CN106276941A - A kind of preparation method of molybdenum boride powder - Google Patents
A kind of preparation method of molybdenum boride powder Download PDFInfo
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- C01B35/00—Boron; Compounds thereof
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Abstract
A kind of preparation method of molybdenum boride powder, by the synthesis mode of High Temperature High Pressure in preparation process, can according to synthesis before B/Mo mol ratio n(n=0.5,1,2,2.5,4) setting, prepare the molybdenum boride powder complying fully with design of material thing phase composition, the synthesis achieving target boronation Mo thing phase composition is controlled, and the molybdenum boride powder size of synthesis is uniform, grain crystalline is complete, excellent performance.The technical process of method own is controlled, and process route is short, and targeted is strong, easy to operate, energy-efficient, and security reliability is good.Finished product molybdenum boride powder diameter is evenly distributed, grain crystalline is complete, chemical purity >=99.8%, product quality good stability, performance has had and has been obviously improved compared with the molybdenum boride material of conventional method synthesis, makes the molybdenum boride material produced show the physicochemical property of excellence in commercial Application.
Description
Technical field
The present invention relates to the preparing technical field of new material, the preparation method of a kind of molybdenum boride powder.
Background technology
Molybdenum boride based compound has high-melting-point, high rigidity, wear-resistant, high temperature resistant, corrosion resistant candle and relatively low coefficient of friction
Etc. feature, modern industry has particularly important status, be widely used in alloy material, coating material, thermal structure
The fields such as material, cathode material, resistant material, high-abrasive material, and along with the progress of science and technology, molybdenum boride based compound
Application also will be expanded further, before this material will show more excellent using value and huge market
Scape.
According to the binary phase diagraml of Mo-B, molybdenum boride based compound can be with Mo2B 、α-MoB、β-MoB、MoB2、Mo2B5、
MoB4Presented in totally 6 kinds of things phases.At present, the research report about B-Mo based compound is less both at home and abroad, and Dalian maritime affairs are big
An entitled " detonation flame spraying has been delivered in " the 6th international thermal spraying Conference Papers " in the Gaoyang learning metal material institute
The forming process of molybdenum boride metal-cermic coating " scientific paper, in paper author use sintering manufacture technique be prepared for 5-
10 μm and two kinds of MoB powder of 10-30 μm, but X line diffraction shows in its powder synthesized containing α-MoB, β-MoB, MoB2With
And Mo2B5These several thing phases, do not obtain the powder of single MoB thing phase, and this limits this material to a certain extent and is giving birth to
Actual application in product technology.Wang Yadong of Wuhan University of Technology et al. delivered in " Science Bulletin " the 27th phase of volume 57 in 2012
The scientific paper of one entitled " metal boride is as the preparation of aqueous solution negative material and volume output performance ", Wen Zhongzuo
The Mo powder that mol ratio is 1:0.5 is synthesized amorphous MoB with B powder by mechanical attrition method by person0.5Mixing with simple substance Mo
Thing, does not the most obtain the boride of the molybdenum of single thing phase, and MoB0.5Or presented in amorphous state.Central South University
Wang Yi in its thesis for the doctorate " preparation of molybdenum-base alloy high-temperature oxidation resistant coating and performance study thereof " by in-situ chemical gas phase
First sedimentation at the boron element that the substrate deposit activity of molybdenum is higher, is then occurred in situ with matrix molybdenum element by boron element
Diffusion reaction, the matrix surface at molybdenum defines one layer of boronation molybdenum layer (MoB), and this method has significant limitation, it is necessary to
Mo substrate could be formed molybdenum boride, and the molybdenum boride of synthesis is only as the coating use of Mo substrate.
Therefore, a kind of grain crystalline of preparation is complete, and finished product is the molybdenum boride powder of single thing phase, improves molybdenum boride material
Using value industrially is the most necessary.
Summary of the invention
For the deficiency of molybdenum boride preparation method in prior art, the invention provides a kind of novel molybdenum boride powder
Preparation method.The present invention is by operations such as High Temperature High Pressure synthesis, it is achieved that the synthesis of target boronation Mo thing phase composition is controlled,
And the molybdenum boride powder size of synthesis is uniform, grain crystalline is complete, excellent performance.There is widely purposes and higher market
Competitiveness.
