CN106756832B - A kind of preparation method of target - Google Patents
A kind of preparation method of target Download PDFInfo
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- CN106756832B CN106756832B CN201611229097.9A CN201611229097A CN106756832B CN 106756832 B CN106756832 B CN 106756832B CN 201611229097 A CN201611229097 A CN 201611229097A CN 106756832 B CN106756832 B CN 106756832B
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- blank
- target
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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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
Abstract
The present invention provides a kind of preparation methods of target, comprising the following steps: A) it will be heat-treated after the blank pickling after forging, the heating rate of the heat treatment is 10~50 DEG C/min；B) blank after heat treatment is placed in the tooling of milling train and is rolled；C the blank after rolling) is subjected to pickling, then is heat-treated, target is obtained；The heating rate of the heat treatment is 10~50 DEG C/min.The present invention is by using special rolling tooling and the heat treatment process that is rapidly heated, diameter can be prepared in 400~1000mm, big specification target of the thickness in 6~30mm, and control { 111 } of the acquisition of this kind of target, { 100 } texture component ratio 20~40%, texture component is distributed undulated control within 10%, is able to satisfy the semiconductor application of 28nm and following processing procedure.
Description
Technical field
The present invention relates to target technical field more particularly to a kind of preparation methods of target.
Background technique
Physical vapour deposition (PVD) (PVD) is one of the technique of most critical in semiconductor chip production process, and the purpose is to gold
Belong to or the compound of metal is deposited in the form of a film on silicon wafer or other substrates, and then passes through the works such as photoetching and corrosion
The cooperation of skill ultimately forms distribution structure complicated in semiconductor chip.Physical vapour deposition (PVD) is completed by sputtering machine table
, sputtering target material is exactly for the very important crucial consumptive material of one in above-mentioned technique.Common sputtering target material has high-purity
Ta, there are also the non-ferrous metals such as Ti, Al, Co and Cu.
As wafer size increases to 300mm (12 inches), 450mm (18 cun), corresponding sputtering target from 200mm (8 inches)
Material size also increases with it the basic demand for being just able to satisfy PVD plated film, meanwhile, line width is reduced to 90~45nm from 130~180nm
And 28nm hereinafter, electric conductivity and barrier layer based on conductor matching performance, then sputtering target material also will from ultra-pure Al/Ti system turn
Turn to ultra-pure Cu/Ta system, Ta target blankss are increasing in the importance of semiconductor sputtering industry, while demand is also increasingly
Greatly.
Currently, manufacturing process becomes smaller since wafer size increases, more harsh requirement is proposed to included a tantalum target base texture.Often
The included a tantalum target base for 300mm wafer of rule technology production, because its texture component is uncontrolled, each component is unevenly distributed, crucial texture
Constituent content and sputtering machine table Base line target are inconsistent, cause properties after spatter film forming not up to standard, are not available,
Influence the scale application of included a tantalum target base.
Summary of the invention
Present invention solves the technical problem that being to provide a kind of preparation method of target, preparation method provided by the present application can
Make 400~1000mm of diameter of preparation, is controlled with a thickness of { 111 } of the target of 9~30mm, { 100 } texture component ratio
20%~40%, texture component is distributed undulated control within 10%.
In view of this, this application provides a kind of preparation methods of target, comprising the following steps:
A), will be heat-treated after the blank pickling after forging, the heating rate of the heat treatment is 10~50 DEG C/min；
B), the blank after heat treatment is placed in the tooling of milling train and is rolled；The contact surface of the tooling and blank
Angle with the plane for crossing top and bottom rolls axis is θ, and the tooling is rolled under with the plane where the minimum point of blank contact surface
The distance of roller horizontal section is δ, the θ=± (55~85 °), the δ=± (20~50) mm；
C), the blank after rolling is subjected to pickling, then is heat-treated, obtain target；The heating rate of the heat treatment
For 10~50 DEG C/min.
Preferably, the target is tantalum target or tantalum alloy target.
Preferably, the θ=± (60~80 °), the δ=± (20~40) mm.
Preferably, the rolling is rotation rolling, and the working modulus of each passage of the rolling is 2%~20%.
