CN108772558A - A kind of compound tungsten crucible of multielement rare earth and its preparation method and application - Google Patents

A kind of compound tungsten crucible of multielement rare earth and its preparation method and application Download PDF

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CN108772558A
CN108772558A CN201810619330.7A CN201810619330A CN108772558A CN 108772558 A CN108772558 A CN 108772558A CN 201810619330 A CN201810619330 A CN 201810619330A CN 108772558 A CN108772558 A CN 108772558A
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tungsten
rare earth
crucible
composite
tungsten powder
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张帆
袁德林
文小强
张金祥
欧阳希
王玉香
普建
钟婷
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GANZHOU NONFERROUS METALLURGICAL INSTITUTE
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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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • B22F3/24—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
    • 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
    • B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
    • 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

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Abstract

A kind of compound tungsten crucible of multielement rare earth of present invention offer and its preparation method and application, tungsten crucible prepared by this method has longer service life.The preparation method includes the following steps：1) the RE composite ultrasonic disperse of lanthana, cerium oxide and yttrium oxide composition is obtained into RE composite dispersion liquid in alcohol；2) tungsten powder and the RE composite dispersion liquid are uniformly mixed under vacuum, are dried in vacuo to obtain mixture later；3) mixture obtained by step 2) is fitted into progress isostatic cool pressing compacting in mold, obtains green compact；4) green compact that step 3) obtains is sintered under vacuum, sintering temperature is 1800-2100 DEG C, and soaking time is 4-10 hours, later cooling down.It is in terms of 100% by the gross mass of tungsten powder used in RE composite used in step 1) and step 2), the mass fraction of tungsten powder is 97.5%-99%, the mass fraction of RE composite is 1%~2.5%, and the mass fraction of lanthana, cerium oxide and yttrium oxide is respectively 0.2%~1%.

Description

A kind of compound tungsten crucible of multielement rare earth and its preparation method and application
Technical field
The present invention relates to tungsten crucible technical field, more particularly to a kind of compound tungsten crucible of multielement rare earth and preparation method thereof and Using.
Background technology
Tungsten crucible because of it with excellent elevated temperature strength, strong anti-friction corrosion resistance, coefficient of thermal expansion is small, quenching degree is good etc. Feature is widely used in the industries such as rare-earth smelting, crystal growth.Tungsten crucible can be in 2600 DEG C of vacuum inert gas below It uses, is the cord cage in the industrial furnaces such as rare-earth smelting stove, monocrystal growing furnace.It is existing to prepare tungsten crucible technology mainly including burning Form type, punch forming, spun type, welding fabrication etc..
The tungsten crucible of welding fabrication, due to weld seam existing defects, service life is shorter at high temperature.
The tungsten crucible of rotary press modelling is process using pure tungsten plate, leaf and pure tungsten stick through corresponding technique, due to processing Deformation generates defective wood, and material consumption is very fast at high temperature, and production cost is excessively high.
The tungsten crucible of sinter molding utilize PM technique, it is easily prepared go out the less tungsten crucible of the uniform defect of material, But its service life is still shorter, causes high pure rare earth metals production cost higher.
Therefore, high-purity, material is uniform, and the longer tungsten crucible of service life urgently researches and develops preparation.
Invention content
The present invention is to make up the deficiencies in the prior art, provides a kind of preparation side of the compound tungsten crucible of multielement rare earth Method, this method preparation process is simple, and tungsten crucible obtained more dense uniform and hardness height, can largely reduce tungsten crucible Defect has longer service life.
