CN108941584A - A kind of preparation method of long molybdenum tube sputtering target material - Google Patents
A kind of preparation method of long molybdenum tube sputtering target material Download PDFInfo
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- CN108941584A CN108941584A CN201811042186.1A CN201811042186A CN108941584A CN 108941584 A CN108941584 A CN 108941584A CN 201811042186 A CN201811042186 A CN 201811042186A CN 108941584 A CN108941584 A CN 108941584A
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- molybdenum tube
- long
- molybdenum
- sputtering target
- target material
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 272
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 231
- 239000011733 molybdenum Substances 0.000 title claims abstract description 231
- 239000013077 target material Substances 0.000 title claims abstract description 63
- 238000005477 sputtering target Methods 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 48
- 238000005245 sintering Methods 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 238000012797 qualification Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000005452 bending Methods 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 238000000137 annealing Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 13
- 238000007789 sealing Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 11
- 239000001301 oxygen Substances 0.000 description 11
- 229910052760 oxygen Inorganic materials 0.000 description 11
- 238000005304 joining Methods 0.000 description 8
- 238000009770 conventional sintering Methods 0.000 description 6
- 238000003754 machining Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000011324 bead Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000006837 decompression Effects 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 238000005242 forging Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
- 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
- B22F3/24—After-treatment of workpieces or articles
-
- 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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
- B22F5/106—Tube or ring forms
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
-
- 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
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The present invention relates to a kind of preparation methods of long molybdenum tube sputtering target material, it is the following steps are included: S1 suppresses molybdenum tube base: the molybdenum powder after mixing is fitted into the tubular cavity of cold isostatic mould, molybdenum powder is suppressed at 150-200MPa into tubulose, then it sloughs cold isostatic mould and obtains molybdenum tube base, molybdenum tube base end and outer circle are modified；S2 is sintered molybdenum tube base: molybdenum tube base being placed in hydrogen environment in 1800-2000 DEG C of sintering 4-10h, and modifies sintered molybdenum tube base；S3 splices long molybdenum tube: the resulting molybdenum tube base of several step S2 is longitudinally sequentially overlapped in the tubular cavity of hot isostatic pressing mold, then the air-tightness of tubular cavity is checked, the carry out hip treatment for filtering out air-tightness qualification obtains a root long molybdenum tube, and the long molybdenum tube is coated in hot isostatic pressing mold；S4 is straightened long molybdenum tube: carrying out hot alignment processing to the hot isostatic pressing mold for being coated with long molybdenum tube, then sloughs mold and obtain long molybdenum tube sputtering target material.
Description
Technical field
The present invention relates to target production technical fields, more particularly to a kind of preparation method of long molybdenum tube sputtering target material.
Background technique
Molybdenum target material is widely used in the industries such as electro-conductive glass, STN/TN/TFT-LCD, optical glass, ion film plating, is applicable in institute
There are facet coatings and rotary plating system.
The method of preparation large scale molybdenum tube target is mainly sintering process at present, but this method requires very starting material particle size
Height, and sintered density is relatively low, it is difficult to reach 99.5% density requirements, in addition long molybdenum tube is easily bent deformation in sintering process,
Yield rate is low.There are also three kinds of pressure sinterings, extrusion and forging method preparation methods in addition to sintering process, and still, pressure sintering is easily led to
Impurity and oxygen content are exceeded, are unable to satisfy the purity requirement greater than 99.95%；Extrusion equipment used in extrusion need to be able to bear
Pressure greater than 5000 tons, the high requirements on the equipment；Forging method is difficult to reach 99.5% density requirements, simultaneously because in forging process
In be difficult to control molybdenum tube thermal deformation, also cause uniformity inside molybdenum tube poor.
Summary of the invention
Based on this, the object of the present invention is to provide it is a kind of using device simple, density is high, purity is good, uniformity is good,
The long molybdenum tube preparation method of high yield rate.
