Source: http://www.google.com/patents/US6958253?dq=4316055
Timestamp: 2014-12-29 04:50:21
Document Index: 148848491

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 US6958253 - Process for deposition of semiconductor films - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inAdvanced Patent SearchPatentsChemical vapor deposition processes utilize higher order silanes and germanium precursors as chemical precursors. The processes have high deposition rates yet produce more uniform films, both compositionally and in thickness, than films prepared using conventional chemical precursors. In preferred embodiments,...http://www.google.com/patents/US6958253?utm_source=gb-gplus-sharePatent US6958253 - Process for deposition of semiconductor filmsAdvanced Patent SearchPublication numberUS6958253 B2Publication typeGrantApplication numberUS 10/074,534Publication dateOct 25, 2005Filing dateFeb 11, 2002Priority dateFeb 12, 2001Fee statusPaidAlso published asDE60223662D1, DE60223662T2, DE60227350D1, EP1374290A2, EP1374290B1, EP1374291A2, EP1374291B1, EP1421607A2, US6716713, US6716751, US6743738, US6821825, US6900115, US6962859, 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 number074534, 10074534, US 6958253 B2, US 6958253B2, US-B2-6958253, US6958253 B2, US6958253B2InventorsMichael A. ToddOriginal AssigneeAsm America, Inc.Export CitationBiBTeX, EndNote, RefManPatent Citations (68), Non-Patent Citations (9), Referenced by (28), Classifications (129), Legal Events (4) External Links: USPTO, USPTO Assignment, EspacenetProcess for deposition of semiconductor filmsUS 6958253 B2Abstract Chemical vapor deposition processes utilize higher order silanes and germanium precursors as chemical precursors. The processes have high deposition rates yet produce more uniform films, both compositionally and in thickness, than films prepared using conventional chemical precursors. In preferred embodiments, higher order silanes are employed to deposit SiGe-containing films that are useful in the semiconductor industry in various applications such as transistor gate electrodes.
providing a chemical vapor deposition chamber having disposed therein a substrate; introducing a gas comprised of a higher-order silane of the formula SinH2n+2 and a germanium precursor to the chamber, wherein n=3-6; and depositing a non-single crystalline SiGe-containing film onto the substrate. 2. The process as claimed in claim 1, wherein the higher-order silane is selected from the group consisting of trisilane and tetrasilane.
5. The process as claimed in claim 1, wherein the non-single crystalline SiGe-containing film is polycrystalline and the depositing is carried out at a temperature in the range of about 550� C. to about 700� C.
6. The process as claimed in claim 1, wherein the non-single crystalline SiGe-containing film is amorphous and the depositing is carried out at a temperature in the range of about 450� C. to about 600� C.
7. The process as claimed in claim 1, wherein the depositing is carried out at a rate of about 50 Å per minute or higher.
8. The process as claimed in claim 1, wherein the depositing is carried out at a rate of about 100 Å per minute or higher.
12. The process as claimed in claim 1, wherein the SiGe-containing film has greater uniformity than a comparable film using silane in place of the higher-order silane.
16. A process for making a graded SiGe-containing film, comprising:
providing a substrate disposed within a CVD chamber; and depositing a graded SiGe-containing film onto the substrate by thermal CVD using a deposition gas comprising trisilane and a germanium precursor. 17. The process of claim 16, wherein the amounts are varied to produce a germanium concentration that is a substantially linear function of the amount of germanium precursor.
18. The process of claim 16, wherein the germanium precursor is selected from the group consisting of germane and digermane.
19. The process of claim 18, wherein the graded SiGe-containing film is deposited at a deposition rate that is a substantially linear function of the amount of germanium precursor.
20. The process of claim 18, wherein the deposition gas further comprises an amount of silane.
21. The process of claim 20, wherein the amount of silane is varied during deposition.
22. The process of claim 20, wherein a weight ratio of trisilane to silane in the deposition gas is about 1:1 or greater.
