CN106591613B - The method that tungsten-molybdenum alloy is prepared using beneficial element doping - Google Patents
The method that tungsten-molybdenum alloy is prepared using beneficial element doping Download PDFInfo
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- CN106591613B CN106591613B CN201610989720.4A CN201610989720A CN106591613B CN 106591613 B CN106591613 B CN 106591613B CN 201610989720 A CN201610989720 A CN 201610989720A CN 106591613 B CN106591613 B CN 106591613B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0031—Matrix based on refractory metals, W, Mo, Nb, Hf, Ta, Zr, Ti, V or alloys thereof
Abstract
The method that tungsten-molybdenum alloy is prepared using beneficial element doping, the step of the step of including doping type molybdenum powder is made, the step of doping type tungsten powder being made, and tungsten-molybdenum alloy is made using 82 ~ 87.5% doping type molybdenum powders, 11 ~ 15% doping type tungsten powders, 1.5 ~ 3.0% vanadium oxide.Tungsten-molybdenum alloy produced by the present invention not only has excellent high-temperature creep resistance, tensile strength, also there is good low temperature intensity, because lanthana and praseodymium oxide are after plastic deformation, be separated into tiny second phase particles at relatively high temperatures, and it is regularly arranged, play invigoration effect.
Description
Technical field
Present invention relates particularly to a kind of method that tungsten-molybdenum alloy is prepared using beneficial element doping.
Background technology
Tungsten-molybdenum alloy has the corrosiveness of excellent tolerance of liquid zinc, to manufacture the agitator in zinc metallurgy industry, pipeline
With container inside lining and miscellaneous part.Tungsten-molybdenum alloy is because elevated temperature strength is good, and performance is close with tungsten and proportion is smaller than tungsten, so available
Make high-temperature component, filament, part and other high-temperature materials of electron tube under corresponding hot conditions in rocket, guided missile.Molybdenum
Manufactured with the alloy of metal in weapon, and have critical role in the leading-edge field such as guided missile rocket.In addition, tungsten filament is used to make lamp
Silk, the heater element of high-temperature electric resistance furnace.Metal molybdenum easy processing is widely used in the electronics industry into silk, band, piece, rod etc..Molybdenum filament
Small hook, the grid of electron tube etc. as heater strip in support bulb.Tungsten-molybdenum alloy powder is commonly used to prepare sintered metal product,
But tungsten-molybdenum alloy the shortcomings that fragility big, poor processability be present, it is necessary to doped alloys element is strengthened to it, improves its property
Energy.
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to provide a kind of side that tungsten-molybdenum alloy is prepared using beneficial element doping
Method.
The used to achieve the above object technical scheme of the present invention is：Tungsten-molybdenum alloy is prepared using beneficial element doping
Method, comprise the following steps：
Step 1: will be according to Pr：Re：Mo=1：1：0.5 mol ratio, it is molten that praseodymium nitrate, nitric acid rhenium and ammonium molybdate are weighed successively
In citric acid solution, mixed solution is formed, the pH to 1.0 ~ 1.5 of nitric acid regulation mixed solution is added, in 85 ~ 100 DEG C of bars
Heating water bath mixed solution under part, colloidal sol is made；Colloidal sol is added by 100 ~ 120 DEG C of 0.5 ~ 0.8h of heating, 450 ~ 600 DEG C successively
2 ~ 4h of heat, obtains solid powder, by solid powder after reduction treatment, then by 1450 ~ 1550 DEG C of 10 ~ 20min of roasting, is made
Doping type molybdenum powder, it is standby；
Step 2: according to La：W=1：0.25 mol ratio, weighs lanthanum nitrate and tungsten oxide successively, and lanthanum nitrate is all molten
Yu Shuizhong, form molar concentration and be 0.4mol/L lanthanum nitrate hexahydrate, and lanthanum nitrate hexahydrate is doped to oxidation using spray-on process
In tungsten, then add the sodium hydroxide solution that molar concentration is 1.2mol/L and adjust pH to 9.0 ~ 9.5, filter and much filtrate exists
Dried at 100 ~ 110 DEG C, 2 ~ 2.5h is then calcined under 750 ~ 900 DEG C, hydrogen atmosphere, doping type tungsten powder is made, it is standby；
Step 3: according to mass percent, doping type molybdenum powder made from 82 ~ 87.5% step 1,11 ~ 15% steps are taken respectively
Doping type tungsten powder made from two and 1.5 ~ 3.0% vanadium oxide, above-mentioned each component percentage by weight sum are 100%, then will
Doping type molybdenum powder, doping type tungsten powder and vanadium oxide, which are added in batch mixer, mixes 24h, and is carried out using vacuumizing in drying receptacle
Spread 8h, then under 200 ~ 300MPa carry out 10 ~ 30min of cold isostatic compaction, then at 2100 ~ 2900 DEG C sintering 10 ~
24h, and be machined out, the tungsten-molybdenum alloy of required shape is made.