The present invention solves that the technical scheme that above-mentioned technical problem is used is: the preparation method of a kind of molybdenum boride powder,
Comprise the following steps:
Step one, take B powder and be positioned in the graphite crucible that inwall scribbles BN powder, afterwards, graphite crucible is placed in hydrogen reducing
In stove, reduce under the conditions of 1000-1500 DEG C, must reduce B powder, standby;
Step 2, take Mo powder and be positioned in metal molybdenum crucible, afterwards, metal molybdenum crucible is placed in hydrogen reducing furnace, at 600-
Reduce under the conditions of 1200 DEG C, must reduce Mo powder, standby;
Step 3, be 0.5 or 1 or 2 or the ratio of 2.5 or 4 according to the mol ratio of B and Mo, weigh that step one prepares respectively also
The reduction Mo powder that former B powder and step 2 prepare joins in ball grinder, carries out ball milling 2-96 h;
Step 4, the material after step 3 ball milling is poured in rustless steel pallet, then, pallet is positioned over vacuum drying oven
In, it is dried under the conditions of 60-120 DEG C;
Step 5, by dried for step 4 gained material transposition in inwall scribbles the graphite crucible of BN powder, then, by graphite
Crucible is placed in vacuum drying oven, under conditions of in control vacuum drying oven, pressure is 0.5-30GPa, with the intensification speed of 0.5-30 DEG C/min
Rate intensification 800-2400 DEG C, is sintered 0.5-8h, obtains molybdenum boride granule, standby;
Step 6, the molybdenum boride granule that step 5 prepares is put into and is ground into powder in pulverizer, afterwards, according to the granularity of product
Spreading requirements selects the screen cloth of suitable mesh number to sieve, and obtaining the mol ratio of B and Mo is 0.5 or 1 or 2 or the boronation of 2.5 or 4
Molybdenum powder.
In described step one, the percent mass purity of B powder is not less than 99.5%.
In described step 2, the percent mass purity of Mo powder is not less than 99.5%.
In step 3, ball-milling medium used is ethanol, and the material of ball grinder used and ball milling ball is polytetrafluoro
Ethylene.
In step 5, the sintering temperature in described vacuum drying oven is 1200-2400 DEG C, and sintering time is 1-8h.
Beneficial effect:
1, the present invention before High Temperature High Pressure synthesizes first with material being added the processing mode of thermal reduction in hydrogen reducing furnace,
Can effectively reduce the content of the impurity such as oxygen in the water in B powder, hydrogen peroxide insoluble matter, oxygen and Mo powder, substantially increase
Synthesize raw materials used purity;Ball milling step in preparation method uses edible ethanol as ball-milling medium, selects polytetrafluoroethyl-ne
Alkene, as ball grinder and the material of ball milling ball, effectively prevent the addition of impurity element in mechanical milling process;Vacuum is used after ball milling
Mixed material is dried by drying baker, it is to avoid B powder and the secondary oxidation of Mo powder;Use the synthesis technique of High Temperature High Pressure, add
Fast B powder and the reaction rate of Mo powder, it is achieved that synthetic crystal structure the most controlled, improve molybdenum boride powder grain knot
Brilliant integrity, and ensure that the molybdenum boride product of release cooling synthesis later can keep its High Temperature High Pressure under normal pressure and temperature
Crystal structure under state and material property.
2, the present invention uses the synthesis mode of High Temperature High Pressure, can according to synthesis before B/Mo mol ratio n(n=0.5,1,2,
2.5,4) setting, prepares the molybdenum boride powder complying fully with design of material thing phase composition, and this powder can be
Mo2B、α-MoB、β-MoB、MoB2、 Mo2B5、MoB4Or the mixture of several person, the technical process of method own is controlled, process route
Short, targeted is strong, easy to operate, energy-efficient, and security reliability is good.Finished product molybdenum boride powder diameter is evenly distributed, crystal grain
Perfect crystalline, chemical purity >=99.8%, product quality good stability, performance compared with the molybdenum boride material of conventional method synthesis
Have and be obviously improved, made the molybdenum boride material produced show the physicochemical property of excellence in commercial Application.Can be used for alloy
Additive, coating material, high-temperature structural material, cathode material, hard alloy, resistant material, rub resistance material, target, earthenware
The field such as crucible and functional material.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the α-MoB powder prepared by embodiment 1;
Fig. 2 is the SEM sem image of the α-MoB powder prepared by embodiment 1;
Fig. 3 is the SEM sem image of the α-MoB powder prepared by embodiment 1;
Fig. 4 is the SEM sem image of the MoB base hot spray powder prepared by the present invention;
Fig. 5 is the cross section metallographic shape appearance figure of the MoB base hot-spraying coating prepared by the present invention.
