CN113275589B - Preparation method and system of high-purity titanium powder and tungsten-titanium alloy sputtering target material - Google Patents
Preparation method and system of high-purity titanium powder and tungsten-titanium alloy sputtering target material Download PDFInfo
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- CN113275589B CN113275589B CN202110553332.2A CN202110553332A CN113275589B CN 113275589 B CN113275589 B CN 113275589B CN 202110553332 A CN202110553332 A CN 202110553332A CN 113275589 B CN113275589 B CN 113275589B
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- MAKDTFFYCIMFQP-UHFFFAOYSA-N titanium tungsten Chemical compound [Ti].[W] MAKDTFFYCIMFQP-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000005477 sputtering target Methods 0.000 title claims abstract description 38
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 24
- 239000013077 target material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000001301 oxygen Substances 0.000 claims abstract description 23
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000010936 titanium Substances 0.000 claims abstract description 17
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 150000004820 halides Chemical class 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 23
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 claims description 20
- NXHILIPIEUBEPD-UHFFFAOYSA-H tungsten hexafluoride Chemical compound F[W](F)(F)(F)(F)F NXHILIPIEUBEPD-UHFFFAOYSA-H 0.000 claims description 19
- 229910052786 argon Inorganic materials 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 10
- -1 titanium halide Chemical class 0.000 claims description 9
- 239000010937 tungsten Substances 0.000 claims description 9
- 229910052721 tungsten Inorganic materials 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 3
- 238000007740 vapor deposition Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- B22F1/0003—
-
- 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
-
- 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
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
- C23C16/08—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metal halides
- C23C16/14—Deposition of only one other metal element
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/20—Refractory metals
- B22F2301/205—Titanium, zirconium or hafnium
Abstract
The invention belongs to the technical field of sputtering targets, and particularly relates to a preparation method and a system of a high-purity titanium powder and tungsten-titanium alloy sputtering target. The preparation method of the high-purity titanium powder adopts a vapor deposition method to decompose the halide of titanium by heating so as to prepare the high-purity titanium powder. The high-purity titanium powder is prepared by adopting a vapor deposition method, and is directly used for preparing the tungsten titanium sputtering target, so that the purity of the tungsten titanium sputtering target is improved, and the increase of the oxygen content caused by the reaction of the titanium powder and oxygen is avoided; the purity of the tungsten-titanium sputtering target material prepared by the method is not lower than 99.999%, the oxygen content is not higher than 300ppm, the purity and the oxygen content are far higher than those of products in the current market, and the requirements of the electronic industry are completely met.
Description
Technical Field
The invention belongs to the technical field of sputtering targets, and particularly relates to a preparation method and a system of a high-purity titanium powder and tungsten-titanium alloy sputtering target.
Background
The sputtering target material is mainly applied to the electronic and information industries, such as integrated circuits, information storage, liquid crystal display screens, laser memories, electronic control devices and the like; can also be applied to the field of glass coating; can also be applied to industries such as wear-resistant materials, high-temperature corrosion resistance, high-grade decorative articles and the like.
The tungsten-titanium target is a typical alloy target, and a large-scale semiconductor integrated circuit, a solar cell and the like can be coated by using the tungsten-titanium target to form a barrier layer.
At present, tungsten-titanium targets are produced by a powder metallurgy process, and a preparation method of mixing tungsten powder and titanium powder and then forming is adopted, but the hardness value of the obtained tungsten-titanium targets is higher, and cracks are easy to occur.
Disclosure of Invention
The invention provides a preparation method and a system of a high-purity titanium powder and tungsten-titanium alloy sputtering target material.
In order to solve the technical problems, the invention provides a preparation method of high-purity titanium powder, which adopts a vapor deposition method to heat and decompose titanium halide so as to prepare the high-purity titanium powder.
In a second aspect, the present invention also provides a high purity titanium powder prepared by the preparation method as described above, wherein the purity of the high purity titanium powder is not less than 99.99%.
In a third aspect, the present invention also provides a method for preparing a tungsten-titanium alloy sputtering target, comprising the following steps: step S1, after purging the whole pipeline by argon, closing each pipeline to remove residual air in each pipeline; step S2, respectively introducing hydrogen and tungsten hexafluoride into the reactor so that the hydrogen reduces the tungsten hexafluoride into high-purity metal tungsten and deposits the high-purity metal tungsten on the matrix material; and S3, introducing argon into a titanium halide raw material tank, heating the titanium halide raw material tank to decompose titanium tetraiodide, introducing the titanium tetraiodide into a reactor, and depositing the titanium tetraiodide on a base material to prepare the tungsten-titanium alloy sputtering target.