The present invention is to reach its purpose, and the technical solution of use is as follows：
The present invention provides a kind of preparation method of the compound tungsten crucible of multielement rare earth, includes the following steps：
1) it is multiple to be obtained into rare earth in alcohol for the RE composite ultrasonic disperse of lanthana, cerium oxide and yttrium oxide composition Close object dispersion liquid；
2) tungsten powder and the RE composite dispersion liquid are uniformly mixed under vacuum, are dried in vacuo to obtain mixing later Material；Tungsten powder used in the step includes that mass ratio is 15:1-20:The tungsten powder of 1-3 μm of the tungsten powder and granularity of 1 4-6 μm of granularity；
3) mixture obtained by step 2) is fitted into progress isostatic cool pressing compacting in mold, obtains green compact；
4) green compact that step 3) obtains is sintered under vacuum, sintering temperature is 1800-2100 DEG C, and soaking time is 4-10 hours, cooling down later；
It is tungsten powder in terms of 100% by the gross mass of tungsten powder used in RE composite used in step 1) and step 2) Mass fraction be 97.5%-99%, the mass fraction of RE composite is 1%~2.5%, and lanthana, cerium oxide and oxygen The mass fraction for changing yttrium is respectively 0.2%~1%.It is respectively 0.2%~1% lanthana, cerium oxide and oxidation using dosage Yttrium, and be 1%~2.5% by three's overall control, with mass ratio 15:1-20:1-3 μm of the tungsten powder and granularity of 1 4-6 μm of granularity Tungsten powder combination, can be very good enhancing tungsten crucible performance, realize oxide between interaction, avoid rare earth oxide Reunite and causes to be segregated；And rare earth oxide dosage is more, easily causes reunion, influences tungsten crucible performance, and if dosage is very few, nothing Method effectively enhances tungsten crucible performance, and rare earth oxide can not preferably play the role of crystal grain thinning and purification crystal boundary.
The preparation method of the present invention, using micro RE composite, the RE composite is with trace rare-earth lanthana, oxygen Change cerium and yttrium oxide composition, three combines according to specific dosage, in the present invention prepares tungsten crucible technique, can play purification crystal boundary With the effect of crystal grain thinning, the tungsten powder of 1-3 μm of tungsten powder and granularity further using 4-6 μm of granularity is according to mass ratio 15:1-20: 1 addition, using a vacuum-sintering, there is the tungsten crucible of preparation crystal structure evenly, grain-boundary strength higher can have more High service life.
RE composite is carried out ultrasonic disperse by the present invention in alcohol in advance, can preferably realize that RE composite is uniform Distribution, and be easier to RE composite package tungsten powder, avoid be directly appended to occur in batch mixer oxide be unevenly distributed, Phenomena such as reunion.Preferably, in step 1), the ultrasonic disperse is ultrasonic disperse 1- under the conditions of power density 20-40W/L 10min is conducive to RE composite dispersion and is more uniformly distributed using preferred ultrasound condition.
Preferably, in step 2), for tungsten powder and the RE composite dispersion liquid are mixed 10- in Vacuum mixer 30min carries out the vacuum drying again later.
Preferably, mold described in step 3) includes crucible mold core and gum cover, which is mold commonly used in the art, is not made It repeats.In preferred embodiment, the diameter (internal diameter) of the gum cover is bigger 15- than the diameter (outer diameter) of crucible film core 16mm.The material of crucible mold core preferably uses 45# steel.In a particular embodiment, specially mixture is transferred in gum cover, is used Isostatic cool pressing compacting is carried out after rubber plug sealing.
Preferably, in step 3), the process conditions for carrying out isostatic cool pressing compacting include：Forming pressure is 220~270Mpa, Pressurize 10~30 minutes, venting duration are 5~20 minutes.
Further include following steps after step 4) as a kind of specific implementation mode：The tungsten crucible that step 4) is obtained Carry out surface rubbing down.
The preparation method of the present invention, step 4) is described to be sintered to disposal vacuum sintering, and sintering specifically can be in vacuum-sintering It is carried out in stove.
The present invention also provides the compound tungsten crucibles of multielement rare earth made from a kind of preparation method as described above.
The compound tungsten crucible of multielement rare earth produced by the present invention in rare-earth smelting or field of crystal growth particularly suitable for answering With.