23. The process of claim 20, wherein the weight ratio of trisilane to silane in the deposition gas is about 4:1 or greater.
24. The process of claim 16, wherein the SiGe-containing film is epitaxial.
25. The process of claim 16, wherein the SiGe-containing film comprises carbon.
26. The process of claim 16, wherein the SiGe-containing film is polycrystalline.
27. The process of claim 16, wherein the SiGe-containing film is amorphous.
28. The process of claim 26, wherein the SiGe-containing film is formed directly over a dielectric.
29. The process of claim 28, wherein the dielectric comprises silicon oxide.
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 10/074,564, all of which were filed on Feb. 11, 2002.
It has been found that this problem may be addressed by adjusting the amount of trisilane supplied to the substrate surface, e.g., by increasing the flow rate of the feed gas, so that the rate at which trisilane is supplied to the surface is equal to or greater than the rate at which the trisilane is consumed by the deposition process. In practice, the flow rate of the feed gas is preferably selected in conjunction with the deposition temperature to provide the film with a greater degree of uniformity than a comparable film made using silane in place of trisilane, as illustrated in working Examples 16-19 below. Increasing the flow rate of trisilane is also advantageous because it allows for higher deposition rates. However, even when the trisilane flow rate is less than silane, all other conditions being equal, the deposition rate can be higher because of tile greater deposition efficiency of trisilane, as illustrated in working Examples 5-15 below. Preferred flow rates thus may be adjusted to provide the desired degree of uniformity and the desired deposition rate, taking into account the deposition temperature and the partial pressure of trisilane in the feed gas, as well as practical considerations such as reactor size and configuration.
Dopant precursors include diborane, deuterated diborane, phosphine, and arsine. Silylphosphines [(H3Si)3-xPRx] and silylarsines [(H3Si)3-xAsRx] where x=0-2 an Rx=H and/or D are preferred dopant sources of phosphorous and arsenic. SbH3 and trimethylindium are preferred sources of antimony and indium, respectively. Such dopants and dopant sources are useful for the preparation of preferred films such as boron-, phosphorous-, antimony-, indium-, and arsenic-doped silicon, SiGe and SiGeC films, by the methods described herein. The dopant concentration in these materials, when doped, is preferably in the range of from about 1�1014 to about 1�1022 atoms/cm3. Dopants can be incorporated using very low concentrations of the dopant sources, e.g., as mixtures in hydrogen with concentration ranging from about 1 ppm to about 1%, by weight based on total. These diluted mixtures can then be delivered to the reactor via a mass flow controller with set points ranging from 10 to 200 standard cubic centimeters per minute (sccm), depending on desired dopant concentration and dopant gas concentration. The dopant source is also preferably further diluted in the carrier gas delivered to the reactor with the silicon/germanium/carbon sources. Since flow rates often range from about 20 standard liters per minute (slm) to about 180 slm, the concentration of the dopant used in a typical process is usually very small.
The use of a deposition gas that contains trisilane greatly simplifies the task of depositing a graded Si-containing film using thermal CVD. For example, the effect of changing the amount of Ge precursor during CVD, deposition using a trisilane-containing deposition gas is shown in FIGS. 9-10. The data shown in FIGS. 9-10 were obtained under the conditions described in the Examples below. In contrast to the non-linearities apparent in FIGS. 5-8, FIG. 9 shows that the Ge incorporation into the film is a substantially linear function of the germane flow rate. FIG. 9 also illustrates preferred linearity in the deposition rate as a function of the germane flow rate. The data is taken over a large range of Ge concentrations and Ge deposition rates of interest in IC fabrication contexts. It is preferred that both Ge incorporation and deposition rate be substantially linear functions of flow rate in order to facilitate the process of depositing graded Si�Ge films. Those skilled in the art will appreciate that data such as that shown in FIGS. 9 and 10 can be used to determine preferred conditions for the deposition of graded films, preferably graded Si�Ge films. FIG. 10 also illustrates preferred linearity of Ge incorporation and deposition rate for trisilane/germane under higher H2 flow rate conditions and a different germane concentration than illustrated in FIG. 9, demonstrating that the advantages of using trisilane are not limited to the specific conditions used to obtain the data in FIG. 9.
