CN109609926A - A kind of chemical vapor deposition high purity tungsten sputtering target material production method - Google Patents
A kind of chemical vapor deposition high purity tungsten sputtering target material production method Download PDFInfo
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- CN109609926A CN109609926A CN201910128681.2A CN201910128681A CN109609926A CN 109609926 A CN109609926 A CN 109609926A CN 201910128681 A CN201910128681 A CN 201910128681A CN 109609926 A CN109609926 A CN 109609926A
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- tungsten
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- vapor deposition
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Electrodes Of Semiconductors (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of chemical vapor deposition high purity tungsten sputtering target material production method, includes the following steps: that (1) prepares raw material: being gaseous tungsten hexafluoride as raw material using normal temperature and pressure；(2) it prepares high pure metal tungsten: by chemical vapor depsotition equipment, tungsten hexafluoride being reduced into high pure metal tungsten with reducing gas；(3) high pure metal tungsten obtained in step (2) is deposited on basis material, One-step production high-purity tungsten target material or tungsten target material blank.The problems such as present invention is low to solve existing tungsten target material Purity, not easy to be processed, and surface is easy to pollute, and quality conformance is poor, vapor deposition reaction are continuous vapor reaction, and reaction process is uniform, good product consistency；Tungsten target material is prepared using one-step method, secondary operation is avoided to pollute, advantageously ensures that tungsten target material product quality, and production cost is low.
Description
Technical field
The present invention relates to a kind of chemical vapor deposition high purity tungsten sputtering target material production methods, more particularly, to form big rule
The high purity tungsten sputtering target material production method of vlsi die diffusion contact layer film.
Background technique
Large scale integrated circuit carries out vacuum sputtering film forming commonly using tungsten target material, it is especially desirable to using large-sized high-purity
Tungsten target material, in current semiconductor integrated circuit field, the purity of tungsten target material is in 99.995%-99.999%, diameter 300-
450mm, with a thickness of 5-15mm.But with the development of semicon industry, large scale integrated circuit proposes tungsten target material higher
It is required that.
Tungsten belongs to infusibility difficult-to-machine metal, and the method production tungsten target material of powder metallurgy, the powder smelting are generallyd use in industry
Gold process is the processing method by high purity tungsten metal powder by shaping, being sintered, blank or product is made.Specific
In powder metallurgy process, by the way that ready tungsten powder to be mounted in particular manufacturing craft or jacket, then through isostatic cool pressing equipment
Through vacuum or gas-protecting sintering after (Cold Isostatic Pressing, abbreviation CIP) molding, or through hot isostatic apparatus
(Hot Isostatic Pressing, abbreviation HIP) sinter molding, or it is placed in hot pressing (Hot in vacuum hotpressing stove
Pressing, abbreviation HP) molding.Need the mold to be matched according to the size design of target and the vacuum hotpressing that matches or
Hot isostatic pressure stove.However, the processing for large-sized high-purity tungsten target material, quiet by die size and hot pressing, heat etc.
It presses furnace to use the limitation of size and temperature, one-pass molding is difficult to using powder metallurgy production large scale tungsten target material, is needed tungsten powder
It is last first pre-formed, that is, a large scale tungsten target material blank is formed, then uses the calendering technologies such as cogging, rolling by this large scale
Tungsten target material blank carries out hot rolling and cold rolling processing, to reach size required for qualified tungsten target material and physical property requirements.Due to
Tungsten is hard crisp at normal temperature, is not easy to be rolled at normal temperature, tungsten metal slabs need hot rolling thus, and tungsten metal rolls after heating
The oxidation rate that process processed is such as exposed to the atmosphere is very fast, and the operation of rolling is easy to cause high purity tungsten surface second to pollute.It is complicated
Processing technology and complicated molding, sintering, rolling equipment, cause tungsten target material that secondary dirt occurs in subsequent calendering process
Dye, and Quality Control Links are more, are easy to cause quality fluctuation, influence the spatter film forming quality of tungsten target material and the performance of film.Have
In consideration of it, it is proposed that a kind of production method of new high-purity tungsten target material, the especially production of high-purity, large-sized tungsten target material
Method, to overcome the deficiencies of existing technologies.
