CN105714253A - Preparation method of large-size and fine-grain molybdenum tantalum alloy sputtering target material - Google Patents
Preparation method of large-size and fine-grain molybdenum tantalum alloy sputtering target material Download PDFInfo
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- CN105714253A CN105714253A CN201610133824.5A CN201610133824A CN105714253A CN 105714253 A CN105714253 A CN 105714253A CN 201610133824 A CN201610133824 A CN 201610133824A CN 105714253 A CN105714253 A CN 105714253A
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- JZLMRQMUNCKZTP-UHFFFAOYSA-N molybdenum tantalum Chemical compound [Mo].[Ta] JZLMRQMUNCKZTP-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000005477 sputtering target Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910001362 Ta alloys Inorganic materials 0.000 title claims abstract description 8
- 239000013077 target material Substances 0.000 title abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 16
- 238000011282 treatment Methods 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims description 73
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 37
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 36
- 238000003825 pressing Methods 0.000 claims description 34
- 239000011812 mixed powder Substances 0.000 claims description 24
- 238000004080 punching Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 13
- 238000012216 screening Methods 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 238000012545 processing Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000003068 static effect Effects 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 238000007493 shaping process Methods 0.000 claims description 6
- 238000004513 sizing Methods 0.000 claims description 6
- 229910052715 tantalum Inorganic materials 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 5
- 239000011247 coating layer Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 235000019698 starch Nutrition 0.000 claims description 5
- 239000008107 starch Substances 0.000 claims description 5
- 238000007751 thermal spraying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 abstract description 8
- 238000005096 rolling process Methods 0.000 abstract description 7
- 238000001513 hot isostatic pressing Methods 0.000 abstract description 3
- 229910000831 Steel Inorganic materials 0.000 abstract description 2
- 238000003754 machining Methods 0.000 abstract description 2
- 239000010959 steel Substances 0.000 abstract description 2
- 238000009694 cold isostatic pressing Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- 238000005056 compaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000004531 microgranule Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000010849 ion bombardment Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000011800 void material Substances 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
A preparation method of a large-size and fine-grain molybdenum tantalum alloy sputtering target material comprises steps of cold isostatic pressing molding through combination of a steel mold with a rubber plate, sintering, levelling and reshaping, hot isostatic pressing treatment, rolling and machining. The grain size of the produced target material is smaller than 50 microns, the change of the grain size is maintained within 20%, and grains are evenly distributed in the plane direction and the thickness direction of the target material; the relative density of the target material is higher than 97%; besides, the large-size sputtering target material with the length being about 2 m and the width being about 1.3 m can be produced.
Description
Technical field
The present invention relates to target technical field, the preparation method being specifically related to a kind of large scale, thin brilliant molybdenum tantalum alloy-sputtering targets material.
Background technology
Sputtering is one of major technique preparing thin-film material.With the ion bom bardment surface of solids accelerated, ion and surface of solids atom exchange momentum, making the atom of the surface of solids leave solid and be deposited on substrate surface, this process is called sputtering.The solid bombarded is the source material depositing thin film with sputtering method, is commonly referred to target.
High by the thin film consistency of target as sputter deposition, and the tack between base material is good.No matter sputtered film material shows in semiconductor integrated circuit, record medium, plane and is obtained in surface coating etc. and be widely applied.Therefore, to sputtering target material, this functional material demand with high added value increases year by year.In recent years, China's electronics and information industry develops rapidly, and integrated circuit, CD and display production line all have joint in a large number or Sole Proprietorship's appearance, one of China greatest requirements area being increasingly becoming thin film target in the world.But up to now, China is still without the special professional major company producing target, and a large amount of targets are still from external import.Especially for alloy target material, alloy temperature high-ductility is low, it is impossible to utilize Rolling Production.When utilizing powder metallurgy forming; after carrying out isostatic cool pressing process by molybdenum powder; be sintered, roll, machine after with backboard bind; the target made is in the process of sputter coating; when sputtering target is bombarded; gas owing to existing in target internal void discharges suddenly, causes large-sized target granule or microgranule to splash, or the caudacoria material of film forming is caused microgranule to splash by secondary electron bombardment.Due to the delayed development of domestic target industry, China's target market significant portion is captured by offshore company at present.Along with the high speed development of the high-tech industries such as microelectronics, the target market of China, by expanding day, provides opportunities and challenges for China's manufacturing development of target.
