CN109047781A - A method of preparing large scale tungsten product - Google Patents
A method of preparing large scale tungsten product Download PDFInfo
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- CN109047781A CN109047781A CN201810932485.6A CN201810932485A CN109047781A CN 109047781 A CN109047781 A CN 109047781A CN 201810932485 A CN201810932485 A CN 201810932485A CN 109047781 A CN109047781 A CN 109047781A
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- 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
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- 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]
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- 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
- B22F3/101—Changing atmosphere
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- 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
- B22F9/026—Spray drying of solutions or suspensions
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- 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
- B22F2009/044—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by jet milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
A method of large scale tungsten product is prepared, powder metallurgical technology is belonged to.First to restore tungsten powder as raw material, handle to obtain fine grain tungsten powder using airflow milling.Then tungsten powder aggregate is prepared by atomizing granulating technology, aggregate is in that complete spherical and size distribution is controllable, can reach the powder accumulation state of rule.Tungsten granulation aggregate is pressed by green compact using isostatic cool pressing mode.Then it is slowly heated up and sintering method that high temperature is rapidly heated using low temperature, obtains the large scale tungsten slab of high-compactness, excellent dimensions uniformity.The low-temperature sintering stage slowly heats up, and restoring green body sufficiently, to keep its sintering activity, the high temperature sintering stage is rapidly heated, and can be reduced crystal grain and grows up to reduce oxygen content in green body.The preparation method solves the problems, such as that previous large scale thick tungsten plate is easy to appear the loose, crackle in part, and for the tungsten slab thickness prepared in 30mm or so, consistency reaches 97% or more, and can guarantee the dimensional homogeneity of steel slab surface and center.
Description
Technical field
The invention belongs to powder metallurgical technologies, specifically provide a kind of method for preparing large scale tungsten product.
Background technique
Tungsten is shown at high temperature because having the characteristics that high-melting-point, thermal conductivity are good, thermal expansion is small and capability of resistance to radiation is excellent
Good ermal physics and mechanical property are the irreplaceable critical materials of the high-temperature applications such as national defence, core or space flight.It is wherein big
Size tungsten product is widely used in important component and the ion sputtering, ion implanting, plated film industry etc. of superhigh temperature furnace.Greatly
The development of the high-end equipment such as type crystal growth, plated film proposes the tungsten crucible, thermal field element and high-purity target of big specification more next
Higher requirement.For example, tungsten crucible is the critical component that melt is contained in sapphire crystallization furnace, it is single as chip size increases
Brilliant furnace develops towards enlarged direction, and tungsten crucible size used is increasing.The manufacture of tungsten product generally uses powder metallurgy work
Skill, i.e. " preparation-isostatic cool pressing of tungsten powder-Medium frequency induction sintering-deformation process ".However, for large-sized tungsten product
It develops, to pay close attention to two problems of density uniformity and dimensional accuracy.Compared with small sized article, large scale product blanks
Various pieces often result in material crystalline substance in forming, heat/power history experienced, environment can have larger difference in sintering process
Grain is non-homogeneous to grow up, internal stress and deformation of products.Different-thickness position density has a larger difference, and thickness is thicker to be more difficult to reduction, more
Hard-to-sinter is fine and close, and surface densification and center densification degree are different, cause slab each position shrink uniform sex differernce compared with
Greatly, the case where being easy to appear loose part, crackle, this will lead to slab and cracking phenomena occurs in deformation after unloading processing, seriously
Influence board quality；In addition, large scale slab is each in compacting process since serious agglomeration phenomenon often occurs in raw material tungsten powder
The sintering temperature difference of each position, leads to the receipts of slab each position in the powder accumulation state difference and sintering process of position
Contracting uniformity is different, so that prepared tungsten product dimensional accuracy is poor.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing large scale tungsten product.The present invention is from improving raw material powder
The angle of mobility and sintering activity is set out, and is handled using airflow milling and is carried out dispersing to be crushed to tungsten powder, and the sintering for improving powder is living
Property；And granulation tungsten powder, the powder accumulation state of implementation rule, eventually by isostatic cool pressing are prepared using the technique of mist projection granulating
Forming and the slow sintering process of low temperature, are prepared the large scale thick tungsten plate base of high-compactness, excellent dimensions uniformity.Prepare work
Skill is as shown in Figure 1.