Technical solution provided by the invention has the advantages that：
1, the compound tungsten crucible of lanthanum cerium yttrium ternary RE prepared by the present invention, wherein using lanthana, cerium oxide and yttrium oxide Three kinds of rare earth oxides are combined according to specific proportioning, have given full play to the complex effect of three, and the stability of product is excellent.In advance First ultrasonic disperse RE composite, and mixed according to a certain ratio using 2 kinds of varigrained tungsten powders, make three kinds of rare earth oxides It is uniformly distributed in tungsten crucible finished product so that the complex effect of ternary RE compound is more given full play to.
2, the present invention suppresses green compact by isostatic cool pressing, effectively prevents the Density inhomogeneity of green compact, improves billet and causes Density and uniformity.Finally, using disposal vacuum sintering process, reduce process, reduce energy consumption.
3, according to the compound tungsten crucible of lanthanum cerium yttrium ternary RE made of the present invention, tungsten crucible can not only greatly be reduced Defect makes it have higher service life；And the preparation method is easy, is easy to grasp and operate, and production cost is small, uses Effect is good.
Specific implementation mode
For a better understanding of the technical solution of the present invention, with reference to the embodiment content that the present invention is further explained, But present disclosure is not limited only to following embodiment.
Part detection method involved in embodiment is described as follows：Density Detection method is with reference to GB/T 3850-2015；It causes Density calculation is density/theoretical density；Mean grain size detection method is with reference to GB/T 6394-2002；Hardness determination standard With reference to GB/T 230.1-2004.
Embodiment 1
A kind of compound tungsten crucible of multielement rare earth, preparation method includes the following steps：
1) rare earth dispensing：Cerium oxide 30g, yttrium oxide 15g are weighed, lanthana 15g is placed in alcoholic solution, with 20W/L's Ultrasonic echography disperses 3min, obtains rare earth composite dispersion liquid.
2) tungsten powder dispensing：The tungsten powder 2760g that granularity is 5 μm is weighed, 2.5 μm of tungsten powder 180g is weighed.By above-mentioned tungsten powder with The rare earth composite dispersion liquid obtained through ultrasonic disperse is collectively disposed in Vacuum mixer, then batch mixing 15min is dried in vacuo, obtains Mixture.
3) above-mentioned dried mixture is put into crucible die, is put into isostatic pressing machine and carries out isostatic cool pressing compacting, pressure Green compact, pressing pressure (shaping pressure) 220MPa, dwell time 10min, venting duration 5min is made.
4) above-mentioned green compact is placed in vacuum sintering furnace and is sintered, 2000 DEG C of sintering temperature, soaking time 5 hours, with Stove cools down.
The tungsten crucible density of institute's sinter molding is 18.22g/cm3, consistency 94.4%, 7 μm of mean grain size, hardness 71HRA。
Embodiment 2
A kind of compound tungsten crucible of multielement rare earth, preparation method includes the following steps：
1) rare earth dispensing：Cerium oxide 20g, yttrium oxide 20g are weighed, lanthana 20g is placed in alcoholic solution, with 30W/L's Ultrasonic echography disperses 6min, obtains rare earth composite dispersion liquid.
2) tungsten powder dispensing：The tungsten powder 2760g that granularity is 6 μm is weighed, 3 μm of tungsten powder 180g is weighed.By above-mentioned tungsten powder and warp The rare earth composite dispersion liquid that ultrasonic disperse obtains is collectively disposed in Vacuum mixer, and then batch mixing 20min is dried in vacuo, obtain mixed Close material.
3) above-mentioned dried mixture is put into crucible die, is put into isostatic pressing machine and carries out isostatic cool pressing compacting, pressure Green compact, pressing pressure 240MPa, dwell time 15min, venting duration 10min is made.
