CN103752840B - A kind of fast preparation method of nanometer Mg alloyed powder - Google Patents
A kind of fast preparation method of nanometer Mg alloyed powder Download PDFInfo
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- CN103752840B CN103752840B CN201410011985.8A CN201410011985A CN103752840B CN 103752840 B CN103752840 B CN 103752840B CN 201410011985 A CN201410011985 A CN 201410011985A CN 103752840 B CN103752840 B CN 103752840B
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Abstract
The present invention relates to a kind of fast preparation method of nanometer Mg alloyed powder, be the situation for magnesium alloy powder grain refinement difficulty, adopt HDH method, through pulverizing magnesium alloy block, sieve, hydrogenation, heating, dehydrogenation, vacuum drying, make nanoscale magnesium alloy powder, this preparation method's technique is advanced, and fast simple and direct, informative data is accurate, the magnesium alloy powder crystal grain diameter≤30nm of preparation, product purity is high, reaches 99.5%, is the very good quick method preparing nanometer Mg alloyed powder.
Description
Technical field
The present invention relates to a kind of fast preparation method of nanometer Mg alloyed powder, belong to the technical field of the preparations and applicatio of non-ferrous alloy powder.
Background technology
Magnesium alloy is a kind of coloured light metal alloy, obtains apply more widely in electronics, automobile, aerospace industry field, and because the intensity of magnesium alloy is lower, deformability is poor, the mechanical property of magnesium alloy remains at low levels; In order to improve the combination property of magnesium alloy, the range of application of expansion magnesium alloy, crystal grain thinning is a kind of effective method.
At present, the crystal fining method of magnesium alloy have high-energy ball milling, etc. channel pressings and fast melt-quenching etc., these methods can only make magnesium alloy refining to micron order, are difficult to reach nanoscale, make the application of magnesium alloy receive great limitation.
Summary of the invention
goal of the invention
The object of the invention is the deficiency for background technology, adopt HDH method, through pulverizing, hydrogenation, heating, dehydrogenation, obtained nanoscale magnesium alloy powder, to increase substantially mechanical property and the Chemical Physics performance of magnesium alloy, expands the range of application of magnesium alloy.
technical scheme
The chemical substance material that the present invention uses is: magnesium alloy block, hydrogen, argon gas, and it is as follows that its combination prepares consumption: with gram, centimetre
3for measurement unit
Magnesium alloy block: AZ91,1000g ± 1g
Hydrogen: H
2, 100000cm
3± 100cm
3
Argon gas: Ar, 100000cm
3± 100cm
3
Preparation method is as follows:
(1) selected chemical substance material
To carry out selected to the chemical substance material that preparation uses, and carry out quality purity control:
Magnesium alloy block: solid state 99.9%
Hydrogen: gaseous atmospheres 99.5%
Argon gas: gaseous atmospheres 99.5%
(2) pretreatment magnesium alloy block
The pretreatment of magnesium alloy block is pulverized and is carried out in seal box, completes under argon shield;
1. in seal box, put pulverizer, magnesium alloy block is placed in pulverizer, pulverizer rotating speed 100r/min;
2. in seal box, argon gas is passed into, argon gas input speed 200cm
3/ min;
3. sieve with 400 eye mesh screens after seal box is pulverized;
4. pulverize, sieving repeats, after pulverizing, magnesium alloy block becomes fine powder, fine particle diameter≤0.038mm;
(3) hydrogenation treatment magnesium alloy powder
The hydrogenation treatment of magnesium alloy powder is carried out in hydrogenation furnace, completes under heating, the domestic and abroad water circulation state of defeated hydrogen, pressure process;
1. magnesium alloy powder is placed in quartz container, and adds a cover stainless steel cloth on quartz container top;
2. the quartz container filling magnesium alloy powder is placed in hydrogenation furnace, and airtight;
3. extract hydrogenation furnace air, make pressure in stove reach 0.005Pa, and constant;
4. to inputting hydrogen in stove, hydrogen input speed 100cm
3/ min, to make in stove under hydrogen atmosphere invariablenes pressure of liquid at 4MPa ± 0.1MPa;
5. open the heater of hydrogenation furnace, in stove, heating-up temperature 450 DEG C ± 2 DEG C, opens outer water circulation cooling tube, carries out outer water circulation cooling;
6. constant temperature and pressure hydrogenation 12h at pressurized with hydrogen 4MPa ± 0.1MPa, heating-up temperature 450 DEG C ± 2 DEG C;
7. close heater after hydrogenation, stop heating, open air outlet valve when making in-furnace temperature naturally be down to 70 DEG C, discharge hydrogen;
8. heating in vacuum, constant temperature isothermal holding
Open hydrogenation furnace vavuum pump, extract furnace air, make pressure in stove reach 0.005Pa;
Heater, heating-up temperature 350 DEG C ± 2 DEG C;
At 0.005Pa, constant temperature isothermal holding 4h at 350 DEG C ± 2 DEG C;
9. close heater, stop exhaust, when in-furnace temperature is down to 30 DEG C, in stove, inputting hydrogen is to normal pressure, hydrogen input speed 100cm
3/ min;
10. open hydrogenation furnace, take out quartz container and product, product is nanoscale magnesium alloy powder;
(4) detect, analyze, characterize
The pattern of nanometer Mg alloyed powder of preparation, color and luster, crystal grain, Chemical Physics performance are detected, analyze, characterized;
Grain size analysis is carried out with transmission electron microscope;
Crystal species analysis is carried out with powder x-ray diffraction;
Conclusion: nanometer Mg alloyed powder is silver gray powder, powder grain diameter≤30nm, product purity reaches 99.5%.
