CN105714253B - The preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material - Google Patents
The preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material Download PDFInfo
- Publication number
- CN105714253B CN105714253B CN201610133824.5A CN201610133824A CN105714253B CN 105714253 B CN105714253 B CN 105714253B CN 201610133824 A CN201610133824 A CN 201610133824A CN 105714253 B CN105714253 B CN 105714253B
- Authority
- CN
- China
- Prior art keywords
- powder
- molybdenum
- tantalum
- sequence
- standby
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- JZLMRQMUNCKZTP-UHFFFAOYSA-N molybdenum tantalum Chemical compound [Mo].[Ta] JZLMRQMUNCKZTP-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000005477 sputtering target Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000004080 punching Methods 0.000 claims abstract description 23
- 238000007493 shaping process Methods 0.000 claims abstract description 8
- 239000013077 target material Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims description 75
- 238000003825 pressing Methods 0.000 claims description 36
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 32
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 29
- 239000011812 mixed powder Substances 0.000 claims description 19
- 235000013339 cereals Nutrition 0.000 claims description 17
- 238000009413 insulation Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 13
- 238000012216 screening Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 238000000137 annealing Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000465 moulding 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
- 238000004513 sizing Methods 0.000 claims description 6
- 230000003068 static effect Effects 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000002002 slurry 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
- 235000007164 Oryza sativa Nutrition 0.000 claims description 4
- 239000011247 coating layer Substances 0.000 claims description 4
- 235000009566 rice Nutrition 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 7
- 238000005096 rolling process Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005056 compaction Methods 0.000 abstract description 4
- 238000009499 grossing Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 7
- 229910001362 Ta alloys Inorganic materials 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- 241000209094 Oryza Species 0.000 description 3
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 235000011187 glycerol Nutrition 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
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000012528 membrane Substances 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
- 239000002345 surface coating layer Substances 0.000 description 1
- 239000010409 thin film Substances 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
Abstract
The preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material, the step of the step of combining the step of carrying out cold isostatic compaction, sintering using punching block and rubber slab, smoothing shaping, hip treatment the step of, rolling the step of, mach step.The crystallite dimension for the target produced is less than 50 microns, and the change of grain size is maintained within 20%, and on target plane direction and thickness direction, crystal grain is to be uniformly distributed；The relative density ＞ 97% of target；Furthermore, it is possible to production length 2m or so, width 1.3m or so large-size sputtering target material.
Description
Technical field
The present invention relates to target technical field, and in particular to the preparation of a kind of large scale, fine grain molybdenum tantalum alloy-sputtering targets material
Method.
Background technology
Sputtering is to prepare one of major technique of thin-film material.With the Ions Bombardment surface of solids of acceleration, ion and solid
Surface atom exchanges momentum, the atom of the surface of solids is left solid and is deposited on substrate surface, and this process is referred to as sputtering.Quilt
The solid of bombardment is the source material with sputtering method deposition film, commonly referred to as target.
The film consistency deposited with target as sputter is high, and the tack between base material is good.Sputtered film material no matter
Semiconductor integrated circuit, recording medium, plane are shown and surface coating etc. is obtained for and is widely applied.Cause
This, to sputtering target material, there is the functional material demand of high added value to increase year by year for this.In recent years, China's electronics and information industry flies
Speed development, integrated circuit, CD and display production line have a large amount of joint or Sole Proprietorships to occur, and China has been increasingly becoming
One of greatest requirements area of film target in the world.But so far, professional grand duke of the China still without special production target
Department, 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 utilizes Rolling Production.
During using powder metallurgy forming, i.e., tied up after after molybdenum powder progress isostatic cool pressing processing, being sintered, roll, machining with backboard
Fixed, manufactured target is during sputter coating, when sputtering target is bombarded, because existing gas is dashed forward in target internal void
So release, large-sized target particle or particulate is caused to splash, or membrane material is caused particulate to fly by secondary electron bombardment after film forming
Splash.Because the hysteresis of domestic target industry develops, current Chinese target market significant portion is captured by offshore company.With micro- electricity
The high speed development of the high-tech industries such as son, Chinese target market will expand day by day, and be provided for the manufacturing development of Chinese target
Opportunities and challenges.
The content of the invention
It is an object of the invention to provide a kind of crystal grain is tiny, the sputtering of relative density ＞ 97% large scale, fine grain molybdenum tantalum alloy
The preparation method of target.