Preferably, step C) in, the heating rate of the heat treatment is 20~40 DEG C/min.
Preferably, step C) in, the temperature of the heat treatment is the 25%~45% of blank fusing point, soaking time is 0~
240min。
Preferably, step A) described in heat treatment temperature be blank fusing point 25%~45%.
Preferably, step A) with step C) described in pickling mixed liquor be volume ratio be 5:3:2 HCl, HF and
H2SO4Mixed liquor.
Preferably, the blank is cake blank, diameter >=100mm of the blank, thickness≤50mm.
Preferably, the diameter of the target is 400mm~1000mm, with a thickness of 6~30mm.
This application provides a kind of preparation method of target, this method will be heat-treated after the blank pickling after forging first,
The blank after heat treatment is placed in the tooling of milling train again and is rolled, it finally will be at reheating after the blank pickling after rolling
Reason, obtains target；The application introduces shear strain by introducing tooling during the rolling process, so that sotck thinkness direction
Surface and middle layer rolling texture type are variant, and by introducing the heat treatment process that is rapidly heated, so that target blankss are in thickness side
There are temperature gradients from surface to middle layer upwards, finally make thickness direction rolling texture difference and heat treatment temperature gradient
It is formed and is corresponded to, so that target texture is evenly distributed, texture type and ratio are controllable, realize { 111 }, { 100 } texture group of target
Divide ratio control 20%~40%, texture component is distributed undulated control within 10%.
Detailed description of the invention
Fig. 1 is the schematic diagram that tooling and blank are placed in the operation of rolling of the present invention；
Fig. 2 is the texture distribution statistics figure of tantalum target prepared by the embodiment of the present invention 1；
Fig. 3 is the textile analysis IPF figure of tantalum target prepared by the embodiment of the present invention 1；
Fig. 4 is the texture distribution statistics figure of tantalum target prepared by the embodiment of the present invention 2；
Fig. 5 is the textile analysis IPF figure of tantalum target prepared by the embodiment of the present invention 2；
Fig. 6 is the texture distribution statistics figure of tantalum target prepared by the embodiment of the present invention 3；
Fig. 7 is the textile analysis IPF figure of tantalum target prepared by the embodiment of the present invention 3.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
The embodiment of the invention discloses a kind of preparation methods of target, comprising the following steps:
A), will be heat-treated after the blank pickling after forging, the heating rate of the heat treatment is 10~50 DEG C/min；
B), the blank after heat treatment is placed in the tooling of milling train and is rolled；The contact surface of the tooling and blank
It is θ, the tooling and the plane and bottom roll level where the minimum point of blank contact surface with the angle for crossing top and bottom rolls axis
The distance of section is δ, the θ=± (55~85 °), the δ=± (20~50) mm；
C), the blank after rolling is subjected to pickling, then is heat-treated, obtain target；The heating rate of the heat treatment
For 10~50 DEG C/min.
During preparing target, rolling tooling and be rapidly heated heat treatment process of the application by design, so that
Target texture is evenly distributed, texture type and ratio are controllable, realizes that { 111 } of target, the control of { 100 } texture component ratio exist
20%~40%, texture component is distributed undulated control within 10%.
According to the present invention, the pretreatment of blank is carried out first, i.e., is heat-treated after the blank after forging being carried out pickling.It is described
It is forged to technological means well known to those skilled in the art, the application is without particularly limiting herein.The pickling is to remove
Surface impurity visually observes blank gloss without miscellaneous spot；The pickling preferably uses volume ratio for the mix acid liquor of 5:3:2.
Herein described preparation method is suitable for the alloy that those skilled in the art generally use, and can be tantalum material, or its
His material, in embodiment, the blank is preferably tantalum base, can be pure tantalum base, or tantalum alloy base.The heat treatment
Temperature be preferably the 25%~45% of blank fusing point, soaking time be 0~240min；The blank is described by taking tantalum base as an example
The temperature of heat treatment is preferably the 25%~45% of tantalum base, in embodiment, the heat treatment temperature of the tantalum base is 1000 DEG C~
1300℃.Diameter is 400~1000mm in order to obtain, with a thickness of the target of 6~30mm, the size for the blank that the application is forged
Specifically: diameter >=100mm, thickness≤50mm.During above-mentioned heat treatment, heating of the application to the heat treatment temperature
Rate is not particularly limited, and can directly be warming up to the temperature of heat treatment, can also be with heating rate liter well known in the art
Temperature is to heat treatment temperature.
