CN106363166A - Composite powder formed by uniformly doping nano-La2O3 in nano-Mo and preparation method thereof - Google Patents
Composite powder formed by uniformly doping nano-La2O3 in nano-Mo and preparation method thereof Download PDFInfo
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- CN106363166A CN106363166A CN201610816583.4A CN201610816583A CN106363166A CN 106363166 A CN106363166 A CN 106363166A CN 201610816583 A CN201610816583 A CN 201610816583A CN 106363166 A CN106363166 A CN 106363166A
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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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses composite powder formed by uniformly doping nano-La2O3 in nano-Mo. The size of the La2O3 and Mo composite powder is 30-100 nm, and the La2O3 content is 0.5-5.0wt.%. The invention further discloses a preparation method of the composite powder. The method includes the technological processes of solution preparing, solution heating, glucose adding, precursor synthesizing, precursor reduction and forming of the composite powder through uniformly doping of the nano-La2O3 in the nano-Mo. According to the composite powder formed by uniformly doping the nano-La2O3 in the nano-Mo and the preparation method thereof, uniform dispersion and stability of nano-particles are guaranteed, and moreover, the powder size can be effectively adjusted and controlled; and meanwhile, the precursor reaction synthesis temperature is low, the reaction time is short, the efficiency is high, energy saving is achieved, and operation is simple.
Description
Technical field
The present invention relates to nanometer la2o3The technical field of doping, refers in particular to a kind of nanometer la2o3Uniform Doped nanometer molybdenum is combined
Powder and preparation method thereof.
Background technology
Metal molybdenum is important refractory metal material, because under the room temperature of molybdenum, toughness is poor, ductil-brittle transition temperature (dbtt)
Higher, toughness is still not enough at relatively high temperatures, the molybdenum and molybdenum alloy application in terms of structural material of these drawbacks limit.Using
la2o3Rare-earth oxide doping molybdenum alloys Deng the preparation of rare earth oxide doping techniques have good room/elevated temperature strength and tough
Property.The dispersed and refinement of rare earth oxide particle is difficult point and the key point of rare earth oxide doping techniques.
At present, rare earth oxide doping molybdenum raw powder's production technology has three kinds: Gu solid doping (s s), solid-liquid doping (s
L) adulterate (l l) with liquid liquid.Gu admittedly doping typically adopts mechanical mixing, directly mo powder is mixed with rare earth oxide particles
Ball milling, or by moo2Carry out calcining reduction process after solution and rare earth oxide mix particles;Solid-liquid doping is then by rare earth nitre
Acid salt solution and moo2Mixing, through hydrogen reducing moo2With decomposition rare earth nitrate, obtain doping powder;The doping of liquid liquid is general
Using sol-gal process, by ammonium molybdate ((nh4)2moo4) solution mix with rare earth nitrate solution and dried after formed molten
Glue gel presoma, is calcined to presoma and reduction treatment obtains doping powder.Comparatively, admittedly admittedly doping process letter
Single, but uniform doping is poor, and doping particle is relatively thick and is readily incorporated impurity;The uniformity of solid-liquid doping is preferable, but difficult to form
Tiny doping particle;The doping of liquid liquid is the mixing of molecule and atomic scale, achievable particle refinement and dispersed.As in
State's patent cn103273071a discloses the preparation method of nano-second-phase granule dipping molybdenum alloy powder and product, and the method is
By way of spray dosing, nano-second-phase granule is doped in molybdenum dioxide powder, through reduction, sieves, obtain nanometer
Second Phase Particle dipping molybdenum alloy powder, this method ensure that scattered uniformity coefficient and the stability of Second Phase Particle, but no
Method obtains the molybdenum alloy powder of nano-particle.And for example Chinese patent cn103706802a discloses a kind of system of lanthanum-doped alloy molybdenum powder
Preparation Method, this method solves la dispersing uniformity and la content regulation and control problem, but is not directed to the controlling party of powder size aspect
Method.At present, still suffer from that technique is more complicated due to existing liquid liquid doping techniques, cycle length and the low problem of efficiency, industrial metaplasia
Product aspect is still most to prepare rare-earth oxidation molybdenum doping molybdenum powder using solid doping and solid-liquid doping techniques.Seek a kind of simple
Efficiently prepare the new method of rare earth oxide doping molybdenum composite granule, there is important practical value.
Therefore, the present inventor makes further research to this, develops a kind of nanometer la2o3Uniform Doped nanometer molybdenum composite powder
End and preparation method thereof, this case thus produces.