The used to achieve the above object technical scheme of the present invention is：Large scale, fine grain molybdenum tantalum alloy-sputtering targets material
Preparation method, comprise the following steps：
Step 1: sieved respectively after molybdenum powder and tantalum powder are pre-processed, the Fei Shi grains of tantalum powder and molybdenum powder after screening
The ratio between degree is 1.6：1, by the molybdenum powder after screening and tantalum powder according to 90 ~ 94：6 ~ 10 quality is made than more than ball milling mixing 16h
Molybdenum tantalum mixed powder, it is standby；
Step 2: according to the target size of required pressed compact, the matter to form the molybdenum tantalum mixed powder needed for a pressed compact is weighed
Amount or volume, and inner chamber and the isometric cold isostatic mould of molybdenum tantalum mixed powder are manufactured, mix molybdenum tantalum using powder feeder
Close powder to freely fall into the molding cavity of cold isostatic mould, isostatic cool pressing process conditions are：The pressurize 5 under 150 ~ 200MPa
~10min；A sequence pressed compact is obtained by processing, it is standby；
Step 3: the demoulding, takes out a sequence pressed compact, a sequence pressed compact is placed in body of heater, with 30 ~ 40 DEG C/min heating rate
2150 ~ 2200 DEG C are warming up to, and naturally cools to room temperature with stove after 8 ~ 9h of insulation at such a temperature, takes out base substrate, it is standby；
Step 4: after base substrate is placed in straight die is smoothed, base substrate is placed in sizing die and carries out shaping, it is standby；
Step 5: hip treatment will be carried out after base substrate surface treated, two sequence base substrates are obtained, it is standby；Wherein, heat etc.
Static pressure technique is：Pre-burning 30min at 800 ~ 1000 DEG C, then increasing temperature and pressure to 1450 ~ 1500 DEG C, 180 ~ 200MPa, insulation are protected
Press 1 ~ 3h；
Step 6: the longitudinal direction in 1400 DEG C of sequence base substrates of lower edge two is rolled, when a deflection of two sequence base substrates
For 20 ~ 60% when, rolled in the horizontal direction of 1200 DEG C of sequence base substrates of lower edge two, when two sequence base substrates secondary deformation amount be 70%
When, two sequence base substrates are incubated 2h at 1250 DEG C, it is standby；
Step 7: being machined out to two sequence base substrates, its profile is reached target shape size, be connected with backboard, is made
Molybdenum tantalum alloy target.
Further, the preprocess method in step 1 is：Molybdenum powder and tantalum powder are made annealing treatment under vacuum
2h, annealing temperature are 1300 DEG C.
In the present invention, cold isostatic mould in step 2 include punching block, be laid on the rubber slab of punching block opening with
And the pressing plate on rubber slab is laid in, wherein, it is bolted between punching block, rubber slab and pressing plate three, and punching block and spiral shell
Sealing gasket is equipped between bolt, between punching block and rubber slab, the connecting portion of punching block upper end and rubber slab on the inside of bolt
Provided with semicircular groove, be embedded with rubber seal in groove, described pressing plate be provided be used for pressing plate and rubber slab it
Between 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, the aperture of hand-hole is 10mm.
Further, the technique of the billet surface processing in step 5 is：Molybdenum powder and tantalum powder are milled to 100 respectively ~
200nm, after mixing, by compound with water disperse into slurry, using thermal spraying by slip coating to billet surface, billet surface
Coating layer thickness is 100 ~ 300 microns.Base substrate is surface-treated using nanocrystalline molybdenum powder and tantalum powder, it is all to eliminate billet surface
Such as the defects of stomata, crackle etc, the consistency of final products is improved.
Further, the heat and other static pressuring processes in step 5 are：Surface treated base substrate is placed at 1000 DEG C in advance
30min is burnt, then increasing temperature and pressure to 1500 DEG C, 200MPa, heat-insulation pressure keeping 3h.
The present invention carries out crisscross rolling after the hot isostatic pressing, and vertically and horizontally tissue mutually overlap joint interlocks, crystal grain row
Cloth is more uniformly distributed, can be effectively prevented from it is each to discontinuity when produce defect, moreover, the trend of tandem rolling crackle and roll to
Synchronism it is small, and extensions path effective length grow, retardation has been further expanded to crackle.