In a fourth aspect, the invention also provides a tungsten-titanium alloy sputtering target material prepared by the preparation method, wherein the purity of the tungsten-titanium alloy sputtering target material is not lower than 99.999 percent, and the oxygen content is lower than 300ppm.
In a fifth aspect, the present invention also provides a system for preparing a tungsten titanium alloy sputtering target, comprising: a reactor, each raw material tank connected with the reactor; wherein, each raw material tank is provided with a control valve on a pipeline connected with the reactor.
The method has the beneficial effects that the high-purity titanium powder is prepared by adopting a vapor deposition method, and is directly used for preparing the tungsten titanium sputtering target, so that the purity of the tungsten titanium sputtering target is improved, and the increase of the oxygen content caused by the reaction of the titanium powder and oxygen is avoided; the purity of the tungsten-titanium sputtering target material prepared by the method is not lower than 99.999%, the oxygen content is not higher than 300ppm, the purity and the oxygen content are far higher than those of products in the current market, and the requirements of the electronic industry are completely met.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
In order to make the above objects, features and advantages of the present invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of a system for preparing a tungsten titanium alloy sputter target according to the present invention.
In the figure:
1-a first control valve; 2-a second control valve; 3-a third control valve; 4-a fourth control valve; 5-a fifth control valve; 6-a sixth control valve; 7-a hydrogen tank; 8-a first feedstock tank; 9-argon tank; 10-a second raw material tank; 11-a reactor; 12-tail gas treatment device.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The existing methods for preparing tungsten-titanium targets are all powder methods, have various steps, and need to use high-purity titanium powder and tungsten powder as raw materials; titanium powder is a hazardous chemical because of the fact that the titanium powder is easy to react with oxygen, the oxygen content is generally high, and the sputtering target has very strict requirements on the oxygen content, and generally, the lower the oxygen content is, the better the oxygen content is; after qualified raw materials are obtained, the target material blank can be prepared generally by mixing, stirring, cold pressing, sintering, hot pressing and other links, and the parameters such as pressure, temperature, vacuum degree and the like are very strictly controlled in the whole process.
In order to solve the technical problems, the invention provides a preparation method of high-purity titanium powder, which is characterized in that a vapor deposition method is adopted to heat and decompose titanium halide to prepare the high-purity titanium powder.
Wherein, optionally, the halide of titanium comprises: tiCl 4 、TiI 4 、TiBr 4 And TiF 4 The method comprises the steps of carrying out a first treatment on the surface of the TiI is preferred because titanium-iodine bonds are more prone to cleavage than other titanium-halogen bonds (e.g., titanium-chlorine bonds) 4 。
Optionally, the heating temperature for the thermal decomposition of the halide of titanium is 1000-1500 ℃.
Specifically, the titanium tetraiodide is decomposed at high temperature to generate Ti and I 2 The deposition thickness of the target material is generally millimeter-scale and different from the nanometer-scale thickness of the deposited film, so that the high-purity titanium powder can be prepared by adopting a pyrolysis mode; in another aspect, the high temperature deposited film also causes a change in film properties, and the substrate material of the deposited target is typically a refractory material, so that the high purity titanium powder can be deposited on the substrate after being prepared by pyrolysis.
Further, the invention also provides the high-purity titanium powder prepared by the preparation method, and the purity of the high-purity titanium powder is not lower than 99.99%.
Further, the invention also provides a preparation method of the tungsten-titanium alloy sputtering target material, which comprises the following steps: step S1, after purging the whole pipeline by argon, closing each pipeline to remove residual air in each pipeline; step S2, respectively introducing hydrogen and tungsten hexafluoride into the reactor so that the hydrogen reduces the tungsten hexafluoride into high-purity metal tungsten and deposits the high-purity metal tungsten on the matrix material; and S3, introducing argon into a titanium halide raw material tank, heating the titanium halide raw material tank to decompose titanium tetraiodide, introducing the titanium tetraiodide into a reactor, and depositing the titanium tetraiodide on a base material to prepare the tungsten-titanium alloy sputtering target.
Wherein optionally, the matrix material may be, but is not limited to, copper or copper alloy, titanium or titanium alloy.
Optionally, the molar ratio of the hydrogen to the tungsten hexafluoride is 3:1.
optionally, in the step S2, tungsten hexafluoride is heated to 120-180 ℃, and the temperature of the matrix material is 550-650 ℃.
Optionally, in the step S3, the heating temperature for heating the halide of titanium is 200-350 ℃; the temperature of the matrix material is 900-1500 ℃.
Optionally, the ratio of tungsten to titanium in the tungsten-titanium sputtering target is controlled by adjusting the time of steps S2 and S3.