Content of the invention
The technical problem to be solved is to provide a kind of nanometer la2o3Uniform Doped nanometer molybdenum composite powder and
Its preparation method, with the problem overcoming prior art to exist.
For solving above-mentioned technical problem, the technical solution of the present invention is:
A kind of nanometer la2o3Uniform Doped nanometer molybdenum composite powder, nanometer la2o3Uniform Doped forms composite powder in nanometer molybdenum
End, la2o3Size with the composite powder of mo is 30 ~ 100nm, la2o3Content be 0.5 ~ 5.0wt.%.
Further, la2o3Size with mo composite powder is 80nm, la2o3Content be 1.2wt.%.
Further, la2o3Size with mo composite powder is 50nm, la2o3Content be 3wt.%.
A kind of nanometer la2o3The preparation method of Uniform Doped nanometer molybdenum composite powder, with four water ammonium paramolybdates as molybdenum source, six
Water Lanthanum (III) nitrate is lanthanum source, and ammonium nitrate and glycine are reaction combustion agent, and the nanometer carbon plate being generated using glucose response is to oxide
The absorption of granule, refinement and dispersed effect, and the order by controlling glucose to add, make solution form low decomposition temperature
Complex, realize synthesis under 100 ~ 160 DEG C of low temperature for the presoma, prepare a nanometer la in conjunction with method of reducing2o3Uniform Doped
Nanometer molybdenum composite powder, its preparation technology flow process is: prepare solution → solution heat → add glucose → synthesis presoma →
Presoma reduction → nanometer la2o3Uniform Doped nanometer molybdenum composite powder.
Further, in preparing solution step, four water ammonium paramolybdates that certain proportion is weighed, lanthanum nitrate hexahydrate, nitric acid
Ammonium and glycine are put in beaker simultaneously, and add the deionized water of 100ml, stir to being completely dissolved;Four water ammonium paramolybdates, nitre
The mass ratio of sour ammonium and glycine is: four water ammonium paramolybdates are 25~50 wt.%, and ammonium nitrate+glycine is 50~75 wt.%,
Wherein ammonium nitrate and the mol ratio of glycine are 2~4;The mol ratio of lanthanum nitrate hexahydrate and four water ammonium paramolybdates be 0.02~
0.22;Mentioned reagent purity should reach the pure specification of analysis.
Four water ammonium paramolybdate ratios solution can be led to precipitate molybdic acid more than 50 wt.% it is impossible to smooth synthesize, less than 25
Then corresponding ammonium nitrate+glycine is that ratio is excessive to wt.%, makes reaction temperature too high, leads to moo3Volatilization loss, serious reduce
Combined coefficient;The mol ratio of ammonium nitrate and glycine is more than 2, and heat of reaction is not enough it is impossible to complete synthetic reaction, ammonium nitrate with sweet
The mol ratio of propylhomoserin is less than 2, then glycine reactant not exclusively, easily forms impurity.
Further, in solution heating stepses, carry out adding in 200 DEG C by filling the beaker preparing solution and being placed on heating furnace
Heat, after waiting solution to seethe with excitement 3 ~ 5 minutes, adds glucose, the mol ratio of glucose and four water ammonium paramolybdates is 1.5~5;Glucose
Purity should reach the pure specification of analysis.
Further, drive before the synthesis in body step, the solution after heating is continued to be held in 200 DEG C and is heated, make molten
Liquid is shaped as light blue collosol state, low decomposition temperature complex because moisture persistently volatilizees, and heating-up temperature is dropped to
160 DEG C, solution reacts and forms fluffy foam-like material, and after 3~5 minutes, reaction terminates, and obtains la2o3/mooxForerunner
Body powder;Wherein mooxFor moo3、moo2And mo4o11Mixture.Further, in presoma reduction step, by la2o3/
mooxPrecursor powder is put in atmosphere heating furnace, is under 800~1000ml/min hydrogen atmosphere 650~850 in hydrogen flowing quantity
DEG C carry out reductase 12~5 hour, be down to after room temperature after furnace temperature and powder is taken out, that is, obtain nanometer la2o3Uniform Doped nanometer molybdenum is multiple
Close powder;In reduction and temperature-fall period, remain flowing hydrogen atmosphere state.
