CN109338314A - A kind of processing method of Ultra-fine grain copper manganese alloy target - Google Patents
A kind of processing method of Ultra-fine grain copper manganese alloy target Download PDFInfo
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- CN109338314A CN109338314A CN201811471674.4A CN201811471674A CN109338314A CN 109338314 A CN109338314 A CN 109338314A CN 201811471674 A CN201811471674 A CN 201811471674A CN 109338314 A CN109338314 A CN 109338314A
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- HPDFFVBPXCTEDN-UHFFFAOYSA-N copper manganese Chemical compound [Mn].[Cu] HPDFFVBPXCTEDN-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910000914 Mn alloy Inorganic materials 0.000 title claims abstract description 21
- 238000003672 processing method Methods 0.000 title claims abstract description 8
- 238000005242 forging Methods 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 36
- 238000000137 annealing Methods 0.000 claims abstract description 31
- 238000011084 recovery Methods 0.000 claims abstract description 26
- 238000005266 casting Methods 0.000 claims abstract description 11
- 238000001953 recrystallisation Methods 0.000 claims abstract description 7
- 238000011282 treatment Methods 0.000 claims abstract description 6
- 239000011572 manganese Substances 0.000 claims description 3
- 239000013077 target material Substances 0.000 abstract description 19
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 238000005477 sputtering target Methods 0.000 abstract description 14
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 description 13
- 239000010949 copper Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 4
- 238000001887 electron backscatter diffraction Methods 0.000 description 4
- 230000035515 penetration Effects 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 229910000881 Cu alloy Inorganic materials 0.000 description 3
- 230000008602 contraction Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000011265 semifinished product Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 235000013618 yogurt Nutrition 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- -1 includes Al Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
Classifications
-
- 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
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention belongs to integrated circuit sputtering target material manufacturing technology fields, disclose a kind of processing method of Ultra-fine grain copper manganese alloy target.This method mainly includes the following steps: 1) to carry out high temperature forging cogging to cupromanganese ingot casting；2) forging of the low temperature three-dimensional of round more than 150-250 DEG C is carried out to step 1) gains；3) to step 2) gains in 425-475 DEG C of progress dynamic recrystallization treatment；4) multiple cold deformation+recovery annealing is carried out to step 3) gains, obtains Ultra-fine grain copper manganese alloy target.Its service life of long-life cupromanganese target that the present invention obtains is up to 3000kwh, average grain size is at 1 μm or less, Vickers hardness is more than 140HV, (220) orientation percentage is more than 80%, it can effectively improve target utilization, can satisfy the requirement of integrated circuit 28nm and following manufacturing process.
Description
Technical field
The invention belongs to target manufacturing technology field, in particular to a kind of processing method of Ultra-fine grain copper manganese alloy target.
Background technique
Currently, the top company Samsung of integrated circuit industry technology has been carried out 7nm technique volume production, it is contemplated that the year two thousand twenty
Realize 5nm volume production；The maximum chip foundry company's T SMC mainstream technology in the whole world equally comes into 7nm technique, carry out 5~
3nm technique development.On the whole in terms of technological level, global IC chip 10nm and following technique account for world market predominantly
Position；It was predicted that mainstream will be become to 7nm in 2019 and following technique.
The ratio that current whole world 45nm and following production capacity account for semiconductors manufacture aggregated capacity is increasing, the reduction of characteristic size
The update of new material is set to develop into certainty.It is cured in the metal line width of 45nm and following process stage, integrated circuit chip circuits
Come more small, the interconnection line number of plies is more and more.45nm or less process requirements replace high purity copper as interconnection line using copper alloy, with solution
Certainly as line width reduces the problems such as bring electromigration, RC retardation ratio.Can be had using the metal-doped Cu alloy material such as aluminium, manganese
The stability that effect inhibits electromigration, improves Cu seed layer, is the important development direction in copper wiring technique.