Detailed description of the invention
With specific embodiment technical scheme done further details of elaboration and explanation below in conjunction with the accompanying drawings.
The preparation method of a kind of novel boronation molybdenum powder material, this preparation method uses the mode of High Temperature High Pressure to synthesize first
Molybdenum boride powder, does not all find the report of similar synthetic method in the documents such as current patent, report and paper.It is concrete
Preparation method comprise the steps:
Step one, the most respectively B powder and Mo powder are placed on inwall and scribble profit in the graphite crucible of BN powder and metal molybdenum crucible
Reducing with hydrogen reducing furnace, wherein the reduction temperature of boron powder is 1000-1500 DEG C, and the reduction temperature of molybdenum powder is 600-1200
℃;
Step 2, it is 0.5 or 1 or 2 or the ratio of 2.5 or 4 by the B powder after reduction and Mo powder according to mol ratio, is added separately to
Ball milling mixing 2-96h in ball mill mixing tank, wherein, ball-milling medium is edible ethanol, and ball grinder and ball milling ball all use polytetrafluoro
The material of ethylene;
Step 3, the compound after ball milling is poured in rustless steel pallet, be dried in being then placed into vacuum drying oven, dry
Dry temperature is 60-120 DEG C;
Step 4, by dried for step 3 material transposition in inwall scribbles the graphite crucible of BN powder, then, by graphite earthenware
Crucible is placed in high temperature and high pressure containers, under conditions of in control container, pressure is 0.5-30 GPa, with the liter of 0.5-30 DEG C/min
Temperature ramp, to 1200-2400 DEG C, is sintered 1-8 h, obtains molybdenum boride granule, standby;
Step 5, the molybdenum boride granule that step 4 prepares is put into and is ground into powder in pulverizer, afterwards, according to the granularity of product
Spreading requirements selects the screen cloth of suitable mesh number to sieve, and obtaining the mol ratio of B and Mo is 0.5 or 1 or 2 or the boronation of 2.5 or 4
Molybdenum powder.
Embodiment 1:
(1) the most respectively B powder and Mo powder are placed in inwall scribbles the graphite crucible of BN powder and metal molybdenum crucible and utilize hydrogen
Gas reduction furnace reduces, and wherein the reduction temperature of boron powder is 1200 DEG C, and the reduction temperature of molybdenum powder is 1050 DEG C;
(2) B powder and Mo powder after reducing are the ratio of 1:1 according to mol ratio, are added separately to ball milling in ball mill mixing tank and mix
Closing 48 h, ball-milling medium is edible ethanol, and ball grinder and ball milling ball all use the material of politef;
(3) compound after ball milling is poured in rustless steel pallet, be dried in being then placed into vacuum drying oven, be dried temperature
Degree is 100 DEG C;
(4) by dried for step 3 material transposition in inwall scribbles the graphite crucible of BN powder, then, by graphite crucible
It is placed in high temperature and high pressure containers, under conditions of pressure is 20 GPa in control container, is warming up to the heating rate of 3 DEG C/min
1600 DEG C, it is sintered 4 h, obtains α-MoB granule;
(5) the molybdenum boride granule that step 4 prepares is put into and is ground into powder in pulverizer, afterwards, according to the particle size distribution of product
Require select suitable mesh number screen cloth sieve, through X ray diffracting spectrum measure display: obtain be chemical formula be α-MoB
Molybdenum boride powder.
Embodiment 2:
(1) the most respectively B powder and Mo powder are placed in inwall scribbles the graphite crucible of BN powder and metal molybdenum crucible and utilize hydrogen
Gas reduction furnace reduces, and wherein the reduction temperature of boron powder is 1200 DEG C, and the reduction temperature of molybdenum powder is 1050 DEG C;
(2) B powder and Mo powder after reducing are the ratio of 1:1 according to mol ratio, are added separately to ball milling in ball mill mixing tank and mix
Closing 48 h, ball-milling medium is edible ethanol, and ball grinder and ball milling ball all use the material of politef;
(3) compound after ball milling is poured in rustless steel pallet, be dried in being then placed into vacuum drying oven, be dried temperature
Degree is 100 DEG C;
(4) by dried for step 3 material transposition in inwall scribbles the graphite crucible of BN powder, then, by graphite crucible
It is placed in high temperature and high pressure containers, under conditions of pressure is 28 GPa in control container, is warming up to the heating rate of 3 DEG C/min
2200 DEG C, it is sintered 4 h, obtains β-MoB granule;
(5) the molybdenum boride granule that step 4 prepares is put into and is ground into powder in pulverizer, afterwards, according to the particle size distribution of product
Require select suitable mesh number screen cloth sieve, through X ray diffracting spectrum measure display: obtain be chemical formula be β-MoB
Molybdenum boride powder.
