CN107052356A - A kind of preparation method of the tungsten yittrium oxide superfine composite precursor powder of core shell structure - Google Patents
A kind of preparation method of the tungsten yittrium oxide superfine composite precursor powder of core shell structure Download PDFInfo
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- CN107052356A CN107052356A CN201710035239.6A CN201710035239A CN107052356A CN 107052356 A CN107052356 A CN 107052356A CN 201710035239 A CN201710035239 A CN 201710035239A CN 107052356 A CN107052356 A CN 107052356A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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Abstract
The present invention relates to a kind of preparation method of the tungsten yittrium oxide superfine composite precursor powder of core shell structure, by surfactant and Y2O3Powder is dissolved in deionized water or distilled water obtained solution, and ammonium paratungstate is added in solution；By dense HNO3Progress chemical precipitation reaction in above-mentioned solution is added under mechanical agitation and ultrasound condition, suspension is formed；Absolute ethyl alcohol is added in suspension and continues to react, mechanical agitation and ultrasonically treated working condition is in and rotating speed and power are constant, the sediment that reacted suspension is filtered and obtained with washes of absolute alcohol in whole course of reaction；In tube furnace composite oxide power is obtained in calcining under nitrogen or argon stream；The reduction of two steps is carried out with pure hydrogen and obtains the W Y with core shell structure2O3Superfine composite precursor powder.The invention enables to the average grain size of composite precursor powder reach 10~40nm, and grain size distribution has good uniformity.
Description
Technical field
The present invention proposes a kind of a kind of tungsten-yittrium oxide superfine composite forerunner that core shell structure is prepared using wet chemistry method
The preparation method of body powder, belongs to powder preparation engineering technical field.
Background technology
Tungsten and its alloy are because with good machinery, hot property, such as high-melting-point, high thermal conductivity, hardness are big, thermal expansion system
The small, elevated temperature strengths of number are good, ductility is good, toughness is good and ray absorption capacity is good etc. and are taken as being widely used in high temperature
Material, such as turbine, heating element heater, kinetic energy penetrator.Meanwhile, in following fusion reactor, tungsten sill also by
Be considered most future towards plasma (PFM) and Divertor Materials.But, the tungsten base material under recrystallization and radiation parameter
The had fragility of material is always to limit its problem applied in nuclear fusion field.The second phase developed in the recent period (is predominantly carbonized
Thing and oxide) disperse tungsten sill achieves preferable effect in this regard, wherein the Y stablized especially with high temperature properties2O3Add
Plus effect is notable.The tiny Y of grain boundaries2O3Second Phase Particle can effectively hinder the tungsten grain produced in sintering process to grow up, brilliant
The Y of intragranular portion Dispersed precipitate2O3Second Phase Particle can effectively pin accumulating dislocation so that improve material work hardening capacity, most
Crystal grain thinning is reached eventually and improves the effect of tungsten sill properties.There are some researches show in crystal grain thinning and promotion material
In terms of densification, Y2O3It is optimal dispersed oxide phase.Importantly, the Y of Dispersed precipitate2O3Tungsten can effectively be hindered
High-temperature reply and recrystallization process, improve recrystallization temperature, so as to improve the elevated temperature strength and croop property of tungsten alloy, reduce
The ductile-brittle transition temperature of tungsten, and improve the Radiation hardness of tungsten.
Current W-Y2O3The preparation of composite Nano precursor powder uses tungsten powder and Y mostly2O3The route of sphere of powder break-in aurification.
In real process, mechanical alloying is vulnerable to the limitation for the factors such as powder pollution, mass production be difficult and interior energy is excessive.It is this
Method can cause Y2O3Second Phase Particle size is uneven and main segregation is in tungsten basal body grain boundaries, it is impossible to Dispersed precipitate well
Into tungsten crystal.Although in addition, many emerging chemical methods, sol-gal process are improving W-Y2O3The purity of composite powder, tungsten are brilliant
The size and dimensional homogeneity, Y of grain2O3Good achievement is achieved in terms of the uniform distribution of Second Phase Particle, but formerly
Drive Y in powder2O3Second Phase Particle is still mainly distributed on tungsten crystal boundary, is seldom distributed in transgranular, and this can cause the sintering in postorder
During grain boundaries Y2O3Second Phase Particle is reunited, grown up, so as to largely reducing Y2O3To the improvement effect of tungsten alloy performance
Really, the especially index such as ductile-brittle transition temperature, recrystallization temperature and structural homogenity.For above present Research, the present invention exists
Prepare W-Y2O3On the basis of the conventional wet chemical method of composite precursor powder, its raw material is modified and during the course of the reaction
Apply surfactant and ultrasonically treated next W-Y of the preparation with core shell structure in situ2O3Superfine composite precursor powder.