(5) product storage
The nanometer Mg alloyed powder of preparation is stored in the glass container of amber transparent, and airtight lucifuge stores, and moistureproof, sun-proof, anti-acid-alkali salt to corrode, storage temperature 20 DEG C, relative humidity≤10%.
beneficial effect
The present invention has obvious advance compared with background technology, be the situation for magnesium alloy powder grain refinement difficulty, adopt HDH method, through pulverizing magnesium alloy block, sieve, hydrogenation, heating, dehydrogenation, vacuum drying, make nanoscale magnesium alloy powder, this preparation method's technique is advanced, and fast simple and direct, informative data is accurate, the magnesium alloy powder crystal grain diameter≤30nm of preparation, product purity is high, reaches 99.5%, is the very good quick method preparing nanometer Mg alloyed powder.
Accompanying drawing explanation
Fig. 1 is that the state diagram of nanometer Mg alloyed powder prepared by hydrogenation furnace
Fig. 2 is nanometer Mg alloyed powder transmission shape appearance figure
Fig. 3 is nanometer Mg alloyed powder diffracted intensity collection of illustrative plates
Shown in figure, list of numerals is as follows:
1, hydrogenation furnace, 2, workbench, 3, quartz container, 4, stainless steel cloth, 5, outer water circulation cooling tube, 6, outer water circulation cooling valve, 7, hydrogen cylinder, 8, hydrogen pipe, 9, hydrogen valve, 10, hydrogen table, 11, hydrogen, 12, vavuum pump, 13, vacuum tube, 14, vacuum valve, 15, vacuum meter, 16, electric cabinet, 17, display screen, 18, indicator lamp, 19, power switch, 20, heating temperature control, 21, controller for vacuum pump, 22, furnace chamber, 23, nanometer Mg alloyed powder.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described:
Shown in Fig. 1, for the state diagram of nanometer Mg alloyed powder prepared by hydrogenation furnace, each position, annexation wants correct, and proportioning according to quantity, operates according to the order of sequence.
The value of the chemical substance that preparation uses determines by the scope pre-set, with gram, centimetre
3for measurement unit.
The preparation of nanometer Mg alloyed powder is carried out in hydrogenation furnace, completes under heating, the domestic and abroad water circulation state of cooling of defeated hydrogen, pressure process;
Hydrogenation furnace is that rectangle is vertical, and being furnace chamber 22 in hydrogenation furnace 1, is workbench 2 at furnace chamber 22 inner bottom part, quartz container 3 is put on workbench 2 top, quartz container 3 top, by stainless steel cloth 4 capping, is nanometer Mg alloyed powder 23 in quartz container 3, by hydrogen 11 filling in furnace chamber 22; Cool valve 6 around, outer water circulation cooling tube 5 by outer water circulation by outer water circulation cooling tube 5 in hydrogenation furnace 1 outside to control; Be provided with hydrogen cylinder 7 at the left part of hydrogenation furnace 1, hydrogen cylinder 7 top is hydrogen pipe 8, and hydrogen pipe 8 is provided with hydrogen valve 9, hydrogen table 10, and hydrogen pipe 8 stretches in furnace chamber 22, and inputting hydrogen 11; Be provided with vavuum pump 12 at the right part of hydrogenation furnace 1, vavuum pump 12 top is vacuum tube 13, and vacuum tube 13 is provided with vacuum valve 14, vacuum meter 15, and vacuum tube 13 stretches in furnace chamber 22, extracts furnace air out; Be provided with electric cabinet 16 in the bottom of hydrogenation furnace 1, electric cabinet 16 is provided with display screen 17, indicator lamp 18, power switch 19, heating temperature control 20, controller for vacuum pump 21.
