CN108930020A - Molybdenum niobium target manufacture craft - Google Patents
Molybdenum niobium target manufacture craft Download PDFInfo
- Publication number
- CN108930020A CN108930020A CN201810974197.7A CN201810974197A CN108930020A CN 108930020 A CN108930020 A CN 108930020A CN 201810974197 A CN201810974197 A CN 201810974197A CN 108930020 A CN108930020 A CN 108930020A
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- CN
- China
- Prior art keywords
- powder
- manufacture craft
- jacket
- molybdenum
- layer jacket
- 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.)
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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 invention discloses a kind of molybdenum niobium target manufacture crafts, including Step 1: raw material mixes；Step 2: gum cover fills powder operation；Step 3: isostatic cool pressing operation, room temperature boosting, and after being kept for the predetermined time, remove pressure；Step 4: hot isostatic pressing step, will carry out jacket operation by the molding finished product of isostatic cool pressing operation, internal layer jacket, outer layer jacket are successively sheathed on internal material, outer layer jacket is carried out welded seal；It will be removed by gas between the internal material and internal layer jacket of the post-job finished product of jacket；After degasification, hot isostatic pressing operation is carried out to product.The density of MoNb alloy target material can be improved.
Description
Technical field
The present invention relates to molybdenum niobium target manufacture crafts.
Background technique
The raw material of MoNb alloy target material are Mo powder, Nb powder, for the Coating Materials of TFT liquid crystal display panel, Mo-at%
The theoretical density of 10Nb: 9.99g/cm3.It is only capable of reaching materials theory density using the manufacture craft of molybdenum niobium target currently on the market
98%, a large amount of gas hole defect is contained in low density target, leachy place can be abnormal electric discharge in use,
In addition, reverse sputtering accumulation (mura) can occur for the target of low-density, target use is influenced.
Summary of the invention
To overcome disadvantages mentioned above, the purpose of the present invention is to provide stomata, the reduction paradoxical discharges in a kind of reduction target
The molybdenum niobium target manufacture craft of the MoNb alloy target material of phenomenon, guarantee target normal use.
In order to reach the goals above, the technical solution adopted by the present invention is that: a kind of molybdenum niobium target manufacture craft, including step
One, raw material mixes；Step 2: gum cover fills powder operation；Step 3: isostatic cool pressing operation, room temperature boosting, and kept for the predetermined time
Afterwards, pressure is removed；Step 4: hot isostatic pressing step industry, will carry out jacket operation by the molding finished product of isostatic cool pressing operation, according to
It is secondary that internal layer jacket, outer layer jacket are sheathed on internal material, outer layer jacket is subjected to welded seal；It will be after jacket operation
Finished product internal material and internal layer jacket between gas remove；After degasification, hot isostatic pressing operation is carried out to product.
The beneficial effect of molybdenum niobium target manufacture craft of the present invention is after isostatic cool pressing operation, then to carry out hot isostatic pressing step
Suddenly, molybdenum niobium target manufacture craft uses isostatic cool pressing operation, hot isostatic pressing step combined process, so that the density of product can reach
98% or more of theoretical density realizes high density, and highdensity target reduces a large amount of gas hole defect, in use,
Reduce paradoxical discharge phenomenon, in addition, highdensity target is susceptible to reverse sputtering accumulation (mura), ensure that target just
It is often used.
Preferably, isostatic cool pressing operation, room temperature boosts to 150-180MPa, and removes pressure after keeping at least 200s.
Using isostatic cool pressing, make the initial stage compacted density of powder increase powder dress real density in 34-37%, isostatic cool pressing is logical
The compacted density that 67-70% can be achieved is crossed after this process operation.
Preferably, in the hot isostatic pressing step, temperature range control when degasification is at 350-500 DEG C, vacuum degree 1
×10- 4- 1 × 10- 3Pa, time are maintained at 2.5h-5h.Degasification operation is to remove the gas in jacket as far as possible, is formed opposite
The state of vacuum, increase certain temperature the purpose of be to be conducive to material internal gas discharge, the time it is longer also can be conducive to material in
Portion's gas discharge.
Preferably, the temperature of the hot isostatic pressing operation controls within the scope of 1000-1500 DEG C, while pressure control exists
130MPa-180MPa continues 2.5-6h, so that 98% or more the density accessibility theory density of product.Mo alloy is made in high temperature
Contraction can be generated under industry, in the case where there is pressure in outside, further achieved the effect that contraction, realized high density.
