CN109609925A - A kind of chemical vapor deposition high-purity tantalum sputtering target material production method - Google Patents
A kind of chemical vapor deposition high-purity tantalum sputtering target material production method Download PDFInfo
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- CN109609925A CN109609925A CN201910128675.7A CN201910128675A CN109609925A CN 109609925 A CN109609925 A CN 109609925A CN 201910128675 A CN201910128675 A CN 201910128675A CN 109609925 A CN109609925 A CN 109609925A
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- Prior art keywords
- tantalum
- target
- purity
- chemical vapor
- vapor deposition
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Classifications
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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
-
- 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
Abstract
The invention discloses a kind of chemical vapor deposition high-purity tantalum sputtering target material production method, include the following steps: that (1) prepares raw material: using tantalum pentafluoride as raw material；(2) it prepares high pure metal tantalum: by chemical vapor depsotition equipment, tantalum pentafluoride being reduced into high pure metal tantalum with reducing gas；(3) high pure metal tantalum obtained in step (2) is deposited on basis material, One-step production high-purity tantalum target or tantalum target blank.The present invention is continuous vapor reaction to make high-purity, high density, large-sized tantalum spattering target material, vapor deposition reaction, and reaction process is uniform, good product consistency；Tantalum target is prepared using one-step method, secondary operation is avoided to pollute, advantageously ensures that tantalum target product quality, and production cost is low.
Description
Technical field
The present invention relates to a kind of chemical vapor deposition high-purity tantalum sputtering target material production method, more particularly, to formation conducts
Tantalum (Ta) film of the diffusion barrier layer of thin copper film in integrated circuit or the tantalum spattering target material production method of tantalum nitride (TaN) film.
Background technique
Copper resistance is small, highly effective as integrated circuit wiring material, but since copper itself is active metal, exists
Diffuse to interlayer dielectric and cause pollute and fail the problem of, need between thin copper film and interlayer dielectric formed Ta film,
The diffusion barrier layers such as TaN film.
In general, Ta film, TaN film are especially needed commonly using tantalum target progress vacuum sputtering film forming in large scale integrated circuit
Large-sized high-purity tantalum target is used, in current semiconductor integrated circuit field, the purity of tantalum target is on 99.995% left side
The right side, diameter 200-450mm, with a thickness of 5-15mm.But with the development of semicon industry, large scale integrated circuit is to tantalum
Target is put forward higher requirements.
Up to the present, it is known that various impurity, gas componant, density, crystallite dimension, the crystal planar orientation contained in included a tantalum target
It will cause influence Deng on the filming performances such as Ta film, TaN film film forming speed, the uniformity of film thickness, particle generation when sputtering.Tradition
Tantalum spattering target material be all the size for guaranteeing tantalum target by complicated technologies such as vacuum melting, forging, annealing, rolling, heat treatments,
The performance indicators such as impurity content, crystallite dimension, crystal orientation.Traditional tantalum target target preparation process is complicated, process is long, leads to tantalum
In subsequent calendering process secondary pollution occurs for target, and Quality Control Links are more, are easy to cause quality fluctuation, influences
The spatter film forming quality of tantalum target and the performance of film.
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 Tantalum
Sputtering target material production method, to make high-purity, high density, large-sized tantalum spattering target material.
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 tantalum sputtering target material production method, includes the following steps:
(1) prepare raw material: using tantalum pentafluoride as raw material；
(2) it prepares high pure metal tantalum: by chemical vapor depsotition equipment, tantalum pentafluoride being reduced into high pure metal with reducing gas
Tantalum；
(3) high pure metal tantalum obtained in step (2) is deposited on basis material, One-step production high-purity tantalum target or tantalum
Target blank.
As a preferred embodiment, high pure metal tantalum obtained in step (2) is deposited to through chemical vapor depsotition equipment
Tantalum target on back veneer material is fabricated to finished product tantalum target after thermally treated and Precision Machining.
As a preferred embodiment, high pure metal tantalum obtained in step (2) is deposited to through chemical vapor depsotition equipment
Tantalum target blank on back veneer material is bound after cutting, high-temperature heat treatment, surface treatment with backboard, after subsequent technique
It is fabricated to product tantalum target.
As a preferred embodiment, in the step (3) high pure metal tantalum deposition can be deposited on copper, tantalum or copper, tungsten or
On other basis materials, basis material can be copper, copper alloy, tantalum, nickel or other basis materials.
As a preferred embodiment, tantalum content exists in the high-purity tantalum target or tantalum target blank that the step (3) obtains
99.999-99.9999% or more.
As a preferred embodiment, the high-purity tantalum target or tantalum target blank density that the step (3) obtains can reach
99.5% or more of theoretical density.