High-purity copper alloy sputtering target material is Nanometer integrated circuit copper-connection critical support material.Due to the property of sputtering target material
Can directly determine the quality level of metallic film, the quality requirements of integrated circuit technology then to the chemical purity of target and its
Microstructure proposes high requirement.Currently, the maximum target of 28nm processing procedure volume production dosage is cupromanganese target, main quilt
Electronic material giant company monopolizing of the foreign countries such as Nikko, Honeywell, wherein great representative for the production of Honeywell company
Ultra-fine grain copper manganese alloy target, have the advantage that (1) target crystalline grains size fine uniform；(2) target Vickers hardness is up to
140HV or more, non-deformability is strong in sputtering process, and target deformation is no more than 0.5mm；(3) Ultra-fine Grained target has overlength
Service life greatly improves the utilization rate of target up to 3000kwh or more, saves target replacement and board safeguards institute
The time and efforts needed, reduces the production cost of semiconductor producer to greatest extent.This target is widely used in entirely at present
Ball 28nm advanced process.
Super fine crystal material refers to nanocrystalline or sub-micron crystal material of the average grain size at 0.1-1 μm, has excellent
Physical and mechanical properties are one of research hotspots of Material Field.Equal channel angular pressing technology (ECAP) is using by two phases
Hand over isometrical channel composition mold obtain metal big plasticity is shear-deformable, the shape and size before and after sample deformation are not sent out
It is raw to change, therefore can repeatedly be deformed.This method is up to the strain of target by repeated multiple times equal channel angular pressing
6-8, to obtain ultrafine-grained (UFG) microstructure.But due to equipment limit, the whole world, which only has Honeywell, at present the channels such as large size bent angle
Extrusion equipment can process large scale Ultra-fine Grained target using this method, it is therefore desirable to develop the processing of other Novel super-thin crystalline substance targets
Method.
The method that patent CN1484711A discloses physical vapor deposition target and manufactures metal material, this method is with scheduled
Path and number carry out equal channel angular pressing, and tandem rolling or forging are carried out after equal channel angular pressing, most pass through afterwards
Recrystallization annealing is crossed, obtaining average grain size is 1-30 μm, and (220) are orientated the target blankss of percentage > 90%.
Patent CN1592797A discloses a kind of high-strength sputtering target and its manufacturing method, this method using etc. channels bent angle squeeze
Pressure refinement crystal grain, target crystalline grains size < 1 μm finally obtained are orientated random sputtering target material, and sputtering target material material mainly includes
Al、Ti、Cu、Ta、Ni、Mo、Au、Ag、Pt。
Patent CN1681960 discloses the method for a kind of copper sputtering target material and formation copper sputtering target material, and this method uses 300
DEG C hot forging falls to height and is at least about 40%, only progress extrusion process, makes to be hot-forged blank and passes through equal channels bent angle
It squeezes at least 4 times, is during which heat-treated, is finally cold-rolled to drafts less than 90%, so that semi-finished product are formed, the target of acquisition
Average grain diameter is less than 1 μm, and grain size uniformity standard deviation is less than or equal to 15% in entire target.
Patent CN102925832A discloses a kind of large plastometric set method for preparing ultra-fine contraction crystalline substance copper, and this method is using more
Shear stress during the asynchronous pack rolling of passage and accumulation strain effect promote the stacking mistake row of material internal, crystal grain refinement and
Interface it is compound, by the slidings of annealing process Dislocations and climb later, change local dot matrix and crystal boundary planar orientation, promote
Then the formation of contraction crystalline substance in annealing process cools to room temperature removal with the furnace to get ultra-fine contraction crystalline substance copper material is arrived.But this method is only fitted
It is processed for thin strip, sputtering target material manufacture field can not be applied to.
Patent CN105039670A discloses a kind of two-sided mixing yoghurt Ultra-fine Grained plate device and method, this method
By reasonably designing two-sided mixing yoghurt device and method, the heat engine that can be effectively eliminated between adjacent stirring area influences
Area and heat affected area effectively improve the mechanical property of Ultra-fine Grained plate.