Being as a further improvement of the present invention further includes step 5, rolls operation, and the calendering operation will be outside script
Layer removal；The outer layer jacket of calendering, then welded seal are remake, the thickness for remaking the outer layer jacket of calendering is greater than
The thickness of the outer layer jacket of hot isostatic pressing step；Temperature is heated to 1400 DEG C, duration 3h by heating work；Push work
Make, each volume under pressure is maintained at 25%.After rolling operation, the density of product can reach 99.8% or more theoretical density.
Preferably, the raw material uses molybdenum powder, niobium powder, and weight 8.5:1 carries out investment charge according to the ratio for the molybdenum powder, niobium powder
Storehouse, molybdenum powder, niobium powder are mixed in storage bin.
Preferably, the hybrid technique that the molybdenum powder, niobium powder are mixed in storage bin are as follows: be passed through Ar gas progress air and set
10-20min is changed, mixes rotation speed are as follows: 6-12 revolution/min, activity duration long 60-120min.Powder mixture operation, by
It is made of in raw material two kinds of powder, needs uniformly to combine the two, niobium powder is a kind of element of easy oxygen uptake, so needing to carry out gas
Body protection, such as Ar gas, the purpose of rotational time and revolving speed is that it is sufficiently stirred.
Preferably, the powder completed mixing in the gum cover dress powder operation, weighs the weight of requirement, gum cover will be arrived by filling out
In, every to need to carry out jolt ramming when filling 25% weight, point 4 vibrations so that 1-5min sufficiently, is vibrated in vibration, final height into
Row measurement.The tap density of powder can reach the 35% of theoretical density in advance at this time.
Preferably, further include between step 3 and step 4 six faces processing job step, by the product of isostatic cool pressing into
The processing of 6 face of row, the flatness < 1mm in each face of product.
Preferably, after the step of calendering operation, product is once by alignment operation, vacuum heat treatment operation and machine
Tool processes the production of final finished shape.
Detailed description of the invention
Fig. 1 is the photograph after the MoNb target material structure made by the molybdenum niobium target manufacture craft of embodiment one amplifies 50 times
Piece；
Fig. 2 is the photograph after the MoNb target material structure made by the molybdenum niobium target manufacture craft of embodiment one amplifies 400 times
Piece.
Specific embodiment
It is described in detail below with reference to preferred embodiment, so that advantages and features of the invention can be easier to by this field
Technical staff's understanding, so as to make a clearer definition of the protection scope of the present invention.
Embodiment one,
A kind of molybdenum niobium target manufacture craft of the present embodiment, includes the following steps:
Step 1, raw material mixing
By raw material (Mo powder, Nb powder), weight 8.5:1 is carried out in investment storage bin according to the ratio, hybrid technique are as follows: be passed through Ar gas
Carry out air displacement 15min；Mix rotation speed are as follows: 8 revolutions/min, activity duration long 120min.
Step 2, gum cover fill powder operation
The powder that mixing is completed, weighs the weight of requirement, fills out into gum cover, every to need to carry out when filling 25% weight
1-5min is vibrated in jolt ramming, and preferably 2min finally highly measures, it is therefore an objective to guarantee to reach theoretical density 35% with
On.In this step, it needs first to set in advance, when reaching the 35% of theoretical density, after jolt ramming operation, the height of powder is answered
To be how many, reach this height once the powder after jolt ramming, then can guarantee to reach the 35% of theoretical density.
Step 3, isostatic cool pressing operation (CIP)
Room temperature boosts to after 160MPa used time 400s reaches 160MPa holding 200s and removes pressure, is reaching reason density
66% 68% or more ~.
Step 4, six faces process operation
The product of isostatic cool pressing is subjected to 6 face processing, guarantees the flatness < 1mm in each face, purpose: for hot isostatic pressing step
(HIP) product flatness guarantees.
Step 5, hot isostatic pressing step (HIP)
1) six faces to be processed into complete finished product and carries out jacket operation, first layer is internal layer jacket, using SUS304, with a thickness of
0.3mm, the second layer is outer layer jacket, using 45# steel, with a thickness of 3mm, by outer layer jacket and internal material welded seal.