Beneficial effect：1st, the present invention is combined using punching block and rubber slab and carries out cold isostatic compaction, by being set on pressing plate
Hand-hole to isostatic cool pressing medium is at the uniform velocity injected between pressing plate and rubber slab, the mould solves sealing problem, breaches steel
Boundary between mould and cold isostatic compaction, the defects of overcoming traditional isostatic cool pressing pressed compact poor dimensional precision, it can not only reach
The requirement of traditional steel mold pressing product, can also produce large-scale workpiece.
2nd, it is sintered after cold isostatic compaction, is warming up to 2150 ~ 2200 DEG C with 30 ~ 40 DEG C/min heating rate, energy
Enough make the mobility of crystal grain optimal, be not easy to form bubble and segregation defects；The collocation of the temperature and heating rate, avoids base substrate
Occur rolling the problem of splitting in follow-up machining process；Moreover, being able to verify that by experiment, more than the temperature range, it is easily caused
The situation of green body edge chap.Before blank sintering, the molybdenum powder of crystalline state nanometer and tantalum powder thermal jet are coated onto its surface, with disperse shape
State is distributed, and improves the crack resistance of product；The present invention by the way of isostatic cool pressing, sintering and hip treatment are combined,
Molybdenum tantalum powder is handled, makes the dislocation density of interiors of products high, dislocation mutually hands over section shape into jog, improve product intensity and
Hardness.The crystallite dimension for the target produced is less than 50 microns, and the change of grain size is maintained within 20%, is put down in target
On face direction and thickness direction, crystal grain is to be uniformly distributed；The relative density ＞ 97% of target；Furthermore, it is possible to production length 2m is left
Right, width 1.3m or so large-size sputtering target material.
3rd, the present invention is handled using the mode of isostatic cool pressing and sintering before hip treatment, contributes to molybdenum
Diffusion, flowing of the tantalum powder particle in sintering process, shorten the sintering period, additionally it is possible to effectively suppress crystallite dimension in target
Grow up.Base substrate after sintering is subjected to hip treatment, due to being carried out at high temperature by the use of gas such as Ar as pressure medium
Pressure sintering, target are not easy to be reduced.Hot isostatic pressing of the present invention is handled through preamble, obtained uniformly without using jacket
, isotropic heterogeneous microstructure, through high temperature insostatic pressing (HIP) and rolling, stomata and defect inside blank are compacted, and are eliminated
Internal porosity, and make crystal grain uniform, isotropism is good, the relative density after rolling close to theoretical value more than 99%.Meanwhile heat
The fibr tissue for the base substrate that isostatic pressing makes to be formed by isostatic cool pressing is again off, and is recrystallized, and avoids the occurrence of tissue point
The situation that layer, crystal grain distribution are uneven and grain size is uneven, obtained even tissue is tiny, and crystallite dimension is less than 50 microns.
Brief description of the drawings
Fig. 1 is the cold isostatic mould in the present invention.
Reference：1st, punching block, 2, rubber slab, 3, pressing plate, 4, bolt, 5, groove, 6, hand-hole.
Embodiment
With reference to specific embodiment, the invention will be further described, so that those skilled in the art can be more preferable
Understand the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
The preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material, comprises the following steps：Step 1: by molybdenum powder and tantalum
Powder is sieved respectively after being pre-processed, and the ratio between tantalum powder and the Fisher particle size of molybdenum powder are 1.6 after screening：1, by the molybdenum after screening
Powder and tantalum powder are according to 90 ~ 94：6 ~ 10 quality is more standby than more than ball milling mixing 16h, obtained molybdenum tantalum mixed powder；
Step 2: according to the target size of required pressed compact, the matter to form the molybdenum tantalum mixed powder needed for a pressed compact is weighed
Amount or volume, and inner chamber and the isometric cold isostatic mould of molybdenum tantalum mixed powder are manufactured, mix molybdenum tantalum using powder feeder
Close powder to freely fall into the molding cavity of cold isostatic mould, isostatic cool pressing process conditions are：The pressurize 5 under 150 ~ 200MPa
~10min；A sequence pressed compact is obtained by processing, it is standby；
Step 3: the demoulding, takes out a sequence pressed compact, a sequence pressed compact is placed in body of heater, with 30 ~ 40 DEG C/min heating rate
2150 ~ 2200 DEG C are warming up to, and naturally cools to room temperature with stove after 8 ~ 9h of insulation at such a temperature, takes out base substrate, it is standby；
Step 4: after base substrate is placed in straight die is smoothed, base substrate is placed in sizing die and carries out shaping, it is standby；
Step 5: hip treatment will be carried out after base substrate surface treated, two sequence base substrates are obtained, it is standby；Wherein, heat etc.