A kind of preparation method of long molybdenum tube sputtering target material of the invention, comprising the following steps:
S1 suppresses molybdenum tube base: after weighing and mixing molybdenum powder, molybdenum powder being fitted into the tubular cavity of cold isostatic mould, cold
Under equal static pressure 150-200MPa then compacting molybdenum powder sloughs cold isostatic mould and obtains molybdenum tube base, to molybdenum tube base end at tubulose
And outer surface is modified；
S2 is sintered molybdenum tube base: the molybdenum tube base after finishing is placed in hydrogen environment in 1800-2000 DEG C of sintering 4-10h, and
Modify end and the surfaces externally and internally of sintered molybdenum tube base；
S3 splices long molybdenum tube: the resulting molybdenum tube base of several step S2 is longitudinally sequentially overlapped to the pipe in hot isostatic pressing mold
In shape cavity, then checks the air-tightness in tubular cavity, filter out the heat for being coated with several molybdenum tube bases of air-tightness qualification
Isostatic tooling carries out hip treatment, obtains a root long molybdenum tube, the long molybdenum tube is coated in hot isostatic pressing mold；
S4 is straightened long molybdenum tube: detection is coated with the bending position of the hot isostatic pressing mold of long molybdenum tube, and to the bending position
Alignment processing is carried out, then the stress relief annealing in vacuum environment；Hot isostatic pressing mold is sloughed after annealing, and modifies long molybdenum tube
End obtains long molybdenum tube sputtering target material；
Wherein, the standard of air-tightness qualification is that practical vacuum degree is less than or equal to 10 in tubular cavity-3pa。
Compared with the existing technology, the preparation method of long molybdenum tube sputtering target material of the present invention, which has the advantage that, passes through
Molybdenum tube base growth molybdenum tube sputtering target material is spliced using hip treatment mode, it is easy to operate, and each joining place uniform force,
So that the long molybdenum tube sputtering target material being spliced is in molybdenum tube base junction also even density；It handles and suppresses by using isostatic cool pressing
Molybdenum powder is at molybdenum tube base, so that all directions uniform stressed of molybdenum powder, so that molybdenum tube base even density is consistent, further such that
The even density of long molybdenum tube sputtering target material is consistent；By airtight test screened out air-tightness it is bad be coated on hot isostatic pressing mould
Molybdenum tube base in tool, to improve yield rate；By carrying out hot isostatic pressing under sintering and vacuum condition under hydrogen atmosphere
The processes such as processing and stress relief annealing, avoid being mixed into for oxygen as far as possible, have ensured that oxygen content is low in obtained long molybdenum tube,
Improve the purity of long molybdenum tube；By constantly modifying molybdenum tube base, when so that molybdenum tube base stacking splicing, the gap of joining place is small,
To be conducive to splicing, it helps improve the uniformity of long molybdenum tube sputtering target material；By using hip treatment by molybdenum tube base
Before splicing growth molybdenum tube, air-tightness is checked, to ensure that the joining place of molybdenum tube base is not mixed into air, to further decrease
Oxygen content；But also the density of molybdenum tube base joining place and the consistent in density of other parts, further improve entire long molybdenum tube
The even density degree of sputtering target material；Everywhere details it is comprehensive so that the density and purity of molybdenum tube reach the 99.5% of theoretical value with
On.Mould therefor is simple, and sintering, airtight test and alignment process device therefor are common, without using setting for complicated height
Standby large scale, the length of can be prepared by is the molybdenum tube of 1000-3500mm.
Further, in step S1, molybdenum powder is put into batch mixer, argon gas is filled with after vacuumizing, then in ar gas environment
In fill and be stirred 5-8h, obtain mixing powder.It is mixed using applying argon gas, the oxygen content of long molybdenum tube sputtering target material can be reduced；
The uniformity that can be improved long molybdenum tube sputtering target material is sufficiently stirred；Using high pure molybdenum powder, long molybdenum tube sputtering target material can be improved
Purity is also conducive to improve density.
Further, the cold isostatic mould includes mandrel, gum cover and support plate；During the gum cover with the mandrel is
Mandrel forms tubular cavity between the gum cover and the mandrel, for holding molybdenum powder at cylindrical shape；The mandrel and gum cover hang down
Disposed upright on the support plate, be uniformly provided on the support plate diameter be 20-40mm aperture；The material of the gum cover is
Multiple resin；The material of the support plate is stainless steel.By opening aperture on support plate, filled convenient for bottom liquid when isostatic cool pressing
Tap touching gum cover keeps the even density of molybdenum tube base consistent so that molybdenum powder is pressurized uniformly.
Further, in step S3, the hot isostatic pressing mold includes Hollow Cylindrical Shaft, cylinder jacket and two sealing covers；
Tubular cavity is formed between the Hollow Cylindrical Shaft and the cylinder jacket, for stacking molybdenum tube base obtained by step S2；It is described
Two sealing covers are respectively arranged at the both ends of long molybdenum tube made of stacking, are wherein provided with aspirating hole on the sealing cover of one end, institute
State aspirating hole connection vacuum pump.
Further, the quantity of the aspirating hole is two, is set on sealing cover using the Hollow Cylindrical Shaft as symmetry axis,
The aspirating hole present position face tubular cavity.
Further, in step S3, the air-leakage test process is the hot isostatic pressing that will be coated with several molybdenum tube bases
Mold is evacuated to 10 after being heated to 500-600 DEG C of heat preservation 5-12h-3Then Pa seals aspirating hole and cooling, in cooling procedure
Detect air-tightness.