2) it will be removed by the gas between the internal material and internal layer jacket of the post-job finished product of jacket: temperature when degasification
Scope control is spent at 350-500 DEG C, and vacuum degree control is 1 × 10- 4- 1 × 10- 3Within the scope of Pa, vacuum degree is preferably 1 × 10- 3Pa, time are maintained at 2.5h-5h, it is preferable that the time continues 3h.
3) after degasification, carry out hot isostatic pressing operation to product: temperature and pressure are controlled respectively at 1000-1500 DEG C
Range, 130MPa-180MPa, continue 2.5-6h (preferably 4h) pressure and heating operation carries out simultaneously.
The density of product can reach 98% or more theoretical density.
Step 6 rolls operation
1) the HIP jacket made is removed, is specifically got rid of, outer layer jacket: 45# steel, due to passing through hot isostatic pressing
Outer layer jacket after step can damage, and can not play the role of preventing heat dissipation, so to replace.
2) jacket (outer layer jacket) of production calendering: 45# steel, 10mm are sealed welding, remake the outer of calendering
The thickness of layer jacket is greater than the thickness of the outer layer jacket of hot isostatic pressing step, to guarantee the outer layer jacket in calendering operation process
It is not damaged.
3) heating operation: at least 1400 DEG C, duration at least 3h are heated to, the present embodiment is (real using 1400 DEG C × 3hr
Object guarantees 1350 DEG C).
4) each drafts: 25%, the pushing of multi-frequency, the density of product can reach theoretical density 99.89%.
Step 7, more straight operation
1) removal calendering jacket；
2) 1200 DEG C × 30min is heated；
3) oil pressure planisher is relatively flat under the condition of high temperature, flatness < 2mm.
Step 8, vacuum heat treatment operation
1) vacuum degree: 1.0E-1Pa；
2) it is heated to 1000-1300 DEG C, is kept for 3-5 hours.
Step 9, machining final finished shape production
Product is finally machined into the target of needs, length, width, thickness, chamfering etc..It is processed by customer drawings
Shape.Finally obtained molybdenum niobium target material structure is as shown in Figure 1, 2.
Embodiment two,
What is different from the first embodiment is that a kind of following parameter of molybdenum niobium target manufacture craft of the present embodiment is different.
It is every to need to carry out jolt ramming when filling 25% weight in the dress powder operation of step 2 gum cover, vibrate 3min.
In step 5,2) temperature range when degasification is controlled at 350 DEG C, and vacuum degree control is 1 × 10- 4Within the scope of Pa,
Time is maintained at 2.5h.3) after degasification, carry out hot isostatic pressing operation to product: temperature and pressure are controlled respectively 1500
DEG C, 150MPa, continue 6h pressure and heating operation carry out simultaneously.After eventually passing through calendering operation, it is close that product can reach its theory
The 99.85% of degree.
Embodiment three,
What is different from the first embodiment is that a kind of following parameter of molybdenum niobium target manufacture craft of the present embodiment is different.
It is every to need to carry out jolt ramming when filling 25% weight in the dress powder operation of step 2 gum cover, vibrate 5min.
In step 5,2) temperature when degasification is controlled at 350 DEG C, and vacuum degree control is 5 × 10- 4Within the scope of Pa, the time
It is maintained at 4h.3) after degasification, hot isostatic pressing operation carried out to product: temperature and pressure control respectively 1400 DEG C,
130MPa, continues 2.5h pressure and heating operation carries out simultaneously.The density of product can reach 98% or more theoretical density.Final warp
After crossing calendering operation, product up to its theoretical density 99.83%.
The technical concepts and features of embodiment of above only to illustrate the invention, its object is to allow be familiar with technique
People understands the contents of the present invention and is implemented, and it is not intended to limit the scope of the present invention, all spiritual according to the present invention
The equivalent change or modification that essence is done, should be covered by the scope of protection of the present invention.
Claims (9)
1. a kind of molybdenum niobium target manufacture craft, including Step 1: raw material mixes；Step 2: gum cover fills powder operation；Its feature exists
In: further include
Step 3: isostatic cool pressing operation, room temperature boosting, and after being kept for the predetermined time, remove pressure；
Step 4: hot isostatic pressing step, will carry out jacket operation by the molding finished product of isostatic cool pressing operation, successively in internal material
It is sheathed with internal layer jacket, outer layer jacket on material, outer layer jacket is subjected to welded seal；It will be by the post-job finished product of jacket
Gas removes between portion's material and internal layer jacket；After degasification, hot isostatic pressing operation is carried out to product.