Static pressure technique is：Pre-burning 30min at 800 ~ 1000 DEG C, then increasing temperature and pressure to 1450 ~ 1500 DEG C, 180 ~ 200MPa, insulation are protected
Press 1 ~ 3h；
Step 6: the longitudinal direction in 1400 DEG C of sequence base substrates of lower edge two is rolled, when a deflection of two sequence base substrates
For 20 ~ 60% when, rolled in the horizontal direction of 1200 DEG C of sequence base substrates of lower edge two, when two sequence base substrates secondary deformation amount be 70%
When, two sequence base substrates are incubated 2h at 1250 DEG C, it is standby；
Step 7: being machined out to two sequence base substrates, its profile is reached target shape size, be connected with backboard, is made
Molybdenum tantalum alloy target.
Wherein, the cold isostatic mould in step 2 is as shown in figure 1, including punching block 1, be laid on the opening of punching block 1
Rubber slab 2 and the pressing plate 3 being laid on rubber slab 2, wherein, pass through bolt 4 between punching block 1, rubber slab 2 and the three of pressing plate 3
Connection, and sealing gasket is equipped between punching block 1 and bolt 4, between punching block 1 and rubber slab 2, on the punching block 1 of the inner side of bolt 4
End is provided with semicircular groove 5 with the connecting portion of rubber slab 2, is embedded with rubber seal in groove 5, on described pressing plate 3
Provided between pressing plate 3 and rubber slab 2 inject isostatic cool pressing medium hand-hole 6；The interior knuckle of the upper end of punching block 1 is rounding
Angle, 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, fine grain molybdenum tantalum alloy-sputtering targets material, comprises the following steps：Step 1: by molybdenum powder and tantalum
Powder is sieved respectively after being pre-processed, and the Fisher particle size of tantalum powder is 9.6 microns after screening, and the Fisher particle size of molybdenum powder is micro- for 6
Rice, by the molybdenum powder after screening and tantalum powder according to 94：6 quality is more standby than ball milling mixing 16h, obtained molybdenum tantalum mixed powder；Its
In, preprocess method is：Molybdenum powder and tantalum powder are subjected to annealing 2h under vacuum, annealing temperature is 1300 DEG C.
Step 2: according to the target size of required pressed compact, the matter to form the molybdenum tantalum mixed powder needed for a pressed compact is weighed
Amount or volume, and inner chamber and the isometric cold isostatic mould of molybdenum tantalum mixed powder are manufactured, mix molybdenum tantalum using powder feeder
Close powder to freely fall into the molding cavity of cold isostatic mould, isostatic cool pressing process conditions are：The pressurize 5min under 200MPa；
A sequence pressed compact is obtained by processing, it is standby；
Step 3: the demoulding, takes out a sequence pressed compact, a sequence pressed compact is placed in body of heater, with 40 DEG C/min heating rate liter
Temperature naturally cools to room temperature after insulation 8.5h with stove at such a temperature to 2165 DEG C, takes out base substrate, standby；
Step 4: after base substrate is placed in straight die is smoothed, base substrate is placed in sizing die and carries out shaping, it is standby；
Step 5: hip treatment will be carried out after base substrate surface treated, two sequence base substrates are obtained, it is standby；Wherein, heat etc.
Static pressure technique is：Pre-burning 30min at 1000 DEG C, then increasing temperature and pressure to 1450 DEG C, 190MPa, heat-insulation pressure keeping 3h；Wherein, base substrate
The technique of surface treatment is：Molybdenum powder and tantalum powder are milled to 100nm respectively, it is sharp by compound with water disperse into slurry after mixing
With thermal spraying by slip coating to billet surface, the coating layer thickness of billet surface is 100 microns.
Step 6: the longitudinal direction in 1400 DEG C of sequence base substrates of lower edge two is rolled, when a deflection of two sequence base substrates
For 60% when, rolled in the horizontal direction of 1200 DEG C of sequence base substrates of lower edge two, when two sequence base substrates secondary deformation amount be 70% when,
Two sequence base substrates are incubated 2h at 1250 DEG C, it is standby；
Step 7: being machined out to two sequence base substrates, its profile is reached target shape size, be connected with backboard, is made
Molybdenum tantalum alloy target.