According to the present invention, then the blank after heat treatment is rolled, it is herein described to roll the work for being placed in milling train
Load onto and rolled, i.e., during rolling, tooling is contacted with blank, specifically, the contact surface of the tooling and blank with
The angle for crossing the plane of top and bottom rolls axis is θ, the tooling and the plane and bottom roll where the minimum point of blank contact surface
The distance of horizontal section is δ, the θ=± (55~85 °), the δ=± (20~50) mm；Specific schematic diagram is as shown in Figure 1.
The rolling tooling of the application design, so that the macro-strain tensor of crystal is to be shown below under plate appearance coordinate when rolling；
It is asymmetric that the rolling tooling being arranged in the application operation of rolling deforms contact in rolling with respect to blank middle layer,
Unsymmetrical rolling is caused, is formed in " area Cuo Zha "；Wherein, in above formula ε ,-ε be plate along R to N to principal strain, Δ be the face N on
Be parallel to R to shear strain；(flow of metal can be considered simple compression, i.e. Δ is 0) to compare, this rolling mode with pair rolling
Under, in " area Cuo Zha " metal other than having the principal strain ε under simple compression, also act on the face N, be parallel to R to shear strain
Δ, total deformation are the superposition of compression and shear strain；Because of the introducing of shear strain, so that the type and ratio of rolling deformation texture
It is different from conventional synchronous rolling, the final texture type for influencing tantalum target and distribution；It can be by shear strain Δ introduction volume
Adjustment is to influence final target texture type and ratio；And the change to this tooling θ, δ parameter, shear strain Δ can be introduced
Amount is adjusted.The parameter θ, δ of tooling will affect shear strain Δ introduction volume in the application, the final texture class for influencing target
Type, component and distributing homogeneity.In certain embodiments, the θ=± (60~80 °), the δ=± (20~40) mm.?
In embodiment, the rolling rolls circle for rotation, and each pass reduction of the rolling is preferably 2%~20%；In certain implementations
In example, the number of the rolling is preferably 8~12 times, and the working modulus of each passage of the rolling is preferably 7%~15%.
Then blank after rolling is carried out pickling by the application, to remove surface impurity.The acid solution of the pickling is preferably adopted
The mix acid liquor for being 5:3:2 with volume ratio.Finally the blank after pickling is heat-treated, obtains target.The heat treatment
Heating rate is 10~50 DEG C/min, and in embodiment, the heating rate is 20~40 DEG C/min.The temperature of the heat treatment
It is the 25%~45% of blank fusing point, the time of heat preservation is 0~240min；The blank is by taking tantalum base as an example, in some embodiments
In, the temperature of the heat treatment is preferably 1100~1300 DEG C, and the time of the heat preservation is preferably 5~60min.In the above process
The heat treatment process that is rapidly heated is introduced, which makes target blankss thickness direction, and there are temperature from surface to middle layer
Gradient forms target blankss thickness direction rolling texture difference with heat treatment temperature gradient corresponding, finally makes entire target blankss texture point
Cloth uniformly, texture type and ratio it is controllable.The size of heating rate described herein will affect the temperature of target blankss inside and outside
Gradient, and then influence target blankss texture distributing homogeneity, type and component.
The application is during preparing target, by the rolling tooling speed heating heat treatment process of designed, designed, with solution
Certainly included a tantalum target base texture component ratio is uncontrolled, does not meet sputtering machine table Base line target requirement and through-thickness texture
The sharp problem of distribution gradient, has obtained the included a tantalum target base for meeting semiconductor requirement, and main feature has a two o'clock: first, included a tantalum target
Base specification is diameter in 400~1000mm, and thickness is in 6~30mm；Second, { 111 }, { 100 } texture component ratio are controlled 20
~40%, texture composite distribution undulated control is within 10%.