Summary of the invention
It is an object of the invention to provide that a kind of crystal grain is tiny, the preparation method of the large scale of relative density > 97%, thin brilliant molybdenum tantalum alloy-sputtering targets material.
The technical scheme that the present invention adopts for achieving the above object is: the preparation method of large scale, carefully brilliant molybdenum tantalum alloy-sputtering targets material, comprises the following steps:
Step one, molybdenum powder and tantalum powder are carried out pretreatment after sieve respectively, after screening, the ratio of the Fisher particle size of tantalum powder and molybdenum powder is 1.6:1, by the molybdenum powder after screening and tantalum powder according to the quality of 90 ~ 94:6 ~ 10 than ball milling more than mixing 16h, prepared molybdenum tantalum mixed powder, standby；
Step 2, target size according to required pressed compact, weigh the quality or volume that form the molybdenum tantalum mixed powder needed for a pressed compact, and manufacture molding cavity and the molybdenum isopyknic cold isostatic mould of tantalum mixed powder, utilizing powder feeder to make molybdenum tantalum mixed powder freely fall in the molding cavity of cold isostatic mould, isostatic cool pressing process conditions are: pressurize 5 ~ 10min under 150 ~ 200MPa；A sequence pressed compact is obtained through processing, standby；
Step 3, the demoulding, take out a sequence pressed compact, is placed in body of heater by a sequence pressed compact, is warming up to 2150 ~ 2200 DEG C with the heating rate of 30 ~ 40 DEG C/min, and after being incubated 8 ~ 9h at such a temperature, naturally cools to room temperature with stove, takes out base substrate, standby；
Step 4, base substrate is placed in straight die is smoothed after, base substrate is placed in sizing die and carries out shaping, standby；
Step 5, carry out hip treatment by after base substrate surface treated, obtain two sequence base substrates, standby；Wherein, heat and other static pressuring processes is: pre-burning 30min at 800 ~ 1000 DEG C, and then increasing temperature and pressure is to 1450 ~ 1500 DEG C, 180 ~ 200MPa, heat-insulation pressure keeping 1 ~ 3h；
Step 6, roll along the longitudinal direction of two sequence base substrates at 1400 DEG C, when a deflection of two sequence base substrates is 20 ~ 60%, roll along the horizontal direction of two sequence base substrates at 1200 DEG C, when the secondary deformation amount of two sequence base substrates is 70%, two sequence base substrates are incubated at 1250 DEG C 2h, standby；
Step 7, two sequence base substrates are machined out so that it is profile reaches target shape size, is connected with backboard, makes molybdenum tantalum alloy target.
Further, the preprocess method in step one is: being annealed under vacuum processing 2h by molybdenum powder and tantalum powder, annealing temperature is 1300 DEG C.
In the present invention, cold isostatic mould in step 2 includes punching block, be laid on punching block opening rubber slab and the pressing plate being laid on rubber slab, wherein, it is bolted between punching block, rubber slab and pressing plate three, and between punching block and bolt, be equipped with sealing gasket between punching block and rubber slab, the connecting portion being positioned at the punching block upper end inside bolt and rubber slab is provided with semicircular groove, be embedded with rubber seal in groove, described pressing plate be provided with between pressing plate and rubber slab inject isostatic cool pressing medium hand-hole.
Further, the interior knuckle of punching block upper end is rounding, and the thickness of rubber slab is 5 ~ 10mm, and the thickness of pressing plate is 10 ~ 15mm, and the aperture of hand-hole is 10mm.
Further, the technique that billet surface in step 5 processes is: molybdenum powder and tantalum powder are milled to 100 ~ 200nm respectively, after mixing, become powder to starch compound water disperse, utilizing thermal spraying by slip coating to billet surface, the coating layer thickness of billet surface is 100 ~ 300 microns.Utilize nanocrystalline molybdenum powder and tantalum powder that base substrate is carried out surface treatment, eliminate the defect of billet surface such as pore, crackle etc, improve the consistency of final products.