Further, in step S3, the condition of the hip treatment is that the open circles of mold are depressured to described heat etc.
After filling up the ceramic bead of diameter 5-30mm in axis, at a temperature of 130-180MPa pressure and 1100-1500 DEG C, heat-insulation pressure keeping 2-
6h。
Further, in step S4, that detects the hot isostatic pressing mold for being coated with long molybdenum tube detects that bending bounce is maximum
Then bending bounce maximum point position is placed in induction coil and is heated to 1100-1250 DEG C, keeps the temperature 20-60min by point position；
Bending bounce maximum point position is placed under 150-250T pressure again and carries out pressurization alignment.
Further, in step S4, the condition of the stress relief annealing keeps the temperature 3h at a temperature of being 850-900 DEG C.
Further, in step S1, purity >=99.99% of molybdenum powder used.
In order to better understand and implement, the invention will now be described in detail with reference to the accompanying drawings.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of cold isostatic mould of the invention；
Fig. 2 is the structural schematic diagram of hot isostatic pressing mold of the invention；
Fig. 3 is the end cross-sectional view of hot isostatic pressing mold of the invention；
Wherein, 10- cold equal decompression mold, 11- mandrel, 12- gum cover, 13- support plate, 131- aperture, 20- molybdenum powder, 30- heat
Deng decompression mold, 31- Hollow Cylindrical Shaft, 32- housing, 33- sealing cover, 331- aspirating hole, 40- molybdenum tube base.
Fig. 4 is the metallographic microscope of long molybdenum tube sputtering target material obtained by the embodiment of the present invention one；
Fig. 5 is long molybdenum tube sputtering target material C-SCAN figure obtained by the embodiment of the present invention one；
Fig. 6 is the metallographic microscope of long molybdenum tube sputtering target material obtained by the embodiment of the present invention two；
Fig. 7 is long molybdenum tube sputtering target material C-SCAN figure obtained by the embodiment of the present invention two；
Fig. 8 is the metallographic microscope of long molybdenum tube sputtering target material obtained by the embodiment of the present invention three；
Fig. 9 is long molybdenum tube sputtering target material C-SCAN figure obtained by the embodiment of the present invention three；
Figure 10 is the metallographic microscope of long molybdenum tube sputtering target material made from conventional sintering method；
Figure 11 is long molybdenum tube sputtering target material C-SCAN figure made from conventional sintering method.
Specific embodiment
The preparation method of long molybdenum tube sputtering target material of the invention, comprising the following steps:
S1 suppresses molybdenum tube base: weighing purity >=99.99% molybdenum powder and is put into batch mixer, argon gas is filled with after vacuumizing, then
It fills in an argon atmosphere and is stirred 5-8h, obtain mixing molybdenum powder, the tubular cavity of molybdenum powder loading cold isostatic mould will be mixed
In, molybdenum powder is suppressed at isostatic cool pressing 150-200MPa into tubulose, is then sloughed cold isostatic mould and is obtained molybdenum tube base, to molybdenum tube
Base end and outer surface are modified, and keep it smooth；
S2 is sintered molybdenum tube base: the molybdenum tube base after finishing is placed in hydrogen environment in 1800-2000 DEG C of sintering 4-10h, and
Modify end and the surfaces externally and internally of sintered molybdenum tube base；
S3 splices long molybdenum tube: the resulting molybdenum tube base of several step S2 is longitudinally sequentially overlapped to the pipe in hot isostatic pressing mold
In shape cavity, the air-tightness in tubular cavity is then checked, filter out practical vacuum degree less than or equal to 10-3Being coated with for pa is several
The hot isostatic pressing mold of root molybdenum tube base carries out hip treatment, obtains a root long molybdenum tube, it is quiet that the long molybdenum tube is coated on heat etc.
In compression mould；
S4 is straightened long molybdenum tube: detection is coated with the bending position of the hot isostatic pressing mold of long molybdenum tube, and to the bending position
Alignment processing is carried out, then the stress relief annealing in vacuum environment；Hot isostatic pressing mold is sloughed after annealing, and modifies long molybdenum tube
End obtains long molybdenum tube sputtering target material.
Isostatic pressing technology be it is a kind of processed powder is placed in the closed container for filling with liquid, to each of powder
A surface applies with equal pressure, to make the technology of powder coagulation forming.
