CN105903976A - Molybdenum alloy doping method - Google Patents
Molybdenum alloy doping method Download PDFInfo
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- CN105903976A CN105903976A CN201610272344.7A CN201610272344A CN105903976A CN 105903976 A CN105903976 A CN 105903976A CN 201610272344 A CN201610272344 A CN 201610272344A CN 105903976 A CN105903976 A CN 105903976A
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 229910001182 Mo alloy Inorganic materials 0.000 title claims abstract description 18
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 claims abstract description 40
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002270 dispersing agent Substances 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 239000002019 doping agent Substances 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims description 26
- 238000001914 filtration Methods 0.000 claims description 21
- 238000006703 hydration reaction Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 14
- 230000036571 hydration Effects 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 11
- 238000004663 powder metallurgy Methods 0.000 abstract description 3
- 239000003595 mist Substances 0.000 abstract 1
- 238000011085 pressure filtration Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 35
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 16
- 239000000463 material Substances 0.000 description 10
- 238000005275 alloying Methods 0.000 description 4
- 229910000420 cerium oxide Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
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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
-
- B22F1/0003—
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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
- B22F1/14—Treatment of metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/026—Spray drying of solutions or suspensions
-
- 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
- C22C1/045—Alloys based on refractory metals
-
- 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
-
- 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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- 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
Abstract
The invention belongs to the technical field of powder metallurgy, and particularly relates to a molybdenum alloy doping method. The method comprises the steps that (1) a solid dopant with the grain size being in nanometer scale or submicron scale and a dispersing agent are mixed with the weight ratio being 1:0.5-10 and then ground, and the grinding time is 1-20 h; (2) the dispersing agent is added into slurry obtained after grinding again for dispersing, the weight ratio of the slurry to the dispersing agent is 1:1-50, and the dispersing time is 1-24 h; (3) a solution obtained after dispersing is subjected to still standing; (4) the solution is filtered, and a hydrate gellike solution and filter residues are obtained; and (5) the hydrate gellike solution is sprayed on the surface of molybdenum dioxide or the surface of molybdenum trioxide in a mist mode. Nano-scale or submicron-scale reagents are dispersed through a grinding-gellike dispersing method, large-grain reagents are filtered through a vacuum negative pressure filtration method, and the uniformity of solid-solid doping can be effectively achieved.
Description
Technical field
The invention belongs to powder metallurgical technology, be specifically related to the doping method of a kind of molybdenum alloy.
Background technology
Alloying is the inevitable direction of Materials, can be obviously improved the performance of material by alloying, fully excavates the use potentiality of material.Molybdenum is typically to prepare through powder metallurgy process, and the method for powder metallurgy can effectively reduce cost, prepares grained material.Molybdenum realizes the approach of alloying and is mainly added in molybdenum dioxide or molybdenum trioxide or ammonium molybdate by the way of doping by alloying element.Doping method mainly has at present: sol-gel, liquid-solid doping, solid-solid doping.The doping of liquid liquid mainly has the generation of waste liquid to limit it and promote the use of, liquid-solid doping application relatively wide but produce waste gas, waste liquor contamination, hostile environment and limited；Admittedly Gu doping nonstaining property waste liquid, waste gas are discharged, and raw materials recovery rate is high, but there is dispute in uniformity.
Summary of the invention
The problem existed for above-mentioned prior art, the present invention provides the doping method of a kind of molybdenum alloy, it is possible to effectively solve the homogeneity question of solid-solid doping.
The present invention is achieved by the following technical solutions:
The doping method of a kind of molybdenum alloy, it is characterised in that described method step includes:
(1) by granularity be nanometer, the solid dopant thing of submicron order be to be ground after 1:0.5 ~ 10 mix with dispersant according to weight ratio, milling time is 1 ~ 20h；
(2) again adding dispersant in the slurry obtained after grinding to disperse, slurry is 1:1 ~ 50 with the weight ratio of dispersant, and jitter time is 1 ~ 24h；
(3) solution obtained after dispersion is stood；
(4) solution is filtered, obtain being hydrated gellike solution and filtering residue；
(5) hydration gellike solution 10～50:1 is doped with hydration gellike solution by volume with vaporific molybdenum dioxide or molybdenum trioxide surface, molybdenum dioxide or the molybdenum trioxide of being sprayed on.