4) above-mentioned green compact is placed in vacuum sintering furnace and is sintered, 2100 DEG C of sintering temperature, soaking time 6 hours, with Stove cools down.
The tungsten crucible density of institute's sinter molding is 18.29g/cm3, consistency 94.8%, 7 μm of mean grain size, hardness 73HRA。
Embodiment 3
A kind of compound tungsten crucible of multielement rare earth, preparation method includes the following steps：
1) rare earth dispensing：Cerium oxide 20g, yttrium oxide 20g are weighed, lanthana 20g is placed in alcoholic solution, with 30W/L's Ultrasonic echography disperses 6min, obtains rare earth composite dispersion liquid.
2) tungsten powder dispensing：The tungsten powder 2780g that granularity is 6 μm is weighed, 3 μm of tungsten powder 160g is weighed.By above-mentioned tungsten powder and warp The rare earth composite dispersion liquid that ultrasonic disperse obtains is collectively disposed in Vacuum mixer, and then batch mixing 30min is dried in vacuo, obtain mixed Close material.
3) above-mentioned dried mixture is put into crucible die, is put into isostatic pressing machine and carries out isostatic cool pressing compacting, pressure Green compact, pressing pressure 250MPa, dwell time 30min, venting duration 15min is made.
4) above-mentioned green compact is placed in vacuum sintering furnace and is sintered, 2100 DEG C of sintering temperature, soaking time 6 hours, with Stove cools down.
The tungsten crucible density of institute's sinter molding is 18.42g/cm3, consistency 95.4%, 7 μm of mean grain size, hardness 72HRA。
Embodiment 4
A kind of compound tungsten crucible of multielement rare earth, preparation method includes the following steps：
1) rare earth dispensing：Cerium oxide 12g, yttrium oxide 30g are weighed, lanthana 18g is placed in alcoholic solution, with 20W/L's Ultrasonic echography disperses 10min, obtains rare earth composite dispersion liquid.
2) tungsten powder dispensing：The tungsten powder 2800g that granularity is 4 μm is weighed, 3 μm of tungsten powder 140g is weighed.By above-mentioned tungsten powder and warp Ultrasonic disperse obtains rare earth composite dispersion liquid and is collectively disposed in Vacuum mixer, and then batch mixing 20min is dried in vacuo, must mix Material.
3) above-mentioned dried mixture is put into crucible die, is put into isostatic pressing machine and carries out isostatic cool pressing compacting, pressure Green compact, pressing pressure 270MPa, dwell time 10min, venting duration 10min is made.
4) above-mentioned green compact is placed in vacuum sintering furnace and is sintered, 2050 DEG C of sintering temperature, soaking time 8 hours, with Stove cools down.
The tungsten crucible density of institute's sinter molding is 18.32g/cm3, consistency 94.9%, 6 μm of mean grain size, hardness 74HRA。
Comparative example 1
A kind of compound tungsten crucible of multielement rare earth, preparation method includes the following steps：
1) rare earth dispensing：Lanthana 60g is weighed, is placed in alcoholic solution, disperses 10min with the ultrasonic echography of 20W/L, Obtain rare earth dispersion liquid.
2) tungsten powder dispensing：The tungsten powder 2780g that granularity is 6 μm is weighed, 3 μm of tungsten powder 160g is weighed.By above-mentioned tungsten powder and warp Ultrasonic disperse obtains rare earth composite dispersion liquid and is collectively disposed in Vacuum mixer, and then batch mixing 20min is dried in vacuo, must mix Material.
3) above-mentioned dried mixture is put into crucible die, is put into isostatic pressing machine and carries out isostatic cool pressing compacting, pressure Green compact, pressing pressure 220MPa, dwell time 10min, venting duration 5min is made.
4) above-mentioned green compact is placed in vacuum sintering furnace and is sintered, 2100 DEG C of sintering temperature, soaking time 4 hours, with Stove cools down.