The preparation principle of long molybdenum tube sputtering target material of the invention are as follows: handled using isostatic cool pressing and be pressed into high-purity molybdenum powder
The molybdenum tube base of even density is spliced the lesser molybdenum tube base of several root long degree using hip treatment after the sintering of molybdenum tube base
It is pressed into the biggish long molybdenum tube sputtering target material of a root long degree.During the preparation process, length is improved using cold equal and hot isostatic pressing technique
The density uniformity of molybdenum tube sputtering target material avoids molybdenum tube base joining place and other parts Density inhomogeneity by airtight test,
Further increase density uniformity；Heat alignment is carried out to long molybdenum tube and guarantees that long molybdenum tube sputtering target material is straight.
Wherein, the specific structure of the cold isostatic mould sees attached drawing 1.The cold isostatic mould 10 includes mandrel
11, gum cover 12 and support plate 13；The gum cover 12 is center axis into cylindrical shape, the gum cover 12 and the core with the mandrel 11
Tubular cavity is formed between axis 11, for holding molybdenum powder；The mandrel 11 and gum cover 12 are vertically arranged on the support plate 13, institute
The aperture 131 for being uniformly provided with that diameter is 20-40mm on support plate 13 is stated, comes into full contact with glue convenient for bottom liquid when isostatic cool pressing
Set, so that molybdenum powder is pressurized uniformly.The material of the gum cover is multiple resin；The material of the support plate is stainless steel；The mandrel
For solid 45# steel pipe, and 1-3mm taper is had, pipe outside diameter polishing smoothness reaches Ra≤0.3, and surface is coated with release agent, institute
Stating release agent is glycerine mixed liquor, is taken off on decompression mold convenient for molybdenum tube base from cold wait.
The specific structure of the hot isostatic pressing mold sees attached drawing 2 and attached drawing 3.The hot isostatic pressing mold 30 includes hollow
Circular shaft 31, cylinder jacket 32 and two sealing covers 33；Tubular sky is formed between the Hollow Cylindrical Shaft 31 and the cylinder jacket 32
Chamber, for stacking molybdenum tube base obtained by step S2；Described two sealing covers 33 are respectively arranged at long molybdenum tube made of stacking
Both ends, wherein aperture is 8-10mm aspirating hole 331 there are two settings on one end sealing cover 33；Described two aspirating holes 331 are with institute
Stating Hollow Cylindrical Shaft 31 is that symmetry axis is set on sealing cover 33, present position face tubular cavity, the aspirating hole 33 with it is true
Sky pump connection, for evacuating between molybdenum tube base and stacking the air between molybdenum tube base and Hollow Cylindrical Shaft 31 and cylinder jacket 32.
The Hollow Cylindrical Shaft 31 is hollow round steel pipe, and mandrel wall thickness is 20-45mm, and the gap with molybdenum tube base is 0.2-0.5mm；It is described
The material of cylinder jacket 32 is 20# steel, and wall thickness 5-30mm is 0.5-2mm with molybdenum tube base gap；Splicing between the molybdenum tube base
Gap≤0.3mm.
Detailed process is as follows states shown in embodiment for the preparation method of long molybdenum tube sputtering target material of the present invention.
Embodiment one
S1 suppresses molybdenum tube base
Take purity >=99.99%, averagely Fisher particle size is 2-6 μm, the molybdenum powder of oxygen content < 500ppm is put into V-type batch mixer
It is interior, it is filled with argon gas after vacuumizing, 5h is then thoroughly mixed in argon gas, obtains uniformly mixed molybdenum powder；
Uniformly mixed molybdenum powder is uniformly packed into isostatic cool pressing cylinder mould by shaking platform, is filled to molybdenum powder tubular
After cavity, compacting is uniform and tightens gum cover end, molybdenum powder is suppressed under isostatic cool pressing 150Pa pressure into tubulose, then demoulding is gone
Except mandrel obtains the molybdenum tube base that theoretical density is 60%-65%, length is 520-530mm, then molybdenum tube base is modified in machining
Two ends and outer surface, it is ensured that outer surface is uniformly without recess or protrusion.
S2 is sintered molybdenum tube base
Molybdenum tube base after finishing is placed in hydrogen environment and is sintered 4h, sintering temperature is 1800 DEG C, and obtaining theoretical density is
96%-98%, the molybdenum tube base that length is 420-430mm continue the machining finishing two ends of molybdenum tube base and interior after the completion of sintering
Outer surface, so that surface roughness Ra≤0.4 of molybdenum tube base.