Wherein, the method for reduction treatment of solid powder is in step 1：Solid powder is placed in the reduction furnace for being passed through hydrogen
In, carry out 5 ~ 6h of processing, obtain the mixed-powder containing molybdenum dioxide, wherein, 10 ~ 15m/s of hydrogen flow rate, dew point of hydrogen for-
70 ~ -60 DEG C, and be followed successively by using five warm areas reduction system, the temperature of each warm area：530 DEG C, 550 DEG C, 580 DEG C, 600 DEG C and 620
℃；Continue to be passed through hydrogen, 5 ~ 8h of processing carried out to the mixed-powder containing molybdenum dioxide, obtains the mixed-powder containing molybdenum powder,
Wherein, 20 ~ 35m/s of hydrogen flow rate, dew point of hydrogen are -75 ~ -60 DEG C, and using five warm areas reduction system, the temperature of each warm area according to
It is secondary to be：750 DEG C, 800 DEG C, 850 DEG C, 900 DEG C and 950 DEG C.
Wherein, the preparation method of the vanadium oxide in step 3 is：According to W：V=0.03：10 mol ratio, weighs tungsten successively
Sour ammonium and ammonium metavanadate, and ammonium tungstate and ammonium metavanadate is all soluble in water, solution is formed, then adds a certain amount of formic acid,
After the pH to 2.0 ~ 3.0 for adjusting solution, solution is placed in reactor, after heating 4 ~ 36h at 100 ~ 200 DEG C, filters and adopts
Much filtrate is washed with deionized, dries, vanadium oxide is made.Contain W in the vanadium oxide of preparation6+, and W6+Occupy in lattice position
Put, reach the rock-steady structure of thermodynamic significance.Vanadium adds the heat resistance of alloy and the drag to creep, can effectively fix conjunction
Carbon and nitrogen impurity in gold, and the carbide and nitride particulate of highly dispersed distribution are formed, play refined crystalline strengthening and precipitation is strong
The effect of change.
Beneficial effects of the present invention are：1st, step 1 is final to be made using praseodymium nitrate, nitric acid rhenium and the doping of liquid ammonium molybdate liquid
Nano level batch mixing doping type molybdenum powder.In the present invention, in reduction reaction, praseodymium and lanthanum are to exist in the form of an oxide, are
The also volatilization of molybdenum oxide and tungsten oxide provides nucleus, limits the reunion of molybdenum atom and tungsten atom, is formed largely with rare earth oxygen
Compound is the fine particle of nucleus；Rhenium exists with simple substance form, it is possible to increase the recrystallization temperature and high-temperature behavior of alloy, and rhenium
MoReO can be formed4Compound, prevent O in grain boundaries segregation；Meanwhile rhenium can reduce the directionality of molybdenum Central Plains sub-key, prevent
Molybdenum is changed from metallic bond to covalent bond, improves shearing abrasive material, the black brittleness for solving molybdenum.
2nd, tungsten-molybdenum alloy produced by the present invention not only has excellent high-temperature creep resistance, tensile strength, also has good
Low temperature intensity, because lanthana and praseodymium oxide are after plastic deformation, be separated into the second tiny phase grain at relatively high temperatures
Son, and it is regularly arranged, play invigoration effect.