The tungsten crucible density of institute's sinter molding is 18.16g/cm3, consistency 94.1%, 10 μm of mean grain size, hardness 68HRA。
Comparative example 2
A kind of compound tungsten crucible of multielement rare earth, preparation method includes the following steps：
1) rare earth dispensing：Yttrium oxide 20g is weighed, lanthana 40 is placed in alcoholic solution, with the ultrasonic echography of 20W/L Disperse 10min, obtains rare earth composite dispersion liquid.
2) tungsten powder dispensing：The tungsten powder 2800g that granularity is 5 μm is weighed, 3 μm of tungsten powder 140g is weighed.By above-mentioned tungsten powder and warp Ultrasonic disperse obtains rare earth composite dispersion liquid and is collectively disposed in Vacuum mixer, and then batch mixing 20min is dried in vacuo, must mix Material.
3) above-mentioned dried mixture is put into crucible die, is put into isostatic pressing machine and carries out isostatic cool pressing compacting, pressure Green compact, pressing pressure 240MPa, dwell time 10min, venting duration 10min is made.
4) above-mentioned green compact is placed in vacuum sintering furnace and is sintered, 2050 DEG C of sintering temperature, soaking time 6 hours, with Stove cools down.
The tungsten crucible density of institute's sinter molding is 18.18g/cm3, consistency 94.2%, 9 μm of mean grain size, hardness 67HRA。
Comparative example 1-2 and embodiment 1-4's the experimental results showed that, the present invention uses lanthana, cerium oxide and yttrium oxide three It plants rare earth oxide to combine according to specific proportioning, technique according to the invention prepares tungsten crucible, answers between three kinds of rare earth oxides Cooperation is used, and tungsten crucible obtained is compared with comparative example 1-2, more dense uniform, and mean grain size is small, and product hardness is high so that Product has more preferably stability and longer service life.
Comparative example 3
A kind of compound tungsten crucible of multielement rare earth, preparation method includes the following steps：
1) rare earth dispensing：Cerium oxide 20g, yttrium oxide 20g are weighed, lanthana 20g is placed in alcoholic solution, with 20W/L's Ultrasonic echography disperses 10min, obtains rare earth composite dispersion liquid.
2) tungsten powder dispensing：The tungsten powder 3000g that granularity is 6 μm is weighed, it is total with rare earth composite dispersion liquid is obtained through ultrasonic disperse With being placed in Vacuum mixer, then batch mixing 20min is dried in vacuo, obtains mixture.
3) above-mentioned dried mixture is put into crucible die, is put into isostatic pressing machine and carries out isostatic cool pressing compacting, pressure Green compact, pressing pressure 250MPa, dwell time 10min, venting duration 15min is made.
4) above-mentioned green compact is placed in vacuum sintering furnace and is sintered, 2000 DEG C of sintering temperature, soaking time 8 hours, with Stove cools down.
The tungsten crucible density of institute's sinter molding is 18.08g/cm3, consistency 93.7%, 9 μm of mean grain size, hardness 67HRA。
Comparative example 4
A kind of compound tungsten crucible of multielement rare earth, preparation method includes the following steps：
1) rare earth dispensing：Cerium oxide 20g, yttrium oxide 15g are weighed, lanthana 25g is placed in alcoholic solution, with 20W/L's Ultrasonic echography disperses 10min, obtains rare earth composite dispersion liquid.
2) tungsten powder dispensing：The tungsten powder 1470g that granularity is 6 μm is weighed, 4 μm of tungsten powder 1470g is weighed and is obtained with through ultrasonic disperse It is collectively disposed in Vacuum mixer to rare earth composite dispersion liquid, then batch mixing 20min is dried in vacuo, obtains mixture.
3) above-mentioned dried mixture is put into crucible die, is put into isostatic pressing machine and carries out isostatic cool pressing compacting, pressure Green compact, pressing pressure 2670MPa, dwell time 15min, venting duration 5min is made.