For a further understanding of the present invention, carried out below with reference to preparation method of the embodiment to target provided by the invention detailed
Describe in detail bright, protection scope of the present invention is not limited by the following examples.
Embodiment 1
1, the pure tantalum blank of cake of forging, diameter >=100mm of blank, thickness≤50mm are completed；
2, by the cake blank pickling after pickling, to remove surface impurity, visible tantalum metallic luster is visually observed without miscellaneous spot
: the mixed solution of pickling is HCl:HF:H2SO4=5:3:2 (volume ratio)；
3, be heat-treated the blank after pickling: the temperature of heat treatment is the 25%~45% of pure tantalum material fusing point, when heat preservation
Between be 0~240min；
4, installation rolling tooling: by designed tilt rolling tooling on milling train, θ=± (55~85 °), δ=±
(20~50mm), as shown in Figure 1；Rolling: circle is rolled in rotation, and each pass reduction control is 2%~20%；
5, by the blank pickling after rolling, to remove surface impurity, visible tantalum metallic luster is visually observed without miscellaneous spot；
The acid solution of pickling is specially HCl:HF:H2SO4=5: 3:2 (volume ratio)；
6, the blank after pickling is rapidly heated heat treatment, obtains tantalum target；Heat treatment temperature is tantalum material fusing point
25%~45%, soaking time is 0~240min, 10~50 DEG C/min of heating rate；
7, the tantalum target being prepared is subjected to textile analysis: analysis thickness direction { 111 }, { 100 } texture ratio.
Embodiment 2
It uses specification for Φ 250mm × δ 45mm and the pure tantalum cake blank of forging is completed, using the side of such as embodiment 1
Method prepares tantalum target, obtains Φ 500mm × δ 11mm included a tantalum target base, and be sampled textile analysis；The technological parameter of preparation is specifically shown in
Table 1, textile analysis result are as shown in Figure 2 and Figure 3；
1 embodiment 2 of table prepares the technological parameter of tantalum target
By Fig. 2 and Fig. 3 it is found that (100) mean value 6.4, standard deviation 3.1, (111) mean value 48.4, standard deviation are
11.1, (111) are dominant, and the distribution fluctuation of texture ratio is small；It can be seen that from IPF figure, form the logical thickness based on (111) texture and knit
The included a tantalum target base of structure distribution uniform.
Embodiment 3
It uses specification for Φ 250mm × δ 45mm and the pure tantalum cake blank of forging is completed, using the embodiment of the present application 1
Method prepare tantalum target, obtain the included a tantalum target base of Φ 500mm × δ 11mm, and be sampled textile analysis, the technological parameter of preparation
Specifically it is shown in Table 2；Textile analysis is as shown in Figure 4, Figure 5；
2 embodiment 3 of table prepares the technological parameter of tantalum target
By Fig. 4 and Fig. 5 it is found that (100) mean value 22.0, standard deviation 2.2, (111) mean value 23.5, standard deviation are
1.5, (100), (111) are dominant jointly, and the distribution fluctuation of texture ratio is less than 10%；Can be seen that from IPF figure, formed with (100),
(111) the included a tantalum target base that the logical thickness texture based on texture is evenly distributed has reached and " has obtained { 111 }, { 100 } texture component ratio
20~40%, texture component is distributed undulated control within 10% for control " target compared with implementation 2, because introducing more multiplexing
Sequence be rapidly heated heat treatment and using rolling tooling after rolling pass adjustment, promote included a tantalum target base texture component ratio and uniformly
Property variation so that (100) ratio increase, (111) ratio decline.
Embodiment 4
It uses specification for 310 × δ of Φ 45 and the tantalum-tungsten alloy cake blank of forging is completed, using the method for embodiment 1
Tantalum target is prepared, obtains the included a tantalum target base of Φ 500mm × δ 17mm, and be sampled textile analysis, the technological parameter of preparation is shown in Table 3；
Textile analysis is as shown in Figure 6, Figure 7；
3 embodiment 4 of table prepares the technological parameter of tantalum target
By Fig. 6 and Fig. 7 it is found that (100) mean value 29.1, standard deviation 7.8, (111) mean value 33.7, standard deviation are
7.1, (100), (111) are dominant jointly and accounting increases, and the distribution fluctuation of texture ratio is smaller；Can be seen that from IPF figure, formed with
(100), the included a tantalum target base that the logical thickness texture based on (111) texture is evenly distributed has reached { 111 }, { 100 } texture component ratio
Control the target 20~40%；Compared with Example 3, to the adjustment for the heat treatment parameter that is rapidly heated, texture group is also resulted in
The variation of part ratio.
