WO1999002288A1 - Intermetallic aluminides and silicides sputtering targets, and methods of making same - Google Patents
Intermetallic aluminides and silicides sputtering targets, and methods of making same Download PDFInfo
- Publication number
- WO1999002288A1 WO1999002288A1 PCT/US1998/013719 US9813719W WO9902288A1 WO 1999002288 A1 WO1999002288 A1 WO 1999002288A1 US 9813719 W US9813719 W US 9813719W WO 9902288 A1 WO9902288 A1 WO 9902288A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- die
- pressure
- vacuum
- powders
- article
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/04—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbonitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Definitions
- Refractory metals and their suicides are widely used in CMOS DRAMs and logic circuits. Suicides offer lower resistivity compared to doped silicon. In addition, suicides also offer higher ⁇ thermal stability compared to conventional interconnect materials such as aluminum. There are several ways to obtain refractory metal silicide films on the wafer. The most common method to obtain metal silicide is through the salicide process. The salicide process for obtaining titanium silicide film on a wafer is described below:
- a layer of Ti is deposited on a wafer by sputtering; -, r 2.
- This step is done in a nitrogen atmosphere to avoid forming TiSi 2 on the oxide and forms a TiN layer on the titanium;
- the wafer is removed and selectively etched to the TiN and unreacted Ti; a. a second RTA step is performed whereby TiSi 2 is transformed from the high 2 resistivity phase (C49) to the low resistivity phase (C54).
- the process involves four steps including two high temperature rapid annealing steps.
- the advantage of RTA versus conventional annealing is that RTA reduces the "thermal budget", defined as the time the wafer stays in the furnace at high temperature. In general, reducing the thermal budget is desirable. 2 ⁇ r
- An alternative way to obtain a silicide film on a wafer would be by depositing a silicide film by sputtering a silicide target. Sputter deposition of silicide film using a silicide target offers the following advantages:
- Aluminides of Ti and Ta are useful barrier materials in the manufacture of integrated circuits.
- Ti and Al layers often react to form r titanium aluminide during wafer processing.
- formation of titanium aluminide during wafer processing is detrimental to the wafer because it introduces additional stresses in the film and also consumes Ti and Al from interconnect wiring.
- Depositing a titanium _• aluminide film eliminates the introduction of stresses associated with formation of titanium aluminide and unnecessary consumption of interconnect metal.
- the invention relates to a method of making enhanced purity stoichiometric and non- ⁇ stoichiometric articles, such as targets for sputtering and related microelectronics applications, and to such articles, including targets.
- Stoichiometric articles are defined as single phase microstructure having a chemical composition as predicted by the phase diagram of the constituent elements e.g. T1AI3, WSi2, TiSi 2 , etc.
- Non-stoichiometric articles are defined as articles, such as targets, having a composition slightly away from the stoichiometric composition ⁇ r as predicted by the phase diagram of the constituent elements e.g. TiSi 2 4, WSi2,8, etc.
- Enhanced purity articles such as targets, are defined as having an overall purity
- the articles may be manufactured by using a combination of reactive sintering, sintering and vacuum hot pressing. It has been found that such a combination can be performed in situ in a vacuum hot press which enables the process to be a one-step process to manufacture stoichiometric and non-stoichiometric, such as sputtering targets starting from elemental
- T powders i.e. elements in powder form.
- FIG. 1 is a photomicrograph of the grain structure of T1AI3 target produced in accordance with an embodiment of the invention (100X, grain size 18 microns); o FIG. 2 is a graph showing the x-ray diffraction pattern of a target produced in accordance with one embodiment of the invention;
- FIG. 3 is a graph of an analysis of titanium silicide
- FIG. 4 is a photomicrograph of the grain structure of TiSi 2 target produced in accordance with one embodiment of the invention (100X, grain size, 18 microns; cracks observed are an artifact of the sample mounting, grinding and polishing process).
- One aspect of the invention comprises a one-step method of making enhanced purity, high
- the invention includes a method of making an article particularly useful as a sputtering target having enhanced purity comprising metal (M) and either silicon (Si) or aluminum (Al), from powder.
- M comprises Ti, Fe, Co,
- M comprises Ti, Ta, Ni, Cr, Co and/or Pt.