4) above-mentioned green compact is placed in vacuum sintering furnace and is sintered, 2050 DEG C of sintering temperature, soaking time 6 hours, with Stove cools down.
The tungsten crucible density of institute's sinter molding is 18.1g/cm3, consistency 93.8%, 13 μm of mean grain size, hardness 66HRA。
Comparative example 3-4 and embodiment 1-4's the experimental results showed that, using lanthana, cerium oxide and the specific proportioning of yttrium oxide The composite rare-earth oxide of dosage, with certain mass than the tungsten powder of 4-6 μm of granularity and the tungsten powder of 1-3 μm of granularity combine, according to The technique of the present invention prepares tungsten crucible, and products obtained therefrom not only more dense uniform, mean grain size is small, and product hardness is high, tungsten earthenware The performance of crucible is enhanced.
1 each embodiment and comparative example experimental result of table
It will be understood by those skilled in the art that under the introduction of this specification, the present invention can be made some modifications or Adjustment.These modifications or adjustment should also be as within the scope of the claims in the present invention.

Claims (9)

1. a kind of preparation method of the compound tungsten crucible of multielement rare earth, which is characterized in that include the following steps：
1) the RE composite ultrasonic disperse of lanthana, cerium oxide and yttrium oxide composition is obtained into RE composite in alcohol Dispersion liquid；
2) tungsten powder and the RE composite dispersion liquid are uniformly mixed under vacuum, are dried in vacuo to obtain mixture later； Tungsten powder used in the step includes that mass ratio is 15:1-20:The tungsten powder of 1-3 μm of the tungsten powder and granularity of 1 4-6 μm of granularity；
3) mixture obtained by step 2) is fitted into progress isostatic cool pressing compacting in mold, obtains green compact；
4) green compact that step 3) obtains is sintered under vacuum, sintering temperature is 1800-2100 DEG C, soaking time 4-10 Hour, cooling down later；
It is the matter of tungsten powder in terms of 100% by the gross mass of tungsten powder used in RE composite used in step 1) and step 2) Amount score is 97.5%-99%, and the mass fraction of RE composite is 1%~2.5%, and lanthana, cerium oxide and yttrium oxide Mass fraction be respectively 0.2%~1%.
2. preparation method according to claim 1, which is characterized in that in step 1), the ultrasonic disperse is close in power Ultrasonic disperse 1-10min under the conditions of degree 20-40W/L.
3. preparation method according to claim 1 or 2, which is characterized in that in step 2), to answer tungsten powder and the rare earth It closes object dispersion liquid and mixes 10-30min in Vacuum mixer, carry out the vacuum drying again later.
4. according to claim 1-3 any one of them preparation methods, which is characterized in that mold described in step 3) includes crucible The internal diameter of mold core and gum cover, the gum cover is bigger 15-16mm than the outer diameter of crucible film core.
5. according to claim 1-4 any one of them preparation methods, which is characterized in that in step 3), carry out isostatic cool pressing pressure The process conditions of system include：Forming pressure is 220~270Mpa, and pressurize 10~30 minutes, venting duration is 5~20 minutes.
6. according to claim 1-5 any one of them preparation methods, which is characterized in that after the step 4) further include walking as follows Suddenly：The tungsten crucible that step 4) is obtained carries out surface rubbing down.
7. according to claim 1-6 any one of them preparation methods, which is characterized in that step 4) is described to be sintered to disposably very Sky sintering.
8. a kind of compound tungsten crucible of multielement rare earth as made from claim 1-7 any one of them preparation methods.
9. the application of the compound tungsten crucible of multielement rare earth according to any one of claims 8, which is characterized in that the multielement rare earth composite tungsten earthenware Crucible is applied in rare-earth smelting or crystal growth.
CN201810619330.7A 2018-06-15 2018-06-15 A kind of compound tungsten crucible of multielement rare earth and its preparation method and application Pending CN108772558A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
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