Shown in Fig. 2, be nanometer Mg alloyed powder transmission shape appearance figure, nanometer Mg alloyed powder crystal grain≤30nm, in irregular stacking.
Shown in Fig. 3, be nanometer Mg alloyed powder diffracted intensity collection of illustrative plates, known in figure: after hydrogenation, powder becomes hydrogenation phase, after dehydrogenation, the phase composition of powder is consistent with starting powder, is still magnesium alloy powder.
Claims (2)
1. a fast preparation method for nanometer Mg alloyed powder, is characterized in that: the chemical substance material of use is: magnesium alloy block, hydrogen, argon gas, and it is as follows that its combination prepares consumption: with gram, centimetre
3for measurement unit
Magnesium alloy block: AZ91,1000g ± 1g
Hydrogen: H
2, 100000cm
3± 100cm
3
Argon gas: Ar, 100000cm
3± 100cm
3
Preparation method is as follows:
(1) selected chemical substance material
To carry out selected to the chemical substance material that preparation uses, and carry out quality purity control:
Magnesium alloy block: solid 99.9%
Hydrogen: gas 99.5%
Argon gas: gas 99.5%
(2) pretreatment magnesium alloy block
The pretreatment of magnesium alloy block is pulverized and is carried out in seal box, completes under argon shield;
1. in seal box, put pulverizer, magnesium alloy block is placed in pulverizer, pulverizer rotating speed 100r/min;
2. in seal box, argon gas is passed into, argon gas input speed 200cm
3/ min;
3. sieve with 400 eye mesh screens after seal box is pulverized;
4. pulverize, sieving repeats, after pulverizing, magnesium alloy block becomes fine powder, fine particle diameter≤0.038mm;
(3) hydrogenation treatment magnesium alloy powder
The hydrogenation treatment of magnesium alloy powder is carried out in hydrogenation furnace, completes under heating, the domestic and abroad water circulation state of defeated hydrogen, pressure process;
1. magnesium alloy powder is placed in quartz container, and adds a cover stainless steel cloth on quartz container top;
2. the quartz container filling magnesium alloy powder is placed in hydrogenation furnace, and airtight;
3. extract hydrogenation furnace air, make pressure in stove reach 0.005Pa, and constant;
4. to inputting hydrogen in stove, hydrogen input speed 100cm
3/ min, to make in stove under hydrogen atmosphere invariablenes pressure of liquid at 4MPa ± 0.1MPa;
5. open the heater of hydrogenation furnace, in stove, heating-up temperature 450 DEG C ± 2 DEG C, opens outer water circulation cooling tube, carries out outer water circulation cooling;
6. constant temperature and pressure hydrogenation 12h at pressurized with hydrogen 4MPa ± 0.1MPa, heating-up temperature 450 DEG C ± 2 DEG C;
7. close heater after hydrogenation, stop heating, open air outlet valve when making in-furnace temperature naturally be down to 70 DEG C, discharge hydrogen;
8. heating in vacuum, constant temperature isothermal holding
Open hydrogenation furnace vavuum pump, extract furnace air, make pressure in stove reach 0.005Pa;
Heater, heating-up temperature 350 DEG C ± 2 DEG C;
At 0.005Pa, constant temperature isothermal holding 4h at 350 DEG C ± 2 DEG C;
9. close heater, stop exhaust, when in-furnace temperature is down to 30 DEG C, in stove, inputting hydrogen is to normal pressure, hydrogen input speed 100cm
3/ min;
10. open hydrogenation furnace, take out quartz container and product, product is nanoscale magnesium alloy powder;
(4) detect, analyze, characterize
The pattern of nanometer Mg alloyed powder of preparation, color and luster, crystal grain, Chemical Physics performance are detected, analyze, characterized;
Grain size analysis is carried out with transmission electron microscope;
Crystal species analysis is carried out with powder x-ray diffraction;
Conclusion: nanometer Mg alloyed powder is silver gray powder, powder grain diameter≤30nm, product purity reaches 99.5%;
(5) product storage
The nanometer Mg alloyed powder of preparation is stored in the glass container of amber transparent, and airtight lucifuge stores, and moistureproof, sun-proof, anti-acid-alkali salt to corrode, storage temperature 20 DEG C, relative humidity≤10%.