The content of the invention
The present invention is preparing W-Y2O3On the basis of the conventional wet chemical method of composite precursor powder, its raw material is carried out more
Change and apply surfactant during the course of the reaction and ultrasonically treated prepare the W-Y with core shell structure2O3Superfine composite forerunner
Body powder.The technology enables to Y2O3Particle is coated on inside tungsten grain well；Meanwhile, the average grain size of tungsten reaches
10-40nm, and crystallite dimension has good uniformity；Y is obtained for postorder sintering2O3Second Phase Particle is mainly distributed on tungsten grain
The tungsten-bast alloy of internal, fine grain densification is laid a good foundation.
Concrete technical scheme is as follows:
A kind of preparation method of the tungsten of core shell structure-yittrium oxide superfine composite precursor powder, comprises the following steps：
(1) by surfactant and Y2O3Powder is dissolved in deionized water or distilled water, with mechanical agitation and ultrasonically treated is made
Ammonium paratungstate (APT), is then added thereto by its fully dispersed, dissolving；
(2) by concentration be 65%~68% HNO3Add and changed in above-mentioned solution under mechanical agitation and ultrasound condition
Precipitation reaction is learned, suspension is formed；
(3) absolute ethyl alcohol is added in suspension and continues to react, in whole course of reaction mechanical agitation and it is ultrasonically treated
In running order and its rotating speed and power keep constant, and reacted suspension is filtered and washes of absolute alcohol institute is used
The sediment of acquisition；
(4) obtained sediment is placed in grinding after being dried in drying box and obtains composite powder, then by the composite powder
It is placed in tube furnace, calcining obtains composite oxide power in nitrogen or argon stream；
(5) in tube furnace with pure hydrogen in 580~650 DEG C, first step reductase 12~5h；Again at 700~800 DEG C,
Second step reductase 12~6h；Obtain the W-Y with core shell structure2O3Superfine composite precursor powder.
Surfactant selects one of the following in the step (1)：Polyvinylpyrrolidone (PVP) and dodecyl
Sodium sulphate (SDS).
The concentration of ammonium paratungstate in the solution is in the step (1)：0.08~0.33g/mL；The quality of yittrium oxide is secondary
The 0.38%~3.8% of ammonium tungstate quality；The quality of surfactant is the 5%~15% of ammonium paratungstate quality.
65%~68%HNO in the step (2)3The volume ratio of consumption and deionized water or distilled water be：1/12~
1/4。
In the step (2) chemical precipitation reaction time be：20~60min.
The volume of addition absolute ethyl alcohol in the step (3) is 0.5~3 times of suspension cumulative volume.
The time for continuing reaction after addition absolute ethyl alcohol in the step (3) is 2~5h.
Churned mechanically rotating speed is 1000~5000rpm in the step, and ultrasonically treated power is 100~400W.
Calcining heat in the step (4) is 450~500 DEG C；Calcination time is 1~3h.
Y in the step (1)2O3Powder diameter<50nm.
Advantages of the present invention is as follows：
1st, with preparing W-Y2O3The conventional wet chemical method of composite precursor powder, sol-gal process are compared, and the preparation method can
So that Y2O3Second Phase Particle is wrapped in inside tungsten grain very well；Surfactant is used simultaneously and ultrasonically treated so that forerunner
The crystallite dimension and dimensional homogeneity of body powder are controlled very well.
2nd, compared with traditional Mechanical Alloying, this method can be on the basis of precursor powder purity be ensured to crystalline substance
Size, the shape of grain realize accurate regulation and control；Y2O3Second Phase Particle is also uniformly distributed in precursor powder.
3rd, the W-Y with core shell structure is prepared into using this method2O3Superfine composite precursor powder, is that postorder sintering is obtained
Obtain the high fine and close, Y of fine grain2O3Second Phase Particle is mainly distributed on the W-Y inside tungsten grain2O3Alloy is laid a good foundation.