After such scheme, because the present invention is with four water ammonium paramolybdates (also referred to as " ammonium paramolybdate ") as molybdenum source, six water
Lanthanum (III) nitrate (also becoming " Lanthanum (III) nitrate ") is lanthanum source, and ammonium nitrate glycine is reaction promoter, the nanometer being generated using glucose response
Carbon plate, to the absorption of oxide particle and peptizaiton, prepares a nanometer la in conjunction with method of reducing2o3Uniform Doped nanometer molybdenum is combined
Powder is a kind of simply efficient and the new method of energy-conservation, has important practical value.The method has the advantage that
First, ensure that homodisperse degree and the stability of granule, prepare granule uniformly and la2o3The nanometer of Uniform Doped
Molybdenum composite powder;
2nd, can achieve the Effective Regulation to powder size, obtain a size of la of 30 ~ 100nm2o3Uniform Doped nanometer molybdenum is multiple
Close powder, this can provide high-quality powder stock for preparing high performance nanometer molybdenum alloy and rear-earth-doped alloy.
3rd, presoma is synthesized that temperature is low, the response time is short, efficiency high, energy-conservation and simple to operate;
4th, present invention employs ammonium nitrate is reaction combustion agent, and it not only can have and the effect of nitric acid identical, and ammonium nitrate
Substantial amounts of nh can be released in heating combustion process3、no、n2The gases such as o, more favourable powder nanometer and dispersed;
5th, first glucose and other raw material are mixed together and can form the higher complex of decomposition temperature, when leading to combustion reaction
Decompose slow, releasing gas is few, and powder bulkiness is poor;The present invention can form the complex of low decomposition temperature using rear plus glucose,
Product bulkiness is good, and synthesis temperature can be reduced to 100 ~ 160 DEG C.
Brief description
Fig. 1 is nanometer la of the present invention2o3The preparation technology flow process of Uniform Doped nanometer molybdenum composite powder;
Fig. 2 is nanometer la of the present invention2o3The tg/dsc curve of the synthesis presoma of Uniform Doped nanometer molybdenum composite powder;
Fig. 3 is nanometer la of the present invention2o3The electron scanning micrograph of Uniform Doped nanometer molybdenum composite powder;
Fig. 4 is nanometer la of the present invention2o3The xrd diffraction spectra of Uniform Doped nanometer molybdenum composite powder.
Specific embodiment
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Embodiment one:
A kind of nanometer la2o3The preparation technology flow process of Uniform Doped nanometer molybdenum composite powder is as shown in Figure 1.
(1) 12.4g tetra- water ammonium molybdate, 16g ammonium nitrate, 8g glycine and 0.22g lanthanum nitrate hexahydrate are put into simultaneously
In the beaker of 1000ml, and add 100ml deionized water, be stirred to and be completely dissolved formation mixed solution.
(2) beaker filling above-mentioned mixed solution is placed on heating furnace, is heated at 200 DEG C.
(3) add the glucose of 4.5g after solution seethes with excitement 3~5 minutes, be fully stirred simultaneously.
(4) heated adding the solution after glucose to continue at 200 DEG C, when solution forms light blue colloidal sol, will
To 160 DEG C, reaction proceeds by and is formed fluffy foam-like material, and after 3~5 minutes, reaction terminates for temperature drop, obtains
la2o3/mooxPrecursor powder.Its tg/dsc curve is as shown in Figure 2.
(5) by above-mentioned la2o3/mooxPrecursor powder is put in atmosphere heating furnace, under the flowing hydrogen of 800ml/min,
Carry out reductase 12 hour in 850 DEG C, reduction terminates rear furnace cooling, and remains the flowing hydrogen of 800ml/min in cooling procedure
Gas atmosphere.
Etc. (6) powder is taken out after being down to room temperature by furnace temperature, obtains la2o3Mass percentage content is the nanometer of 1.2wt.%
la2o3Uniform Doped nanometer molybdenum composite powder.
Nanometer la by process above preparation2o3The la of Uniform Doped nanometer molybdenum composite granule2o3Content is 1.2wt.%,
The size about 80nm of (wt.% herein represents mass percent) composite powder.The scanning electron microscope of this composite powder is shone
Piece is as shown in figure 3, xrd diffraction spectra is as shown in Figure 4.
Embodiment two:
(1) 12.4g tetra- water ammonium molybdate, 20g ammonium nitrate, 8g glycine and 0.55g lanthanum nitrate hexahydrate are put into 1000ml's simultaneously
In beaker, and add 100ml deionized water, be stirred to and be completely dissolved formation mixed solution.
(2) beaker filling above-mentioned mixed solution is placed on heating furnace, is heated at 200 DEG C.
(3) add the glucose of 6.8g after solution seethes with excitement 3~5 minutes, be fully stirred simultaneously.