According to above-mentioned method, it is characterised in that the composition composition of described dispersant is by volume: deionized water, ethanol, acetone=0 ~ 10:0 ~ 10:0 ~ 10, be wherein zero during three's content difference.
According to above-mentioned method, it is characterised in that in step (1), solid dopant thing joins in diamond lap tank with dispersant and is ground.
According to above-mentioned method, it is characterised in that the slurry obtained after grinding in step (2) joins and carries out vibration dispersion in multi-frequency ultrasonic vibra shoot.
According to above-mentioned method, it is characterised in that step (3) time of repose is 0.5h ~ 2h.
According to above-mentioned method, it is characterized in that, after the solution obtained through dispersion is stood, use wide strip filter paper to insert in solution and keep taking-up after 30s, putting into and be dried 0.5h in drying baker, paper slip immerses the part in solution, and to be cut into isometric size some, weigh, when each section of deviation of weight is more than 5%, repeat step (2).
According to above-mentioned method, it is characterised in that solution is poured in vacuum filter tank and filtered by step (4), filter mesh number more than 300 mesh.
According to above-mentioned method, it is characterized in that, after step (5) will be hydrated gellike solution pressurization 0.2 ~ 0.8MPa, by nozzle with the vaporific molybdenum dioxide being sprayed in doping tank or molybdenum trioxide surface, in described doping tank tank, negative pressure is 0.02 ~ 0.1MPa, and tank body rotates with 300～1000 turns/min.
According to above-mentioned method, it is characterised in that in step (4) when filtering residue weight is higher than the 10% of former solid dopant thing weight, filtering residue is repeated step (1) and (2).
According to above-mentioned method, it is characterised in that after spraying terminates, utilize the humidity change at each position in hygronom detection doping tank, when the psychrometric difference at each position is more than ± 5% and less than ± 10%, increase mixing time 1h ~ 4h；When psychrometric difference is more than ± 10% and less than ± 20%, increase mixing time 2h ~ 6h.
The technique effect of the present invention: the invention provides the doping method of a kind of molybdenum alloy, this method passes through grinding-gellike dispersion method by nanometer and the dispensing reagents of submicron order, negative pressure of vacuum suction method carries out bulky grain reagent filtration, it is possible to the effective homogeneity question solving solid-solid doping.
Detailed description of the invention
A kind of doping method of molybdenum alloy, described method step includes:
(1) by granularity be nanometer, submicron order solid dopant thing and dispersant according to weight ratio be 1:0.5 ~ 10 add grinding pot mixes after be ground, milling time is 1 ~ 20h；
(2) slurry obtained after grinding joins in multi-frequency ultrasonic vibra shoot, again adds dispersant and carries out vibration dispersion, and slurry is 1:1 ~ 50 with the weight ratio of dispersant, and jitter time is 1 ~ 24h；
(3) being stood by the solution obtained after dispersion, time of repose is 0.5 ~ 2h, observes gellike solution and forms effect；
(4) use wide strip filter paper to insert in solution to be slowly withdrawn after holding 30s, putting into and be dried 0.5h in drying baker, paper slip immerses the part in solution, and to be cut into isometric size some, weigh, each section of deviation of weight, less than 5%, shows that the grinding-hydration gellike dispersion of reagent meets doping requirement；Otherwise, the dispersion grinding-be hydrated gellike reagent need to repeat.
(5) solution is poured in vacuum filter tank filter, filter mesh number more than 300 mesh, obtain being hydrated gellike solution and filtering residue；When filtering residue weighs less than the 10% of former solid dopant thing weight, proceed next step, when filtering residue weight is higher than the 10% of former solid dopant thing weight, filtering residue is scraped and repeats step (1) and (2)；
(6) by after the hydration gellike solution pressurization 0.2 ~ 0.8MPa through being filtrated to get, by nozzle with the vaporific molybdenum dioxide being sprayed in doping tank or molybdenum trioxide surface, this nozzle inserts in the bearing at doping tank charging aperture, in doping tank tank, negative pressure is 0.02 ~ 0.1MPa, tank body rotates with 300～1000 turns/min, and molybdenum dioxide or molybdenum trioxide 10～50:1 are doped by volume with hydration gellike solution.
