherein establishing trisilane chemical vapor deposition conditions comprises heating the substrate to a temperature in the range of about 450� C. to about 650� C. in the absence of a plasma.
18. The method of claim 1, wherein the amorphous Si-containing film is a Si�N film.
19. The method of claim 18, wherein the gas further comprises a nitrogen precursor.
20. The method of claim 19, wherein the nitrogen precursor is atomic nitrogen.
21. The method of claim 19, wherein the amorphous Si-containing film has a hydrogen content that is less than about 4 atomic %.
22. The method of claim 1, wherein establishing trisilane deposition conditions comprises maintaining a chamber pressure between about 1 Torr and 100 Torr.
23. A method for depositing a thin film, comprising:
introducing a gas comprising trisilane to a chamber, wherein the chamber contains a substrate having a substrate surface roughness; establishing trisilane chemical vapor deposition conditions in the chamber; depositing an amorphous Si-containing film onto the substrate, the amorphous Si-containing film having a thickness in the range of 10 Å to 150 Å and a film surface roughness that is greater than the substrate surface roughness by an amount of about 5 Å rms or less, over a surface area of about one square micron or greater; depositing an oxide layer directly onto the amorphous Si-containing film; and annealing the amorphous Si-containing film to form a plurality of quantum dots. 24. A method for depositing a thin film, comprising:
introducing a gas comprising trisilane to a chamber, wherein the chamber contains a substrate having a substrate surface roughness; establishing trisilane chemical vapor deposition conditions in the chamber; depositing a Si-containing film onto the substrate, the Si-containing film having a thickness in the range of 10 Å to 150 Å and a film surface roughness that is greater than the substrate surface roughness by an amount of about 5 Å rms or less, over a surface area of about one square micron or greater; and depositing a doped Si-containing layer directly onto the Si-containing film; wherein the Si-containing film is deposited directly onto a dielectric material. 25. The method of claim 24, wherein the doped Si-containing layer further comprises germanium.
26. The method of claim 25, wherein the doped Si-containing layer further comprises carbon.
27. A method for depositing a thin film, comprising:
introducing a gas comprising trisilane to a chamber, wherein the chamber contains a substrate having a substrate surface roughness; establishing trisilane chemical vapor deposition conditions in the chamber; depositing an amorphous Si-containing film onto the substrate, the amorphous Si-containing film having a thickness in the range of 10 Å to 150 Å and a film surface roughness that is greater than the substrate surface roughness by an amount of about 5 Å rms or less, over a surface area of about one square micron or greater; wherein the amorphous Si-containing film has a thickness non-uniformity of about 10% or less for a mean film thickness in the range of 100 Å to 150 Å, a thickness non-uniformity of about 15% or less for a mean film thickness in the range of 50 Å to 99 Å, and a thickness non-uniformity of about 20% or less for a mean film thickness of less than 50 Å. 28. A method for depositing a thin film, comprising:
introducing a gas comprising trisilane to a chamber, wherein the chamber contains a substrate having a substrate surface roughness; establishing trisilane chemical vapor deposition conditions in the chamber; depositing an amorphous Si-containing film onto the substrate, the amorphous Si-containing film having a thickness in the range of 10 Å to 150 Å and a film surface roughness that is greater than the substrate surface roughness by an amount of about 5 Å rms or less, over a surface area of about one square micron or greater; wherein the substrate comprises a step or trench. 29. The method of claim 28, further comprising annealing the amorphous Si-containing film to form hemispherical grained silicon.
30. A method for depositing a thin film, comprising:
introducing a gas comprising trisilane to a chamber, wherein the chamber contains a substrate having a substrate surface roughness; establishing trisilane chemical vapor deposition conditions in the chamber; depositing an amorphous Si-containing film onto the substrate, the amorphous Si-containing film having a thickness in the range of 10 Å to 150 Å and a film surface roughness that is greater than the substrate surface roughness by an amount of about 5 Å rms or less, over a surface area of about one square micron or greater; wherein the gas further comprises a dopant element selected from the group consisting of boron, arsenic, antimony, indium, and phosphorous. 31. The method of claim 30, wherein the amorphous Si-containing film is a diffusion layer.
32. The method of claim 30, wherein the depositing of the amorphous Si-containing film onto the substrate results in uniform incorporation of the dopant element throughout the amorphous Si-containing film.
33. A method for depositing a thin film, comprising:
introducing a gas comprising trisilane to a chamber, wherein the chamber contains a substrate having a substrate surface roughness; establishing trisilane chemical vapor deposition conditions in the chamber; and depositing a Si�N film onto the substrate, the Si�N film having a thickness in the range of 10 Å to 150 Å and a film surface roughness that is greater than the substrate surface roughness by an amount of about 5 Å rms or less, over a surface area of about one square micron or greater. 34. The method of claim 33, wherein the gas further comprises a nitrogen precursor.