- the preferred embodiment of the method may comprise the following steps, which may be combined or rearranged in order:
- the die is further cooled by a flowing inert gas;
- the inert gas used to cool the die is helium;
- ⁇ the stoichiometric product, for example a sputtering target comprises or consists essentially of one phase with the second phase not exceeding more than about 1%;
- the non-stoichiometric product, for example a sputtering target comprises or consists essentially of two phases with any and all additional phases not exceeding about 1%;
- the characteristics of the enhanced purity stoichiometric and non-stoichiometric ⁇ ⁇ - article, for example a sputtering target has a density of at least 95% of theoretical density, substantially no porosity, and impurities that have been reduced by at least 5%; the density is at least equal to the theoretical density; and the cooled compact has substantially the desired dimensions of the article, for example a sputtering target
- the process parameters are defined in ranges because it has been found that in order to achieve the desired chemical composition and phases in the sputtering target, temperatures, heating and cooling rates, vacuum, hold times and pressure should be controlled.
- the specific process parameters will depend on the starting materials and desired composition.
- a compaction step prior to reactive sintering assists in increasing the reaction rate.
- the degassing step removes moisture.
- the titanium and aluminum powders in this example react to produce T1AI3.
- Control of process parameters ensures that the reaction occurs uniformly throughout the powder mixture resulting in a fine-grained (due to several nucleating sites) single phase near-net shaped TiAl 3 blank.
- the exothermic nature of the reaction leads to a temperature increase which makes the reacted powder mixture plastic and thus easy to densify.
- the second degassing step removes the gases given out during the exothermic reactive process.
- the combination of two degassing steps at low and elevated temperatures prior to and after the reactive sintering step results in reduction of alkali and gaseous impurities and an enhanced purity article especially useful as a sputtering target.
- the advantage of the process is reflected by absence of elemental Ti and Al powders in the finished article. This is determined by analyzing the near-net shaped blank using x-ray diffraction, SEM/EDS, and Atomic Absorption.
- FIG. 1 shows the grain structure of a T1AI3 target processed using the process described above.
- the photomicrograph clearly sows that the grain size is less than 20 microns.
- FIG. 2 shows the x-ray diffraction pattern of a sample piece obtained from the target. The x-ray diffraction pattern shows the presence of a single phase TiAl compound.
- FIG. 3 which represents the analysis of titanium silicide target using x-ray diffraction revealed that the target contained two phases as expected.
- the two phases were TiSi 2 and Si. Further analysis indicated that the TiSi 2 is in the C54 phase, which is a low resistivity phase.
- the microstructural analysis showed a fine microstructure with an average grain size less than 20 microns (FIG. 4). GDMS, LECO and SIMS analysis showed that the overall purity of the target was higher than that of the staring powders.
- Tables 4, 5 and 6 describe typical compositions of titanium aluminide, titanium silicide and tungsten silicide, respectively, which may be produced. Furthermore, when these compositions are produced as sputtering targets, it has been confirmed that the targets will produce films of titanium aluminide, titanium silicide and tungsten silicide, respectively, on a substrate.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP98933058A EP1021265A4 (en) | 1997-07-11 | 1998-07-01 | Intermetallic aluminides and silicides sputtering targets, and methods of making same |
JP2000501855A JP2003535969A (en) | 1997-07-11 | 1998-07-01 | Intermetallic aluminide and silicide sputtering target and method of manufacturing the same |
KR1020007000281A KR20010021722A (en) | 1997-07-11 | 1998-07-01 | Intermetallic aluminides and silicides sputtering targets, and methods of making same |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US5226297P | 1997-07-11 | 1997-07-11 | |