Summary of the invention
The object of the present invention is to provide a kind of processing methods of Ultra-fine grain copper manganese alloy target, which is characterized in that comprising such as
Lower step:
1) high temperature (900-950 DEG C) hammer cogging is carried out to ingot casting, carries out the forging of the low temperature three-dimensional of round more than 150-250 DEG C later
It makes, sufficiently broken blank tissue.To blank after forging in 425-475 DEG C of progress dynamic recrystallization treatment, tiny crystallite dimension is obtained.
2) multiple cold deformation+recovery annealing is carried out to blank, further refines crystal grain, realize Ultra-fine grain copper manganese alloy target
Preparation, obtain the service life up to 3000kwh, average grain size is at 1 μm hereinafter, Vickers hardness is more than 140HV, (220) orientation
Percentage is more than 80% Ultra-fine grain copper manganese alloy sputtering target material
Mn content is 0.3at%-1at% in the cupromanganese.
The low temperature three-dimensional forging, it is desirable that final forging temperature is no more than 400 DEG C, and forging times are 2-3 times.
Multiple cold deformation+the recovery annealing, number of processes are 3-4 times, and single cold deformation is 40-60%, are replied
Annealing temperature is 300-350 DEG C.
Beneficial effects of the present invention: the preparation of Ultra-fine grain copper manganese alloy target may be implemented in processing method of the invention, obtains
Its service life of long-life cupromanganese target arrived, average grain size was at 1 μm hereinafter, Vickers hardness is more than up to 3000kwh
140HV, (220) be orientated percentage be more than 80%, can effectively improve target utilization, can satisfy integrated circuit 28nm and with
The requirement of lower manufacturing process.
Detailed description of the invention
Fig. 1 is typical Ultra-fine grain copper manganese alloy target EBSD photo (× 6000).
Fig. 2 is typical Ultra-fine grain copper manganese alloy target crystalline grains distribution histogram (× 6000).
Fig. 3 is copper manganese target material EBSD photo (× 6000) after 1 low temperature three-dimensional forging.
Fig. 4 is copper manganese target material crystal grain distribution histogram (× 6000) after 1 low temperature three-dimensional forging
Fig. 5 is copper manganese target material EBSD photo (× 6000) after 2 cold deformation+recovery annealings
Fig. 6 is copper manganese target material crystal grain distribution histogram (× 6000) after 2 cold deformation+recovery annealings
Fig. 7 is copper manganese target material EBSD photo (× 300) after 5 cold deformation+recovery annealings
Fig. 8 is copper manganese target material crystal grain distribution histogram (× 300) after 5 cold deformation+recovery annealings
Specific embodiment
The present invention provides a kind of processing method of Ultra-fine grain copper manganese alloy target, comprises the following steps:
1) high temperature forging cogging is carried out to ingot casting, carries out the forging of the low temperature three-dimensional of round more than 150-250 DEG C later, it is sufficiently broken
Blank tissue.To blank after forging in 425-475 DEG C of progress dynamic recrystallization treatment, tiny crystallite dimension is obtained.
2) multiple cold deformation+recovery annealing is carried out to blank, further refines crystal grain, realize Ultra-fine grain copper manganese alloy target
Preparation, obtain average grain size 1 μm or less, Vickers hardness be more than 140HV, (220) orientation percentage be more than 80%
Ultra-fine grain copper manganese alloy sputtering target material, the service life is up to 3000kwh.
With reference to the accompanying drawings and examples to the detailed description of the invention.