S3 splices long molybdenum tube
The resulting molybdenum tube base of several step S2 is longitudinally sequentially overlapped in the tubular cavity of hot isostatic pressing mold, molybdenum tube
Base superposition height is 1700mm；Then the hot isostatic pressing mold for being coated with several molybdenum tube bases is put into Muffle furnace and is heated to
500-600 DEG C of heat preservation 5-12h, is evacuated to 10-3Pa seals aspirating hole after Muffle furnace cooling during welding, detect airtight
Property；Then, by air-tightness qualification, i.e., practical vacuum degree is less than or equal to 10-3The heat for being coated with several molybdenum tube bases of pa etc. is quiet
The ceramic bead that full diameter is 5-30mm is filled in the Hollow Cylindrical Shaft 31 of compression mould；Then above-mentioned mold is placed in hot isostatic pressing furnace
It is interior, hip treatment is carried out under the conditions of 130MPa, 1100 DEG C, obtains that a root long degree is longer, is spelled by several molybdenum tube bases
The long molybdenum tube being connected into, the long molybdenum tube are coated in hot isostatic pressing mold.
S4 is straightened long molybdenum tube
The resulting hot isostatic pressing mold for being coated with long molybdenum tube of detecting step S3 detects bending bounce maximum point position,
Then bending bounce maximum point position is placed in induction coil and is heated to 1100-1250 DEG C, keep the temperature 20-60min；It again will bending
Bounce maximum point position is placed on the surface plate of four column hydraulic presses under 150-250T pressure, is carried out pressurization alignment, is measured simultaneously
Bending bounce, until true topic bending bounce is less than 1mm.Then in a vacuum, 850 DEG C of heat preservation 3h progress destressings are heated to move back
Fire；Hot isostatic pressing mold is taken off after annealing, and finishing is machined out to the two ends of long molybdenum tube, and obtaining length is 1500mm's
Long molybdenum tube sputtering target material.
Embodiment two
S1 suppresses molybdenum tube base
Take purity >=99.99%, averagely Fisher particle size is 2-6 μm, the molybdenum powder of oxygen content < 500ppm is put into V-type batch mixer
It is interior, it is filled with argon gas after vacuumizing, 8h is then thoroughly mixed in argon gas, obtains uniformly mixed molybdenum powder；
Uniformly mixed molybdenum powder is uniformly packed into isostatic cool pressing cylinder mould by shaking platform, is filled to molybdenum powder tubular
After cavity, compacting is uniform and tightens gum cover end, molybdenum powder is suppressed under isostatic cool pressing 200MPa pressure into tubulose, then demoulding is gone
Except mandrel obtains the molybdenum tube base that theoretical density is 60%-65%, length is 700-710mm, then molybdenum tube base is modified in machining
Two ends and outer surface, it is ensured that outer surface is uniformly without recess or protrusion.
S2 is sintered molybdenum tube base
Molybdenum tube base after finishing is placed in hydrogen environment and is sintered 10h, sintering temperature is 2000 DEG C, and obtaining theoretical density is
96%-98%, the molybdenum tube base that length is 580-590mm continue the machining finishing two ends of molybdenum tube base and interior after the completion of sintering
Outer surface, so that surface roughness Ra≤0.4 of molybdenum tube base.
S3 splices long molybdenum tube
The resulting molybdenum tube base of several step S2 is longitudinally sequentially overlapped in the tubular cavity of hot isostatic pressing mold, molybdenum tube
Base superposition height is 2900mm；Then the hot isostatic pressing mold for being coated with several molybdenum tube bases is put into Muffle furnace and is heated to
600 DEG C of heat preservation 5-12h, are evacuated to 10-3Pa seals aspirating hole after Muffle furnace cooling during welding, detect air-tightness；
Then, by by air-tightness qualification, i.e., practical vacuum degree is less than or equal to 10-3The hot isostatic pressing for being coated with several molybdenum tube bases of pa
The ceramic bead that full diameter is 5-30mm is filled in the Hollow Cylindrical Shaft 31 of mold；Then above-mentioned mold is placed in hot isostatic pressing furnace,
Hip treatment is carried out under the conditions of 180MPa, 1500 DEG C, obtains that a root long degree is longer, is spliced by several molybdenum tube bases
Long molybdenum tube, the long molybdenum tube is coated in hot isostatic pressing mold.
S4 is straightened long molybdenum tube
The resulting hot isostatic pressing mold for being coated with long molybdenum tube of detecting step S3 detects bending bounce maximum point position,
Then bending bounce maximum point position is placed in induction coil and is heated to 1250 DEG C, keep the temperature 60min；It is again that bending bounce is maximum
Point position is placed on the surface plate of four column hydraulic presses under 250T pressure, carries out pressurization alignment, while measuring bending bounce, until
True topic bending bounce is less than 1mm.Then in a vacuum, it is heated to 900 DEG C of heat preservation 3h and carries out stress relief annealing；Heat is taken off after annealing
Isostatic tooling, and finishing is machined out to the two ends of long molybdenum tube, obtain the long molybdenum tube sputtering target material that length is 2700mm.