A method of preparing large scale tungsten product, it is characterised in that: to restore tungsten powder as raw material, handle using airflow milling
It is uniformly dispersed, narrow particle size distribution, subsphaeroidal fine grain tungsten powder, powder flowbility and sintering activity at this time increases
By force.Then tungsten powder aggregate is prepared by atomizing granulating technology, aggregate is in that complete spherical and size distribution is controllable, can be reached
To the powder accumulation state of rule, to greatly reduce the formation for being closed hole during the sintering process.In addition, forming technology uses
The method of isostatic cool pressing, sintering process are slowly heated up and method that high temperature is rapidly heated using low temperature, and high cause is finally prepared
The thick tungsten plate base of density, excellent dimensions uniformity, specific process step are as follows:
Step 1: carrying out airflow milling twice using to spray formula air-flow mill apparatus to raw material tungsten powder and handling；First time airflow milling
Keep powder surface rounder and more smooth, further increases the mobility of powder；Airflow milling is all made of nitrogen as abrasive media twice, makes
Oxygen content≤0.05% in grinding chamber.Finally obtain airflow milling processing fine grain tungsten powder；
Step 2: airflow milling, which is handled fine grain tungsten powder, binder, deionized water, is mixed and made into slurry.Specifically, first
Binder and deionized water are uniformly mixed and made into solution A, the binder content in the solution A is 5~15wt.%, then
Airflow milling processing fine grain tungsten powder is added in solution A and carries out mechanical stirring to being uniformly mixed, slurry is made, in the slurry
Solid concentration is 60~85wt.%；
Step 3: using centrifugal spray dryer to affiliated slurry carry out mist projection granulating, the range of speeds be 16000~
20000r/min, atomizing pressure are 100~300kPa, and drying temperature is at 90~150 DEG C；
Step 4: tungsten powder aggregate is put into tube furnace be passed through high-purity hydrogen carry out degreasing, skimming temp be 650~
1000 DEG C, heating rate be 5~10 DEG C/min, soaking time be 60~120min, obtain degreasing tungsten powder aggregate；By degreasing tungsten
Powder ball aggressiveness is pre-sintered in hydrogen atmosphere at 1400~1800 DEG C, obtains the granulation tungsten powder of low oxygen content；
Step 5: the granulation tungsten powder is fitted into swaging mold, and Vacuum Package is carried out, then uses cold isostatic pressing
Green compact, isostatic cool pressing suppress pressure be 200~280MPa, the dwell time be 5~10min；
Step 6: using the two-step sintering method of low temperature hydrogen reduction and high temperature argon sintering；The first step is in hydrogen shield
Frequency sintering furnace carries out low-temperature reduction sintering to the green compact, and low-temperature reduction slab is transferred in high-purity argon gas atmosphere protection by second step
High temperature sintering is carried out in frequency furnace, finally obtains the tungsten slab of high-compactness, high structural homogenity.
Further, step 1 is using jet milling process twice, first time airflow milling set grinding chamber pressure as 0.75~
0.80MPa, the frequency of separation wheel are 10~30Hz, realize the dispersion of powder and are crushed；Second of airflow milling sets grinding chamber pressure
It is by force 0.65~0.70MPa, the frequency of separation wheel is 40~60Hz；Treated particulate handles the average grain of tungsten powder through tungsten powder
Diameter < 6 μm；The tungsten aggregate obtained using mist projection granulating, even particle size distribution, particle size range are 20~50 μm, and pattern has been presented
Global type.
Further, binder described in step 2 can be the polymer such as polyvinyl alcohol, polyethylene glycol, stearic acid, paraffin
Based binder.