Examples 1 and 2
It the results are shown in Table shown in 1 and Fig. 1, Fig. 2；
Cupromanganese ingot casting specification is 180 × 310t of φ, high temperature hot forging is carried out after 900-950 DEG C of heat penetration, later
In 200 DEG C of progress low temperature three-dimensional hot forgings.Blank specification is 205 × 240t of φ after forging；450 DEG C of heats are carried out to blank after forging
Processing；First round cold deformation+recovery annealing is carried out later, and blank specification is 290 × 120t of φ after deformation, and heat treatment temperature is
300℃；Second wheel cold deformation+recovery annealing is carried out later, and blank specification is 410 × 60t of φ after deformation, and heat treatment temperature is
300℃；Third round cold deformation+recovery annealing is eventually passed through, blank specification is 580 × 30t of φ after deformation, and heat treatment temperature is
300 DEG C, obtain semi-finished product target blankss.
What is obtained the results are shown in Table 1, it can be seen that carry out under conditions of cryogenic forging number is 2-3 times to ingot casting sufficiently thin
Change, using 3 wheel cold deformation+recovery annealings, obtained Ultra-fine grain copper manganese alloy sputtering target material average grain size is at 1 μm or less
(see Fig. 1,2), with the increase of cryogenic forging number, average grain size is gradually reduced.
Embodiment 3 and 4
It the results are shown in Table shown in 1 and Fig. 1, Fig. 2；
Cupromanganese ingot casting specification is 180 × 310t of φ, hot forging is carried out after 900-950 DEG C of heat penetration, later 200
DEG C carry out low temperature three-dimensional hot forging 2 wheel, after forging blank specification be 205 × 240t of φ, to after forging blank carry out 450 DEG C of heats at
Reason；3-4 is carried out later takes turns cold deformation+recovery annealing, blank specification is 580 × 30t of φ after deformation, and heat treatment temperature is 300 DEG C,
Obtain semi-finished product target blankss.
What is obtained the results are shown in Table 1, it can be seen that ingot casting is sufficiently refined under conditions of low temperature three-dimensional is hot-forged 2 times,
Using 3-4 take turns cold deformation+recovery annealing, obtained Ultra-fine grain copper manganese alloy sputtering target material average grain size at 1 μm hereinafter,
With the increase of cold deformation+recovery annealing number, average grain size is gradually reduced.Comparative example 1 and 2
It the results are shown in Table shown in 1 and Fig. 3, Fig. 4
The range of Ultra-fine grain copper manganese alloy target low temperature three-dimensional hot forging number in order to obtain, carries out 1 low temperature three-dimensional respectively
Forging and 4 low temperature three-dimensional forging tests, compare with embodiment.
Cupromanganese ingot casting specification is 180 × 310t of φ, hot forging is carried out after 900-950 DEG C of heat penetration, later 200
1 time and 4 low temperature three-dimensionals forgings are carried out DEG C respectively, and blank specification is 205 × 240t of φ after forging, to 450 DEG C of blank progress after forging
Dynamic recrystallization treatment；First round cold deformation+recovery annealing is carried out later, and blank specification is 290 × 120t of φ, heat treatment after deformation
Temperature is 300 DEG C；Second wheel cold deformation+recovery annealing is carried out later, and blank specification is 410 × 60t of φ, heat treatment temperature after deformation
Degree is 300 DEG C；Third round cold deformation+recovery annealing is eventually passed through, blank specification is 580 × 30t of φ, heat treatment temperature after deformation
It is 300 DEG C, obtains finished product target blankss.
What is obtained the results are shown in Table 1, it can be seen that when low temperature three-dimensional forging times are lower than 2 times, ingot casting cylindrical crystalline substance is broken not
Sufficiently, target blankss average grain size is more than 1 μm, and sub-micron rank is not achieved；When low temperature three-dimensional forging times are more than 3 times, target blankss
Average grain size at 1 μm hereinafter, crystal grain refinement is without essential distinction, and when low temperature three-dimensional forging times are more than 3 times,
Target production efficiency, which will receive, to be seriously affected, and hinders target to produce production capacity, therefore it is not recommended that continue to improve the forging time of low temperature three-dimensional
Number.
Comparative example 3 and 4
It the results are shown in Table shown in 1 and figure 5-8
Ultra-fine grain copper manganese alloy target cold deformation+recovery annealing number range in order to obtain carries out 2 cold deformations respectively
+ recovery annealing and 5 cold deformations+recovery annealing test, are compared with embodiment.