3rd, the present invention is adulterated using the oxide form of molybdenum, and the rupture of molybdenum oxide improves the uniform of the distribution of rare-earth phase
Property, but the less stable due to lanthana in molybdenum, the praseodymium oxide of addition can reduce the reciprocation of lanthana and molybdenum.
4th, the doped processing of the present invention, inside contain high-temperature-phase and alloying element, prevent oxygen to continue to invade to molybdenum product
Erosion.Moreover, have the rare earth element of very big affinity by oxide grain boundary to the higher surface migration of oxidation activity to oxygen
Trend, during travel motion, larger active rare-earth ion convergent collection is segregated at oxide grain boundary, has blocked oxidation
To the passage of molybdenum depths diffusible oxydation, the oxidation mechanism of molybdenum and tungsten is changed, makes molybdenum and the outside diffusible oxydation reduced capability of tungsten, makes
More than 45% can be improved with the life-span.
Embodiment
Technological means, creation characteristic and the purpose reached to realize the present invention readily appreciate, with reference to specific
Embodiment, the present invention is expanded on further, but scope of the present invention is not limited to be retouched in embodiment
The scope stated.
Embodiment 1
The method that tungsten-molybdenum alloy is prepared using beneficial element doping, is comprised the following steps：
Step 1: will be according to Pr：Re：Mo=1：1：0.5 mol ratio, it is molten that praseodymium nitrate, nitric acid rhenium and ammonium molybdate are weighed successively
In molar concentration be 0.1mol/L citric acid solution in, formed mixed solution, add nitric acid regulation mixed solution pH to
1.0, the heating water bath mixed solution under the conditions of 100 DEG C, colloidal sol is made；By colloidal sol successively by 120 DEG C heating 0.8h, 600 DEG C
2h is heated, obtains solid powder, by solid powder after reduction treatment, then by 1450 DEG C of roasting 20min, doping type molybdenum is made
Powder, it is standby；Its own, the method for reduction treatment of solid powder is：Solid powder is placed in the reduction furnace for being passed through hydrogen, carried out
6h is handled, obtains the mixed-powder containing molybdenum dioxide, wherein, hydrogen flow rate 15m/s, dew point of hydrogen is -70 DEG C, and using five
Warm area reduces system, and the temperature of each warm area is followed successively by：530 DEG C, 550 DEG C, 580 DEG C, 600 DEG C and 620 DEG C；Continue to be passed through hydrogen,
Processing 8h is carried out to the mixed-powder containing molybdenum dioxide, obtains the mixed-powder containing molybdenum powder, wherein, hydrogen flow rate 35m/s,
Dew point of hydrogen is -75 DEG C, and is followed successively by using five warm areas reduction system, the temperature of each warm area：750℃、800℃、850℃、900
DEG C and 950 DEG C.
Step 2: according to La：W=1：0.25 mol ratio, weighs lanthanum nitrate and tungsten oxide successively, and lanthanum nitrate is all molten
Yu Shuizhong, form molar concentration and be 0.4mol/L lanthanum nitrate hexahydrate, and lanthanum nitrate hexahydrate is doped to oxidation using spray-on process
In tungsten, then add the sodium hydroxide solution that molar concentration is 1.2mol/L and adjust pH to 9.0, filter and by much filtrate 110
Dried at DEG C, then calcine 2.1h under 880 DEG C, hydrogen atmosphere, doping type tungsten powder is made, it is standby；
Step 3: according to mass percent, doping type molybdenum powder made from 87.5% step 1,11% step 2 is taken to be made respectively
Doping type tungsten powder and 1.5% vanadium oxide, then by doping type molybdenum powder, doping type tungsten powder and vanadium oxide add batch mixer
Middle mixing 24h, and 8h is diffused in drying receptacle using vacuumizing, vacuum its 10-1Torr, rotating speed 100r/min, then
Cold isostatic compaction 20min is carried out under 220MPa, 22h is then sintered at 2150 DEG C, and is machined out, required shape is made
The tungsten-molybdenum alloy of shape.
The compound of the tungsten of the present invention is ammonium tungstate, blue tungsten, preferably tungsten dioxide, blue tungsten, and activity is larger, carries out hydrogen
After reduction, the tungsten alloy containing beneficial element and oxide is formed.