It has been found that a temperature set point, or a set of reactor conditions affecting temperature control more generally, that results in a film that is relatively uniform in composition and thickness for the first 5 Å to 1,000 Å of film deposition can be found empirically, but the film then typically becomes less uniform as deposition continues. The reasons for this are not well understood, and this invention is not limited by theory, but emissivity and other properties of the substrate, and SiC-coated graphite reactor components, that change as a function of deposition lime, can affect the temperature control system. This, in turn, can produce temperature variations that result in compositional and thickness variations.
Having determined the desired set points T1, T2, T3, T4, etc., the preferred embodiment may be practiced using a CVD chamber that is equipped with a temperature controller configured to allow programming with multiple temperature set points for a single recipe. The process is preferably conducted by entering a temperature set point T1 into a temperature controller and introducing a first gas comprised of X1 % of a first Si-containing chemical precursor to the CVD chamber. A first Si-containing layer is then deposited onto a substrate contained within the chamber. The process is preferably continued by entering a temperature set point T2 into the temperature controller, introducing a second gas comprised of X2 % of a second Si-containing chemical precursor to the CVD chamber, and depositing a second Si-containing layer onto the first Si-containing layer, thereby forming a multi-layer Si-containing film. The second Si-containing chemical precursor may be chemically identical to the first Si-containing chemical precursor or may be different, as discussed below and illustrated by FIG. 3 and Example 39.
The process can be continued further by, e.g., entering a temperature set point T3 into the temperature controller, introducing a third gas comprised of X3 % of a third Si-containing chemical precursor to the CVD chamber, and depositing a third Si-containing layer onto the second Si-containing layer, and so on, producing as many layers as desired.
Preferred Si-containing chemical precursors include higher order silanes as described elsewhere herein, as well as conventional chemical precursors such as silane. Preferably at least one of the first Si-containing chemical precursor and the second Si-containing chemical precursor is selected from the group consisting of silane, disilane and trisilane. At least one of the first gas, second gas and third gas includes an additional germanium and/or other dopant source, preferably a compound selected from the group consisting of germane, digermane, trigermane, NF3, monosilylmethane, disilylmethane, trisilylmethane, tetrasilylmethane, and an electrical dopant precursor, as described elsewhere herein. Preferably, the amount of each Si-containing chemical precursor Xn, for X1 %, X2 %, X3 %, X4 %, etc., in the gas is independently in the range of about 1�10−6% to about 100%, preferably about 1�10−4% to about 100%, by volume based on total volume, at any particular stage of the deposition process.
The processes of the preferred embodiments may be practiced by depositing the multiple layers of the film in a stepwise or continuous fashion. Advantageously, when the deposition is paused to adjust the temperature set point, process variables such as flow rate, partial pressure and gas composition can also be adjusted as desired to produce films having varied compositions. For instance, the deposited film may have a homogenous or uniform composition as discussed above, or may vary in composition step-wise or continuously. The identity of the Si-containing chemical precursor can be altered during the pause, and/or the amount in the gas X1 %, X2 %, X3 %, X4 %, etc. can be varied. In a preferred embodiment, the process involves the growth of a graded germanium concentration layer by non-continuous or step-wise changes in germanium concentration, preferably achieved by preparing a superlattice with discontinuous periodicity by depositing layers of selected germanium concentration on top of each other. Example 39 below and FIG. 3 illustrate this embodiment.