Summary of the invention
In view of the deficienciess of the prior art, the object of the invention is that providing a kind of chemical vapor deposition high purity tungsten
Sputtering target material production method, low to solve existing tungsten target material Purity, not easy to be processed, surface is easy to pollute, quality conformance
The problems such as poor.
To achieve the goals above, the technical solution adopted by the present invention is that it is such:
A kind of chemical vapor deposition high purity tungsten sputtering target material production method, includes the following steps:
(1) prepare raw material: being gaseous tungsten hexafluoride as raw material using normal temperature and pressure；
(2) it prepares high pure metal tungsten: by chemical vapor depsotition equipment, tungsten hexafluoride being reduced into high pure metal with reducing gas
Tungsten；
(3) high pure metal tungsten obtained in step (2) is deposited on basis material, One-step production high-purity tungsten target material or tungsten
Target blank.
As a preferred embodiment, high pure metal tungsten obtained in step (2) is deposited to through chemical vapor depsotition equipment
Tungsten target material on back veneer material is fabricated to finished product tungsten target material after thermally treated and Precision Machining.
As a preferred embodiment, high pure metal tungsten obtained in step (2) is deposited to through chemical vapor depsotition equipment
Tungsten target material blank on non-back veneer material is bound after cutting, high-temperature heat treatment, surface treatment with backboard, through subsequent technique
After be fabricated to product tungsten target material.
As a preferred embodiment, in the step (3) high pure metal tungsten deposition can be deposited on copper, tungsten, nickel, titanium or its
On his basis material.
As a preferred embodiment, W content exists in the high-purity tungsten target material or tungsten target material blank that the step (3) obtains
99.999-99.99999% or more.
As a preferred embodiment, the high-purity tungsten target material or tungsten target material blank density that the step (3) obtains can reach
99.5% or more of theoretical density.
As a preferred embodiment, the high-purity tungsten target material or tungsten target material billet size that the step (3) obtains are length
In 100 ~ 600mm, width in 100 ~ 600mm or diameter in 100-600mm, thickness in 1-35mm.
As a preferred embodiment, sputter face is hung down in the high-purity tungsten target material or tungsten target material blank that the step (3) obtains
Histogram is to for high pure metal tungsten deposition direction or crystal grain production mode reform, sputter face vertical direction crystallite dimension and crystal planar orientation one
It causes.
As a preferred embodiment, in the high-purity tungsten target material or tungsten target material blank that the step (3) obtains in sputter face
Average grain size at 20 μm or more and 200 μm or less.
Compared with prior art, beneficial effects of the present invention: it is entirely different with the production technology of conventional tungsten sputtering target material, change
By reduction tungsten hexafluoride, a step in chemical vapor depsotition equipment has been deposited for the production of vapor deposition (CVD) tungsten sputtering target material
At not needing to carry out powder preparation, hammer cogging, the processes such as rolling, simple process, production process are easily-controllable, are not easy to produce target
Raw pollution, target of the invention are easier the technical requirements for making material property reach semiconductor circuit diffusion contact layer film,
By controlling the deposition velocity, control crystallite dimension and crystal planar orientation of tungsten target material, there is the discharge voltage for reducing tungsten sputtering target
To be easy to produce plasma, and inhibit the effect of the voltage drift in film forming.
Specific embodiment
The invention will be further described combined with specific embodiments below.Following embodiment is only used for clearly illustrating
Technical solution of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment:
A kind of chemical vapor deposition high purity tungsten sputtering target material production method, includes the following steps:
(1) prepare raw material: being gaseous tungsten hexafluoride as raw material using normal temperature and pressure；
(2) it prepares high pure metal tungsten: by chemical vapor depsotition equipment, tungsten hexafluoride being reduced into high pure metal with reducing gas
Tungsten；
(3) high pure metal tungsten obtained in step (2) is deposited on basis material, One-step production high-purity tungsten target material or tungsten
Target blank.