35. The method of claim 34, wherein the nitrogen precursor is atomic nitrogen.
36. The method of claim 34, wherein the Si-containing film has a hydrogen content that is less than about 4 atomic %.
37. A method for depositing a thin film, comprising:
introducing trisilane to a chamber, wherein the chamber contains a substrate; depositing a continuous amorphous Si-containing film having a thickness of less than about 100 Å and a surface area of about one square micron or larger onto the substrate by thermal chemical vapor deposition; depositing an oxide layer over the amorphous Si-containing film; and annealing the amorphous Si-containing film to form a plurality of quantum dots. 38. A method for depositing a thin film, comprising:
introducing trisilane to a chamber, wherein the chamber contains a substrate; depositing a continuous amorphous Si-containing film having a thickness of less than about 100 Å and a surface area of about one square micron or larger onto the substrate by thermal chemical vapor deposition; and depositing a doped Si-containing layer directly onto the amorphous Si-containing film. 39. The method of claim 38, wherein the doped Si-containing layer further comprises germanium.
40. The method of claim 39, wherein the doped Si-containing layer further comprises carbon.
RELATED APPLICATION INFORMATION This application claims priority to U.S. Provisional Application No. 60/268,337, filed Feb. 12, 2001; U.S. Provisional Application No. 60/279,256, filed Mar. 27, 2001; U.S. Provisional Application No. 60/311,609, filed Aug. 9, 2001; U.S. Provisional Application No. 60/323,649, filed Sep. 19, 2001; U.S. Provisional Application No. 60/332,696, filed Nov. 13, 2001; U.S. Provisional Application No. 60/333,724, filed Nov. 28, 2001; and U.S. Provisional Application No. 60/340,454, filed Dec. 7, 2001; all of which are hereby incorporated by reference in their entireties. This application is related to, and incorporates by reference in their entireties, co-owned and co-pending U.S. patent application Ser. Nos.: 10/074,563; 10/074,149; 10/074,722; 10/074,633; and 10/074,534, all of which were filed on Feb. 11, 2002.
Tuning involves depositing a large number of films, each under a different pre-selected set of deposition conditions. The thickness variations within each film are then id measured and the results analyzed to identify conditions that reduce or eliminate the thickness variations. The inventor has realized, however, that tuning does not necessarily achieve uniform temperature distributions throughout the process; rather, the result of the tuning process is to time-average the thickness variations, produced by the temperature variations for a specific reaction temperature set point.
Incorporation of dopants into Si-containing films by CVD using trisilane is preferably accomplished by in situ doping using gas phase dopant precursors. Precursors for electrical dopants include diborane, deuterated diborane, phosphine, arsenic vapor, and arsine. Silylphosphines [(H3Si)3-xPRx] and silylarsines [(H3Si)3-xAsRx] where x=0-2 and Rx=H and/or D are preferred precursors for phosphorous and arsenic as dopants. SbH3 and trimethylindium are preferred sources of antimony and indium, respectively. Such dopant precursors are useful for the preparation of preferred semiconductor films as described below, preferably boron-, phosphorous-, antimony-, indium-, and arsenic-doped silicon, Si�C, Si�Ge and Si�Ge�C films and alloys.
For thermal CVD using trisilane, deposition is preferably conducted at a substrate temperature of about 400� C. or greater, more preferably about 450� C. or greater, even more preferably about 500� C. or greater. Preferably, deposition of amorphous films takes place at a temperature of about 750� C. or less, more preferably about 650� C. or less, most preferably about 600� C. or less. Such temperatures are preferably achieved by heating the substrate to the indicated temperature. As temperatures are increased beyond about 600� C., surface roughness tends to increase due to the transition to microcrystalline and polycrystalline structures and deposition rates tend to be higher. Epitaxial films may be obtained by deposition at sufficiently high temperatures onto properly prepared substrates. Those skilled in the art can adjust these temperature ranges to take into account the realities of actual manufacturing, e.g., preservation of thermal budget, tolerance for surface roughness in a particular application, tolerance for compositional variations, etc. For example, deposition temperatures in the range of about 450� C. to about 525� C. are preferred for the deposition of extremely thin (e.g., about 10 Å to about 50 Å) amorphous Si-containing films A onto an oxide substrate using trisilane. Preferred deposition temperatures thus depend on the desired application, but are typically in the range of about 400� C. to about 750� C., preferably about 425� C. to about 700� C., more preferably about 450� C. to about 650� C.