Further, the heat and other static pressuring processes in step 5 is: be placed at 1000 DEG C by surface treated base substrate pre-burning 30min, and then increasing temperature and pressure is to 1500 DEG C, 200MPa, heat-insulation pressure keeping 3h.
The present invention carries out crisscross rolling after the hot isostatic pressing, vertically and horizontally tissue overlap joint mutually is staggered, crystal grain arrangement is more uniformly distributed, can be effectively prevented from each to discontinuity time produce defect, and, the trend of tandem rolling crackle with roll to synchronicity little, and extensions path effective length is long, and crackle has been further expanded retardation.
Beneficial effect: 1, the present invention utilizes punching block and rubber slab combination to carry out cold isostatic compaction, by the hand-hole of setting on pressing plate at the uniform velocity injecting isostatic cool pressing medium between pressing plate and rubber slab, this mould solves sealing problem, breach the boundary between punching block and cold isostatic compaction, overcome the defect of traditional cold isostatic pressed pressed compact poor dimensional precision, the requirement of tradition steel mold pressing product can not only be reached, it is also possible to produce large-scale workpiece.
2, it is sintered after cold isostatic compaction, is warming up to 2150 ~ 2200 DEG C with the heating rate of 30 ~ 40 DEG C/min, it is possible to the mobility making crystal grain is best, is not easily formed bubble and segregation defects；The collocation of this temperature and heating rate, it is to avoid base substrate occurs rolling the problem split in follow-up machining process；And, it is able to verify that by experiment, exceedes this temperature range, be easily caused the situation that green body edge is chapped.Before blank sintering, the molybdenum powder of crystalline state nanometer and tantalum powder thermal jet are coated onto its surface, are distributed with disperse state, improve the crack resistance of product；The present invention adopts the mode that isostatic cool pressing, sintering and hip treatment combine, and molybdenum tantalum powder is processed, and the dislocation density making interiors of products is high, and dislocation is mutually handed over and cut formation jog, improves intensity and the hardness of product.The crystallite dimension of the target produced is less than 50 microns, and the change of grain size maintains within 20%, and on target plane direction and thickness direction, crystal grain is and is uniformly distributed；The relative density > 97% of target；Furthermore, it is possible to produce the large-size sputtering target material of about length 2m, width about 1.3m.
3, the present invention is before hip treatment, utilizes the mode of isostatic cool pressing and sintering to process, and contributes to the diffusion in sintering process of the molybdenum tantalum powder granule, flowing, shortens the sintering period, additionally it is possible in effective suppression target, crystallite dimension grows up.Base substrate after sintering is carried out hip treatment, and owing at high temperature carrying out pressure sintering with gas such as Ar as pressure medium, target is not easily reduced.Hot isostatic pressing of the present invention is without using jacket, process through preamble, obtain heterogeneous microstructure uniform, isotropic, through high temperature insostatic pressing (HIP) and rolling, pore and defect within blank are compacted, and eliminate internal porosity, and make crystal grain uniform, isotropism is good, and the relative density after rolling is close to more than the 99% of theoretical value.Meanwhile, hip moulding makes the fibrous tissue of the base substrate through isostatic cool pressing formation be again off, and crystallization again, it is to avoid the situation that organizational hierarchy, crystal grain skewness and grain size are uneven occur, the even tissue obtained is tiny, crystallite dimension is less than 50 microns.
Accompanying drawing explanation
Fig. 1 is the cold isostatic mould in the present invention.