Furthermore, the invention also provides a tungsten-titanium alloy sputtering target material prepared by the preparation method, wherein the purity of the tungsten-titanium alloy sputtering target material is not lower than 99.999 percent, and the oxygen content is lower than 300ppm.
Further, as shown in fig. 1, the present invention further provides a system for preparing a tungsten-titanium alloy sputtering target, which comprises: a reactor 11, and each raw material tank connected to the reactor 11; wherein, each raw material tank is provided with a control valve on a pipeline connected with the reactor.
Specifically, tungsten hexafluoride and titanium tetraiodide are respectively added into the first raw material tank 8 and the second raw material tank 10; and connecting each raw material tank with the reactor 11 through a connecting pipe to form a closed system; the tightness of the whole system is checked, and if a leakage point is found, the system must be repaired.
The third control valve 3 and the fifth control valve 5 are opened, the first control valve 1, the second control valve 2, the fourth control valve 4 and the sixth control valve 6 are closed to switch on the argon tank 9, the lines of the whole system are purged with argon to remove the residual air in each line, and then all the control valves are closed.
Opening the first control valve 1, the second control valve 2 and the third control valve 3, while closing the other control valves; the heaters of the first raw material tank 8 and the reactor 11 are turned on to heat the tungsten hexafluoride and the base material; hydrogen gas and tungsten hexafluoride are introduced into the reactor 11 to reduce the tungsten hexafluoride to high purity metallic tungsten and deposit on the base material.
Turning on the heaters of the second raw material tank 10 and the reactor 11 to heat the titanium tetraiodide and the base material; closing the first control valve 1, the second control valve 2, the third control valve 3 and the fifth control valve 5, and opening the fourth control valve 4 and the sixth control valve 6; argon is introduced into titanium tetraiodide, so that the titanium tetraiodide is heated and decomposed, then introduced into a reactor 11 and deposited on a base material, and the tungsten-titanium alloy sputtering target is prepared.
Wherein, optionally, the reactor 11 is made of stainless steel, and each connecting pipeline is made of stainless steel.
Optionally, an exhaust gas treatment device 12 is further arranged downstream of the reactor 11.
Optionally, each connecting pipeline is also provided with a flowmeter respectively.
Example 1
Respectively adding tungsten hexafluoride and titanium tetraiodide into the first raw material tank 8 and the second raw material tank 10; and connecting each raw material tank with the reactor 11 through a connecting pipe to form a closed system; the tightness of the whole system is checked, and if a leakage point is found, the system must be repaired.
The third control valve 3 and the fifth control valve 5 are opened, the first control valve 1, the second control valve 2, the fourth control valve 4 and the sixth control valve 6 are closed to switch on the argon tank 9, the lines of the whole system are purged with argon to remove the residual air in each line, and then all the control valves are closed.
Opening the first control valve 1, the second control valve 2 and the third control valve 3, while closing the other control valves; turning on a heater of the first raw material tank 8 and controlling the temperature to 150 ℃; turning on a heater of the reactor 11 to control a first heating temperature of the base material to 550 ℃; passing hydrogen and tungsten hexafluoride into the reactor 11 to reduce the tungsten hexafluoride to high purity metallic tungsten and deposit on the base material; the molar ratio of the hydrogen to the tungsten hexafluoride is controlled to be 3:1, a step of; the introduction time of hydrogen and tungsten hexafluoride was controlled to be 80s.
Turning on a heater of the second raw material tank 10 to control the heating temperature of the titanium tetraiodide to 250 ℃; turning on a heater of the reactor 11 to control the second heating temperature of the base material to 1000 ℃; closing the first control valve 1, the second control valve 2, the third control valve 3 and the fifth control valve 5, and opening the fourth control valve 4 and the sixth control valve 6; argon is introduced into titanium tetraiodide, so that the titanium tetraiodide is heated and decomposed, then introduced into a reactor 11 and deposited on a matrix material, and a tungsten-titanium alloy sputtering target is prepared; wherein, the introducing time of argon and titanium tetraiodide is controlled to be 20s. The valve time control is switched by a computer according to a set program.
The remaining examples were prepared according to the procedure of example 1 and the process conditions are summarized in table 1.
Table 1 process conditions for each example
Performance tests were performed on the tungsten titanium sputtering targets prepared in the above examples, and the test results are summarized in table 2.