Wherein, tungsten hexafluoride is with 99.999% or more purity tungsten hexafluoride in step (1), and general tungsten hexafluoride gas phase is heavy
Product tungsten reaction temperature is at 550 ~ 650 DEG C.
Specifically, high pure metal tungsten obtained in step (2) is deposited on back veneer material through chemical vapor depsotition equipment
Tungsten target material, be fabricated to finished product tungsten target material after thermally treated and Precision Machining.
Specifically, high pure metal tungsten obtained in step (2) is deposited to non-back veneer material through chemical vapor depsotition equipment
On tungsten target material blank, after cutting, high-temperature heat treatment, surface treatment with backboard bind, production is fabricated to after subsequent technique
Product tungsten target material.Wherein, subsequent technique includes Precision Machining, cleaning etc..
Specifically, high pure metal tungsten deposition can be deposited on copper, tungsten, nickel, titanium or other basis materials in the step (3)
On.Further basis material can be metal material, be also possible to nonmetallic materials.
More specifically, big diffusion contact layer is formed in semiconductor silicon on piece by magnetron sputtering mode by high-purity tungsten target material
Film forming mechanism enlightenment, and form large scale integrated circuit W film technique using tungsten hexafluoride chemical vapor deposition process and open
Hair, gaseous state high-purity tungsten hexafluoride by vapor deposition apparatus, continuously restored with hydrogen or other reducing gas and deposit to copper
Or on other organism materials, by adjusting substrate size and continuous vapor deposition reaction, large scale, high-purity, high density are realized
The batch production of tungsten sputtering target material.
Specifically, W content is in 99.999- in high-purity tungsten target material or tungsten target material blank that the step (3) obtains
99.99999% or more.Further, principle is purified using tungsten hexafluoride rectification and purification and gas phase deposited crystal oriented growth, it can
To produce the metal tungsten target material product of ultra-high purity, material purity can achieve 99.9999% or more.
Specifically, high-purity tungsten target material or tungsten target material blank density that the step (3) obtains can reach theoretical density
99.5% or more.Further, since vapor deposition is that tungsten atom state is accumulated, tungsten target material or target blank density can be with after deposition
It is close to or up to 99.5% or more the theoretical density of tungsten material.
Specifically, high-purity tungsten target material or tungsten target material billet size that the step (3) obtains be length 100 ~
600mm, width are in 100 ~ 600mm or diameter in 100-600mm, thickness in 1-35mm.Further, heavy using continuous gas phase
Product grain growth principle, the tungsten target material or target blank product, thickness that deposition production different-thickness may be implemented can control
1-35mm。
Specifically, sputter face vertical direction is height in high-purity tungsten target material or tungsten target material blank that the step (3) obtains
Pure metal tungsten deposition direction or crystal grain production mode reform, sputter face vertical direction crystallite dimension are consistent with crystal planar orientation.More have
Body, by control reaction gas flow velocity, flow direction, it can control deposits tungsten target crystalline grains size and crystal planar orientation, there is it
Conducive to sputtering process film forming speed and quality of forming film is improved, improve diffusion contact layer film performance.Further, the present invention makes
High purity tungsten sputtering target material or tungsten target material blank in sputter face vertical direction be tungsten deposition direction or crystal grain production mode reform, sputter face
Vertical direction crystallite dimension is consistent with crystal planar orientation.
Specifically, the average crystal grain in high-purity tungsten target material or tungsten target material blank that the step (3) obtains in sputter face
Size is at 20 μm or more and 200 μm or less.
More specifically, by adjusting deposition substrate material, shape and size, different sizes or different shape can be deposited
Tungsten target material or tungsten target material blank；If high purity tungsten to be deposited directly to the copper for meeting target requirement or copper alloy body material
On material, high-purity, the large scale tungsten target material for meeting requirement can be produced with a step.Further, vapor deposition reaction is to connect
Continuous vapor reaction, reaction process is uniform, good product consistency；Tungsten target material is prepared using one-step method, secondary operation is avoided to pollute, is had
Conducive to guarantee tungsten target material product quality, and production cost is low.