Further, the two-step sintering method described in step 6 is: first by heating of plate blank to 1400~1800 DEG C, heating
Rate is 4~6 DEG C/min, and soaking time is 3~5h；Then by heating of plate blank to 2100~2400 DEG C, heating rate is 10~
15 DEG C/min, soaking time is 20~35h；The low-temperature sintering stage slowly heats up, and restores green body sufficiently to reduce oxygen in green body
Content, green body oxygen content≤0.02%；The high temperature sintering stage is rapidly heated, and can be reduced crystal grain and grows up, and crystallite dimension is fine powder
2~5 times of grain diameter.
Further, the target tungsten slab, consistency 97% or more, and steel slab surface dimensional accuracy be ±
0.5mm。
Compared with prior art, the invention has the following advantages that
One, it is handled using airflow milling and de-agglomerated is carried out to raw material tungsten powder, obtain particulate through tungsten powder, and use mist projection granulating work
The bulky grain that skill is handled to obtain full spherical through tungsten powder to particulate is granulated tungsten aggregate.On the one hand, it is made with fine grain powder
Grain, fine powder have higher surface energy, the sintering activity of prilling powder are improved, to promote densification；On the other hand, it makes
Grain powder realizes the accumulation of rule, is conducive to even green body in sintering stage and shrinks, improves dimensional homogeneity；
Two, slowly heated up using low temperature and sintering method that high temperature is rapidly heated.The low-temperature sintering stage slowly heats up, and makes base
Body is sufficiently restored to reduce oxygen content in green body to keep its sintering activity.In addition, the high temperature sintering stage is rapidly heated, can subtract
Few crystal grain is grown up；
Three, the tungsten slab finally prepared is large scale slab, and thickness can reach 97% or more in 30mm or so, consistency,
And it can guarantee the dimensional accuracy of steel slab surface each position.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Embodiment 1:
Using to spray formula air-flow mill apparatus, to particle diameter distribution be (d10=1.1 μm, d50=4.8 μm, d90=15.3 μm)
Raw material tungsten powder carries out airflow milling twice and handles.First time airflow milling sets grinding chamber pressure as 0.80MPa, and the frequency of separation wheel is
30Hz realizes the dispersion of powder and is crushed.Second of airflow milling sets grinding chamber pressure as 0.70MPa, and the frequency of separation wheel is
60Hz keeps powder surface rounder and more smooth, further increases the mobility of powder.Airflow milling is all made of nitrogen as grinding medium twice
Matter makes oxygen content≤0.05% in grinding chamber.Airflow milling processing fine grain tungsten powder is finally obtained, particle diameter distribution is (d10=1.3 μ
M, d50=1.9 μm, d90=2.8 μm).Airflow milling is handled into fine grain tungsten powder, paraffin, deionized water and is mixed and made into slurry, it is first
Paraffin and deionized water are uniformly first mixed and made into solution A, the paraffin content in the solution A is 10wt.%, then in solution
Airflow milling processing fine grain tungsten powder is added in A and carries out mechanical stirring to being uniformly mixed, slurry is made, solid phase contains in the slurry
Amount is 90wt.%.Mist projection granulating is carried out to affiliated slurry using centrifugal spray dryer.Revolving speed is 16000r/min, atomization
Pressure is 100kPa, and for drying temperature at 90 DEG C, the average grain diameter for obtaining tungsten powder aggregate is 20 μm.Tungsten powder aggregate is put into pipe
Be passed through in formula furnace high-purity hydrogen carry out degreasing, 1000 DEG C of skimming temp, heating rate be 5 DEG C/min, soaking time 120min,
Obtain degreasing tungsten powder aggregate.Degreasing tungsten powder aggregate is pre-sintered in hydrogen atmosphere at 1400 DEG C, hypoxemia is obtained and contains
The granulation tungsten powder of amount, oxygen content in power≤0.05%.The granulation tungsten powder is fitted into swaging mold, and carries out Vacuum Package,
Then the green compact of cold isostatic pressing are used, it is 280MPa, dwell time 10min that isostatic cool pressing, which suppresses pressure,.Sintering is in hydrogen
It is carried out in protection Intermediate frequency sintering furnace, first by heating of plate blank to 1500 DEG C, heating rate is 6 DEG C/min, soaking time 3h；So
Afterwards by heating of plate blank to 2100 DEG C, heating rate is 15 DEG C/min, soaking time 20h.Sintering is completed can be obtained high-densit
The tungsten slab of degree, excellent dimensions uniformity, consistency reach 97% or more.