Preferred values of compositional non-uniformity vary, depending on the amount of the element in the Si-containing film. If the amount of element is 1 atomic % or greater, the compositional non-uniformity for the Si-containing film is preferably about 22% or less, more preferably about 17% or less, even more preferably about 12% or less, and most preferably about 70% or less. Ge content in SiGe films, for example, will typically represent greater than about 1 atomic % of such films, such that the above preferences apply to SiGe films. If the amount of element is in the range of 0.001 atomic percent up to 1 atomic %, the compositional non-uniformity for the Si-containing film is preferably about 90% or less, more preferably about 65% or less, even more preferably about 40% or less, and most preferably about 22% or less. If the amount of element is below 0.001 atomic percent, the compositional non-uniformity for the Si-containing film is preferably about 375% or less, more preferably about 275% or less, even more preferably about 175% or less, and most preferably about 75% or less. Ge content in graded SiGe films, for example, may vary over a broad range, and thus more than one of the above ranges may apply depending on the profile.
C: Comparative Examples 16-19 Si-containing films were deposited using trisilane and silane as chemical precursors, according to the parameters shown in Table 3. Deposition times were adjusted so that the films each had an average thickness of about 500 Å. Deposition rates were determined by measuring average film thickness using a Nanometrics ellipsometer and then dividing this number by the deposition time. Film thickness non-uniformity was determined from a 49-point thickness map of the film thickness. The results show that a much more uniform film was obtained at a much higher deposition rate by using trisilane at the indicated temperature in place of silane. This is true at 550� C., but dramatically more so at 600� C.
Atomic % Ge in Film
Examples 77-80 A series of films was deposited under the conditions described above for Examples 40-48 under the flow rate conditions shown in Table 8 below, except that trisilane was used in place of si lane, the pressure was 40 torr, and the germane concentration in the H2 was 10%. Trisilane was supplied to the reactor via a H2 bubbler at a flow rate set point of 25 sccm. The Ge concentrations in the resulting films and the deposition rates were determined as described above for Examples 40-48. The Ge concentration and deposition rate data are shown in Table 8 below and plotted in FIG. 9.
EXAMPLE 87 A Si-containing film having a mean thickness of 1,038 Å was deposited onto a SiO2 substrate (without a nucleation layer) using trisilane and germane as chemical precursors at a deposition temperature of 650� C. and a pressure of 40 torr. The set points for gas flow injectors had been empirically tuned in the usual manner in a series of previous runs. The resulting SiGe film had a thickness non uniformity of 0.37% (range of 8 Å) as measured by a 49 point linear diameter scan with 6 mm edge exclusion. FIG. 11 is a plot of film thickness as a function of measurement site for this film.
Examples 90-110 A series of Si-containing films were deposited onto a SiO2 substrate (without a nucleation layer) at a pressure of 40 torr using trisilane and germane. The trisilane flow rate was constant at 77 sccm (hydrogen carrier, bubbler) for the examples of Table 10. Germane flow (10% germane, 90% H2) and deposition temperature were varied as shown in Table 10. Germanium concentration (atomic %) and thickness of the resulting SiGe films were determined by RBS, and surface roughness was determined by atomic force microscopy (AFM). The results shown in Table 10 demonstrate that highly uniform films can be prepared over a range of temperatures and flow rate conditions, particularly over a large range of germane concentration. High deposition rates are achieved at relatively low temperatures without sacrificing uniformity.
*Thickness measured by optical technique nd: not determined It will be appreciated by those skilled in the art that various omissions, additions and modifications may be made to the processes described above without departing from the scope of the invention, and all such modifications and changes are intended to fall within the scope of the invention, as defined by the appended claims.