Preferably, the composition composition of dispersant is by volume: deionized water, ethanol, acetone=0 ~ 10:0 ~ 10:0 ~ 10, be wherein zero during three's content difference.
After spraying terminates, utilize central authorities, edge, upper strata, intermediate layer, the humidity change of bottom in hygronom detection doping tank, when the humidity at each position differs less than ± 5%, i.e. preliminary judgement uniform doping；Otherwise psychrometric difference exceedes ± 5% and less than ± 10%, then judge time uniformly, mixing time to be increased 1h ~ 4h；As psychrometric difference exceed ± 10% and less than ± 20%, then judge to owe uniformly, need mixing time to increase 2h ~ 6h；Increase molybdenum dioxide or molybdenum trioxide and hydration gellike solution proportion 10% ~ 50% when rear batch, and batch mixing speed is accelerated 20% ~ 50%.
Embodiment 1
With the ratio of 1:0.5, nano-cerium oxide 1.24kg and dispersant 0.62kg is added grinding pot be ground, grind 2h, slurry after grinding adds multi-frequency ultrasonic oscillating trough, again adds deionized water dispersion, and nano-cerium oxide slurry and dispersive agent ratio are 1:50；Through 1h vibrations dispersion, pour standing 0.5h in glass jar into, observe solution change；Use wide strip filter paper to insert in solution to be slowly withdrawn after holding 30s, put into and drying baker is dried 0.5h, paper slip is cut into isometric size 3 sections, weigh, on the basis of the top, each section of deviation of weight is respectively 2%, 3%, shows that the grinding-hydration gellike dispersion of reagent meets doping requirement；Dispersion being formed after hydration gellike solution pours vacuum filter tank into and seal, filter mesh number 300 mesh, after filtration, filtering residue 353g on filter screen, scraped by filtering residue and repeat grinding, dispersive process, it is 45g that second time weighs filtering residue, it is determined that can continue next step；By being entered the doping tank of 0.02MPa negative pressure after the hydration gellike solution pressurization 0.2MPa in tank by nozzle, with the vaporific molybdenum dioxide surface being sprayed in doping tank；According to material: solution carries out gellike solute doping than 20:1, molybdenum dioxide stirs in the tank body of 300 turns/min of rotating speed, when hydrojet is complete, hygronom is utilized to detect the humidity change of mixing tank central authorities, edge, upper strata, intermediate layer, bottom, the psychrometric difference-1% ,-1%, 1.5% ,-1.5% at each position, preliminary judgement uniform doping is tested with top guide center；Adulterate complete, carry out doping material heating vacuumizing and drying.After doping molybdenum dioxide carries out two sections of reduction, batch mixing 2h, every barrel of different parts samples 3, detection composition 0.88%, 0.9%, the former set component of 0.91%(0.9%)；Alloyed powder is suppressed diameter 20mm rod base and is sintered densification, sintered bar base takes 5 samples, preparation metallographic phase sample, by 100 times of metallographic observations, crystallite dimension 10 ~ 20um, size uniformity, is doped scanning phase, to sample grid division 3 again by high power (being not less than 5000 times) scanning electron microscope JSM 6700F and energy disperse spectroscopy2Each grid beaten power spectrum and determines composition, adding up 80% grid and cerium oxide can be detected, and cerium oxide particle size 30nm ~ 90nm determines that doping dispersion is uniform.