Embodiment 2:
Using to spray formula air-flow mill apparatus, to particle diameter distribution be (d10=1.5 μm, d50=5.2 μm, d90=16.8 μm)
Raw material tungsten powder carries out airflow milling twice and handles.First time airflow milling sets grinding chamber pressure as 0.78MPa, and the frequency of separation wheel is
30Hz realizes the dispersion of powder and is crushed.Second of airflow milling sets grinding chamber pressure as 0.68MPa, and the frequency of separation wheel is
55Hz keeps powder surface rounder and more smooth, further increases the mobility of powder.Airflow milling is all made of nitrogen as grinding medium twice
Matter makes oxygen content≤0.05% in grinding chamber.Airflow milling processing fine grain tungsten powder is finally obtained, particle diameter distribution is (d10=1.8 μ
M, d50=2.5 μm, d90=3.9 μm).Airflow milling is handled into fine grain tungsten powder, paraffin, deionized water and is mixed and made into slurry, it is first
Paraffin and deionized water are uniformly first mixed and made into solution B, the paraffin content in the solution B is 9wt.%, then in solution B
Middle addition airflow milling handles fine grain tungsten powder and carries out mechanical stirring to being uniformly mixed, and slurry is made, solid phase contains in the slurry
Amount is 80wt.%.Mist projection granulating is carried out to affiliated slurry using centrifugal spray dryer.Revolving speed is 17000r/min, atomization
Pressure is 150kPa, and for drying temperature at 90 DEG C, the average grain diameter for obtaining tungsten powder aggregate is 24 μm.Tungsten powder aggregate is put into pipe
Be passed through in formula furnace high-purity hydrogen carry out degreasing, 850 DEG C of skimming temp, heating rate be 5 DEG C/min, soaking time 120min,
Obtain degreasing tungsten powder aggregate.Degreasing tungsten powder aggregate is pre-sintered in hydrogen atmosphere at 1500 DEG C, hypoxemia is obtained and contains
The granulation tungsten powder of amount, oxygen content in power≤0.05%.The granulation tungsten powder is fitted into swaging mold, and carries out Vacuum Package,
Then the green compact of cold isostatic pressing are used, it is 260MPa, dwell time 10min that isostatic cool pressing, which suppresses pressure,.Sintering is in hydrogen
It is carried out in protection Intermediate frequency sintering furnace, first by heating of plate blank to 1550 DEG C, heating rate is 6 DEG C/min, soaking time 3h；So
Afterwards by heating of plate blank to 2200 DEG C, heating rate is 15 DEG C/min, soaking time 20h.Sintering is completed can be obtained high-densit
The tungsten slab of degree, excellent dimensions uniformity, consistency reach 97% or more.