Brief description of the drawings
Fig. 1：W-Y prepared by embodiment 12O3The TEM pictures of composite precursor powder；
Fig. 2：W-Y prepared by embodiment 22O3The TEM pictures of composite precursor powder；
Fig. 3：W-Y prepared by embodiment 32O3The HRTEM pictures of composite precursor powder；
Fig. 4：W-Y prepared by conventional method2O3The HRTEM pictures of composite precursor powder.
Embodiment
The feature of the present invention is further described below by example, but the invention is not limited in following examples.
Embodiment 1
(1) by 3gPVP (K30) and 0.15gY2O3(<50nm) it is dissolved in 120mL distilled water, is 4000rpm machineries with rotating speed
After stirring and power is 200W ultrasonically treated fully dispersed dissolvings, 20gAPT adds in the solution prepared to (APT concentration is
0.17g/mL, Y2O3Quality be the 0.76% of ammonium paratungstate quality, the quality of surfactant is ammonium paratungstate quality
15%).
(2) concentrated nitric acid that 20mL concentration is 65%~68% (volume ratio of itself and distilled water is 1/6) is added to above-mentioned
Chemical precipitation reaction is carried out in solution, reaction continues 40min, forms suspension；
(3) 420mL absolute ethyl alcohols (3 times of suspension cumulative volume) are added in the suspension and continues to react 4h, it is whole anti-
Should during mechanical agitation and it is ultrasonically treated be in working condition and its rotating speed and power keep constant, then suspension is entered
Row vacuum filtration and by the precipitation of acquisition washes of absolute alcohol 3 times；
(4) precipitation after cleaning is put into the vacuum drying chamber that design temperature is 60 DEG C and dried 1 day, then at 480 DEG C
3h is calcined in argon stream and obtains composite oxide power；
(5) composite oxide power is carried out to two step reduction (600 DEG C of insulation 4h, 750 DEG C of insulations in hydrogen gas stream
5h), room temperature is then cooled in hydrogen atmosphere, W-Y is obtained2O3Composite precursor powder, heating rate is 5 DEG C/min, air-flow
Measure as 100mL/min.It can be seen that from Fig. 1 TEM figures：The powder grain size uniform, average grain size are 13.5nm.With
Conventional wet chemical is compared with tungsten powder prepared by mechanical alloying, and this method can effectively reduce the size of tungsten grain and improve size
Uniformity.
Embodiment 2
(1) by 1gSDS and 0.38g Y2O3(<50nm) it is dissolved in 120mL distilled water, is 2000rpm mechanical agitations with rotating speed
With power for 100W ultrasonically treated fully dispersed dissolving after, 10gAPT adds in the solution prepared to (APT concentration is
0.08g/mL, Y2O3Quality be the 3.8% of ammonium paratungstate quality, the quality of surfactant is ammonium paratungstate quality
10%).
(2) concentrated nitric acid that 10mL concentration is 65%~68% (volume ratio of itself and distilled water is 1/12) is added to above-mentioned
Chemical precipitation reaction is carried out in solution, reaction continues 30min, forms suspension.
(3) 130mL absolute ethyl alcohols (1 times of suspension cumulative volume) are added in the suspension and continues to react 4h, it is whole anti-
Should during mechanical agitation and it is ultrasonically treated be in working condition and its rotating speed and power keep constant, then suspension is entered
Row vacuum filtration and by the precipitation of acquisition washes of absolute alcohol 3 times.
(4) precipitation after cleaning is put into the vacuum drying chamber that design temperature is 60 DEG C and dried 1 day, then at 450 DEG C
2h is calcined in argon stream and obtains composite oxide power.
(5) composite oxide power is carried out to two step reduction (650 DEG C of insulation 2h, 800 DEG C of insulations in hydrogen gas stream
6h), room temperature is then cooled in hydrogen atmosphere, the W-Y with core shell structure is obtained2O3Composite precursor powder.Heating rate
For 5 DEG C/min, throughput is 100mL/min.It can be seen that from Fig. 2 TEM figures：The even grain size of the powder, average crystalline substance
Particle size is 35.5nm.Meanwhile, yttrium oxide particle can be both coated on inside tungsten grain by this method well, can be avoided again
The shortcomings of high-energy ball milling method is easily introduced impurity, energy consumption is big so that the purity of the composite powder of preparation is increased dramatically.