In conclusion the present invention compared with the technique of the prior art, has a characteristic that
(1) the high purity tungsten sputtering target material that the present invention makes is using high-purity tungsten hexafluoride and reducing gas as raw material, in chemical vapor deposition
A step is completed in product equipment, and reaction process is continuous gas-phase reaction, and product is respectively much better than biography to consistency and batch-to-batch consistency
System tungsten target material；
(2) the high purity tungsten sputtering target material purity that the present invention makes can be to 99.9999% or more, and material purity is much better than conventional powder
The tungsten sputtering target material of metallurgical technology production；
(3) the high purity tungsten sputtering target material density that the present invention makes can reach 99.5% of theoretical density or more；
(4) high purity tungsten sputtering target material production method of the invention, can produce the large scale tungsten target material of diameter 500mm or more, tungsten
Thickness can be controlled by sedimentation time, it is most thick can be with stability contorting between 1-35mm；
(5) average crystal grain in the high purity tungsten sputtering target material sputter face that the present invention makes can according to requirements, crystal grain ruler
Very little control is in 20 μm of -200 μ m；
(6) the high purity tungsten sputtering target material or tungsten target material blank that the present invention makes can be deposited on copper, tungsten, nickel, titanium or other matrix materials
On material；
(7) the high purity tungsten sputtering target material tungsten deposition direction or crystal grain production mode reform that the present invention makes are vertical with sputter face, sputter face
Vertical direction crystal grain distribution is consistent, and quality of forming film is completely the same when ensure that sputtering；
(8) high-purity large scale tungsten target material product produced by the invention has process simple, and product size is big, purity is high, density
High, the at low cost, advantages such as consistency is good, are very suitable to the spatter film forming of semiconductor circuit diffusion contact layer film.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improvement and deformations
Also it should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of chemical vapor deposition high purity tungsten sputtering target material production method, which comprises the steps of:
(1) prepare raw material: being gaseous tungsten hexafluoride as raw material using normal temperature and pressure；
(2) it prepares high pure metal tungsten: by chemical vapor depsotition equipment, tungsten hexafluoride being reduced into high pure metal with reducing gas
Tungsten；
(3) high pure metal tungsten obtained in step (2) is deposited on basis material, One-step production high-purity tungsten target material or tungsten
Target blank.
2. a kind of chemical vapor deposition high purity tungsten sputtering target material production method according to claim 1, it is characterised in that: warp
High pure metal tungsten obtained in step (2) is deposited to the tungsten target material on back veneer material by chemical vapor depsotition equipment, thermally treated
With finished product tungsten target material is fabricated to after Precision Machining.
3. a kind of chemical vapor deposition high purity tungsten sputtering target material production method according to claim 1, it is characterised in that: warp
High pure metal tungsten obtained in step (2) is deposited to the tungsten target material blank on non-back veneer material by chemical vapor depsotition equipment, warp
It is bound after crossing cutting, high-temperature heat treatment, surface treatment with backboard, product tungsten target material is fabricated to after subsequent technique.
4. a kind of chemical vapor deposition high purity tungsten sputtering target material production method according to claim 1, it is characterised in that: institute
Stating high pure metal tungsten deposition in step (3) can be deposited on copper, tungsten, nickel, titanium or other basis materials.
5. a kind of chemical vapor deposition high purity tungsten sputtering target material production method according to claim 1, it is characterised in that: institute
W content is stated in the high-purity tungsten target material or tungsten target material blank that step (3) obtains in 99.999-99.99999% or more.
6. a kind of chemical vapor deposition high purity tungsten sputtering target material production method according to claim 1, it is characterised in that: institute
It states high-purity tungsten target material that step (3) obtains or tungsten target material blank density can reach 99.5% of theoretical density or more.