As a preferred embodiment, the high-purity tantalum target or tantalum target 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 tantalum target or tantalum target blank that the step (3) obtains
Histogram is to for high pure metal tantalum 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 tantalum target or tantalum target 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:, chemistry entirely different with traditional tantalum spattering target material production method
By reduction tantalum pentafluoride, a step in dedicated chemical vapor depsotition equipment has been deposited for the manufacture of vapor deposition (CVD) tantalum spattering target material
At not needing to carry out vacuum melting, hammer cogging, the technical process such as rolling, simple process, production process are easily-controllable, are not easy to target
Material generates secondary pollution, and this patent tantalum target is easier the skill for making material property reach semiconductor circuit diffusion barrier layer film
Art requirement, by controlling the deposition velocity, control crystallite dimension and crystal planar orientation of tantalum target, having reduces putting for tantalum spattering target
Piezoelectric voltage inhibits the effect of the voltage drift in film forming to be easy to produce plasma.
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 tantalum sputtering target material production method, includes the following steps:
(1) prepare raw material: using tantalum pentafluoride as raw material；
(2) it prepares high pure metal tantalum: by chemical vapor depsotition equipment, tantalum pentafluoride being reduced into high pure metal with reducing gas
Tantalum；
(3) high pure metal tantalum obtained in step (2) is deposited on basis material, One-step production high-purity tantalum target or tantalum
Target blank.
Wherein, in step (1) tantalum pentafluoride be with 99.995% or more purity tantalum pentafluoride, 200 DEG C of general tantalum pentafluoride with
Under be solid-state, and tantalum pentafluoride vapor deposited metal tantalum temperature wants 1200 DEG C or more.
Specifically, high pure metal tantalum obtained in step (2) is deposited on back veneer material through chemical vapor depsotition equipment
Tantalum target, be fabricated to finished product tantalum target after thermally treated and Precision Machining.
Specifically, high pure metal tantalum obtained in step (2) is deposited on back veneer material through chemical vapor depsotition equipment
Tantalum target blank, after cutting, high-temperature heat treatment, surface treatment with backboard bind, product is fabricated to after subsequent technique
Tantalum target.Wherein, subsequent technique includes Precision Machining, cleaning etc..
Specifically, high pure metal tantalum deposition can be deposited on copper, tantalum or copper, tungsten or other matrix materials in the step (3)
On material, basis material can be copper, copper alloy, tantalum, nickel or other basis materials.Further basis material can be metal material
Material, is also possible to nonmetallic materials.
More specifically, by high-purity tantalum target by magnetron sputtering mode semiconductor silicon on piece formed diffusion contact layer at
The enlightenment of film principle, and form large scale integrated circuit W film technique using tungsten hexafluoride chemical vapor deposition process and inspire,
By vapor deposition apparatus, with hydrogen or other reducing gas by the high-purity tantalum pentafluoride of gaseous state continuously restore and deposit to copper, tantalum,
On nickel or other basis materials, by adjusting basis material size and continuous vapor deposition reaction, realize large scale, high-purity,
The batch production of high density tantalum spattering target material.
Specifically, tantalum content is in 99.999- in high-purity tantalum target or tantalum target blank that the step (3) obtains
99.9999% or more.Further, principle is purified using tantalum pentafluoride rectification and purification and gas phase deposited crystal oriented growth, it can be with
The metal tantalum target product of high-purity is produced, material purity can achieve 99.999% or more.
Specifically, high-purity tantalum target or tantalum target blank density that the step (3) obtains can reach theoretical density
99.5% or more.Further, since vapor deposition is that tantalum atom state is accumulated, tantalum target or target blank density can be with after deposition
It is close to or up to 99.5% or more the theoretical density of tantalum material.
Specifically, high-purity tantalum target or tantalum target 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 tantalum target 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 tantalum target or tantalum target blank that the step (3) obtains
Pure metal tantalum deposition direction or crystal grain production mode reform, sputter face vertical direction crystallite dimension are consistent with crystal planar orientation.Further
, by control reaction temperature and gas flow rate, flow direction, it can control deposition of tantalum target crystalline grains size and crystal planar orientation,
Make it be conducive to improve sputtering process film forming speed and quality of forming film, improves diffusion barrier film performance, what the present invention made
Sputter face vertical direction is tantalum atom deposition direction or crystal grain production mode reform, sputtering in high-purity tantalum sputtering target material or tantalum target blank
Face vertical direction crystallite dimension is consistent with crystal planar orientation.
Specifically, the average crystal grain in high-purity tantalum target or tantalum target 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
Tantalum target or tantalum target blank；If High-purity Tantalum to be deposited directly to the copper for meeting target requirement or copper alloy matrix material
On material, the high-purity for meeting requirement, high density, large-size tantalum target can be produced with a step.Further, it is vapor-deposited
Reaction is continuous vapor reaction, and reaction process is uniform, good product consistency；Tantalum target is prepared using one-step method, avoids secondary add
Work pollution, advantageously ensures that tantalum target product quality, and production cost is low.