It 2,3,4 can be seen that through the foregoing embodiment, using the special rolling tooling of the present invention and be rapidly heated and be heat-treated work
Skill, and by adjusting with the rolling pass working modulus that combines of rolling tooling, but included a tantalum target base texture component ratio, uniformity
It changes；Included a tantalum target base using the present invention available { 111 }, the control of { 100 } texture component ratio 20~40%.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (10)
1. a kind of preparation method of target, comprising the following steps:
A), will be heat-treated after the blank pickling after forging, the heating rate of the heat treatment is 10~50 DEG C/min；
B), the blank after heat treatment is placed in the tooling of milling train and is rolled；The contact surface and mistake of the tooling and blank
The angle of the plane of top and bottom rolls axis is θ, the tooling and the plane and bottom roll water where the minimum point of blank contact surface
The distance of side grain is δ, the θ=± (55~85 °), the δ=± (20~50) mm；
C), the blank after rolling is subjected to pickling, then is heat-treated, obtain target；The heating rate of the heat treatment is 10
~50 DEG C/min.
2. preparation method according to claim 1, which is characterized in that the target is tantalum target or tantalum alloy target.
3. preparation method according to claim 1, which is characterized in that the θ=± (60~80 °), the δ=± (20
~40) mm.
4. preparation method according to claim 1, which is characterized in that it is described rolling for rotation rolling, the rolling it is each
The working modulus of passage is 2%~20%.
5. preparation method according to claim 1, which is characterized in that step C) in, the heating rate of the heat treatment is
20~40 DEG C/min.
6. preparation method according to claim 1, which is characterized in that step C) in, the temperature of the heat treatment is blank
The 25%~45% of fusing point, soaking time are 0~240min.
7. preparation method according to claim 1, which is characterized in that step A) described in heat treatment temperature it is molten for blank
The 25%~45% of point.
8. preparation method according to claim 1, which is characterized in that step A) with step C) described in pickling mixed liquor
It is HCl, HF and H that volume ratio is 5:3:22SO4Mixed liquor.
9. described in any item preparation methods according to claim 1~8, which is characterized in that the blank is cake blank, described
Diameter >=100mm of blank, thickness≤50mm.
10. preparation method according to claim 9, which is characterized in that the diameter of the target is 400mm~1000mm,
With a thickness of 6~30mm.
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| CN110904364B (en) * | 2019-11-19 | 2021-02-19 | 先导薄膜材料（广东）有限公司 | Preparation method of aluminum alloy target material |
| CN113909414B (en) * | 2021-09-30 | 2023-12-29 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum target blank |
| CN114178527B (en) * | 2021-12-09 | 2023-07-21 | 西北工业大学 | Powder metallurgy preparation method of textured titanium material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704187A (en) * | 2009-11-13 | 2010-05-12 | 西北稀有金属材料研究院 | Texture forming method of tantalum target |
| CN103350108A (en) * | 2007-08-06 | 2013-10-16 | H.C.斯塔克公司 | Methods and apparatus for controlling texture of plates and sheets by tilt rolling |
| CN104741872A (en) * | 2015-01-16 | 2015-07-01 | 宁夏东方钽业股份有限公司 | Tantalum target material preparation method |
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2016
- 2016-12-27 CN CN201611229097.9A patent/CN106756832B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103350108A (en) * | 2007-08-06 | 2013-10-16 | H.C.斯塔克公司 | Methods and apparatus for controlling texture of plates and sheets by tilt rolling |
| CN101704187A (en) * | 2009-11-13 | 2010-05-12 | 西北稀有金属材料研究院 | Texture forming method of tantalum target |
| CN104741872A (en) * | 2015-01-16 | 2015-07-01 | 宁夏东方钽业股份有限公司 | Tantalum target material preparation method |
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