Embodiment 2
With the ratio of 1:5, nano lanthanum oxide 2 kg and dispersant 10kg being added grinding pot be ground, grind 10h, the slurry after grinding adds in multi-frequency ultrasonic oscillating trough, again adds ethanol dispersion, and nano lanthanum oxide slurry and dispersive agent ratio are 1:5；Through 12h vibrations dispersion, pour standing 1h in glass jar into, observe solution change；Use wide strip filter paper to insert in solution to be slowly withdrawn after holding 30s, put into and drying baker is dried 0.5h, paper slip is cut into isometric size 4 sections, weigh, on the basis of the top, each section of deviation of weight is respectively 2%, 2.5%, 3.5%, shows that the grinding-hydration gellike dispersion of reagent meets doping requirement；Dispersion is formed after hydration gellike solution pours vacuum filter tank into and seal, filter mesh number 400 mesh, after filtration, filtering residue 452g on filter screen, being scraped by filtering residue and repeat grinding, dispersive process, second time weighs 267g, repeats to grind, disperse, it is 85g that third time weighs filtering residue, it is determined that can continue next step；By being entered the doping tank of 0.06MPa negative pressure after the hydration gellike solution pressurization 0.5MPa in tank by nozzle, with the vaporific molybdenum dioxide surface being sprayed in doping tank；According to material: solution carries out gellike solute doping than for 10:1, molybdenum dioxide stirs in the tank body of 500 turns/min of rotating speed, when hydrojet is complete, hygronom is utilized to detect the humidity change of mixing tank central authorities, edge, upper strata, intermediate layer, bottom, the psychrometric difference 0.5%, 4.5% ,-5.5% ,-7.5% at each position is tested with top guide center, preliminary judgement doping time is uniformly, by doped raw material batch mixing 2h, in the reagent dilutions of rear batch, increase diluent ratio 20%, and batch mixing speed is adjusted to 800 turns/min.Adulterate complete, carry out doping material heating vacuumizing and drying.After doping molybdenum dioxide is carried out two sections of reduction, batch mixing 3h, every barrel of different parts samples 4, detection composition 1.42%, 1.38%, 1.4%, the former set component of 1.41%(1.4%)；The 1kg slab that alloyed powder is suppressed thickness 12mm is sintered densification, sintering slab takes 5 samples, preparation metallographic phase sample, by 100 times of metallographic observations, crystallite dimension 20 ~ 30um, size uniformity, is doped scanning phase, to sample grid division 4 again by high power (being not less than 5000 times) scanning electron microscope JSM 6700F and energy disperse spectroscopy2Each grid being beaten power spectrum and determines composition, the grid of statistics 90% can detect lanthana, and lanthanum oxide particles size 20nm ~ 0.1 μm, determines that doping dispersion is uniform.
Embodiment 3
With the ratio of 1:10, submicron lanthana 0.6kg and dispersant 6kg is added diamond lap tank be ground, grind 20h, slurry after grinding adds in multi-frequency ultrasonic oscillating trough, again adds acetone dispersion, and nano lanthanum oxide slurry and dispersive agent ratio are 1:20；Through 24h vibrations dispersion, pour standing 2h in glass jar into, observe solution change；Use wide strip filter paper to insert in solution to be slowly withdrawn after holding 30s, put into and drying baker is dried 0.5h, paper slip is cut into isometric size 6 sections, weigh, on the basis of the top, each section of deviation of weight is respectively 0.5%, 0.5%, 0.8%, 0.8%, 1.0%, shows that the grinding-hydration gellike dispersion of reagent meets doping requirement；Dispersion is formed after hydration gellike solution pours vacuum filter tank into and seal, filter mesh number 600 mesh, after filtration, filtering residue 52g on filter screen, it is determined that next step can be continued；Hydration gellike solution in tank is pressurizeed after 0.8MPa, entered the doping tank of 0.1MPa negative pressure by nozzle, with the vaporific molybdenum dioxide surface being sprayed in doping tank；According to material: solution carries out gellike solute doping than for 50:1, molybdenum dioxide stirs in the tank body of 800 turns/min of rotating speed, when hydrojet is complete, hygronom is utilized to detect the humidity change of mixing tank central authorities, edge, upper strata, intermediate layer, bottom, the psychrometric difference 2.5%, 4%, 5.1%, 6.7% at each position is tested with top guide center, preliminary judgement doping time is uniformly, by doped raw material batch mixing 4h, in the reagent dilutions of rear batch, increase diluent ratio 20%, and batch mixing speed is adjusted to 1000 turns/min.Adulterate complete, carry out doping material heating vacuumizing and drying.After doping molybdenum dioxide is carried out two sections of reduction, batch mixing 4h, every barrel of different parts samples 4, detection composition 0.42%, 0.38%, 0.4%, the former set component of 0.41%(0.4%)；The 1kg slab that alloyed powder is suppressed thickness 12mm is sintered densification, sintering slab takes 5 samples, preparation metallographic phase sample, by 100 times of metallographic observations, crystallite dimension 20 ~ 40um, size uniformity, is doped scanning phase, to sample grid division 5 again by high power (being not less than 5000 times) scanning electron microscope JSM 6700F and energy disperse spectroscopy2Each grid being beaten power spectrum and determines composition, the grid of statistics 73% can detect lanthana, and lanthanum oxide particles size 50nm ~ 0.2 μm, determines that doping dispersion is uniform.