Embodiment 2
The preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material, comprises the following steps：Step 1: by molybdenum powder and tantalum
Powder is sieved respectively after being pre-processed, and the Fisher particle size of tantalum powder is 16 microns after screening, and the Fisher particle size of molybdenum powder is micro- for 10
Rice, by the molybdenum powder after screening and tantalum powder according to 90：10 quality is more standby than ball milling mixing 20h, obtained molybdenum tantalum mixed powder；Its
In preprocess method be：Molybdenum powder and tantalum powder are subjected to annealing 2h under vacuum, annealing temperature is 1300 DEG C.
Step 2: according to the target size of required pressed compact, the matter to form the molybdenum tantalum mixed powder needed for a pressed compact is weighed
Amount or volume, and inner chamber and the isometric cold isostatic mould of molybdenum tantalum mixed powder are manufactured, mix molybdenum tantalum using powder feeder
Close powder to freely fall into the molding cavity of cold isostatic mould, glycerine or alcohol, isostatic cool pressing are smeared in molding cavity outer wall
Process conditions are：The pressurize 8min under 170MPa；A sequence pressed compact is obtained by processing, it is standby；
Step 3: the demoulding, takes out a sequence pressed compact, a sequence pressed compact is placed in body of heater, with 36 DEG C/min heating rate liter
Temperature naturally cools to room temperature after insulation 9h with stove at such a temperature to 2150 DEG C, takes out base substrate, standby；
Step 4: after base substrate is placed in straight die is smoothed, base substrate is placed in sizing die and carries out shaping, it is standby；
Step 5: pre-burning 30min at 1000 DEG C will be placed in after base substrate surface treated, then increasing temperature and pressure to 1500 DEG C,
200MPa, heat-insulation pressure keeping 3h, two sequence base substrates are obtained, it is standby；The technique of billet surface therein processing is：By molybdenum powder and tantalum powder point
200nm is not milled to, after mixing, by compound with water disperse into slurry, using thermal spraying by slip coating to billet surface, base
The coating layer thickness in body surface face is 200 microns.
Step 6: the longitudinal direction in 1400 DEG C of sequence base substrates of lower edge two is rolled, when a deflection of two sequence base substrates
For 20% when, rolled in the horizontal direction of 1200 DEG C of sequence base substrates of lower edge two, when two sequence base substrates secondary deformation amount be 70% when,
Two sequence base substrates are incubated 2h at 1250 DEG C, it is standby；
Step 7: being machined out to two sequence base substrates, its profile is reached target shape size, be connected with backboard, is made
Molybdenum tantalum alloy target.
Embodiment 3
The preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material, comprises the following steps：Step 1: by molybdenum powder and tantalum
Powder is sieved respectively after being pre-processed, and the Fisher particle size of tantalum powder is 24 microns after screening, and the Fisher particle size of molybdenum powder is micro- for 15
Rice, by the molybdenum powder after screening and tantalum powder according to 92：8 quality is more standby than ball milling mixing 25h, obtained molybdenum tantalum mixed powder；Wherein
Preprocess method be：Molybdenum powder and tantalum powder are subjected to annealing 2h under vacuum, annealing temperature is 1300 DEG C.
Step 2: according to the target size of required pressed compact, the matter to form the molybdenum tantalum mixed powder needed for a pressed compact is weighed
Amount or volume, and inner chamber and the isometric cold isostatic mould of molybdenum tantalum mixed powder are manufactured, mix molybdenum tantalum using powder feeder
Close powder to freely fall into the molding cavity of cold isostatic mould, isostatic cool pressing process conditions are：The pressurize under 150MPa
10min；A sequence pressed compact is obtained by processing, it is standby；
Step 3: the demoulding, takes out a sequence pressed compact, a sequence pressed compact is placed in body of heater, with 30 DEG C/min heating rate liter
Temperature naturally cools to room temperature after insulation 8h with stove at such a temperature to 2200 DEG C, takes out base substrate, standby；
Step 4: after base substrate is placed in straight die is smoothed, base substrate is placed in sizing die and carries out shaping, it is standby；
Step 5: hip treatment will be carried out after base substrate surface treated, two sequence base substrates are obtained, it is standby；Wherein, heat etc.
Static pressure technique is：Pre-burning 30min at 800 DEG C, then increasing temperature and pressure to 1470 DEG C, 180MPa, heat-insulation pressure keeping 1h；Base substrate therein
The technique of surface treatment is：Molybdenum powder and tantalum powder are milled to 160nm respectively, it is sharp by compound with water disperse into slurry after mixing
With thermal spraying by slip coating to billet surface, the coating layer thickness of billet surface is 300 microns.