Embodiment 3:
Using to spray formula air-flow mill apparatus, to particle diameter distribution be (d10=2.9 μm, d50=7.1 μm, d90=20.3 μm)
Raw material tungsten powder carries out airflow milling twice and handles.First time airflow milling sets grinding chamber pressure as 0.75MPa, and the frequency of separation wheel is
20Hz realizes the dispersion of powder and is crushed.Second of airflow milling sets grinding chamber pressure as 0.70MPa, and the frequency of separation wheel is
50Hz keeps powder surface rounder and more smooth, further increases the mobility of powder.Airflow milling is all made of nitrogen as grinding medium twice
Matter makes oxygen content≤0.05% in grinding chamber.Airflow milling processing fine grain tungsten powder is finally obtained, particle diameter distribution is (d10=3.4 μ
M, d50=4.4 μm, d90=5.9 μm).Airflow milling is handled into fine grain tungsten powder, polyethylene glycol, deionized water and is mixed and made into slurry
Material, is uniformly mixed and made into solution C for polyethylene glycol and deionized water first, the polyethyleneglycol content in the solution C is
Then airflow milling processing fine grain tungsten powder is added in solution C and carries out mechanical stirring to being uniformly mixed, slurry is made by 8wt.%
Expect, solid concentration is 75wt.% in the slurry.Mist projection granulating is carried out to affiliated slurry using centrifugal spray dryer.Turn
Speed is 18000r/min, and atomizing pressure 200kPa, for drying temperature at 130 DEG C, the average grain diameter for obtaining tungsten powder aggregate is 35 μ
m.Tungsten powder aggregate is put into tube furnace and is passed through high-purity hydrogen and carries out degreasing, skimming temp is 750 DEG C, heating rate be 5 DEG C/
Min, soaking time 90min obtain degreasing tungsten powder aggregate.By degreasing tungsten powder aggregate 1600 DEG C in hydrogen atmosphere into
Row is pre-sintered, and obtains the granulation tungsten powder of low oxygen content, oxygen content in power≤0.05%.The granulation tungsten powder is packed into swaging mold
In, and Vacuum Package is carried out, the green compact of cold isostatic pressing are then used, it is 240MPa, dwell time that isostatic cool pressing, which suppresses pressure,
For 8min.Sintering carries out in hydrogen shield Intermediate frequency sintering furnace, first by heating of plate blank to 1600 DEG C, heating rate is 5 DEG C/
Min, soaking time 4h；Then by heating of plate blank to 2300 DEG C, heating rate is 12 DEG C/min, soaking time 25h.Sintering
The tungsten slab of high-compactness, excellent dimensions uniformity can be obtained in completion, and consistency reaches 96% or more.
Embodiment 4:
Using to spray formula air-flow mill apparatus, to particle diameter distribution be (d10=3.3 μm, d50=8.5 μm, d90=23.5 μm)
Raw material tungsten powder carries out airflow milling twice and handles.First time airflow milling sets grinding chamber pressure as 0.70MPa, and the frequency of separation wheel is
10Hz realizes the dispersion of powder and is crushed.Second of airflow milling sets grinding chamber pressure as 0.65MPa, and the frequency of separation wheel is
40Hz keeps powder surface rounder and more smooth, further increases the mobility of powder.Airflow milling is all made of nitrogen as grinding medium twice
Matter makes oxygen content≤0.05% in grinding chamber.Airflow milling processing fine grain tungsten powder is finally obtained, particle diameter distribution is (d10=4.6 μ
M, d50=5.3 μm, d90=6.9 μm).Airflow milling is handled into fine grain tungsten powder, polyvinyl alcohol, deionized water and is mixed and made into slurry
Material, is uniformly mixed and made into solution D for polyvinyl alcohol and deionized water first, the polyvinyl alcohol content in the solution D is
Then airflow milling processing fine grain tungsten powder is added in solution D and carries out mechanical stirring to being uniformly mixed, slurry is made by 5wt.%
Expect, solid concentration is 65wt.% in the slurry.Mist projection granulating is carried out to affiliated slurry using centrifugal spray dryer.Turn
Speed is 20000r/min, and atomizing pressure 300kPa, for drying temperature at 150 DEG C, the average grain diameter for obtaining tungsten powder aggregate is 46 μ
m.Tungsten powder aggregate is put into tube furnace and is passed through high-purity hydrogen and carries out degreasing, skimming temp is 650 DEG C, heating rate be 5 DEG C/
Min, soaking time 60min obtain degreasing tungsten powder aggregate.By degreasing tungsten powder aggregate 1800 DEG C in hydrogen atmosphere into
Row is pre-sintered, and obtains the granulation tungsten powder of low oxygen content, oxygen content in power≤0.05%.The granulation tungsten powder is packed into swaging mold
In, and Vacuum Package is carried out, the green compact of cold isostatic pressing are then used, it is 200MPa, dwell time that isostatic cool pressing, which suppresses pressure,
For 5min.Sintering carries out in hydrogen shield Intermediate frequency sintering furnace, first by heating of plate blank to 1800 DEG C, heating rate is 4 DEG C/
Min, soaking time 5h；Then by heating of plate blank to 2400 DEG C, heating rate is 15 DEG C/min, soaking time 35h.Sintering
The tungsten slab of high-compactness, excellent dimensions uniformity can be obtained in completion, and consistency reaches 95% or more.