Preferred Si-containing films have a thickness that is highly uniform across the surface of the film. In general, measurements of uniformity described herein can be on a film obtained by blanket deposition over a bare or oxide-covered 200 mm or 300 mm wafer, and no measurements are taken within a 3 mm exclusion zone at the wafer periphery. Film thickness uniformity is determined by making multiple-point thickness measurements along a randomly selected diameter, determining the mean thickness by averaging the various thickness measurements, and determining the rms variability. A preferred instrument for measuring film thickness utilizes a Nanospec� 8300 XSE instrument (commercially available from Nanometrics, Inc., Sunnyvale, Calif.), and a preferred measurement method involves using such an instrument to measure the film thickness at 49 points along a randomly selected wafer diameter. In practice, thickness variability is typically obtained directly from the instrument following such a measurement, and thus need not be calculated manually. To enable comparisons, the results can be expressed as percent non-uniformity, calculated by dividing the nms thickness variability by the mean thickness and multiplying by 100 to express the result as a percentage. When measuring thickness uniformity of a film having a surface that is not accessible to such a measurement, e.g., a film onto which one or more additional layers have been applied, or a film contained within an integrated circuit, the film is cross sectioned and examined by electron microscopy. The film thickness is measured at the thinnest part of the cross sectioned film and at the thickest part, and the range in thickness measurements (e.g., �6 Å) between these two points is then divided by the sum of the two measurements. This non-uniformity is expressed as a percentage herein.
Because the film 710 is thin and uniform, the resultant quantum dots 770 have a more uniform size and/or spatial distribution than those made by a comparable silane-based optimized method. Preferred quantum dots have a grain size of about 200 Å or less, preferably about 100 Å or less, depending on the desired application. Size uniformity is preferably determined by measuring average quantum dot size and rms size variability. Preferably, rms size variability is about 15% or less, preferably 10% or less, based on the average quantum dot size. For example, for a structure having an average quantum dot size of 50 Å, the size variability is preferably 7.5 Å rms (15% of 50 Å) or less. Spatial uniformity is preferably determined by measuring the average number of quantum dots per given area and the rms spatial variability. Preferably, the rms spatial variability is about 5% or less. For example, for a structure having an average of 50 quantum dots per 0.1 μm2 the spatial variability is preferably 2.5 per 0.1 μm2 rms (5% of 50) or less. Quantum dots as described herein are useful in a number of applications, e.g., single electron transistors, quantum dot infrared photodetectors, and sparse carrier devices. See U.S. Pat. Nos. 6,194,237; 6,211,013; 6,235,618; 6,239,449; and 6,265,329, all of which are hereby incorporated by reference in their entireties, and particularly for the express purpose of describing quantum structures, fabrication methods, and applications.
The ability to deposit thin, smooth Si-containing films as described herein enables the preparation of HSG silicon over structures with smaller feature sizes than when using silane, permitting extension to smaller critical dimensions. Thus, a preferred embodiment provides a method comprising introducing trisilane to a chamber, depositing an amorphous Si-containing film, and annealing the film to from HSG silicon. The chamber preferably contains a substrate at a temperature of about 450� C. to 600� C., more preferably about 450� C. to about 520� C., and an amorphous Si-containing film is deposited onto the substrate by thermal CVD. Preferably, the amorphous Si-containing film has a thickness in the range of about 10 Å to about 150 Å, preferably about 50 Å to about 100 Å, and a surface roughness of about 5 Å rms or less, preferably about 2 Å rms or less. Preferred ranges of percent thickness non-uniformity for the amorphous Si-containing film are set forth in Table 1 above. The amorphous Si-containing film is then annealed to form HSG silicon, preferably by heating to a temperature in the range of about 600� C. to about 700� C. It has been found that Si-containing films, when annealed as described, form HSG silicon having a finer and more uniform grain structure.
A preferred replacement method involves modifying a CVD process to take advantage of the ability to deposit trisilane at a lower temperature, e.g., using the temperature parameters discussed above for the thermal CVD of trisilane. For example, where the semiconductor device manufacturing process comprises thermal CVD of silane at a temperature Ts, the replacement of silane with trisilane preferably further involves reducing the deposition temperature to Tt, where Ts>Tt. Such temperature reductions advantageously conserve thermal budgets, and are preferably about 10% or greater, more preferably about 20% or greater, calculated as (Ts−Tt)/Ts, and multiplying by 100 to express the result in percentage terms. Preferably, Tt* is in the range of about 450� C. to about 600� C., more preferably in the range of about 450� C. to about 525� C. Preferably, the process of introducing silane to the chamber is also modified when replacing the silane with trisilane to take into account the liquid nature of trisilane at room temperature as discussed above, e.g., by using a bubbler, heated gas lines, etc.