Embodiment 2
The method that tungsten-molybdenum alloy is prepared using beneficial element doping, is comprised the following steps：
Step 1: will be according to Pr：Re：Mo=1：1：0.5 mol ratio, it is molten that praseodymium nitrate, nitric acid rhenium and ammonium molybdate are weighed successively
In molar concentration be 0.1mol/L citric acid solution in, formed mixed solution, add nitric acid regulation mixed solution pH to
1.5, the heating water bath mixed solution under the conditions of 90 DEG C, colloidal sol is made；Colloidal sol is added by 100 DEG C of heating 0.6h, 550 DEG C successively
Hot 3h, obtains solid powder, by solid powder after reduction treatment, then by 1500 DEG C of roasting 12min, doping type molybdenum is made
Powder, it is standby；Its own, the method for reduction treatment of solid powder is：Solid powder is placed in the reduction furnace for being passed through hydrogen, carried out
5.5h is handled, obtains the mixed-powder containing molybdenum dioxide, wherein, hydrogen flow rate 12m/s, dew point of hydrogen is -60 DEG C, and is used
Five warm areas reduce system, and the temperature of each warm area is followed successively by：530 DEG C, 550 DEG C, 580 DEG C, 600 DEG C and 620 DEG C；Continue to be passed through hydrogen
Gas, processing 5h is carried out to the mixed-powder containing molybdenum dioxide, obtains the mixed-powder containing molybdenum powder, wherein, hydrogen flow rate
20m/s, dew point of hydrogen are -70 DEG C, and are followed successively by using five warm areas reduction system, the temperature of each warm area：750℃、800℃、850
DEG C, 900 DEG C and 950 DEG C.
Step 2: according to La：W=1：0.25 mol ratio, weighs lanthanum nitrate and tungsten oxide successively, and lanthanum nitrate is all molten
Yu Shuizhong, form molar concentration and be 0.4mol/L lanthanum nitrate hexahydrate, and lanthanum nitrate hexahydrate is doped to oxidation using spray-on process
In tungsten, then add the sodium hydroxide solution that molar concentration is 1.2mol/L and adjust pH to 9.5, filter and by much filtrate 105
Dried at DEG C, then calcine 2.5h under 750 DEG C, hydrogen atmosphere, doping type tungsten powder is made, it is standby；
Step 3: according to mass percent, doping type molybdenum powder made from 82% step 1 is taken respectively, made from 15% step 2
Doping type tungsten powder and 3% vanadium oxide, then doping type molybdenum powder, doping type tungsten powder and vanadium oxide are added in batch mixer and mixed
Close 24h, and 8h be diffused in drying receptacle using vacuumizing, vacuum its 10-1Torr, rotating speed 100r/min, Ran Hou
Cold isostatic compaction 30min is carried out under 200MPa, 24h is then sintered at 2100 DEG C, and is machined out, required shape is made
Tungsten-molybdenum alloy.
Embodiment 3
The method that tungsten-molybdenum alloy is prepared using beneficial element doping, is comprised the following steps：
Step 1: will be according to Pr：Re：Mo=1：1：0.5 mol ratio, it is molten that praseodymium nitrate, nitric acid rhenium and ammonium molybdate are weighed successively
In molar concentration be 0.1mol/L citric acid solution in, formed mixed solution, add nitric acid regulation mixed solution pH to
1.2, the heating water bath mixed solution under the conditions of 85 DEG C, colloidal sol is made；Colloidal sol is added by 105 DEG C of heating 0.5h, 450 DEG C successively
Hot 2h, obtains solid powder, by solid powder after reduction treatment, then by 1550 DEG C of roasting 10min, doping type molybdenum is made
Powder, it is standby；Its own, the method for reduction treatment of solid powder is：Solid powder is placed in the reduction furnace for being passed through hydrogen, carried out
5h is handled, obtains the mixed-powder containing molybdenum dioxide, wherein, hydrogen flow rate 10m/s, dew point of hydrogen is -65 DEG C, and using five
Warm area reduces system, and the temperature of each warm area is followed successively by：530 DEG C, 550 DEG C, 580 DEG C, 600 DEG C and 620 DEG C；Continue to be passed through hydrogen,
Processing 7h is carried out to the mixed-powder containing molybdenum dioxide, obtains the mixed-powder containing molybdenum powder, wherein, hydrogen flow rate 25m/s,
Dew point of hydrogen is -60 DEG C, and is followed successively by using five warm areas reduction system, the temperature of each warm area：750℃、800℃、850℃、900
DEG C and 950 DEG C.