Embodiment 3:
(1) the most respectively B powder and Mo powder are placed in inwall scribbles the graphite crucible of BN powder and metal molybdenum crucible and utilize hydrogen
Gas reduction furnace reduces, and wherein the reduction temperature of boron powder is 1200 DEG C, and the reduction temperature of molybdenum powder is 1050 DEG C;
(2) B powder and Mo powder after reducing are the ratio of 1.5:1 according to mol ratio, are added separately to ball milling in ball mill mixing tank
48 h are closed in mixing, and ball-milling medium is edible ethanol, and ball grinder and ball milling ball all use the material of politef;
(3) compound after ball milling is poured in rustless steel pallet, be dried in being then placed into vacuum drying oven, be dried temperature
Degree is 100 DEG C;
(4) by dried for step 3 material transposition in inwall scribbles the graphite crucible of BN powder, then, by graphite crucible
It is placed in high temperature and high pressure containers, under conditions of pressure is 20 GPa in control container, is warming up to the heating rate of 3 DEG C/min
1800 DEG C, it is sintered 4 h, obtains α-MoB and MoB2Mixed-powder;
(5) the molybdenum boride granule that step 4 prepares is put into and is ground into powder in pulverizer, afterwards, according to the particle size distribution of product
Require select suitable mesh number screen cloth sieve, through X ray diffracting spectrum measure display: obtain be chemical formula be α-MoB
And MoB2Molybdenum boride mixed-powder.
Embodiment 4:
(1) the most respectively B powder and Mo powder are placed in inwall scribbles the graphite crucible of BN powder and metal molybdenum crucible and utilize hydrogen
Gas reduction furnace reduces, and wherein the reduction temperature of boron powder is 1200 DEG C, and the reduction temperature of molybdenum powder is 1050 DEG C;
(2) B powder and Mo powder after reducing are the ratio of 4:1 according to mol ratio, are added separately to ball milling in ball mill mixing tank and mix
Closing 48 h, ball-milling medium is edible ethanol, and ball grinder and ball milling ball all use the material of politef;
(3) compound after ball milling is poured in rustless steel pallet, be dried in being then placed into vacuum drying oven, be dried temperature
Degree is 100 DEG C;
(4) by dried for step 3 material transposition in inwall scribbles the graphite crucible of BN powder, then, by graphite crucible
It is placed in high temperature and high pressure containers, under conditions of pressure is 20 GPa in control container, is warming up to the heating rate of 3 DEG C/min
2200 DEG C, it is sintered 4 h, obtains MoB4Granule;
(5) the molybdenum boride granule that step 4 prepares is put into and is ground into powder in pulverizer, afterwards, according to the particle size distribution of product
Require select suitable mesh number screen cloth sieve, through X ray diffracting spectrum measure display: obtain be chemical formula be MoB4's
Molybdenum boride powder.
Embodiment 5:
(1) the most respectively B powder and Mo powder are placed in inwall scribbles the graphite crucible of BN powder and metal molybdenum crucible and utilize hydrogen
Gas reduction furnace reduces, and wherein the reduction temperature of boron powder is 1200 DEG C, and the reduction temperature of molybdenum powder is 1050 DEG C;
(2) B powder and Mo powder after reducing are the ratio of 0.5:1 according to mol ratio, are added separately to ball milling in ball mill mixing tank
Mixing 56 h, ball-milling medium is edible ethanol, and ball grinder and ball milling ball all use the material of politef;
(3) compound after ball milling is poured in rustless steel pallet, be dried in being then placed into vacuum drying oven, be dried temperature
Degree is 100 DEG C;
(4) by dried for step 3 material transposition in inwall scribbles the graphite crucible of BN powder, then, by graphite crucible
It is placed in high temperature and high pressure containers, under conditions of pressure is 30 GPa in control container, heats up with the heating rate of 20 DEG C/min
To 2000 DEG C, it is sintered 6 h, obtains Mo2B granule;
(5) the molybdenum boride granule that step 4 prepares is put into and is ground into powder in pulverizer, afterwards, according to the particle size distribution of product
Require select suitable mesh number screen cloth sieve, through X ray diffracting spectrum measure display: obtain be chemical formula be Mo2B's
Molybdenum boride powder.