US60/052,262 | 1997-07-11 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1999002288A1 true WO1999002288A1 (en) | 1999-01-21 |
Family
ID=21976446
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US1998/013719 WO1999002288A1 (en) | 1997-07-11 | 1998-07-01 | Intermetallic aluminides and silicides sputtering targets, and methods of making same |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP1021265A4 (en) |
TW (1) | TW398020B (en) |
WO (1) | WO1999002288A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2798395A1 (en) * | 1999-08-03 | 2001-03-16 | Praxair Technology Inc | METHOD FOR MANUFACTURING HIGH-DENSITY INTER-METAL SPRAYING TARGETS |
EP1350861A1 (en) * | 2002-03-29 | 2003-10-08 | Alloys for Technical Applications S.A. | Process for fabrication and regeneration of sputtering targets |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4663120A (en) * | 1985-04-15 | 1987-05-05 | Gte Products Corporation | Refractory metal silicide sputtering target |
US4762558A (en) * | 1987-05-15 | 1988-08-09 | Rensselaer Polytechnic Institute | Production of reactive sintered nickel aluminide material |
US4889745A (en) * | 1986-11-28 | 1989-12-26 | Japan As Represented By Director General Of Agency Of Industrial Science And Technology | Method for reactive preparation of a shaped body of inorganic compound of metal |
US5330701A (en) * | 1992-02-28 | 1994-07-19 | Xform, Inc. | Process for making finely divided intermetallic |
US5418071A (en) * | 1992-02-05 | 1995-05-23 | Kabushiki Kaisha Toshiba | Sputtering target and method of manufacturing the same |
US5508000A (en) * | 1990-05-15 | 1996-04-16 | Kabushiki Kaisha Toshiba | Sputtering target and method of manufacturing the same |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH01136969A (en) * | 1987-11-24 | 1989-05-30 | Mitsubishi Metal Corp | Manufacture of target for titanium silicide sputtering |
JPH01249619A (en) * | 1988-03-30 | 1989-10-04 | Toshiba Corp | Production of metal silicide target having high melting point |
JP2794382B2 (en) * | 1993-05-07 | 1998-09-03 | 株式会社ジャパンエナジー | Silicide target for sputtering and method for producing the same |
-
1998
- 1998-07-01 WO PCT/US1998/013719 patent/WO1999002288A1/en not_active Application Discontinuation
- 1998-07-01 EP EP98933058A patent/EP1021265A4/en not_active Withdrawn
- 1998-07-08 TW TW087111029A patent/TW398020B/en not_active IP Right Cessation
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4663120A (en) * | 1985-04-15 | 1987-05-05 | Gte Products Corporation | Refractory metal silicide sputtering target |
US4889745A (en) * | 1986-11-28 | 1989-12-26 | Japan As Represented By Director General Of Agency Of Industrial Science And Technology | Method for reactive preparation of a shaped body of inorganic compound of metal |
US4762558A (en) * | 1987-05-15 | 1988-08-09 | Rensselaer Polytechnic Institute | Production of reactive sintered nickel aluminide material |
US5508000A (en) * | 1990-05-15 | 1996-04-16 | Kabushiki Kaisha Toshiba | Sputtering target and method of manufacturing the same |
US5418071A (en) * | 1992-02-05 | 1995-05-23 | Kabushiki Kaisha Toshiba | Sputtering target and method of manufacturing the same |
US5330701A (en) * | 1992-02-28 | 1994-07-19 | Xform, Inc. | Process for making finely divided intermetallic |
US5608911A (en) * | 1992-02-28 | 1997-03-04 | Shaw; Karl G. | Process for producing finely divided intermetallic and ceramic powders and products thereof |
Non-Patent Citations (1)
Title |
---|
See also references of EP1021265A4 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2798395A1 (en) * | 1999-08-03 | 2001-03-16 | Praxair Technology Inc | METHOD FOR MANUFACTURING HIGH-DENSITY INTER-METAL SPRAYING TARGETS |
JP2001073128A (en) * | 1999-08-03 | 2001-03-21 | Praxair St Technol Inc | Production of high density sputtering target composed of two or more kinds of metals |
EP1350861A1 (en) * | 2002-03-29 | 2003-10-08 | Alloys for Technical Applications S.A. | Process for fabrication and regeneration of sputtering targets |
BE1014736A5 (en) * | 2002-03-29 | 2004-03-02 | Alloys For Technical Applic S | Manufacturing method and charging for target sputtering. |
Also Published As
Publication number | Publication date |
---|---|
TW398020B (en) | 2000-07-11 |
EP1021265A4 (en) | 2003-08-27 |
EP1021265A1 (en) | 2000-07-26 |
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