Embodiment three
S1 suppresses molybdenum tube base
Take purity >=99.99%, averagely Fisher particle size is 2-6 μm, the molybdenum powder of oxygen content < 500ppm is put into V-type batch mixer
It is interior, it is filled with argon gas after vacuumizing, 7h is then thoroughly mixed in argon gas, obtains uniformly mixed molybdenum powder；
Uniformly mixed molybdenum powder is uniformly packed into isostatic cool pressing cylinder mould by shaking platform, is filled to molybdenum powder tubular
After cavity, compacting is uniform and tightens gum cover end, molybdenum powder is suppressed under isostatic cool pressing 180MPa pressure into tubulose, then demoulding is gone
Except mandrel obtains the molybdenum tube base that theoretical density is 60%-65%, length is 850-860mm, then molybdenum tube base is modified in machining
Two ends and outer surface, it is ensured that outer surface is uniformly without recess or protrusion.
S2 is sintered molybdenum tube base
Molybdenum tube base after finishing is placed in hydrogen environment and is sintered 7h, sintering temperature is 1900 DEG C, and obtaining theoretical density is
96%-98%, the molybdenum tube base that length is 610-620mm continue the machining finishing two ends of molybdenum tube base and interior after the completion of sintering
Outer surface, so that surface roughness Ra≤0.4 of molybdenum tube base.
S3 splices long molybdenum tube
The resulting molybdenum tube base of several step S2 is longitudinally sequentially overlapped in the tubular cavity of hot isostatic pressing mold, molybdenum tube
Base superposition height is 3700mm；Then the hot isostatic pressing mold for being coated with several molybdenum tube bases is put into Muffle furnace and is heated to
550 DEG C of heat preservation 9h, are evacuated to 10-3Pa seals aspirating hole after Muffle furnace cooling during welding, detect air-tightness；So
Afterwards, by air-tightness qualification, i.e., practical vacuum degree is less than or equal to 10-3The hot isostatic pressing mold for being coated with several molybdenum tube bases of pa
Hollow Cylindrical Shaft 31 in fill the ceramic bead that full diameter is 5-30mm；Then above-mentioned mold is placed in hot isostatic pressing furnace,
155MPa, hip treatment is carried out under the conditions of 1300 DEG C, obtain that a root long degree is longer, is spliced by several molybdenum tube bases
Long molybdenum tube, the long molybdenum tube are coated in hot isostatic pressing mold.
S4 is straightened long molybdenum tube
The resulting hot isostatic pressing mold for being coated with long molybdenum tube of detecting step S3 detects bending bounce maximum point position,
Then bending bounce maximum point position is placed in induction coil and is heated to 1175 DEG C, keep the temperature 40min；It is again that bending bounce is maximum
Point position is placed on the surface plate of four column hydraulic presses under 200T pressure, carries out pressurization alignment, while measuring bending bounce, until
True topic bending bounce is less than 1mm.Then in a vacuum, 875 DEG C of heat preservation 3h carry out stress relief annealing；Hot isostatic pressing is taken off after annealing
Mold, and finishing is machined out to the two ends of long molybdenum tube, obtain the long molybdenum tube sputtering target material that length is 3500mm.
Effect analysis
To according to long molybdenum tube sputtering target material made from step described in embodiment one to three, and according to conventional sintering mode
Long molybdenum tube obtained carries out metallographic examination respectively and C-SCAN is checked.Please refer to Fig. 4-Figure 11, wherein Fig. 4 is that the present invention is implemented
The metallographic microscope of long molybdenum tube sputtering target material obtained by example one；Fig. 5 is long molybdenum tube sputtering target material obtained by the embodiment of the present invention one
C-SCAN figure；Fig. 6 is the metallographic microscope of long molybdenum tube sputtering target material obtained by the embodiment of the present invention two；Fig. 7 is the embodiment of the present invention
Long molybdenum tube sputtering target material C-SCAN figure obtained by two；Fig. 8 is long molybdenum tube sputtering target material obtained by the embodiment of the present invention three
Metallographic microscope；Fig. 9 is long molybdenum tube sputtering target material C-SCAN figure obtained by the embodiment of the present invention three；Figure 10 is made for conventional sintering method
Long molybdenum tube sputtering target material metallographic microscope；Figure 11 is long molybdenum tube sputtering target material C-SCAN figure made from conventional sintering method.