Example 1 An eight-inch diameter (200 mm) <100> silicon wafer substrate having a 1,000 Å SiO2 layer was placed into the reactor chamber and allowed to reach thermal equilibrium at 450� C. at 40 Torr pressure under a flow of 20 standard liters per minute (slm) of high purity hydrogen gas. Trisilane was introduced to the chamber by passing high purity hydrogen gas through liquid trisilane using a bubbler (maintained at room temperature using a water bath around the vessel containing the trisilane) connected by a feed line to the chamber. A flow rate of 180 standard cubic centimeters per minute (sccm) of the hydrogen/trisilane mixture, along with a flow of 90 seem (inject) of diborane (100 ppm, 90 sccm mixed with 2 slm high purity hydrogen), was then passed into the reactor for four minutes. A continuous, boron-doped, amorphous silicon film having a total thickness of 56 Å and a surface roughness of about 2 Å rms (comparable to the underlying silicon dioxide) was deposited on the silicon dioxide layer at a deposition rate of 14 Å per minute. A layer of epoxy was then applied to facilitate cross-sectional sample preparation.
Example 2 (Comparative) The process of Example 1 is repeated except that silane is used instead of trisilane. Since silane is a gas under the experimental conditions, it was introduced to the chamber directly in admixture with hydrogen, without the use of a bubbler. No meaningful deposition was observed after 30 minutes and no Si-containing film was obtained even with a silane flow of 190 sccm.
Example 7 (Comparative) An amorphous boron-doped silicon film was deposited as described in Example 4, except that trisilane was used instead of silane. Silane was supplied in the form of a gas at a flow rate of about 100 sccm. A bubbler was not used because silane is a gas under these conditions. The delivery rate of silane to the substrate was about 0.1 gram per minute, about the same as the delivery rate of trisilane in Examples 4-6. Deposition was carried out for three minutes to produce a film having a total thickness of 16 Å. The deposition rate was 5.3 Å per minute.
Example 8 (Comparative) An amorphous boron-doped silicon film was deposited as described in Example 7, except that deposition was carried out for five minutes to produce a film having a total thickness of 87 Å. The deposition rate was 17.4 Å per minute.
Example 9 (Comparative) An amorphous boron-doped silicon film was deposited as described in Example 7, except that deposition was carried out for ten minutes to produce a film having a total thickness of 284 Å. The deposition rate was 28.4 Å per minute.
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H01L21/28035, H01L21/28194, H01L21/0243, H01L21/0251, H01L29/51, H01L21/02595, H01L21/02576, H01L21/02667, H01L28/84, H01L21/02532, H01L21/02529, H01L21/2257, H01L21/0262, C23C16/24, H01L21/28556, Y02E10/546, H01L29/127, H01L29/66181, C23C16/308, H01L31/1804, H01L21/32055, H01L21/02579, H01L21/02598, H01L31/182, B82Y10/00, B82Y30/00, C23C16/0272European ClassificationB82Y10/00, C23C16/30, H01L29/12W4, H01L21/20C, C23C16/02H, C23C16/36, H01L21/225A4F, H01L31/20B, H01L31/18C, H01L21/205, H01L21/285B4B, C23C16/32B, H01L21/285B4H, C30B25/02, H01L29/51, C23C16/30E, C23C16/22, H01L21/3205N, H01L21/20B, H01L21/28E2C2D, H01L29/51M, H01L31/18C5, C30B29/06, H01L21/28E2B2, H01L21/02K4A1K, H01L21/02K4B1A3, H01L21/02K4B5L7, H01L21/02K4C1A2, H01L21/02K4A5S, B82Y30/00, H01L28/84, H01L29/66M6D6, H01L29/66M6T2H, H01L21/205B, H01L21/28E2B2P, C23C16/24, C23C16/56, C23C16/34C, H01L21/318B, H01L21/02K4C3C2, H01L21/02K4C3C1, H01L21/02K4C5M3, H01L21/02K4C1A3, H01L21/02K4E3C, H01L21/02K4C5M2, H01L21/02K4C5M1Legal EventsDateCodeEventDescriptionMar 7, 2013FPAYFee paymentYear of fee payment: 8May 20, 2009FPAYFee paymentYear of fee payment: 4May 20, 2009SULPSurcharge for late paymentMay 18, 2009REMIMaintenance fee reminder mailedJan 2, 2007CCCertificate of correctionJun 10, 2002ASAssignmentOwner name: ASM AMERICA, INC., ARIZONAFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:TODD, MICHAEL A.;RAAIJMAKERS, IVO;REEL/FRAME:012957/0419;SIGNING DATES FROM 20020422 TO 20020513RotateOriginal ImageGoogle Home - Sitemap - USPTO Bulk Downloads - Privacy Policy - Terms of Service - About Google Patents - Send FeedbackData provided by IFI CLAIMS Patent Services©2012 Google