Accompanying drawing labelling: 1, punching block, 2, rubber slab, 3, pressing plate, 4, bolt, 5, groove, 6, hand-hole.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, so that those skilled in the art can be better understood from the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
The preparation method of large scale, carefully brilliant molybdenum tantalum alloy-sputtering targets material, comprise the following steps: step one, molybdenum powder and tantalum powder are carried out pretreatment after sieve respectively, after screening, the ratio of the Fisher particle size of tantalum powder and molybdenum powder is 1.6:1, by the molybdenum powder after screening and tantalum powder according to the quality of 90 ~ 94:6 ~ 10 than ball milling more than mixing 16h, prepare molybdenum tantalum mixed powder, standby；
Step 2, target size according to required pressed compact, weigh the quality or volume that form the molybdenum tantalum mixed powder needed for a pressed compact, and manufacture molding cavity and the molybdenum isopyknic cold isostatic mould of tantalum mixed powder, utilizing powder feeder to make molybdenum tantalum mixed powder freely fall in the molding cavity of cold isostatic mould, isostatic cool pressing process conditions are: pressurize 5 ~ 10min under 150 ~ 200MPa；A sequence pressed compact is obtained through processing, standby；
Step 3, the demoulding, take out a sequence pressed compact, is placed in body of heater by a sequence pressed compact, is warming up to 2150 ~ 2200 DEG C with the heating rate of 30 ~ 40 DEG C/min, and after being incubated 8 ~ 9h at such a temperature, naturally cools to room temperature with stove, takes out base substrate, standby；
Step 4, base substrate is placed in straight die is smoothed after, base substrate is placed in sizing die and carries out shaping, standby；
Step 5, carry out hip treatment by after base substrate surface treated, obtain two sequence base substrates, standby；Wherein, heat and other static pressuring processes is: pre-burning 30min at 800 ~ 1000 DEG C, and then increasing temperature and pressure is to 1450 ~ 1500 DEG C, 180 ~ 200MPa, heat-insulation pressure keeping 1 ~ 3h；
Step 6, roll along the longitudinal direction of two sequence base substrates at 1400 DEG C, when a deflection of two sequence base substrates is 20 ~ 60%, roll along the horizontal direction of two sequence base substrates at 1200 DEG C, when the secondary deformation amount of two sequence base substrates is 70%, two sequence base substrates are incubated at 1250 DEG C 2h, standby；
Step 7, two sequence base substrates are machined out so that it is profile reaches target shape size, is connected with backboard, makes molybdenum tantalum alloy target.
Wherein, cold isostatic mould in step 2 is as shown in Figure 1, including punching block 1, the rubber slab 2 being laid on punching block 1 opening and the pressing plate 3 being laid on rubber slab 2, wherein, punching block 1, connected by bolt 4 between rubber slab 2 and pressing plate 3 three, and between punching block 1 and bolt 4, it is equipped with sealing gasket between punching block 1 and rubber slab 2, the connecting portion being positioned at punching block 1 upper end inside bolt 4 and rubber slab 2 is provided with semicircular groove 5, it is embedded with rubber seal in groove 5, described pressing plate 3 be provided with between pressing plate 3 and rubber slab 2 inject isostatic cool pressing medium hand-hole 6；The interior knuckle of punching block 1 upper end is rounding, and the thickness of rubber slab 2 is 5 ~ 10mm, and the thickness of pressing plate 3 is 10 ~ 15mm, and the aperture of hand-hole 6 is 10mm.
Embodiment 1
The preparation method of large scale, carefully brilliant molybdenum tantalum alloy-sputtering targets material, comprise the following steps: step one, molybdenum powder and tantalum powder are carried out pretreatment after sieve respectively, after screening, the Fisher particle size of tantalum powder is 9.6 microns, the Fisher particle size of molybdenum powder is 6 microns, by the molybdenum powder after screening and tantalum powder according to the quality of 94:6 than ball milling mixing 16h, prepare molybdenum tantalum mixed powder, standby；Wherein, preprocess method is: being annealed under vacuum processing 2h by molybdenum powder and tantalum powder, annealing temperature is 1300 DEG C.