In conclusion compared with prior art, the present invention having a characteristic that
(1) high-purity tantalum sputtering target material that the present invention makes is using high-purity tantalum pentafluoride 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 tantalum target；
(2) the high-purity tantalum sputtering target material purity that the present invention makes can be to 99.999% or more, and material purity is much better than conventional powder smelting
The tantalum spattering target material of gold process production；
(3) the high-purity tantalum sputtering target material density that the present invention makes can reach 99.5% of theoretical density or more；
(4) high-purity tantalum sputtering target material production method of the invention can produce the large-size tantalum target of diameter 500mm or more, tantalum
Thickness can be controlled by deposition velocity and sedimentation time, and thickness can be with stability contorting between 1-35mm；
(5) average crystal grain in the high-purity tantalum sputtering target material sputter face that the present invention makes can according to requirements, sputter face
Upper crystallite dimension control is in 20 μm of -200 μ m；
(6) the high-purity tantalum sputtering target material tantalum 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；
(7) high-purity large-size tantalum target 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 tantalum sputtering target material production method, which comprises the steps of:
(1) prepare raw material: using tantalum pentafluoride as raw material；
(2) it prepares high pure metal tantalum: by chemical vapor depsotition equipment, tantalum pentafluoride being reduced into high pure metal with reducing gas
Tantalum；
(3) high pure metal tantalum obtained in step (2) is deposited on basis material, One-step production high-purity tantalum target or tantalum
Target blank.
2. a kind of chemical vapor deposition high-purity tantalum sputtering target material production method according to claim 1, it is characterised in that: warp
High pure metal tantalum obtained in step (2) is deposited to the tantalum target on back veneer material by chemical vapor depsotition equipment, thermally treated
With finished product tantalum target is fabricated to after Precision Machining.
3. a kind of chemical vapor deposition high-purity tantalum sputtering target material production method according to claim 1, it is characterised in that: warp
High pure metal tantalum obtained in step (2) is deposited to the tantalum target blank on back veneer material by chemical vapor depsotition equipment, is passed through
It is bound after cutting, high-temperature heat treatment, surface treatment with backboard, product tantalum target is fabricated to after subsequent technique.
4. a kind of chemical vapor deposition high-purity tantalum sputtering target material production method according to claim 1, it is characterised in that: institute
Copper, tantalum or copper can be deposited on, on tungsten or other basis materials by stating in step (3) high pure metal tantalum deposition, and basis material can be with
It is copper, copper alloy, tantalum, nickel or other basis materials.
5. a kind of chemical vapor deposition high-purity tantalum sputtering target material production method according to claim 1, it is characterised in that: institute
Tantalum content is stated in the high-purity tantalum target or tantalum target blank that step (3) obtains in 99.999-99.9999% or more.
6. a kind of chemical vapor deposition high-purity tantalum sputtering target material production method according to claim 1, it is characterised in that: institute
It states high-purity tantalum target that step (3) obtains or tantalum target blank density can reach 99.5% of theoretical density or more.
7. a kind of chemical vapor deposition high-purity tantalum sputtering target material production method according to claim 1, it is characterised in that: institute
It states high-purity tantalum target that step (3) obtains or tantalum target 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 tantalum sputtering target material production method according to claim 1, it is characterised in that: institute
State in the high-purity tantalum target or tantalum target blank that step (3) obtains sputter face vertical direction be high pure metal tantalum 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 tantalum sputtering target material production method according to claim 1, it is characterised in that: institute
The average grain size in the high-purity tantalum target or tantalum target blank that step (3) obtains in sputter face is stated at 20 μm or more and
200 μm or less.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910128675.7A CN109609925A (en) | 2019-02-21 | 2019-02-21 | A kind of chemical vapor deposition high-purity tantalum sputtering target material production method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114438472A (en) * | 2022-01-21 | 2022-05-06 | 亚芯半导体材料(江苏)有限公司 | Large-size ultra-pure vanadium sputtering target material for integrated circuit chip and preparation process thereof |
| CN114457314A (en) * | 2021-09-29 | 2022-05-10 | 中国船舶重工集团公司第七一八研究所 | Preparation method of high-purity tantalum target material |
| CN116143171A (en) * | 2023-02-17 | 2023-05-23 | 中船(邯郸)派瑞特种气体股份有限公司 | Tantalum pentafluoride preparation device and preparation method |
| CN116751979A (en) * | 2023-06-21 | 2023-09-15 | 同创(丽水)特种材料有限公司 | High-purity tantalum ingot and preparation method thereof |
| CN114561628B (en) * | 2022-03-22 | 2024-04-19 | 海朴精密材料(苏州)有限责任公司 | Preparation method and application of high-purity tantalum by cyclic chemical vapor deposition |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114457314A (en) * | 2021-09-29 | 2022-05-10 | 中国船舶重工集团公司第七一八研究所 | Preparation method of high-purity tantalum target material |
| CN114438472A (en) * | 2022-01-21 | 2022-05-06 | 亚芯半导体材料(江苏)有限公司 | Large-size ultra-pure vanadium sputtering target material for integrated circuit chip and preparation process thereof |
| CN114561628B (en) * | 2022-03-22 | 2024-04-19 | 海朴精密材料(苏州)有限责任公司 | Preparation method and application of high-purity tantalum by cyclic chemical vapor deposition |
| CN116143171A (en) * | 2023-02-17 | 2023-05-23 | 中船(邯郸)派瑞特种气体股份有限公司 | Tantalum pentafluoride preparation device and preparation method |
| CN116751979A (en) * | 2023-06-21 | 2023-09-15 | 同创(丽水)特种材料有限公司 | High-purity tantalum ingot and preparation method thereof |
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