Cupromanganese ingot casting specification is 180 × 310t of φ, and hot forging is carried out after 900-950 DEG C of heat penetration, 200 DEG C later
2 wheel of low temperature three-dimensional forging, blank specification is 205 × 240t of φ after forging, carries out 450 DEG C of dynamic recrystallization treatments to blank after forging；It
2 wheels and 5 wheel cold deformation+recovery annealings are carried out afterwards, and blank specification is 580 × 30t of φ after deformation, and heat treatment temperature is 300 DEG C, is obtained
Obtain finished product target blankss.
What is obtained the results are shown in Table 1, it can be seen that after 2 wheel low temperature three-dimensional forgings, after 2 wheel cold deformation+recovery annealings, and target
Base inner tissue is seriously elongated, and crystal grain length is more than 5 μm, and width is at 1 μm hereinafter, the institutional framework of such form is unfavorable for sputtering
The uniformity of film；After 5 wheel cold deformation+recovery annealings, since single cold deformation is too small, the mesh of crystal grain refinement is not achieved
, average grain size is more than 10 μm of
The comparison result of 1 cupromanganese sputtering target material of table
Technical solution of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint
What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.
Claims (5)
1. a kind of processing method of Ultra-fine grain copper manganese alloy target, which is characterized in that comprise the following steps:
1) high temperature forging cogging is carried out to cupromanganese ingot casting；
2) forging of the low temperature three-dimensional of round more than 150-250 DEG C is carried out to step 1) gains；
3) to step 2) gains in 425-475 DEG C of progress dynamic recrystallization treatment；
4) multiple cold deformation+recovery annealing is carried out to step 3) gains, obtains Ultra-fine grain copper manganese alloy target.
2. method according to claim 1, which is characterized in that Mn content is in cupromanganese described in step 1)
0.3at%-1at%.
3. method according to claim 1, which is characterized in that the forging of low temperature three-dimensional described in step 2), it is desirable that finish-forging
Temperature is no more than 400 DEG C, and forging times are 2-3 times.
4. method according to claim 1, which is characterized in that multiple cold deformation+recovery annealing described in step 4), place
Managing number is 2-4 times, and single cold deformation is 40-60%, and annealing temperature is 300-350 DEG C.
5. method according to claim 1, which is characterized in that the temperature of high temperature forging cogging described in step 1) is
900-950℃。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111705276A (en) * | 2020-07-01 | 2020-09-25 | 宁波江丰电子材料股份有限公司 | Ultra-pure copper-manganese alloy and treatment method thereof |
| CN113481475A (en) * | 2021-07-05 | 2021-10-08 | 宁波江丰电子材料股份有限公司 | Method for refining titanium target material grains and titanium target material |
| CN114029356A (en) * | 2021-11-09 | 2022-02-11 | 安徽工程大学 | Preparation method of stainless steel plate with superfine crystal/nanocrystalline laminar microstructure |
| CN115341161A (en) * | 2022-08-22 | 2022-11-15 | 宁波江丰电子材料股份有限公司 | Copper-aluminum alloy target material and preparation method and application thereof |
| CN116240408A (en) * | 2021-12-08 | 2023-06-09 | 中国科学院金属研究所 | A kind of preparation method of manganese-copper alloy sheet and foil material |
| CN116351872A (en) * | 2023-03-03 | 2023-06-30 | 燕山大学 | Grain refinement method and its controllable DS rolling mill by means of asynchronous dislocation rolling |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113481475A (en) * | 2021-07-05 | 2021-10-08 | 宁波江丰电子材料股份有限公司 | Method for refining titanium target material grains and titanium target material |
| CN114029356A (en) * | 2021-11-09 | 2022-02-11 | 安徽工程大学 | Preparation method of stainless steel plate with superfine crystal/nanocrystalline laminar microstructure |
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| CN116240408A (en) * | 2021-12-08 | 2023-06-09 | 中国科学院金属研究所 | A kind of preparation method of manganese-copper alloy sheet and foil material |
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