TABLE 2 Performance data for tungsten-titanium sputter targets
| Purity/% | Relative density/% | Oxygen content/ppm | |
| Example 1 | 99.9996％ | 99.5％ | 180 |
| Example 2 | 99.9995％ | 99.3％ | 190 |
| Example 3 | 99.9996％ | 99.1％ | 195 |
| Example 4 | 99.9993％ | 99.1％ | 190 |
| Example 5 | 99.9992％ | 98.9％ | 210 |
As can be seen from the data in Table 2, the purity of the tungsten titanium sputtering target material prepared in each example was higher than 99.999% and the oxygen content was not more than 300ppm.
In summary, the high-purity titanium powder is prepared by adopting a vapor deposition method, and is directly used for preparing the tungsten titanium sputtering target, so that the purity of the tungsten titanium sputtering target is improved, and the increase of oxygen content caused by the reaction of the titanium powder and oxygen is avoided; the purity of the tungsten-titanium sputtering target material prepared by the method is not lower than 99.999%, the oxygen content is not higher than 300ppm, the purity and the oxygen content are far higher than those of products in the current market, and the requirements of the electronic industry are completely met.
With the above-described preferred embodiments according to the present invention as an illustration, the above-described descriptions can be used by persons skilled in the relevant art to make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the description, but must be determined according to the scope of claims.
Claims (3)
1. The preparation method of the tungsten-titanium alloy sputtering target material is characterized by comprising the following steps of:
step S1, after purging the whole pipeline by argon, closing each pipeline to remove residual air in each pipeline;
step S2, respectively introducing hydrogen and tungsten hexafluoride into the reactor so that the hydrogen reduces the tungsten hexafluoride into high-purity metal tungsten and deposits the high-purity metal tungsten on the matrix material;
step S3, introducing argon into a titanium halide raw material tank, and heating the titanium halide raw material tank to decompose titanium tetraiodide, introducing the decomposed titanium tetraiodide into a reactor, and depositing the decomposed titanium tetraiodide on a matrix material to prepare a tungsten-titanium alloy sputtering target material;
the halide of titanium is titanium tetraiodide;
in the step S2, heating tungsten hexafluoride to 120-180 ℃, wherein the temperature of the matrix material is 550-650 ℃;
in the step S3, the heating temperature for heating the titanium halide is 200-350 ℃; the temperature of the matrix material is 900-1500 ℃;
the purity of the tungsten-titanium alloy sputtering target material is not lower than 99.999 percent, and the oxygen content is lower than 300ppm.
2. The method of claim 1, wherein,
the molar ratio of the hydrogen to the tungsten hexafluoride is 3:1.
3. a tungsten-titanium alloy sputtering target material prepared by the preparation method according to claim 1, which is characterized in that,
the purity of the tungsten-titanium alloy sputtering target material is not lower than 99.999 percent, and the oxygen content is lower than 300ppm.
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Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5160534A (en) * | 1990-06-15 | 1992-11-03 | Hitachi Metals Ltd. | Titanium-tungsten target material for sputtering and manufacturing method therefor |
| US5397050A (en) * | 1993-10-27 | 1995-03-14 | Tosoh Smd, Inc. | Method of bonding tungsten titanium sputter targets to titanium plates and target assemblies produced thereby |
| JPH08165566A (en) * | 1994-03-31 | 1996-06-25 | Sumitomo Sitix Corp | High purity titanium material and its production |
| US5700519A (en) * | 1995-01-06 | 1997-12-23 | Sony Corporation | Method for producing ultra high purity titanium films |
| JP2002105632A (en) * | 2000-09-29 | 2002-04-10 | Toshiba Corp | Tungsten powder and its manufacturing method, and sputtering target and cutting tool |
| CN101438391A (en) * | 2006-05-05 | 2009-05-20 | 应用材料股份有限公司 | Method and apparatus for photo-excitation of chemicals for atomic layer deposition of dielectric film |
| CN103484830A (en) * | 2012-06-12 | 2014-01-01 | 核工业西南物理研究院 | Preparation method of thick tungsten coating material and tungsten coating material |