Embodiment 3
(1) by 1gPVP (K12) and 0.76g Y2O3(<50nm) it is dissolved in 120mL distilled water, is 1000rpm machines with rotating speed
After the ultrasonically treated fully dispersed dissolving that tool is stirred and power is 120W, 20gAPT is added into (APT concentration in the solution prepared
For 0.17g/mL, Y2O3Quality be the 3.8% of ammonium paratungstate quality, the quality of surfactant is ammonium paratungstate quality
5%).
(2) concentrated nitric acid that 20mL concentration is 65%~68% (volume ratio of itself and distilled water is 1/6) is added to above-mentioned
Chemical precipitation reaction is carried out in solution, reaction continues 30min, forms suspension.
(3) 140mL absolute ethyl alcohols (1 times of suspension cumulative volume) are added in the suspension and continues to react 3h, it is whole anti-
Should during mechanical agitation and it is ultrasonically treated be in working condition and its rotating speed and power keep constant, then suspension is entered
Row vacuum filtration and by the precipitation of acquisition washes of absolute alcohol 3 times.
(4) precipitation after cleaning is put into the vacuum drying chamber that design temperature is 60 DEG C and dried 1 day, then at 500 DEG C
1h is calcined in argon stream and obtains composite oxide power.
(5) composite oxide power is carried out to two step reduction (600 DEG C of insulation 3h, 800 DEG C of insulations in hydrogen gas stream
6h), room temperature is then cooled in hydrogen atmosphere, the W-Y with core shell structure is obtained2O3Composite precursor powder.Heating rate
For 5 DEG C/min, throughput is 100mL/min.It can be seen that from Fig. 3 HRTEM figures：Yittrium oxide second phase particles are covered by tungsten
Intra-die.Fig. 4 is the HRTEM figures of the composite precursor powder by traditional wet chemistry method preparation, as can be seen from the figure oxygen
Change yttrium second phase particles and be mainly distributed on tungsten grain boundaries.Therefore, method of the invention can be well by the phase of yittrium oxide second grain
Attached bag is wrapped up in into inside tungsten grain, is that the tungsten-bast alloy that postorder sintering acquisition yittrium oxide is mainly distributed on inside tungsten grain is laid well
Basis.
Embodiment 4
(1) by 4gSDS and 0.6g Y2O3(<50nm) it is dissolved in 120mL distilled water, is 5000rpm mechanical agitations with rotating speed
With power for 200W ultrasonically treated fully dispersed dissolving after, 40gAPT adds in the solution prepared to (APT concentration is
0.33g/mL, Y2O3Quality be the 1.5% of ammonium paratungstate quality, the quality of surfactant is ammonium paratungstate quality
10%).
(2) concentrated nitric acid that 30mL concentration is 65%~68% (volume ratio of itself and distilled water is 1/4) is added to above-mentioned
Chemical precipitation reaction is carried out in solution, reaction continues 60min, forms suspension.
(3) 150mL absolute ethyl alcohols (1 times of suspension cumulative volume) are added in the suspension and continues to react 2h, it is whole anti-
Should during mechanical agitation and it is ultrasonically treated be in working condition and its rotating speed and power keep constant, then suspension is entered
Row vacuum filtration and by the precipitation of acquisition washes of absolute alcohol 3 times.
(4) precipitation after cleaning is put into the vacuum drying chamber that design temperature is 60 DEG C and dried 1 day, then at 450 DEG C
1h is calcined in argon stream and obtains composite oxide power.
(5) composite oxide power is carried out to two step reduction (580 DEG C of insulation 5h, 700 DEG C of insulations in hydrogen gas stream
6h), room temperature is then cooled in hydrogen atmosphere, the W-Y that even grain size, average grain size are 39.4nm is obtained2O3It is multiple
Close precursor powder.Heating rate is 5 DEG C/min, and throughput is 100mL/min.
Embodiment 5
(1) by 2gSDS and 0.076g Y2O3(<50nm) it is dissolved in 120mL distilled water, is that 2000rpm machineries are stirred with rotating speed
Mix and stir after the ultrasonically treated fully dispersed dissolving that power is 400W, 20gAPT adds in the solution prepared to (APT concentration is
0.17g/mL, Y2O3Quality be the 0.38% of ammonium paratungstate quality, the quality of surfactant is ammonium paratungstate quality
10%).
(2) concentrated nitric acid that 20mL concentration is 65%~68% (volume ratio of itself and distilled water is 1/6) is added to above-mentioned
Chemical precipitation reaction is carried out in solution, reaction continues 20min, forms suspension.