As seen from the figure, long molybdenum tube sputtering target material obtained by the preparation method using long molybdenum tube sputtering target material of the present invention
Crystal grain it is fine and closely woven and the abnormal defect such as internal pore-free, the uniformity are high.And according to the crystalline substance of long molybdenum tube obtained by conventional sintering method
Grain is coarse, and grain size is greater than 150 microns, far beyond requiring numberical range；And material inside organization uniformity is poor, passes through C-SCAN
There are the abnormal defects such as internal porosity for inspection.
Compared with the existing technology, the preparation method of long molybdenum tube sputtering target material of the present invention, which has the advantage that, passes through
Molybdenum tube base growth molybdenum tube sputtering target material is spliced using hip treatment mode, it is easy to operate, and each joining place uniform force,
So that the long molybdenum tube sputtering target material even density being spliced；Compacting molybdenum powder is handled into molybdenum tube base by using isostatic cool pressing, is made
The all directions uniform stressed for obtaining molybdenum powder, so that molybdenum tube base even density is consistent, further such that long molybdenum tube sputtering target material
Even density it is consistent；The air-tightness ensured in coating mould is screened out by airtight test, improves hot isostatic pressing mold
In molybdenum tube base consistency degree and yield rate；By being carried out at hot isostatic pressing under the sintering under hydrogen atmosphere and vacuum condition
The processes such as reason and stress relief annealing, avoid being mixed into for oxygen as far as possible, have ensured that oxygen content is low in obtained long molybdenum tube；Pass through
Continuous finishing molybdenum tube base, when so that molybdenum tube base stacking splicing, the gap of joining place is small, to be conducive to splicing, it helps mention
The uniformity of high long molybdenum tube sputtering target material；Before molybdenum tube base is spliced growth molybdenum tube by using hip treatment, gas is checked
Close property, to ensure that the joining place of molybdenum tube base is not mixed into air, to further reduced oxygen content；But also molybdenum tube base is held in the mouth
The density at place and the consistent in density of other parts are connect, the even density degree of entire long molybdenum tube sputtering target material is further improved；
Mould therefor is simple, and sintering, airtight test and alignment process device therefor are common, and the equipment without using complicated height is
Large scale can be made, the molybdenum tube that length is 1000-3500mm.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.
Claims (10)
1. a kind of preparation method of long molybdenum tube sputtering target material, which comprises the following steps:
S1 suppresses molybdenum tube base: after weighing and mixing molybdenum powder, molybdenum powder being fitted into the tubular cavity of cold isostatic mould, cold etc. quiet
Compacting molybdenum powder under 150-200MPa is pressed then to slough cold isostatic mould at tubulose and obtain molybdenum tube base, to molybdenum tube base end and outside
It is modified on surface；
S2 is sintered molybdenum tube base: the molybdenum tube base after finishing being placed in hydrogen environment in 1800-2000 DEG C of sintering 4-10h, and is modified
The end of sintered molybdenum tube base and surfaces externally and internally；
S3 splices long molybdenum tube: the resulting molybdenum tube base of several step S2 is longitudinally sequentially overlapped to the tubular sky in hot isostatic pressing mold
It is intracavitary, it then checks the air-tightness in tubular cavity, it is quiet to filter out heat for being coated with several molybdenum tube bases of air-tightness qualification etc.
Compression mould carries out hip treatment, obtains a root long molybdenum tube, the long molybdenum tube is coated in hot isostatic pressing mold；
S4 is straightened long molybdenum tube: detection is coated with the bending position of the hot isostatic pressing mold of long molybdenum tube, and carries out to the bending position
Alignment is handled, then the stress relief annealing in vacuum environment；Hot isostatic pressing mold is sloughed after annealing, and modifies the end of long molybdenum tube
Head obtains long molybdenum tube sputtering target material；
Wherein, the standard of air-tightness qualification is that practical vacuum degree is less than or equal to 10 in tubular cavity-3pa。
2. the preparation method of long molybdenum tube sputtering target material according to claim 1, it is characterised in that: further, step S1
In, molybdenum powder is put into batch mixer, argon gas is filled with after vacuumizing, then fills in an argon atmosphere and is stirred 5-8h, is mixed
Even powder.
3. the preparation method of long molybdenum tube sputtering target material according to claim 1, it is characterised in that: the cold isostatic mould
Including mandrel, gum cover and support plate；The gum cover is center axis into cylindrical shape using the mandrel, the gum cover and the mandrel it
Between form tubular cavity, for holding molybdenum powder；The mandrel and gum cover are vertically arranged on the support plate, on the support plate
It is even to offer the aperture that diameter is 20-40mm；The material of the gum cover is multiple resin；The material of the support plate is stainless steel.