Claims (5)
1. a kind of method for preparing large scale tungsten product, it is characterised in that: to restore tungsten powder as raw material, handled using airflow milling
To be uniformly dispersed, narrow particle size distribution, subsphaeroidal fine grain tungsten powder；Then tungsten powder is prepared by atomizing granulating technology to reunite
Body；In addition, the method that forming technology uses isostatic cool pressing, sintering process is slowly heated up and side that high temperature is rapidly heated using low temperature
The thick tungsten plate base of high-compactness, excellent dimensions uniformity, specific process step is finally prepared in method are as follows:
Step 1: carrying out airflow milling twice using to spray formula air-flow mill apparatus to raw material tungsten powder and handling；First time airflow milling makes powder
Last surface is rounder and more smooth, further increases the mobility of powder；Airflow milling is all made of nitrogen as abrasive media twice, makes to grind
Intracavitary oxygen content≤0.05% finally obtains airflow milling processing fine grain tungsten powder；
Step 2: airflow milling, which is handled fine grain tungsten powder, binder, deionized water, is mixed and made into slurry；Specifically, will glue first
Knot agent and deionized water are uniformly mixed and made into solution A, and the binder content in the solution A is 5~15wt.%, then molten
Airflow milling processing fine grain tungsten powder is added in liquid A and carries out mechanical stirring to being uniformly mixed, slurry, solid phase in the slurry is made
Content is 60~85wt.%；
Step 3: using centrifugal spray dryer to affiliated slurry carry out mist projection granulating, the range of speeds be 16000~
20000r/min, atomizing pressure are 100~300kPa, and drying temperature is at 90~150 DEG C；
Degreasing is carried out Step 4: tungsten powder aggregate is put into tube furnace and is passed through high-purity hydrogen, skimming temp is 650~1000
DEG C, heating rate be 5~10 DEG C/min, soaking time be 60~120min, obtain degreasing tungsten powder aggregate；By degreasing tungsten powder group
Aggressiveness is pre-sintered in hydrogen atmosphere at 1400~1800 DEG C, obtains the granulation tungsten powder of low oxygen content；
Step 5: the granulation tungsten powder is fitted into swaging mold, and Vacuum Package is carried out, then uses the life of cold isostatic pressing
Base, it is 200~280MPa that isostatic cool pressing, which suppresses pressure, and the dwell time is 5~10min；
Step 6: using the two-step sintering method of low temperature hydrogen reduction and high temperature argon sintering；The first step is burnt in hydrogen shield intermediate frequency
Freezing of a furnace carries out low-temperature reduction sintering to the green compact, and low-temperature reduction slab is transferred to high-purity argon gas atmosphere protection intermediate frequency furnace by second step
Middle carry out high temperature sintering, finally obtains the tungsten slab of high-compactness, high structural homogenity.
2. the method for preparation large scale tungsten product according to claim 1, it is characterised in that: using secondary air-flow grinder twice
Skill, first time airflow milling set grinding chamber pressure as 0.75~0.80MPa, and the frequency of separation wheel is 10~30Hz, realizes powder
Dispersion and broken；Second of airflow milling sets grinding chamber pressure as 0.65~0.70MPa, and the frequency of separation wheel is 40~
60Hz；Treated particulate handles partial size < 6 μm of tungsten powder through tungsten powder；The tungsten aggregate obtained using mist projection granulating, granularity point
Cloth is uniform, and particle size range is 20~50 μm, and full spherical is presented in pattern.
3. the method for preparation large scale tungsten product according to claim 1, it is characterised in that binder described in step 2 is
Polyvinyl alcohol, polyethylene glycol, stearic acid, paraffmic-based polymer based binder.