Claims (10)
1. the doping method of a molybdenum alloy, it is characterised in that described method step includes:
(1) by granularity be nanometer, the solid dopant thing of submicron order be to be ground after 1:0.5 ~ 10 mix with dispersant according to weight ratio, milling time is 1 ~ 20h；
(2) again adding dispersant in the slurry obtained after grinding to disperse, slurry is 1:1 ~ 50 with the weight ratio of dispersant, and jitter time is 1 ~ 24h；
(3) solution obtained after dispersion is stood；
(4) solution is filtered, obtain being hydrated gellike solution and filtering residue；
(5) hydration gellike solution 10～50:1 is doped with hydration gellike solution by volume with vaporific molybdenum dioxide or molybdenum trioxide surface, described molybdenum dioxide or the molybdenum trioxide of being sprayed on.
The doping method of a kind of molybdenum alloy the most according to claim 1, it is characterised in that the composition composition of described dispersant is by volume: deionized water, ethanol, acetone=0 ~ 10:0 ~ 10:0 ~ 10, be wherein zero during three's content difference.
The doping method of a kind of molybdenum alloy the most according to claim 1, it is characterised in that in step (1), solid dopant thing joins in diamond lap tank with dispersant and is ground.
The doping method of a kind of molybdenum alloy the most according to claim 1, it is characterised in that the slurry obtained after grinding in step (2) joins and carries out vibration dispersion in multi-frequency ultrasonic vibra shoot.
The doping method of a kind of molybdenum alloy the most according to claim 1, it is characterised in that step (3) time of repose is 0.5h ~ 2h.
The doping method of a kind of molybdenum alloy the most according to claim 1, it is characterized in that, after the solution obtained through dispersion is stood, use wide strip filter paper to insert in solution and keep taking-up after 30s, putting into and be dried 0.5h in drying baker, paper slip immerses the part in solution, and to be cut into isometric size some, weigh, when each section of deviation of weight is more than 5%, repeat step (2).
The doping method of a kind of molybdenum alloy the most according to claim 1, it is characterised in that solution is poured in vacuum filter tank and filtered by step (4), filters mesh number more than 300 mesh.
The doping method of a kind of molybdenum alloy the most according to claim 1, it is characterized in that, after step (5) will be hydrated gellike solution pressurization 0.2 ~ 0.8MPa, by nozzle with the vaporific molybdenum dioxide being sprayed in doping tank or molybdenum trioxide surface, in described doping tank tank, negative pressure is 0.02 ~ 0.1MPa, and tank body rotates with 300～1000 turns/min.
The doping method of a kind of molybdenum alloy the most according to claim 1, it is characterised in that in step (4) when filtering residue weight is higher than the 10% of former solid dopant thing weight, filtering residue is repeated step (1) and (2).
The doping method of a kind of molybdenum alloy the most according to claim 1, it is characterised in that after spraying terminates, utilizes the humidity change at each position in hygronom detection doping tank, when the psychrometric difference at each position is more than ± 5% and less than ± 10%, increase mixing time 1h ~ 4h；When psychrometric difference is more than ± 10% and less than ± 20%, increase mixing time 2h ~ 6h.
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| CN111547768A (en) * | 2020-04-26 | 2020-08-18 | 金堆城钼业股份有限公司 | Preparation method for preparing rare earth ammonium dimolybdate by nano doping |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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