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LlcIntegrated circuit wafer system with control strategyUS8110503Apr 26, 2011Feb 7, 2012The Board Of Trustees Of The University Of IllinoisSurface preparation for thin film growth by enhanced nucleationUS8282735Nov 26, 2008Oct 9, 2012Asm Genitech Korea Ltd.Atomic layer deposition apparatusUS8329252Jul 31, 2011Dec 11, 2012Widetronix, Inc.Method for the growth of SiC, by chemical vapor deposition, using precursors in modified cold-wall reactorUS8367548Feb 21, 2008Feb 5, 2013Asm America, Inc.Stable silicide films and methods for making the sameUS8530340Sep 9, 2009Sep 10, 2013Asm America, Inc.Epitaxial semiconductor deposition methods and structuresUS8545940Aug 30, 2012Oct 1, 2013Asm Genitech Korea Ltd.Atomic layer deposition apparatus* Cited by examinerClassifications U.S. Classification438/47, 427/124, 257/E21.101, 427/255.21, 257/E21.166, 438/318, 427/255.7, 438/933, 438/320, 257/19, 438/235, 257/E21.119, 438/312, 257/E21.17, 257/E21.102, 257/E21.131International ClassificationH01L21/337, H01L21/469, H01L29/51, H01L21/425, H01L21/285, C23C16/42, H01L21/331, H01L21/205, H01L21/28, C30B25/02, H01L21/316, H01L27/092, H01L21/8238, H01L31/20, C23C16/24, C23C16/02, H01L29/78, H01L29/737, H01L21/20, H01L31/18Cooperative ClassificationY10S438/933, Y02E10/547, H01L21/0243, H01L21/02532, H01L21/02529, H01L21/32055, C23C16/308, H01L21/02592, H01L21/0262, H01L29/127, H01L31/202, H01L28/84, H01L21/28525, H01L21/02598, H01L21/02579, H01L21/02422, H01L21/3185, H01L29/517, C30B25/02, H01L21/28194, C23C16/325, H01L21/0245, C23C16/24, H01L29/66181, H01L21/0251, C23C16/36, H01L29/51, H01L31/1804, H01L29/66242, C23C16/56, H01L21/28035, H01L21/02667, C23C16/22, C23C16/30, H01L31/182, Y02E10/546, H01L21/2257, C30B29/06, H01L21/02595, H01L21/02576, H01L21/28556, C23C16/345, H01L29/518, H01L21/28044, B82Y30/00, B82Y10/00, C23C16/0272European ClassificationB82Y30/00, B82Y10/00, H01L21/02K4C1A3, H01L21/02K4A5S, C30B25/02, H01L21/02K4A1K, H01L21/02K4C3C2, H01L21/02K4B1A3, H01L21/02K4E3C, H01L21/02K4C3C1, C30B29/06, H01L21/02K4C5M1, C23C16/32B, H01L21/28E2C2D, H01L29/51M, H01L29/66M6T2H, H01L21/28E2B2, H01L28/84, H01L21/28E2B2P, C23C16/30, C23C16/36, C23C16/24, H01L21/318B, H01L21/02K4B5L7, H01L21/02K4C5M2, H01L21/02K4C1A2, H01L21/02K4C5M3, C23C16/34C, H01L21/3205N, C23C16/56, C23C16/22, H01L29/66M6D6, H01L29/51, C23C16/30E, H01L29/12W4, H01L21/225A4F, H01L31/18C5, H01L31/18C, H01L31/20B, H01L21/20C, H01L21/20B, H01L21/205B, H01L21/285B4B, H01L21/285B4H, C23C16/02H, H01L21/205Legal EventsDateCodeEventDescriptionMar 6, 2013FPAYFee paymentYear of fee payment: 8Apr 8, 2009FPAYFee paymentYear of fee payment: 4Jul 4, 2006CCCertificate of correctionMay 23, 2002ASAssignmentOwner name: ASM AMERICA, INC., ARIZONAFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:TODD, MICHAEL A.;REEL/FRAME:012910/0463Effective date: 20020422RotateOriginal ImageGoogle Home - Sitemap - USPTO Bulk Downloads - Privacy Policy - Terms of Service - About Google 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