| CN105390370A (en) * | 2014-08-20 | 2016-03-09 | 朗姆研究公司 | method and apparatus to deposit pure titanium thin film at low temperature using titanium tetraiodide precursor |
| CN107447201A (en) * | 2017-08-14 | 2017-12-08 | 北京理工大学 | The preparation facilities and method of a kind of tungsten product |
| CN109182996A (en) * | 2018-11-05 | 2019-01-11 | 中国兵器工业第五九研究所 | Tungsten alloy coating Preparation equipment and method |
| CN109609925A (en) * | 2019-02-21 | 2019-04-12 | 苏州鑫沣电子科技有限公司 | A kind of chemical vapor deposition high-purity tantalum sputtering target material production method |
| CN109609926A (en) * | 2019-02-21 | 2019-04-12 | 苏州鑫沣电子科技有限公司 | A kind of chemical vapor deposition high purity tungsten sputtering target material production method |
| CN111151763A (en) * | 2018-11-07 | 2020-05-15 | 宁波江丰电子材料股份有限公司 | Preparation method of tungsten-titanium alloy target material |
| CN111943725A (en) * | 2020-07-29 | 2020-11-17 | 沈阳中钛装备制造有限公司 | Titanium modified ceramic and preparation method thereof, and ceramic-based metal composite and composite method thereof |
| CN112391596A (en) * | 2020-10-19 | 2021-02-23 | 洛阳高新四丰电子材料有限公司 | Preparation method of high-quality tungsten-titanium sputtering target material |
| CN112501586A (en) * | 2020-10-22 | 2021-03-16 | 季华实验室 | Preparation method and preparation device of high-purity metal film and semiconductor chip |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6444556B2 (en) * | 1999-04-22 | 2002-09-03 | Micron Technology, Inc. | Chemistry for chemical vapor deposition of titanium containing films |
| JP5861839B2 (en) * | 2010-09-30 | 2016-02-16 | 日立金属株式会社 | Method for manufacturing molybdenum target |
-
2021
- 2021-05-20 CN CN202110553332.2A patent/CN113275589B/en active Active
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5160534A (en) * | 1990-06-15 | 1992-11-03 | Hitachi Metals Ltd. | Titanium-tungsten target material for sputtering and manufacturing method therefor |
| US5397050A (en) * | 1993-10-27 | 1995-03-14 | Tosoh Smd, Inc. | Method of bonding tungsten titanium sputter targets to titanium plates and target assemblies produced thereby |
| JPH08165566A (en) * | 1994-03-31 | 1996-06-25 | Sumitomo Sitix Corp | High purity titanium material and its production |
| US5700519A (en) * | 1995-01-06 | 1997-12-23 | Sony Corporation | Method for producing ultra high purity titanium films |
| JP2002105632A (en) * | 2000-09-29 | 2002-04-10 | Toshiba Corp | Tungsten powder and its manufacturing method, and sputtering target and cutting tool |
| CN101438391A (en) * | 2006-05-05 | 2009-05-20 | 应用材料股份有限公司 | Method and apparatus for photo-excitation of chemicals for atomic layer deposition of dielectric film |
| CN103484830A (en) * | 2012-06-12 | 2014-01-01 | 核工业西南物理研究院 | Preparation method of thick tungsten coating material and tungsten coating material |
| CN105390370A (en) * | 2014-08-20 | 2016-03-09 | 朗姆研究公司 | method and apparatus to deposit pure titanium thin film at low temperature using titanium tetraiodide precursor |
| CN107447201A (en) * | 2017-08-14 | 2017-12-08 | 北京理工大学 | The preparation facilities and method of a kind of tungsten product |
| CN109182996A (en) * | 2018-11-05 | 2019-01-11 | 中国兵器工业第五九研究所 | Tungsten alloy coating Preparation equipment and method |
| CN111151763A (en) * | 2018-11-07 | 2020-05-15 | 宁波江丰电子材料股份有限公司 | Preparation method of tungsten-titanium alloy target material |
| CN109609925A (en) * | 2019-02-21 | 2019-04-12 | 苏州鑫沣电子科技有限公司 | A kind of chemical vapor deposition high-purity tantalum sputtering target material production method |
| CN109609926A (en) * | 2019-02-21 | 2019-04-12 | 苏州鑫沣电子科技有限公司 | A kind of chemical vapor deposition high purity tungsten sputtering target material production method |
| CN111943725A (en) * | 2020-07-29 | 2020-11-17 | 沈阳中钛装备制造有限公司 | Titanium modified ceramic and preparation method thereof, and ceramic-based metal composite and composite method thereof |
| CN112391596A (en) * | 2020-10-19 | 2021-02-23 | 洛阳高新四丰电子材料有限公司 | Preparation method of high-quality tungsten-titanium sputtering target material |
| CN112501586A (en) * | 2020-10-22 | 2021-03-16 | 季华实验室 | Preparation method and preparation device of high-purity metal film and semiconductor chip |
Non-Patent Citations (2)
| Title |
|---|
| 中国冶金百科全书总编辑委员会《有色金属冶金》卷编辑委员会，冶金工业出版社《中国冶金百科全书》编辑部编.《中国冶金百科全书 有色金属冶金》.北京：冶金工业出版社,1999,第305页. * |
| 化学气相沉积法制备和修复X射线管旋转阳极靶面材料;颜彬游;吕延伟;宋久鹏;李剑;;真空电子技术(第01期);第1-4页 * |
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