(4) heated adding the solution after glucose to continue at 200 DEG C, when solution forms light blue colloidal sol, will
To 160 DEG C, reaction proceeds by and is formed fluffy foam-like material, and after 3~5 minutes, reaction terminates for temperature drop, obtains
la2o3/mooxPrecursor powder.
(5) by above-mentioned la2o3/mooxPrecursor powder is put in atmosphere heating furnace, under the flowing hydrogen of 900ml/min,
Carry out reducing 3 hours in 750 DEG C, reduction terminates rear furnace cooling, and remains the flowing hydrogen of 900ml/min in cooling procedure
Gas atmosphere.
Etc. (6) powder is taken out after being down to room temperature by furnace temperature, obtains la2o3Mass percentage content is the nanometer of 3.0wt.%
la2o3Uniform Doped nanometer molybdenum composite powder.
Nanometer la by process above preparation2o3The la of Uniform Doped nanometer molybdenum composite granule2o3Mass percentage content is
3.0wt.%, the size about 50nm of composite powder.
Embodiment three:
(1) 12.4g tetra- water ammonium molybdate, 24g ammonium nitrate, 8g glycine and 0.94g lanthanum nitrate hexahydrate are put into 1000ml's simultaneously
In beaker, and add 100ml deionized water, be stirred to and be completely dissolved formation mixed solution.
(2) beaker filling above-mentioned mixed solution is placed on heating furnace, is heated at 200 DEG C.
(3) add the glucose of 9g after solution seethes with excitement 3~5 minutes, be fully stirred simultaneously.
(4) heated adding the solution after glucose to continue at 200 DEG C, when solution forms light blue colloidal sol, will
To 160 DEG C, reaction proceeds by and is formed fluffy foam-like material, and after 3~5 minutes, reaction terminates for temperature drop, obtains
la2o3/mooxPrecursor powder.
(5) by above-mentioned la2o3/mooxPrecursor powder is put in atmosphere heating furnace, in the flowing hydrogen of 1000ml/min
Under, carry out reducing 4 hours in 700 DEG C, reduction terminates rear furnace cooling, and remains the stream of 1000ml/min in cooling procedure
Dynamic hydrogen atmosphere.
Etc. (6) powder is taken out after being down to room temperature by furnace temperature, obtains la2o3Mass percentage content is the nanometer of 5.0wt.%
la2o3Uniform Doped nanometer molybdenum composite powder.
Nanometer la by process above preparation2o3The la of Uniform Doped nanometer molybdenum composite granule2o3Mass percentage content is
5.0wt.%, the size about 30nm of composite powder.
Example IV:
(1) 12.4g tetra- water ammonium molybdate, 26g ammonium nitrate, 8g glycine and 0.11g lanthanum nitrate hexahydrate are put into 1000ml's simultaneously
In beaker, and add 100ml deionized water, be stirred to and be completely dissolved formation mixed solution.
(2) beaker filling above-mentioned mixed solution is placed on heating furnace, is heated at 200 DEG C.
(3) add the glucose of 3g after solution seethes with excitement 3~5 minutes, be fully stirred simultaneously.
(4) heated adding the solution after glucose to continue at 200 DEG C, when solution forms light blue colloidal sol, will
To 160 DEG C, reaction proceeds by and is formed fluffy foam-like material, and after 3~5 minutes, reaction terminates for temperature drop, obtains
la2o3/mooxPrecursor powder.
(5) by above-mentioned la2o3/mooxPrecursor powder is put in atmosphere heating furnace, in the flowing hydrogen of 1000ml/min
Under, carry out reducing 5 hours in 650 DEG C, reduction terminates rear furnace cooling, and remains the stream of 1000ml/min in cooling procedure
Dynamic hydrogen atmosphere.
Etc. (6) powder is taken out after being down to room temperature by furnace temperature, obtains la2o3Mass percentage content is the nanometer of 0.5wt.%
la2o3Uniform Doped nanometer molybdenum composite powder.
Nanometer la by process above preparation2o3The la of Uniform Doped nanometer molybdenum composite granule2o3Mass percentage content is
0.5wt.%, the size about 100nm of composite powder.
In sum, the difference of four embodiment preparations is la2o3The size grain of mass percentage content and composite powder
Degree difference.
The above, be only presently preferred embodiments of the present invention, not the technical scope of the present invention imposed any restrictions,
Therefore the change that in every case claim under this invention and description are done or modification, all should belong to the scope that patent of the present invention covers
Within.