7. a kind of chemical vapor deposition high purity tungsten sputtering target material production method according to claim 1, it is characterised in that: institute
It states high-purity tungsten target material that step (3) obtains or tungsten target material billet size is length in 100 ~ 600mm, width in 100 ~ 600mm,
Or diameter in 100-600mm, thickness in 1-35mm.
8. a kind of chemical vapor deposition high purity tungsten sputtering target material production method according to claim 1, it is characterised in that: institute
State in the high-purity tungsten target material or tungsten target material blank that step (3) obtains sputter face vertical direction be high pure metal tungsten deposition direction or
Crystal grain production mode reform, sputter face vertical direction crystallite dimension are consistent with crystal planar orientation.
9. a kind of chemical vapor deposition high purity tungsten sputtering target material production method according to claim 1, it is characterised in that: institute
The average grain size in the high-purity tungsten target material or tungsten target material blank that step (3) obtains in sputter face is stated at 20 μm or more and
200 μm or less.
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Cited By (7)
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|---|---|---|---|---|
| CN110257909A (en) * | 2019-07-16 | 2019-09-20 | 河北工业大学 | A kind of chemical vapour deposition technique prepares the method and device thereof of polycrystalline silicon target |
| CN113136554A (en) * | 2021-04-26 | 2021-07-20 | 宁波江丰电子材料股份有限公司 | Tantalum target material and preparation method thereof |
| CN113275589A (en) * | 2021-05-20 | 2021-08-20 | 亚芯半导体材料(江苏)有限公司 | Preparation method and system of high-purity titanium powder and tungsten-titanium alloy sputtering target material |
| CN114250444A (en) * | 2021-12-01 | 2022-03-29 | 安徽光智科技有限公司 | Method for plasma-assisted chemical vapor deposition of high-purity tungsten sputtering target material |
| CN114318256A (en) * | 2021-12-28 | 2022-04-12 | 亚芯半导体材料(江苏)有限公司 | Large-size molybdenum sputtering target material and preparation process adopting chemical vapor deposition method |
| CN114369810A (en) * | 2020-10-15 | 2022-04-19 | 尚弘科技股份有限公司 | Tungsten product vapor deposition recovery method |
| CN114525485A (en) * | 2022-01-21 | 2022-05-24 | 亚芯半导体材料(江苏)有限公司 | Large-size high-entropy high-purity refractory metal alloy sputtering target material and preparation process thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257909A (en) * | 2019-07-16 | 2019-09-20 | 河北工业大学 | A kind of chemical vapour deposition technique prepares the method and device thereof of polycrystalline silicon target |
| CN114369810A (en) * | 2020-10-15 | 2022-04-19 | 尚弘科技股份有限公司 | Tungsten product vapor deposition recovery method |
| CN113136554A (en) * | 2021-04-26 | 2021-07-20 | 宁波江丰电子材料股份有限公司 | Tantalum target material and preparation method thereof |
| CN113275589A (en) * | 2021-05-20 | 2021-08-20 | 亚芯半导体材料(江苏)有限公司 | Preparation method and system of high-purity titanium powder and tungsten-titanium alloy sputtering target material |
| CN113275589B (en) * | 2021-05-20 | 2024-01-23 | 亚芯半导体材料(江苏)有限公司 | Preparation method and system of high-purity titanium powder and tungsten-titanium alloy sputtering target material |
| CN114250444A (en) * | 2021-12-01 | 2022-03-29 | 安徽光智科技有限公司 | Method for plasma-assisted chemical vapor deposition of high-purity tungsten sputtering target material |
| CN114318256A (en) * | 2021-12-28 | 2022-04-12 | 亚芯半导体材料(江苏)有限公司 | Large-size molybdenum sputtering target material and preparation process adopting chemical vapor deposition method |
| CN114525485A (en) * | 2022-01-21 | 2022-05-24 | 亚芯半导体材料(江苏)有限公司 | Large-size high-entropy high-purity refractory metal alloy sputtering target material and preparation process thereof |
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Application publication date: 20190412 |