Step 2, target size according to required pressed compact, weigh the quality or volume that form the molybdenum tantalum mixed powder needed for a pressed compact, and manufacture molding cavity and the molybdenum isopyknic cold isostatic mould of tantalum mixed powder, utilizing powder feeder to make molybdenum tantalum mixed powder freely fall in the molding cavity of cold isostatic mould, isostatic cool pressing process conditions are: pressurize 5min under 200MPa；A sequence pressed compact is obtained through processing, standby；
Step 3, the demoulding, take out a sequence pressed compact, is placed in body of heater by a sequence pressed compact, is warming up to 2165 DEG C with the heating rate of 40 DEG C/min, and at such a temperature after insulation 8.5h, naturally cool to room temperature with stove, take out base substrate, standby；
Step 4, base substrate is placed in straight die is smoothed after, base substrate is placed in sizing die and carries out shaping, standby；
Step 5, carry out hip treatment by after base substrate surface treated, obtain two sequence base substrates, standby；Wherein, heat and other static pressuring processes is: pre-burning 30min at 1000 DEG C, and then increasing temperature and pressure is to 1450 DEG C, 19MPa, heat-insulation pressure keeping 3h；Wherein, the technique that billet surface processes is: molybdenum powder and tantalum powder being milled to 100nm respectively, after mixing, becomes powder to starch compound water disperse, utilize thermal spraying by slip coating to billet surface, the coating layer thickness of billet surface is 100 microns.
Step 6, roll along the longitudinal direction of two sequence base substrates at 1400 DEG C, when a deflection of two sequence base substrates is 60%, roll along the horizontal direction of two sequence base substrates at 1200 DEG C, when the secondary deformation amount of two sequence base substrates is 70%, two sequence base substrates are incubated at 1250 DEG C 2h, standby；
Step 7, two sequence base substrates are machined out so that it is profile reaches target shape size, is connected with backboard, makes molybdenum tantalum alloy target.
Embodiment 2
The preparation method of large scale, carefully brilliant molybdenum tantalum alloy-sputtering targets material, comprise the following steps: step one, molybdenum powder and tantalum powder are carried out pretreatment after sieve respectively, after screening, the Fisher particle size of tantalum powder is 16 microns, the Fisher particle size of molybdenum powder is 10 microns, by the molybdenum powder after screening and tantalum powder according to the quality of 90:10 than ball milling mixing 20h, prepare molybdenum tantalum mixed powder, standby；Preprocess method therein is: being annealed under vacuum processing 2h by molybdenum powder and tantalum powder, annealing temperature is 1300 DEG C.
Step 2, target size according to required pressed compact, weigh the quality or volume that form the molybdenum tantalum mixed powder needed for a pressed compact, and manufacture molding cavity and the molybdenum isopyknic cold isostatic mould of tantalum mixed powder, powder feeder is utilized to make molybdenum tantalum mixed powder freely fall in the molding cavity of cold isostatic mould, smear glycerol or ethanol at molding cavity outer wall, isostatic cool pressing process conditions are: pressurize 8min under 170MPa；A sequence pressed compact is obtained through processing, standby；
Step 3, the demoulding, take out a sequence pressed compact, is placed in body of heater by a sequence pressed compact, is warming up to 2150 DEG C with the heating rate of 36 DEG C/min, and at such a temperature after insulation 9h, naturally cool to room temperature with stove, take out base substrate, standby；
Step 4, base substrate is placed in straight die is smoothed after, base substrate is placed in sizing die and carries out shaping, standby；
Step 5, being placed at 1000 DEG C by base substrate surface treated pre-burning 30min, then increasing temperature and pressure is to 1500 DEG C, 200MPa, heat-insulation pressure keeping 3h, obtains two sequence base substrates, standby；The technique that billet surface therein processes is: molybdenum powder and tantalum powder being milled to 200nm respectively, after mixing, becomes powder to starch compound water disperse, utilize thermal spraying by slip coating to billet surface, the coating layer thickness of billet surface is 200 microns.
Step 6, roll along the longitudinal direction of two sequence base substrates at 1400 DEG C, when a deflection of two sequence base substrates is 20%, roll along the horizontal direction of two sequence base substrates at 1200 DEG C, when the secondary deformation amount of two sequence base substrates is 70%, two sequence base substrates are incubated at 1250 DEG C 2h, standby；
Step 7, two sequence base substrates are machined out so that it is profile reaches target shape size, is connected with backboard, makes molybdenum tantalum alloy target.