4. the method for preparation large scale tungsten product according to claim 1, it is characterised in that: the two-step sintering method is:
First by heating of plate blank to 1400~1800 DEG C, heating rate is 4~6 DEG C/min, and soaking time is 3~5h；Then by slab
2100~2400 DEG C are heated to, heating rate is 10~15 DEG C/min, and soaking time is 20~35h；The low-temperature sintering stage is slow
Heating, restores green body sufficiently to reduce oxygen content in green body, green body oxygen content≤0.02%；The high temperature sintering stage quickly rises
Temperature can be reduced crystal grain and grow up, and crystallite dimension is 2~5 times of fine powder granules partial size.
5. the method for preparation large scale tungsten product according to claim 1, it is characterised in that: the target tungsten slab,
Consistency is 97% or more, and steel slab surface dimensional accuracy is ± 0.5mm.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109676124A (en) * | 2018-12-24 | 2019-04-26 | 北京科技大学 | A kind of sintering densification and crystallite dimension control method of metal material |
| CN110699584A (en) * | 2019-11-28 | 2020-01-17 | 西北有色金属研究院 | Preparation method of high-density low-strength low-plasticity alloy material for pulse impact energy absorption |
| CN110722171A (en) * | 2019-09-30 | 2020-01-24 | 北京科技大学 | Method for preparing rare earth oxide doped tungsten and molybdenum spherical powder for 3D printing |
| CN110788318A (en) * | 2019-10-29 | 2020-02-14 | 安泰天龙（宝鸡）钨钼科技有限公司 | Preparation method of high-density rare earth tungsten electrode |
| CN111254396A (en) * | 2020-01-21 | 2020-06-09 | 洛阳高新四丰电子材料有限公司 | Preparation method of molybdenum-tungsten alloy sputtering target material |
| CN111575659A (en) * | 2020-05-19 | 2020-08-25 | 湖南金天铝业高科技股份有限公司 | Preparation method of titanium-aluminum alloy target material |
| CN113385679A (en) * | 2021-06-17 | 2021-09-14 | 安徽寒锐新材料有限公司 | Method for preparing cobalt powder with high apparent density |
| CN115415526A (en) * | 2021-05-13 | 2022-12-02 | 安泰天龙钨钼科技有限公司 | Oversized tungsten tube and preparation method thereof |
| US11673196B2 (en) | 2018-12-24 | 2023-06-13 | University Of Science And Technology Beijing | Metal material sintering densification and grain size control method |
| CN116444263A (en) * | 2023-03-15 | 2023-07-18 | 先导薄膜材料(安徽)有限公司 | Sintering process of indium tin oxide target |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002371301A (en) * | 2001-06-18 | 2002-12-26 | Allied Material Corp | Tungsten sintered compact and manufacturing method therefor |
| CN105382255A (en) * | 2015-12-14 | 2016-03-09 | 北京科技大学 | Nano tungsten powder injection molding method |
| CN105478776A (en) * | 2015-12-14 | 2016-04-13 | 北京科技大学 | Method for preparing high-density pure tungsten product through low-temperature sintering |
| CN105478745A (en) * | 2015-12-04 | 2016-04-13 | 西安瑞福莱钨钼有限公司 | Method for preparing tungsten slab by low-temperature sintering |
| CN106216690A (en) * | 2016-08-24 | 2016-12-14 | 洛阳金鹭硬质合金工具有限公司 | A kind of preparation method of slug type thermal spraying tungsten powder of reuniting |
| KR20170044343A (en) * | 2015-10-15 | 2017-04-25 | 희성금속 주식회사 | Preparation method of reuse tungsten target and the reuse tungsten target prepared thereby |
| CN106944629A (en) * | 2016-10-06 | 2017-07-14 | 江西理工大学 | A kind of preparation method of monodisperse superfine/nano-tungsten powder |
-