Embodiment 6:
(1) the most respectively B powder and Mo powder are placed in inwall scribbles the graphite crucible of BN powder and metal molybdenum crucible and utilize hydrogen
Gas reduction furnace reduces, and wherein the reduction temperature of boron powder is 1200 DEG C, and the reduction temperature of molybdenum powder is 1000 DEG C;
(2) B powder and Mo powder after reducing are the ratio of 2:1 according to mol ratio, are added separately to ball milling in ball mill mixing tank and mix
Closing 24h, ball-milling medium is edible ethanol, and ball grinder and ball milling ball all use the material of politef;
(3) compound after ball milling is poured in rustless steel pallet, be dried in being then placed into vacuum drying oven, be dried temperature
Degree is 90 DEG C;
(4) by dried for step 3 material transposition in inwall scribbles the graphite crucible of BN powder, then, by graphite crucible
It is placed in high temperature and high pressure containers, under conditions of pressure is 0.5GPa in control container, heats up with the heating rate of 30 DEG C/min
To 1700 DEG C, it is sintered 6h, obtains MoB2Granule;
(5) the molybdenum boride granule that step 4 prepares is put into and is ground into powder in pulverizer, afterwards, according to the particle size distribution of product
Require select suitable mesh number screen cloth sieve, through X ray diffracting spectrum measure display: obtain be chemical formula be MoB2's
Molybdenum boride powder.
Embodiment 7:
(1) the most respectively B powder and Mo powder are placed in inwall scribbles the graphite crucible of BN powder and metal molybdenum crucible and utilize hydrogen
Gas reduction furnace reduces, and wherein the reduction temperature of boron powder is 1300 DEG C, and the reduction temperature of molybdenum powder is 800 DEG C;
(2) B powder and Mo powder after reducing are the ratio of 2.5:1 according to mol ratio, are added separately to ball milling in ball mill mixing tank
Mixing 72h, ball-milling medium is edible ethanol, and ball grinder and ball milling ball all use the material of politef;
(3) compound after ball milling is poured in rustless steel pallet, be dried in being then placed into vacuum drying oven, be dried temperature
Degree is 120 DEG C;
(4) by dried for step 3 material transposition in inwall scribbles the graphite crucible of BN powder, then, by graphite crucible
It is placed in high temperature and high pressure containers, under conditions of pressure is 15 GPa in control container, heats up with the heating rate of 0.5 DEG C/min
To 1900 DEG C, it is sintered 0.5 h, obtains Mo2B5Granule;
(5) the molybdenum boride granule that step 4 prepares is put into and is ground into powder in pulverizer, afterwards, according to the particle size distribution of product
Require select suitable mesh number screen cloth sieve, through X ray diffracting spectrum measure display: obtain be chemical formula be Mo2B5's
Molybdenum boride powder.
The molybdenum boride powder using the present invention to prepare below carries out the system of MoB base hot spray powder coating as coating material
Standby, realize especially by following operation:
(1) the boronation molybdenum powder that the present invention is prepared by the supersonic velocity flame plating equipment using U.S.'s Praxair model to be JP8000
End sprays as coating material.
(2) spray parameters is as follows: kerosene amount 6.5 GPH, amount of oxygen 1950 SCFH, carrier gas 23 SCFH, powder feeding rate 65g/
Min, spray distance 380mm.Coating cross sections metallographic pattern after spraying is as shown in Figure 5.