2. the fast preparation method of a kind of nanometer Mg alloyed powder according to claim 1, is characterized in that: the preparation of nanometer Mg alloyed powder is carried out in hydrogenation furnace, is to complete under heating, the domestic and abroad water circulation state of cooling of defeated hydrogen, pressure process; Hydrogenation furnace is that rectangle is vertical, be furnace chamber (22) in hydrogenation furnace (1), be workbench (2) at furnace chamber (22) inner bottom part, quartz container (3) is put on workbench (2) top, quartz container (3) top is by stainless steel cloth (4) capping, be nanometer Mg alloyed powder (23) in quartz container (3), by hydrogen (11) filling in furnace chamber (22); Hydrogenation furnace (1) outside by outer water circulation cooling tube (5) around, outer water circulation cooling tube (5) cools valve (6) by outer water circulation and controls; Hydrogen cylinder (7) is provided with at the left part of hydrogenation furnace (1), hydrogen cylinder (7) top is hydrogen pipe (8), hydrogen pipe (8) is provided with hydrogen valve (9), hydrogen table (10), hydrogen pipe (8) stretches in furnace chamber (22), and inputting hydrogen (11); Vavuum pump (12) is provided with at the right part of hydrogenation furnace (1), vavuum pump (12) top is vacuum tube (13), vacuum tube (13) is provided with vacuum valve (14), vacuum meter (15), vacuum tube (13) stretches in furnace chamber (22), extracts furnace air out; Be provided with electric cabinet (16) in the bottom of hydrogenation furnace (1), electric cabinet (16) is provided with display screen (17), indicator lamp (18), power switch (19), heating temperature control (20), controller for vacuum pump (21).
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| CN103752840B true CN103752840B (en) | 2015-09-16 |
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| CN106583740B (en) * | 2016-11-29 | 2018-10-16 | 太原理工大学 | A kind of preparation method of nano-crystal magnesium alloy block |
| CN107176589B (en) * | 2017-03-31 | 2018-10-26 | 太原理工大学 | It is a kind of to prepare nanosizing Mg3Sb2The method of thermoelectric material |
| CN110273120B (en) * | 2019-07-30 | 2023-07-07 | 太原学院 | Method and device for rapidly nanocrystallizing alloy surface |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4798718A (en) * | 1982-12-22 | 1989-01-17 | Studiengesellschaft Kohle, Gmbh | Method of preparing active magnesium-hydride of magnesium hydrogen-storer systems |
| CN101116913A (en) * | 2007-09-07 | 2008-02-06 | 哈尔滨工业大学 | Method for preparing nanocrystalline magnesium alloy powder |
| CN101403053A (en) * | 2008-11-13 | 2009-04-08 | 哈尔滨工业大学 | Apparatus and method for producing block body nanocrystalline magnesium alloy based on nanocrystalline hydrogenation state magnesium alloy powder |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006077303A (en) * | 2004-09-10 | 2006-03-23 | Seiji Kamasaki | Method for producing hydrogen storage alloy and hydrogen storage obtained by the production method |
| JP2006176802A (en) * | 2004-12-21 | 2006-07-06 | Institute Of National Colleges Of Technology Japan | Method for manufacturing high-strength magnesium alloy using solid-state reaction by hydrogenation and dehydrogenation |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4798718A (en) * | 1982-12-22 | 1989-01-17 | Studiengesellschaft Kohle, Gmbh | Method of preparing active magnesium-hydride of magnesium hydrogen-storer systems |
| CN101116913A (en) * | 2007-09-07 | 2008-02-06 | 哈尔滨工业大学 | Method for preparing nanocrystalline magnesium alloy powder |
| CN101403053A (en) * | 2008-11-13 | 2009-04-08 | 哈尔滨工业大学 | Apparatus and method for producing block body nanocrystalline magnesium alloy based on nanocrystalline hydrogenation state magnesium alloy powder |
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| CB03 | Change of inventor or designer information |
Inventor after: Fan Jianfeng Inventor after: Zhang Hua Inventor after: Zhou Fan Inventor after: Xie Zhongzhu Inventor after: Wang Xin Inventor after: Dong Hongbiao Inventor after: Xu Bingshe Inventor before: Fan Jianfeng Inventor before: Zhou Fan Inventor before: Xie Zhongzhu Inventor before: Wang Xin Inventor before: Dong Hongbiao Inventor before: Xu Bingshe |
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Free format text: CORRECT: INVENTOR; FROM: FAN JIANFENG ZHOU FAN XIE ZHONGZHU WANG XIN DONG HONGBIAO XU BINGSHE TO: FAN JIANFENG ZHANG HUA ZHOU FAN XIE ZHONGZHU WANG XIN DONG HONGBIAO XU BINGSHE |
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