4. the preparation method of long molybdenum tube sputtering target material according to claim 1, it is characterised in that: in step S3, the heat
Isostatic tooling includes Hollow Cylindrical Shaft, cylinder jacket and two sealing covers；Shape between the Hollow Cylindrical Shaft and the cylinder jacket
At tubular cavity, for stacking molybdenum tube base obtained by step S2；Described two sealing covers are respectively arranged at long made of stacking
The both ends of molybdenum tube, are wherein provided with aspirating hole on the sealing cover of one end, the aspirating hole connects vacuum pump.
5. the preparation method of long molybdenum tube sputtering target material according to claim 4, it is characterised in that: the quantity of the aspirating hole
It is two, is set on sealing cover using the Hollow Cylindrical Shaft as symmetry axis, the aspirating hole present position face tubular cavity.
6. the preparation method of long molybdenum tube sputtering target material according to claim 5, it is characterised in that: in step S3, the gas
Close property detection process is to take out after the hot isostatic pressing mold for being coated with several molybdenum tube bases is heated to 500-600 DEG C of heat preservation 5-12h
Vacuum is to 10-3Then Pa seals aspirating hole and cooling, detects air-tightness in cooling procedure.
7. the preparation method of long molybdenum tube sputtering target material according to claim 4-6 any one, it is characterised in that: step S3
In, the condition of the hip treatment is that the ceramics of diameter 5-30mm are filled up in the Hollow Cylindrical Shaft for being depressured mold to described heat etc.
After pearl, at a temperature of 130-180MPa pressure and 1100-1500 DEG C, heat-insulation pressure keeping 2-6h.
8. the preparation method of long molybdenum tube sputtering target material according to claim 1, it is characterised in that: in step S4, detection packet
Be covered with the hot isostatic pressing mold of long molybdenum tube detects bending bounce maximum point position, then sets bending bounce maximum point position
It is heated to 1100-1250 DEG C in induction coil, keeps the temperature 20-60min；Bending bounce maximum point position is placed in 150-250T again
Pressurization alignment is carried out under pressure.
9. according to claim 1 or the preparation method of long molybdenum tube sputtering target material described in 8 any one, it is characterised in that: step
In S4, the condition of the stress relief annealing keeps the temperature 3h at a temperature of being 850-900 DEG C.
10. the preparation method of long molybdenum tube sputtering target material according to claim 1 or 2, it is characterised in that: in step S1, institute
With purity >=99.99% of molybdenum powder.
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| CN110000391A (en) * | 2019-02-28 | 2019-07-12 | 株洲硬质合金集团有限公司 | A kind of preparation method of molybdenum tube |
| CN111607752A (en) * | 2020-06-03 | 2020-09-01 | 福建阿石创新材料股份有限公司 | Internal stress removing correction method for sputtering target material |
| CN112343948A (en) * | 2020-11-05 | 2021-02-09 | 三阳纺织有限公司 | Manufacturing method of mandrel component, mandrel component and textile machine applying mandrel component |
| CN114131026A (en) * | 2021-12-08 | 2022-03-04 | 西安瑞福莱钨钼有限公司 | Process for producing molybdenum tube blank by using mould pressing method |
| CN115488333A (en) * | 2022-09-27 | 2022-12-20 | 宁波江丰电子材料股份有限公司 | Molybdenum-titanium alloy tube target and preparation method and application thereof |
| CN115502403A (en) * | 2022-09-29 | 2022-12-23 | 宁波江丰电子材料股份有限公司 | Preparation method of large-size and high-density molybdenum target |
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Denomination of invention: Preparation method of long molybdenum tube sputtering target material Effective date of registration: 20200622 Granted publication date: 20190903 Pledgee: Shaoguan Branch of China Construction Bank Co.,Ltd. Pledgor: SHAOGUAN OULAI HI-TECH MATERIAL Co.,Ltd.|DONGGUAN OMAT PUTTERING TARGET Co.,Ltd. Registration number: Y2020440000149 |
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Date of cancellation: 20211227 Granted publication date: 20190903 Pledgee: Shaoguan Branch of China Construction Bank Co.,Ltd. Pledgor: SHAOGUAN OULAI HI-TECH MATERIAL Co.,Ltd.|DONGGUAN OMAT PUTTERING TARGET Co.,Ltd. Registration number: Y2020440000149 |
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Denomination of invention: A preparation method of sputtering target for long molybdenum tube Effective date of registration: 20211229 Granted publication date: 20190903 Pledgee: Shaoguan Branch of China Construction Bank Co.,Ltd. Pledgor: Guangdong Oulai high tech materials Co.,Ltd.|DONGGUAN OMAT PUTTERING TARGET Co.,Ltd. Registration number: Y2021980016846 |
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