Embodiment 3
The preparation method of large scale, carefully brilliant molybdenum tantalum alloy-sputtering targets material, comprise the following steps: step one, molybdenum powder and tantalum powder are carried out pretreatment after sieve respectively, after screening, the Fisher particle size of tantalum powder is 24 microns, the Fisher particle size of molybdenum powder is 15 microns, by the molybdenum powder after screening and tantalum powder according to the quality of 92:8 than ball milling mixing 25h, prepare molybdenum tantalum mixed powder, standby；Preprocess method therein is: being annealed under vacuum processing 2h by molybdenum powder and tantalum powder, annealing temperature is 1300 DEG C.
Step 2, target size according to required pressed compact, weigh the quality or volume that form the molybdenum tantalum mixed powder needed for a pressed compact, and manufacture molding cavity and the molybdenum isopyknic cold isostatic mould of tantalum mixed powder, utilizing powder feeder to make molybdenum tantalum mixed powder freely fall in the molding cavity of cold isostatic mould, isostatic cool pressing process conditions are: pressurize 10min under 150MPa；A sequence pressed compact is obtained through processing, standby；
Step 3, the demoulding, take out a sequence pressed compact, is placed in body of heater by a sequence pressed compact, is warming up to 2200 DEG C with the heating rate of 30 DEG C/min, and at such a temperature after insulation 8h, naturally cool to room temperature with stove, take out base substrate, standby；
Step 4, base substrate is placed in straight die is smoothed after, base substrate is placed in sizing die and carries out shaping, standby；
Step 5, carry out hip treatment by after base substrate surface treated, obtain two sequence base substrates, standby；Wherein, heat and other static pressuring processes is: pre-burning 30min at 800 DEG C, and then increasing temperature and pressure is to 1470 DEG C, 180MPa, heat-insulation pressure keeping 1h；The technique that billet surface therein processes is: molybdenum powder and tantalum powder being milled to 160nm respectively, after mixing, becomes powder to starch compound water disperse, utilize thermal spraying by slip coating to billet surface, the coating layer thickness of billet surface is 300 microns.
Step 6, roll along the longitudinal direction of two sequence base substrates at 1400 DEG C, when a deflection of two sequence base substrates is 45%, roll along the horizontal direction of two sequence base substrates at 1200 DEG C, when the secondary deformation amount of two sequence base substrates is 70%, two sequence base substrates are incubated at 1250 DEG C 2h, standby；
Step 7, two sequence base substrates are machined out so that it is profile reaches target shape size, is connected with backboard, makes molybdenum tantalum alloy target.
Sputtering target material relative density prepared by the present invention is higher, and in use, the target surface of target is not likely to produce dross in sputter procedure, and effectively inhibits arcing phenomena, reduces the probability that in the thin film of molding, impurity defect occurs.And in the target of high density target, do not have a large amount of cavity, and then ensure purity and the homogeneity of ingredients of thin film in sputter procedure.
Claims (6)
1. the preparation method of large scale, thin brilliant molybdenum tantalum alloy-sputtering targets material, it is characterised in that comprise the following steps:
Step one, molybdenum powder and tantalum powder are carried out pretreatment after sieve respectively, after screening, the ratio of the Fisher particle size of tantalum powder and molybdenum powder is 1.6:1, by the molybdenum powder after screening and tantalum powder according to the quality of 90 ~ 94:6 ~ 10 than ball milling more than mixing 16h, prepared molybdenum tantalum mixed powder, standby；
Step 2, target size according to required pressed compact, weigh the quality or volume that form the molybdenum tantalum mixed powder needed for a pressed compact, and manufacture molding cavity and the molybdenum isopyknic cold isostatic mould of tantalum mixed powder, utilizing powder feeder to make molybdenum tantalum mixed powder freely fall in the molding cavity of cold isostatic mould, isostatic cool pressing process conditions are: pressurize 5 ~ 10min under 150 ~ 200MPa；A sequence pressed compact is obtained through processing, standby；
Step 3, the demoulding, take out a sequence pressed compact, is placed in body of heater by a sequence pressed compact, is warming up to 2150 ~ 2200 DEG C with the heating rate of 30 ~ 40 DEG C/min, and after being incubated 8 ~ 9h at such a temperature, naturally cools to room temperature with stove, takes out base substrate, standby；
Step 4, base substrate is placed in straight die is smoothed after, base substrate is placed in sizing die and carries out shaping, standby；
Step 5, carry out hip treatment by after base substrate surface treated, obtain two sequence base substrates, standby；Wherein, heat and other static pressuring processes is: pre-burning 30min at 800 ~ 1000 DEG C, and then increasing temperature and pressure is to 1450 ~ 1500 DEG C, 180 ~ 200MPa, heat-insulation pressure keeping 1 ~ 3h；
Step 6, roll along the longitudinal direction of two sequence base substrates at 1400 DEG C, when a deflection of two sequence base substrates is 20 ~ 60%, roll along the horizontal direction of two sequence base substrates at 1200 DEG C, when the secondary deformation amount of two sequence base substrates is 70%, two sequence base substrates are incubated at 1250 DEG C 2h, standby；
Step 7, two sequence base substrates are machined out so that it is profile reaches target shape size, is connected with backboard, makes molybdenum tantalum alloy target.