Step 2: according to La：W=1：0.25 mol ratio, weighs lanthanum nitrate and tungsten oxide successively, and lanthanum nitrate is all molten
Yu Shuizhong, form molar concentration and be 0.4mol/L lanthanum nitrate hexahydrate, and lanthanum nitrate hexahydrate is doped to oxidation using spray-on process
In tungsten, then add the sodium hydroxide solution that molar concentration is 1.2mol/L and adjust pH to 9.2, filter and by much filtrate 100
Dried at DEG C, then calcine 2h under 900 DEG C, hydrogen atmosphere, doping type tungsten powder is made, it is standby；
Step 3: according to mass percent, doping type molybdenum powder made from 85.5% step 1,12% step 2 is taken to be made respectively
Doping type tungsten powder and 2.5% vanadium oxide, then by doping type molybdenum powder, doping type tungsten powder and vanadium oxide add batch mixer
Middle mixing 24h, and 8h is diffused in drying receptacle using vacuumizing, vacuum its 10-1Torr, rotating speed 100r/min, then
Cold isostatic compaction 10min is carried out under 300MPa, 10h is then sintered at 2900 DEG C, and is machined out, required shape is made
The tungsten-molybdenum alloy of shape.
In the present invention preparation method for the vanadium oxide that embodiment 1 ~ 3 uses for：According to W：V=0.03：10 mol ratio, according to
It is secondary to weigh ammonium tungstate and ammonium metavanadate and ammonium tungstate and ammonium metavanadate is all soluble in water, solution is formed, is then added certain
Formic acid is measured, after the pH to 2.0 ~ 3.0 for adjusting solution, solution is placed in reactor, after heating 4 ~ 36h at 100 ~ 200 DEG C, mistake
Filter and adopt and much filtrate is washed with deionized, dry, vanadium oxide is made.
The signified beneficial element of the present invention, it is to refer to the element to the performance generation beneficial effect of tungsten-molybdenum alloy, Neng Gougai
The intensity of kind tungsten-molybdenum alloy and the combination property of plasticity, doping of the present invention prepare beneficial element used by alloy include praseodymium, lanthanum,
Rhenium, vanadium.Molybdenum is bcc structures, and critical resolved shear stress is big, and plasticity is poor, the oxygen inevitably brought into material preparation process,
The impurity elements such as carbon, nitrogen are the main reason for it recrystallize fragility in the aggregation of crystal boundary.Tungsten alloy and molybdenum after present invention reduction
Alloy is intermolecular combination, improves mechanical behavior under high temperature.Rhenium can promote interstitial atom oxygen, nitrogen to be separated out at the defects of molybdenum, from
And the impurity concentration on molybdenum lattice and crystal boundary is reduced, reduce interstitial atom and be harmful to the inhibition of dislocation and its to molybdenum
Effect, so as to improve molybdenum filament elongation percentage.Mechanical behavior under high temperature test shows, the tungsten-molybdenum alloy of embodiment 1 ~ 3,1400 ~
At 1600 DEG C, there is the combination property of higher intensity and plasticity.