Claims (8)
1. a kind of nanometer la2o3Uniform Doped nanometer molybdenum composite powder it is characterised in that: nanometer la2o3Uniform Doped is in nanometer molybdenum
Middle formation composite powder, la2o3Size with mo composite powder is 30 ~ 100nm, la2o3Content be 0.5 ~ 5.0wt.%.
2. a kind of nanometer la according to claim 12o3Uniform Doped nanometer molybdenum composite powder it is characterised in that: la2o3With
The size of mo composite powder is 80nm, la2o3Content be 1.2wt.%.
3. a kind of nanometer la according to claim 12o3Uniform Doped nanometer molybdenum composite powder it is characterised in that: la2o3With
The size of mo composite powder is 50nm, la2o3Content be 3wt.%.
4. a kind of nanometer la2o3The preparation method of Uniform Doped nanometer molybdenum composite powder it is characterised in that: with four water ammonium paramolybdates
For molybdenum source, lanthanum nitrate hexahydrate is lanthanum source, and ammonium nitrate and glycine are reaction combustion agent, the nanometer carbon plate being generated using glucose response
To the absorption of oxide particle, refinement and dispersed effect, and the order by controlling glucose to add, so that solution is formed low
The complex of decomposition temperature, realizes synthesis under 100 ~ 160 DEG C of low temperature for the presoma, prepares a nanometer la in conjunction with method of reducing2o3
Uniform Doped nanometer molybdenum composite powder, its preparation technology flow process is: prepares solution → solution and heats → add glucose → synthesis
Presoma → presoma reduction → nanometer la2o3Uniform Doped nanometer molybdenum composite powder.
5. a kind of nanometer la according to claim 42o3The preparation method of Uniform Doped nanometer molybdenum composite powder, its feature
It is: in preparing solution step, four water ammonium paramolybdates, lanthanum nitrate hexahydrate, ammonium nitrate and glycine that certain proportion is weighed
Put in beaker simultaneously, and add the deionized water of 100ml, stir to being completely dissolved;Four water ammonium paramolybdates, ammonium nitrate and sweet ammonia
The mass ratio of acid is: four water ammonium paramolybdates are 25~50 wt.%, and ammonium nitrate and glycine are 50~75 wt.%, wherein ammonium nitrate
Mol ratio with glycine is 2~4;The mol ratio of lanthanum nitrate hexahydrate and four water ammonium paramolybdates is 0.02~0.22;Mentioned reagent
Purity should reach the pure specification of analysis.
6. a kind of nanometer la according to claim 42o3The preparation method of Uniform Doped nanometer molybdenum composite powder, its feature
It is: in solution heating stepses, heated filling the beaker preparing solution and being placed on heating furnace in 200 DEG C, wait solution
After boiling 3 ~ 5 minutes, add glucose, the mol ratio of glucose and four water ammonium paramolybdates is 1.5~5;Glucose purity should reach
To the pure specification of analysis.
7. a kind of nanometer la according to claim 42o3The preparation method of Uniform Doped nanometer molybdenum composite powder, its feature
It is: drive before the synthesis in body step, the solution after heating is continued to be held in 200 DEG C and is heated, make solution due to moisture
Persistently volatilization is shaped as light blue collosol state, the complex of low decomposition temperature, heating-up temperature is dropped to 160 DEG C, solution
React and form fluffy foam-like material, after 3~5 minutes, reaction terminates, obtain la2o3/mooxPrecursor powder;Wherein
mooxFor moo3、moo2And mo4o11Mixture.
8. a kind of nanometer la according to claim 42o3The preparation method of Uniform Doped nanometer molybdenum composite powder, its feature
It is: in presoma reduction step, by la2o3/mooxPrecursor powder is put in atmosphere heating furnace, is 800 in hydrogen flowing quantity
Under~1000ml/min hydrogen atmosphere, 650~850 DEG C carry out reductase 12~5 hour, are down to after room temperature after furnace temperature and take out powder,
Obtain nanometer la2o3Uniform Doped nanometer molybdenum composite powder;In reduction and temperature-fall period, remain flowing hydrogen atmosphere shape
State.
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CN108905972B (en) * | 2018-07-23 | 2021-01-29 | 成都清境环境科技有限公司 | Heavy metal ion adsorbent and preparation method and application thereof |
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CN115323212B (en) * | 2022-09-23 | 2023-02-03 | 西安稀有金属材料研究院有限公司 | Preparation method of ultrafine molybdenum powder and molybdenum alloy with oxide nanoparticles distributed in crystal |
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