Step 6: the longitudinal direction in 1400 DEG C of sequence base substrates of lower edge two is rolled, when a deflection of two sequence base substrates
For 45% when, rolled in the horizontal direction of 1200 DEG C of sequence base substrates of lower edge two, when two sequence base substrates secondary deformation amount be 70% when,
Two sequence base substrates are incubated 2h at 1250 DEG C, it is standby；
Step 7: being machined out to two sequence base substrates, its profile is reached target shape size, be connected with backboard, is made
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 in sputter procedure
Dross is not likely to produce, and effectively inhibits arcing phenomena, reduces the probability that impurity defect occurs in the film of shaping.It is and high
Be not in a large amount of cavities in the target of density target, and then ensure the purity and homogeneity of ingredients of film in sputter procedure.
Claims (6)
1. the preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material, it is characterised in that comprise the following steps：
Step 1: sieved respectively after molybdenum powder and tantalum powder are pre-processed, after screening tantalum powder and the Fisher particle size of molybdenum powder it
Than for 1.6：1, by the molybdenum powder after screening and tantalum powder according to 90 ~ 94：Molybdenum tantalum is made than more than ball milling mixing 16h in 6 ~ 10 quality
Mixed powder, it is standby；
Step 2: according to the target size of required pressed compact, weigh the quality to form the molybdenum tantalum mixed powder needed for a pressed compact or
Volume, and inner chamber and the isometric cold isostatic mould of molybdenum tantalum mixed powder are manufactured, make molybdenum tantalum mixed powder using powder feeder
Material is freely fallen into the molding cavity of cold isostatic mould, and isostatic cool pressing process conditions are：Under 150 ~ 200MPa pressurize 5 ~
10min；A sequence pressed compact is obtained by processing, it is standby；
Step 3: the demoulding, takes out a sequence pressed compact, a sequence pressed compact is placed in body of heater, heated up with 30 ~ 40 DEG C/min heating rate
To 2150 ~ 2200 DEG C, and room temperature is naturally cooled to stove after 8 ~ 9h of insulation at such a temperature, take out base substrate, it is standby；
Step 4: after base substrate is placed in straight die is smoothed, base substrate is placed in sizing die and carries out shaping, it is standby；
Step 5: hip treatment will be carried out after base substrate surface treated, two sequence base substrates are obtained, it is standby；Wherein, high temperature insostatic pressing (HIP)
Technique is：Pre-burning 30min at 800 ~ 1000 DEG C, then increasing temperature and pressure to 1450 ~ 1500 DEG C, 180 ~ 200MPa, heat-insulation pressure keeping 1 ~
3h；
Step 6: the longitudinal direction in 1400 DEG C of sequence base substrates of lower edge two is rolled, when two sequence base substrates a deflection for 20 ~
When 60%, rolled in the horizontal direction of 1200 DEG C of sequence base substrates of lower edge two, will when the secondary deformation amount of two sequence base substrates is 70%
Two sequence base substrates are incubated 2h at 1250 DEG C, standby；
Step 7: being machined out to two sequence base substrates, its profile is reached target shape size, be connected with backboard, molybdenum tantalum is made
Alloy target material.
2. the preparation method of large scale according to claim 1, fine grain molybdenum tantalum alloy-sputtering targets material, it is characterised in that：Step
Preprocess method in rapid one is：Molybdenum powder and tantalum powder are subjected to annealing 2h under vacuum, annealing temperature is 1300 DEG C.
3. the preparation method of large scale according to claim 1, fine grain molybdenum tantalum alloy-sputtering targets material, it is characterised in that：Step
Cold isostatic mould in rapid two includes punching block（1）, be laid on punching block（1）The rubber slab of opening（2）And it is laid in rubber
Offset plate（2）On pressing plate（3）, wherein, punching block（1）, rubber slab（2）And pressing plate（3）Pass through bolt between three（4）Connection, and
Punching block（1）With bolt（4）Between, punching block（1）With rubber slab（2）Between be equipped with sealing gasket, positioned at bolt（4）The punching block of inner side
（1）Upper end and rubber slab（2）Connecting portion be provided with semicircular groove（5）, groove（5）Rubber seal is inside embedded with, institute
The pressing plate stated（3）It is provided with and is used for pressing plate（3）With rubber slab（2）Between inject isostatic cool pressing medium hand-hole（6）.