2. the preparation method of large scale according to claim 1, thin brilliant molybdenum tantalum alloy-sputtering targets material, it is characterised in that: the preprocess method in step one is: being annealed under vacuum processing 2h by molybdenum powder and tantalum powder, annealing temperature is 1300 DEG C.
3. large scale according to claim 1, the preparation method of thin brilliant molybdenum tantalum alloy-sputtering targets material, it is characterized in that: the cold isostatic mould in step 2 includes punching block (1), the rubber slab (2) being laid on punching block (1) opening and the pressing plate (3) being laid on rubber slab (2), wherein, punching block (1), connected by bolt (4) between rubber slab (2) and pressing plate (3) three, and between punching block (1) and bolt (4), it is equipped with sealing gasket between punching block (1) and rubber slab (2), the connecting portion of punching block (1) upper end and rubber slab (2) that are positioned at bolt (4) inner side is provided with semicircular groove (5), groove is embedded with rubber seal in (5), described pressing plate (3) be provided with between pressing plate (3) and rubber slab (2) inject isostatic cool pressing medium hand-hole (6).
4. the preparation method of large scale according to claim 3, thin brilliant molybdenum tantalum alloy-sputtering targets material, it is characterized in that: the interior knuckle of punching block (1) upper end is rounding, the thickness of rubber slab (2) is 5 ~ 10mm, and the thickness of pressing plate (3) is 10 ~ 15mm, and the aperture of hand-hole (6) is 10mm.
5. the preparation method of large scale according to claim 1, thin brilliant molybdenum tantalum alloy-sputtering targets material, it is characterized in that: the technique that the billet surface in step 5 processes is: molybdenum powder and tantalum powder are milled to 100 ~ 200nm respectively, after mixing, powder is become to starch compound water disperse, utilizing thermal spraying by slip coating to billet surface, the coating layer thickness of billet surface is 100 ~ 300 microns.
6. the preparation method of large scale according to claim 1, thin brilliant molybdenum tantalum alloy-sputtering targets material, it is characterized in that: the heat and other static pressuring processes in step 5 is: be placed at 1000 DEG C by surface treated base substrate pre-burning 30min, then increasing temperature and pressure is to 1500 DEG C, 200MPa, heat-insulation pressure keeping 3h.
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| CN110538993A (en) * | 2019-10-18 | 2019-12-06 | 洛阳高新四丰电子材料有限公司 | preparation process of high-density molybdenum-tantalum alloy sputtering target material |
| CN111390164A (en) * | 2020-04-22 | 2020-07-10 | 宁波江丰钨钼材料有限公司 | Die filling method of large-size molybdenum target blank |
| CN114029484A (en) * | 2021-11-08 | 2022-02-11 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum-titanium alloy target material |
| CN114029484B (en) * | 2021-11-08 | 2023-09-12 | 宁波江丰电子材料股份有限公司 | Preparation method of tantalum-titanium alloy target |
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