(3) 70mL absolute ethyl alcohols (0.5 times of suspension cumulative volume) are added in the suspension and continues to react 5h, it is whole anti-
Should during mechanical agitation and it is ultrasonically treated be in working condition and its rotating speed and power keep constant, then suspension is entered
Row vacuum filtration and by the precipitation of acquisition washes of absolute alcohol 3 times.
(4) precipitation after cleaning is put into the vacuum drying chamber that design temperature is 60 DEG C and dried 1 day, then at 480 DEG C
1h is calcined in argon stream and obtains composite oxide power.
(5) composite oxide power is carried out to two step reduction (650 DEG C of insulation 3h, 800 DEG C of insulations in hydrogen gas stream
2h), room temperature is then cooled in hydrogen atmosphere, the W-Y that even grain size, average grain size are 40.4nm is obtained2O3It is multiple
Close precursor powder.Heating rate is 5 DEG C/min, and throughput is 100mL/min.
The present invention discloses and proposed a kind of preparation side of tungsten-yittrium oxide superfine composite precursor powder of core shell structure
Method, those skilled in the art can be by using for reference present disclosure, and the appropriate links such as condition route that change are realized, although the side of the present invention
Method and technology of preparing are described by preferred embodiment, and person skilled can be not substantially being departed from the present invention
Methods and techniques described herein route is modified or reconfigured in appearance, spirit and scope, to realize final preparation
Technology.In particular, all similar replacements and change are apparent to those skilled in the art,
They are considered as being included in spirit of the invention, scope and content.
Claims (10)
1. a kind of W-Y of core shell structure2O3The preparation method of superfine composite precursor powder, it is characterised in that comprise the following steps：
(1) by surfactant and Y2O3Powder is dissolved in deionized water or distilled water, with mechanical agitation and ultrasonically treated fills it
Ammonium paratungstate, is then added thereto by scattered, dissolving；
(2) it is 65%~68%HNO by concentration3Added under mechanical agitation and ultrasound condition and chemical precipitation is carried out in above-mentioned solution
Reaction, forms suspension；
(3) absolute ethyl alcohol is added in suspension and continues to react, mechanical agitation and ultrasonically treated be in whole course of reaction
Working condition and its rotating speed and power keep constant, and reacted suspension is filtered and obtained with washes of absolute alcohol
Sediment；
(4) obtained sediment is placed in grinding after being dried in drying box and obtains composite powder, then the composite powder is placed in
In tube furnace, calcining obtains composite oxide power in nitrogen or argon stream；
(5) in tube furnace with pure hydrogen in 580~650 DEG C, first step reductase 12~5h；Again in 700~800 DEG C, second
Walk reductase 12~6h；Obtain the W-Y with core shell structure2O3Superfine composite precursor powder.
2. according to the method described in claim 1, it is characterised in that surfactant selects polyvinyl pyrrole in the step (1)
One kind of alkanone or lauryl sodium sulfate.
3. according to the method described in claim 1, it is characterised in that the concentration of ammonium paratungstate in the solution in the step (1)
For：0.08~0.33g/mL；The quality of yittrium oxide is the 0.38%~3.8% of ammonium paratungstate quality；The quality of surfactant
For the 5%~15% of ammonium paratungstate quality.
4. according to the method described in claim 1, it is characterised in that dense HNO in the step (2)3Consumption and deionized water or
The volume ratio of distilled water is：1/12~1/4.
5. according to the method described in claim 1, it is characterised in that the time of the chemical precipitation reaction in the step (2) is：
20~60min.
6. according to the method described in claim 1, it is characterised in that the volume of the addition absolute ethyl alcohol in the step (3) is outstanding
0.5~3 times of supernatant liquid cumulative volume.
7. according to the method described in claim 1, it is characterised in that continue to react after the addition absolute ethyl alcohol in the step (3)
Time be 2~5h.
8. according to the method described in claim 1, it is characterised in that churned mechanically rotating speed 1000 in the step~
5000rpm, ultrasonically treated power is 100~400W.
9. according to the method described in claim 1, it is characterised in that the calcining heat in the step (4) is 450~500 DEG C；
Calcination time is 1~3h.
10. according to the method described in claim 1, it is characterised in that the Y2O3Powder diameter<50nm.
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