4. the preparation method of large scale according to claim 3, fine grain molybdenum tantalum alloy-sputtering targets material, it is characterised in that：Steel
Mould（1）The interior knuckle of upper end is rounding, rubber slab（2）Thickness be 5 ~ 10mm, pressing plate（3）Thickness be 10 ~ 15mm, injection
Hole（6）Aperture be 10mm.
5. the preparation method of large scale according to claim 1, fine grain molybdenum tantalum alloy-sputtering targets material, it is characterised in that：Step
In rapid five billet surface processing technique be：Molybdenum powder and tantalum powder are milled to 100 ~ 200nm respectively, after mixing, by compound
It is using thermal spraying that slip coating to billet surface, the coating layer thickness of billet surface is micro- for 100 ~ 300 with water disperse into slurry
Rice.
6. the preparation method of large scale according to claim 1, fine grain molybdenum tantalum alloy-sputtering targets material, it is characterised in that：Step
Heat and other static pressuring processes in rapid five are：Surface treated base substrate is placed in pre-burning 30min at 1000 DEG C, then increasing temperature and pressure
To 1500 DEG C, 200MPa, heat-insulation pressure keeping 3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610133824.5A CN105714253B (en) | 2016-03-10 | 2016-03-10 | The preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610133824.5A CN105714253B (en) | 2016-03-10 | 2016-03-10 | The preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105714253A CN105714253A (en) | 2016-06-29 |
| CN105714253B true CN105714253B (en) | 2017-11-24 |
Family
ID=56157581
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610133824.5A Active CN105714253B (en) | 2016-03-10 | 2016-03-10 | The preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105714253B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT15356U1 (en) * | 2016-09-29 | 2017-07-15 | Plansee Se | Sputtering target |
| CN107916405B (en) * | 2017-11-23 | 2019-10-15 | 洛阳高新四丰电子材料有限公司 | A kind of preparation method of flat-panel screens molybdenum tantalum alloy-sputtering targets material |
| CN108677151B (en) * | 2018-03-28 | 2023-09-08 | 东莞市欧莱溅射靶材有限公司 | Rotary target section binding device and section binding method |
| CN108642457B (en) * | 2018-04-28 | 2020-07-28 | 湖南有色新材料科技有限公司 | Production method of high-generation molybdenum target |
| 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 |
| 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 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1660526A (en) * | 2004-02-27 | 2005-08-31 | 日立金属株式会社 | Process of mfg. Mo alloyed targeting materials |
| CN102321871A (en) * | 2011-09-19 | 2012-01-18 | 基迈克材料科技（苏州）有限公司 | Hot isostatic pressing is produced the method for flat-panel monitor with the molybdenum alloy sputtering target material |
| CN103071793A (en) * | 2013-02-01 | 2013-05-01 | 基迈克材料科技（苏州）有限公司 | Molybdenum sputtering target material hot isostatic pressure production method |
| CN103302295A (en) * | 2013-06-20 | 2013-09-18 | 安泰科技股份有限公司 | Method for mill processing of high-purity and high-density molybdenum alloy target |
| CN103320756A (en) * | 2013-06-20 | 2013-09-25 | 安泰科技股份有限公司 | Method for preparing high-purity, high-density and large-size molybdenum alloy target |
| CN104439247A (en) * | 2014-12-30 | 2015-03-25 | 山东昊轩电子陶瓷材料有限公司 | Molybdenum alloy target preparation method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2796917B2 (en) * | 1993-02-02 | 1998-09-10 | 株式会社クボタ | Composite sintered alloy for non-ferrous metal melts with excellent corrosion resistance and wear resistance |
| US8153052B2 (en) * | 2003-09-26 | 2012-04-10 | General Electric Company | High-temperature composite articles and associated methods of manufacture |
-
2016
- 2016-03-10 CN CN201610133824.5A patent/CN105714253B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1660526A (en) * | 2004-02-27 | 2005-08-31 | 日立金属株式会社 | Process of mfg. Mo alloyed targeting materials |
| CN102321871A (en) * | 2011-09-19 | 2012-01-18 | 基迈克材料科技（苏州）有限公司 | Hot isostatic pressing is produced the method for flat-panel monitor with the molybdenum alloy sputtering target material |
| CN103071793A (en) * | 2013-02-01 | 2013-05-01 | 基迈克材料科技（苏州）有限公司 | Molybdenum sputtering target material hot isostatic pressure production method |
| CN103302295A (en) * | 2013-06-20 | 2013-09-18 | 安泰科技股份有限公司 | Method for mill processing of high-purity and high-density molybdenum alloy target |