2018
- 2018-08-16 CN CN201810932485.6A patent/CN109047781B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002371301A (en) * | 2001-06-18 | 2002-12-26 | Allied Material Corp | Tungsten sintered compact and manufacturing method therefor |
| KR20170044343A (en) * | 2015-10-15 | 2017-04-25 | 희성금속 주식회사 | Preparation method of reuse tungsten target and the reuse tungsten target prepared thereby |
| CN105478745A (en) * | 2015-12-04 | 2016-04-13 | 西安瑞福莱钨钼有限公司 | Method for preparing tungsten slab by low-temperature sintering |
| CN105382255A (en) * | 2015-12-14 | 2016-03-09 | 北京科技大学 | Nano tungsten powder injection molding method |
| CN105478776A (en) * | 2015-12-14 | 2016-04-13 | 北京科技大学 | Method for preparing high-density pure tungsten product through low-temperature sintering |
| CN106216690A (en) * | 2016-08-24 | 2016-12-14 | 洛阳金鹭硬质合金工具有限公司 | A kind of preparation method of slug type thermal spraying tungsten powder of reuniting |
| CN106944629A (en) * | 2016-10-06 | 2017-07-14 | 江西理工大学 | A kind of preparation method of monodisperse superfine/nano-tungsten powder |
Non-Patent Citations (1)
| Title |
|---|
| 黄化等: "气流磨处理钨粉的研究", 《稀有金属材料与工程》 * |
Cited By (15)
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| US11673196B2 (en) | 2018-12-24 | 2023-06-13 | University Of Science And Technology Beijing | Metal material sintering densification and grain size control method |
| CN109676124A (en) * | 2018-12-24 | 2019-04-26 | 北京科技大学 | A kind of sintering densification and crystallite dimension control method of metal material |
| CN110722171B (en) * | 2019-09-30 | 2024-05-28 | 北京科技大学 | Method for preparing rare earth oxide doped tungsten and molybdenum spherical powder for 3D printing |
| CN110722171A (en) * | 2019-09-30 | 2020-01-24 | 北京科技大学 | Method for preparing rare earth oxide doped tungsten and molybdenum spherical powder for 3D printing |
| CN110788318A (en) * | 2019-10-29 | 2020-02-14 | 安泰天龙（宝鸡）钨钼科技有限公司 | Preparation method of high-density rare earth tungsten electrode |
| CN110788318B (en) * | 2019-10-29 | 2022-08-12 | 安泰天龙（宝鸡）钨钼科技有限公司 | Preparation method of high-density rare earth tungsten electrode |
| CN110699584A (en) * | 2019-11-28 | 2020-01-17 | 西北有色金属研究院 | Preparation method of high-density low-strength low-plasticity alloy material for pulse impact energy absorption |
| CN111254396A (en) * | 2020-01-21 | 2020-06-09 | 洛阳高新四丰电子材料有限公司 | Preparation method of molybdenum-tungsten alloy sputtering target material |
| CN111575659A (en) * | 2020-05-19 | 2020-08-25 | 湖南金天铝业高科技股份有限公司 | Preparation method of titanium-aluminum alloy target material |
| CN115415526A (en) * | 2021-05-13 | 2022-12-02 | 安泰天龙钨钼科技有限公司 | Oversized tungsten tube and preparation method thereof |
| CN113385679A (en) * | 2021-06-17 | 2021-09-14 | 安徽寒锐新材料有限公司 | Method for preparing cobalt powder with high apparent density |
| CN116444263A (en) * | 2023-03-15 | 2023-07-18 | 先导薄膜材料(安徽)有限公司 | Sintering process of indium tin oxide target |
| CN116444263B (en) * | 2023-03-15 | 2024-02-27 | 先导薄膜材料(安徽)有限公司 | Sintering process of indium tin oxide target |
| CN117840437A (en) * | 2024-02-28 | 2024-04-09 | 江西国创院新材料有限公司 | Preparation method of copper-based composite material powder for laser 3D printing |
| CN117840437B (en) * | 2024-02-28 | 2024-06-07 | 江西国创院新材料有限公司 | Preparation method of copper-based composite material powder for laser 3D printing |
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