2. molybdenum niobium target manufacture craft according to claim 1, it is characterised in that: in the hot isostatic pressing step, degasification
When temperature range control at 350-500 DEG C, vacuum degree is 1 × 10-4-1×10-3Pa, time are maintained at 2.5h-5h.
3. molybdenum niobium target manufacture craft according to claim 1, it is characterised in that: the temperature control of the hot isostatic pressing operation
System is within the scope of 1000-1500 DEG C, while pressure control continues 2.5-6h in 130MPa-180MPa.
4. molybdenum niobium target manufacture craft according to claim 1, it is characterised in that: further include step 5, roll operation, institute
Calendering operation is stated to remove the outer layer jacket of script；The outer layer jacket of calendering, then welded seal are remake, pressure is remake
The thickness of the outer layer jacket adopted is greater than the thickness of the outer layer jacket of hot isostatic pressing step；Temperature is heated to by heating work
At least 1400 DEG C, duration at least 3h；Work is pushed, each volume under pressure is maintained at 25%.
5. molybdenum niobium target manufacture craft according to claim 1, it is characterised in that: the raw material uses molybdenum powder, niobium powder, institute
Stating molybdenum powder, niobium powder, weight 8.5:1 carries out investment storage bin according to the ratio, and molybdenum powder, niobium powder are mixed in storage bin.
6. molybdenum niobium target manufacture craft according to claim 5, it is characterised in that: the molybdenum powder, niobium powder are in storage bin
Mixed hybrid technique are as follows: be passed through Ar gas and carry out air displacement 10-20min, mix rotation speed are as follows: 6-12 revolution/
Min, activity duration long 60-120min.
7. molybdenum niobium target manufacture craft according to claim 1, it is characterised in that: will mixing in the gum cover dress powder operation
The powder of completion weighs the weight of requirement, fills out into gum cover, every to need to carry out jolt ramming when filling 25% weight, vibrates 1-
5min is finally highly measured.
8. molybdenum niobium target manufacture craft according to claim 1, it is characterised in that: also wrapped between step 3 and step 4
Six faces processing job step is included, the product of isostatic cool pressing is subjected to 6 face processing, the flatness < 1mm in each face of product.
9. molybdenum niobium target manufacture craft according to claim 1, it is characterised in that: after the step of the calendering operation, produce
Product are successively by alignment operation, vacuum heat treatment operation and machining final finished shape production.
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| CN201810974197.7A CN108930020B (en) | 2018-08-24 | 2018-08-24 | Molybdenum niobium target material manufacturing process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110158042A (en) * | 2019-05-08 | 2019-08-23 | 东莞市欧莱溅射靶材有限公司 | A kind of molybdenum niobium alloy rotary target material and preparation method thereof |
| WO2019237515A1 (en) * | 2018-06-12 | 2019-12-19 | 沈志刚 | Method for improving compacted density of battery pole piece, obtained battery pole piece, and battery comprising battery pole piece |
| CN110670032A (en) * | 2019-10-29 | 2020-01-10 | 金堆城钼业股份有限公司 | Molybdenum-nickel-copper multi-element alloy sputtering target material and preparation method thereof |
| CN111058004A (en) * | 2020-01-02 | 2020-04-24 | 宁波江丰电子材料股份有限公司 | Chromium-silicon alloy sputtering target material and preparation method thereof |
| CN111804908A (en) * | 2020-06-04 | 2020-10-23 | 厦门金鹭硬质合金有限公司 | Isostatic pressing soft die sleeve weight-limiting and equal-volume powder filling process and device thereof |
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| CN111058004A (en) * | 2020-01-02 | 2020-04-24 | 宁波江丰电子材料股份有限公司 | Chromium-silicon alloy sputtering target material and preparation method thereof |
| CN111804908A (en) * | 2020-06-04 | 2020-10-23 | 厦门金鹭硬质合金有限公司 | Isostatic pressing soft die sleeve weight-limiting and equal-volume powder filling process and device thereof |
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