| CN103320756A (en) * | 2013-06-20 | 2013-09-25 | 安泰科技股份有限公司 | Method for preparing high-purity, high-density and large-size molybdenum alloy target |
| CN104439247A (en) * | 2014-12-30 | 2015-03-25 | 山东昊轩电子陶瓷材料有限公司 | Molybdenum alloy target preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105714253A (en) | 2016-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105714253B (en) | The preparation method of large scale, fine grain molybdenum tantalum alloy-sputtering targets material | |
| CN104404508B (en) | A kind of laser gain material manufacture method of aluminum alloy junction component | |
| CN111455223B (en) | Aluminum-scandium alloy target material and preparation method thereof | |
| EP2125270B1 (en) | Process for producing high density refractory metals&alloys sputtering targets | |
| CN113579233B (en) | Tungsten-titanium alloy target material and preparation method and application thereof | |
| CN105728708B (en) | A kind of production method of high density long-life tungsten-molybdenum alloy crucible | |
| CN105525263B (en) | A kind of high-performance tantalum spattering target material preparation method | |
| CN108907211A (en) | A method of preparing large scale molybdenum plate blank | |
| CN102423802B (en) | Preparation method of highly-pure cobalt target | |
| CN104775077B (en) | Ultra-fine Grained invar alloy strip and preparation method thereof | |
| EP1449935B1 (en) | Sputtering target and production method therefor | |
| CN102367568A (en) | Preparation method of high-purity tantalum target material | |
| CN102848135A (en) | Production method of super-thick steel plate with even performance in thickness direction | |
| CN104480439A (en) | Preparation process of tantalum target material | |
| CN110158042A (en) | A kind of molybdenum niobium alloy rotary target material and preparation method thereof | |
| CN106312071A (en) | A tungsten-titanium tube target manufacture method | |
| JP2002129204A (en) | Method for manufacturing porous metal | |
| CN104419901A (en) | Method for manufacturing tantalum target material | |
| CN111101105B (en) | Preparation method of titanium-aluminum alloy target | |
| JP2000345326A (en) | Divided ito sputtering target | |
| CN112111714B (en) | Preparation method of tantalum-aluminum alloy sputtering target material | |
| CN114293159A (en) | Preparation method of nickel-based alloy target material | |
| KR100944437B1 (en) | Roll crown forming method of twin roll type strip caster | |
| CN106475567A (en) | The manufacture method of chrome molybdenum target blankss | |
| US20230024291A1 (en) | Method for producing molybdenum alloy targets |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of large-size and fine-grain molybdenum tantalum alloy sputtering target material Effective date of registration: 20200414 Granted publication date: 20171124 Pledgee: Bank of China Limited by Share Ltd. Luoyang branch Pledgor: Achemetal Tungsten AND Molybdenum Co.,Ltd. Registration number: Y2020980001482 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20210422 Granted publication date: 20171124 Pledgee: Bank of China Limited by Share Ltd. Luoyang branch Pledgor: Achemetal Tungsten AND Molybdenum Co.,Ltd. Registration number: Y2020980001482 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation of Mo TA alloy sputtering target with large size and fine grain Effective date of registration: 20210426 Granted publication date: 20171124 Pledgee: Bank of China Limited by Share Ltd. Luoyang branch Pledgor: Achemetal Tungsten AND Molybdenum Co.,Ltd. Registration number: Y2021980003028 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20220413 Granted publication date: 20171124 Pledgee: Bank of China Limited by Share Ltd. Luoyang branch Pledgor: Achemetal Tungsten AND Molybdenum Co.,Ltd. Registration number: Y2021980003028 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of large-size and fine-grained molybdenum tantalum alloy sputtering target Effective date of registration: 20220418 Granted publication date: 20171124 Pledgee: Bank of China Limited by Share Ltd. Luoyang branch Pledgor: Achemetal Tungsten AND Molybdenum Co.,Ltd. Registration number: Y2022980004337 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Granted publication date: 20171124 Pledgee: Bank of China Limited by Share Ltd. Luoyang branch Pledgor: Achemetal Tungsten AND Molybdenum Co.,Ltd. Registration number: Y2022980004337 |