Claims (3)
1. the method for tungsten-molybdenum alloy is prepared using beneficial element doping, it is characterised in that comprise the following steps：
Step 1: will be according to Pr：Re：Mo=1：1：0.5 mol ratio, praseodymium nitrate, nitric acid rhenium and ammonium molybdate are weighed successively and is dissolved in lemon
In lemon acid solution, mixed solution is formed, the pH to 1.0 ~ 1.5 of nitric acid regulation mixed solution is added, under the conditions of 85 ~ 100 DEG C
Heating water bath mixed solution, colloidal sol is made；By colloidal sol successively by 100 ~ 120 DEG C heating 0.5 ~ 0.8h, 450 ~ 600 DEG C heating 2 ~
4h, solid powder is obtained, by solid powder after reduction treatment, then by 1450 ~ 1550 DEG C of 10 ~ 20min of roasting, doping is made
Type molybdenum powder, it is standby；
Step 2: according to La：W=1：0.25 mol ratio, weighs lanthanum nitrate and tungsten oxide successively, and lanthanum nitrate is all dissolved in into water
In, form molar concentration and be 0.4mol/L lanthanum nitrate hexahydrate, and lanthanum nitrate hexahydrate is doped in tungsten oxide using spray-on process,
Then add the sodium hydroxide solution that molar concentration is 1.2mol/L and adjust pH to 9.0 ~ 9.5, filter and by much filtrate 100 ~
Dried at 110 DEG C, 2 ~ 2.5h is then calcined under 750 ~ 900 DEG C, hydrogen atmosphere, doping type tungsten powder is made, it is standby；
Step 3: according to mass percent, doping type molybdenum powder made from 82 ~ 87.5% step 1,11 ~ 15% step 2 systems are taken respectively
The doping type tungsten powder and 1.5 ~ 3.0% vanadium oxide obtained, above-mentioned each component percentage by weight sum are 100%, then will doping
Type molybdenum powder, doping type tungsten powder and vanadium oxide, which are added in batch mixer, mixes 24h, and is diffused using vacuumizing in drying receptacle
8h, 10 ~ 30min of cold isostatic compaction is then carried out under 200 ~ 300MPa, 10 ~ 24h is then sintered at 2100 ~ 2900 DEG C,
And be machined out, the tungsten-molybdenum alloy of required shape is made.
2. the method according to claim 1 that tungsten-molybdenum alloy is prepared using beneficial element doping, it is characterised in that：Step 1
The method of reduction treatment of middle solid powder is：Solid powder is placed in the reduction furnace for being passed through hydrogen, 5 ~ 6h of processing is carried out, obtains
Mixed-powder containing molybdenum dioxide, wherein, 10 ~ 15m/s of hydrogen flow rate, dew point of hydrogen is -70 ~ -60 DEG C, and uses five warm areas
Reduction system, the temperature of each warm area are followed successively by：530 DEG C, 550 DEG C, 580 DEG C, 600 DEG C and 620 DEG C；Continue to be passed through hydrogen, to containing
The mixed-powder for having molybdenum dioxide carries out 5 ~ 8h of processing, obtains the mixed-powder containing molybdenum powder, wherein, 20 ~ 35m/ of hydrogen flow rate
S, dew point of hydrogen are -75 ~ -60 DEG C, and are followed successively by using five warm areas reduction system, the temperature of each warm area：750℃、800℃、850
DEG C, 900 DEG C and 950 DEG C.
3. the method according to claim 1 that tungsten-molybdenum alloy is prepared using beneficial element doping, it is characterised in that：Step 3
In the preparation method of vanadium oxide be：According to W：V=0.03：10 mol ratio, ammonium tungstate and ammonium metavanadate are weighed successively, and will
Ammonium tungstate and ammonium metavanadate are all soluble in water, form solution, then add a certain amount of formic acid, adjust the pH to 2.0 of solution ~
After 3.0, solution is placed in reactor, after heating 4 ~ 36h at 100 ~ 200 DEG C, filters and adopts to be washed with deionized and filter out
Thing, dry, vanadium oxide is made.
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| CN107254590B (en) * | 2017-06-30 | 2019-07-30 | 马鞍山华盛冶金科技发展有限公司 | A method of W metallurgy is refined using low-grade tungsten mining and metallurgy |
| CN107904466A (en) * | 2017-12-05 | 2018-04-13 | 安徽恒利增材制造科技有限公司 | A kind of high intensity tungsten molybdenum alloy |
| CN113604720B (en) * | 2021-07-28 | 2022-07-01 | 安泰天龙钨钼科技有限公司 | Large-size deformation-resistant molybdenum alloy bar and preparation method thereof |
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