Claims (5)
1. the preparation method of a molybdenum boride powder, it is characterised in that comprise the following steps:
Step one, take B powder and be positioned in the graphite crucible that inwall scribbles BN powder, afterwards, graphite crucible is placed in hydrogen reducing
In stove, reduce under the conditions of 1000-1500 DEG C, must reduce B powder, standby;
Step 2, take Mo powder and be positioned in metal molybdenum crucible, afterwards, metal molybdenum crucible is placed in hydrogen reducing furnace, at 600-
Reduce under the conditions of 1200 DEG C, must reduce Mo powder, standby;
Step 3, be 0.5 or 1 or 2 or the ratio of 2.5 or 4 according to the mol ratio of B and Mo, weigh that step one prepares respectively also
The reduction Mo powder that former B powder and step 2 prepare joins in ball grinder, carries out ball milling 2-96 h;
Step 4, the material after step 3 ball milling is poured in rustless steel pallet, then, pallet is positioned over vacuum drying oven
In, it is dried under the conditions of 60-120 DEG C;
Step 5, by dried for step 4 gained material transposition in inwall scribbles the graphite crucible of BN powder, then, by graphite
Crucible is placed in vacuum drying oven, under conditions of in control vacuum drying oven, pressure is 0.5-30GPa, with the intensification speed of 0.5-30 DEG C/min
Rate is warming up to 800-2400 DEG C, is sintered 0.5-8h, obtains molybdenum boride granule, standby;
Step 6, the molybdenum boride granule that step 5 prepares is put into and is ground into powder in pulverizer, afterwards, according to the granularity of product
Spreading requirements selects the screen cloth of suitable mesh number to sieve, and obtaining the mol ratio of B and Mo is 0.5 or 1 or 2 or the boronation of 2.5 or 4
Molybdenum powder.
The preparation method of a kind of molybdenum boride powder the most according to claim 1, it is characterised in that: B powder in described step one
Percent mass purity not less than 99.5%.
The preparation method of a kind of molybdenum boride powder the most according to claim 1, it is characterised in that: Mo powder in described step 2
Percent mass purity not less than 99.5%.
The preparation method of a kind of molybdenum boride powder the most according to claim 1, it is characterised in that: in step 3, used
Ball-milling medium be ethanol, the material of balls grinding jar and ball milling ball is politef.
The preparation method of a kind of molybdenum boride powder the most according to claim 1, it is characterised in that: in step 5, described
Sintering temperature in vacuum drying oven is 1200-2400 DEG C, and sintering time is 1-8h.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB761311A (en) * | 1954-09-23 | 1956-11-14 | Norton Grinding Wheel Co Ltd | Process for the production of metal borides or mixtures of metal borides and carbon boride |
GB812092A (en) * | 1955-12-28 | 1959-04-15 | Norton Grinding Wheel Co Ltd | Process for the production of borides |
US3334974A (en) * | 1963-08-07 | 1967-08-08 | Atomic Energy Authority Uk | Manufacture of refractory compounds |
CN102530974A (en) * | 2012-02-28 | 2012-07-04 | 吉林大学 | High-temperature high-pressure preparation method of molybdenum boride |
-
2016
- 2016-08-26 CN CN201610729515.4A patent/CN106276941B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB761311A (en) * | 1954-09-23 | 1956-11-14 | Norton Grinding Wheel Co Ltd | Process for the production of metal borides or mixtures of metal borides and carbon boride |
GB812092A (en) * | 1955-12-28 | 1959-04-15 | Norton Grinding Wheel Co Ltd | Process for the production of borides |
US3334974A (en) * | 1963-08-07 | 1967-08-08 | Atomic Energy Authority Uk | Manufacture of refractory compounds |
CN102530974A (en) * | 2012-02-28 | 2012-07-04 | 吉林大学 | High-temperature high-pressure preparation method of molybdenum boride |
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CN107541693A (en) * | 2017-07-29 | 2018-01-05 | 江苏华海冶金机械设备有限公司 | Sinking roller corrosion-resistant finishes preparation technology |
CN107986290A (en) * | 2017-12-30 | 2018-05-04 | 湖南人文科技学院 | A kind of preparation method of chromium boride powder |
CN107986793A (en) * | 2017-12-30 | 2018-05-04 | 湖南人文科技学院 | A kind of preparation method of boronation zirconium powder |
CN109574673A (en) * | 2018-11-01 | 2019-04-05 | 中国科学院上海硅酸盐研究所 | A method of boride powder is prepared using discarded boride ceramics |
CN109574673B (en) * | 2018-11-01 | 2021-11-02 | 中国科学院上海硅酸盐研究所 | Method for preparing boride powder by using waste boride ceramic |
CN111961942A (en) * | 2020-10-10 | 2020-11-20 | 中铁工程装备集团有限公司 | Wear-resistant material, preparation method and application |
CN111961942B (en) * | 2020-10-10 | 2021-09-24 | 中铁工程装备集团有限公司 | Wear-resistant material, preparation method and application |
CN113816392A (en) * | 2021-10-14 | 2021-12-21 | 北京华威锐科化工有限公司 | Preparation method of hafnium boride powder |
CN114605187A (en) * | 2022-03-22 | 2022-06-10 | 河南省龙灯生物科技有限公司 | Rubber tree cutting nutrient solution |
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