CN100485065C - Method for synthesizing MgA1B14 superhard material - Google Patents

Method for synthesizing MgA1B14 superhard material Download PDF

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Publication number
CN100485065C
CN100485065C CNB2007100185968A CN200710018596A CN100485065C CN 100485065 C CN100485065 C CN 100485065C CN B2007100185968 A CNB2007100185968 A CN B2007100185968A CN 200710018596 A CN200710018596 A CN 200710018596A CN 100485065 C CN100485065 C CN 100485065C
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powder
sheet
mgalb
piece
minute
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CNB2007100185968A
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CN101109047A (en
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刘国庆
闫果
王庆阳
李成山
卢亚锋
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Northwest Institute for Non Ferrous Metal Research
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Northwest Institute for Non Ferrous Metal Research
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Abstract

The invention relates to a synthetic method for MgAlB14 super-hard material. The preparation process of the method is that: first, a dried magnesium powder, a dried aluminite powder and a dried boron powder are mixedly grinded and pressed and shaped according to 6:1:14 stoichiometric ratio, and are protected by an argon hydrogen mixture air at constant 800 DEG C. to 900 DEG C. for 3 to 6 hours to get Mg6AlB14 block material, and then the Mg6AlB14 block material is sintered for 10 to 50 hours under the vacuum condition at 700 DEG C. to 1000 DEG C. to finally gain the MgAlB14 block material or the powder. The invention features the easy and feasible method, short preparation cycle, 80 per cent to 90 per cent power saving and free from the impure phase of the Mg, Al and B materials due to the long time high temperature heat treatment.

Description

A kind of synthetic MgAlB 14The method of superhard material
Technical field
The invention belongs to the cermet material preparing technical field, be specifically related to a kind of synthetic MgAlB 14The method of superhard material.
Background technology
MgAlB 14Be a kind of boride superhard material that U.S. Ames National Laboratory in 2000 at first finds, its crystalline structure is for containing B 12Icosahedral orthohormbic structure.MgAlB 14Vickers' hardness reach 32-46GPa, be that a kind of hardness is only second to adamantine superhard material, can be widely used in fields such as thermo-electric device, photodetector, neutron buried body.
At present synthetic MgAlB 14Material mainly adopts direct mixed-sintering method, and U.S. Ames National Laboratory (B.A.Cook et al.Scr.Mater.42 (2000) 597) disclosed technological process in the literature is: with magnesium powder (99.99%), aluminium powder (99.99%) and boron powder (99.99%) according to MgAlB 14The stoichiometric ratio mixed grinding, after the compression moulding, pressed compact is sealed in the Ta pipe, then under 1300 ℃ of-1500 ℃ of conditions the reaction more than 1500 hours, obtain MgAlB at last 14Superhard material.Though this sintering process process is simple, thermal treatment has not only consumed a large amount of electric energy for a long time, and introduces the oxygen in the environment easily, causes a large amount of MgAl 2O 4Dephasign produces, and makes MgAlB in the end product 14Phase content only is 60-70%.
Summary of the invention
The objective of the invention is in order to overcome the deficiencies in the prior art, a kind of synthesis temperature, shortening generated time, MgAlB of preparation of reducing is provided 14Dephasign content is very low in the material, but the synthetic MgAlB of while saves energy 14The method of superhard material.
To achieve these goals, the technical solution used in the present invention is: a kind of synthetic MgAlB 14The method of superhard material is characterized in that its preparation process is:
(1) with exsiccant magnesium powder, aluminium powder and boron powder according to Mg: Al: B=6: 1: 14 ratio thorough mixing, compacting in flakes or piece place vacuum annealing furnace with sheet or the piece that is pressed into, and vacuumize under room temperature, treat that vacuum tightness reaches 10 -3Pa, the gas mixture that charges into argon gas and hydrogen, cooled off it with 20-40 ℃/minute speed of cooling in 800-900 ℃ of constant temperature 3-6 hour with 30-50 ℃/minute temperature rise rate at last, prepared Mg 6AlB 14Sheet or piece, wherein the argon gas volume percent is 95%, hydrogen volume per-cent is 5%;
(2) with the Mg for preparing in the step (1) 6AlB 14Bulk or sheet material place vacuum annealing furnace with Nb or Ta sheet parcel, treat that vacuum tightness reaches 10 2-10 -3Behind the Pa,,, with 20-40 ℃/minute speed of cooling it is cooled off at last, prepare MgAlB in 700-1000 ℃ of insulation 10-50 hour with 30-50 ℃/minute temperature rise rate heating 14Material.
In order to prove MgAlB 14The feasibility of novel synthesis, the inventor furthers investigate the one-tenth phase physical and chemical process of Mg-Al-B system, finds to exist Mg in the Mg-Al-B system 6AlB 14And MgAlB 14Two thermodynamically stable phases, and Mg 6AlB 1410 2-10 -3Under the pressure condition of Pa, because the volatilization of Mg can be decomposed generation MgAlB 14Therefore, can adopt following method to obtain MgAlB 14Material: with magnesium powder, aluminium powder and boron powder according to Mg: Al: B=6: 1: 14 ratio thorough mixing, compacting in flakes or piece equaling sintering under the atmospheric pressure, are prepared Mg 6AlB 14Then 10 2-10 -3Under the pressure condition and certain temperature of Pa, make Mg 6AlB 14Decompose, finally obtain MgAlB 14Material.
The present invention compared with prior art has the following advantages: the present invention prepares MgAlB 14Material can reduce synthesis temperature, shorten generated time, therefore the MgAlB of preparation 14Dephasign content is very low in the material, can save the electric energy of 80-90% simultaneously.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1
With exsiccant magnesium (99%), aluminium (99%) and boron (99%) powder according to Mg: Al: B=6: 1: 14 ratio thorough mixing, compacting are in flakes.The sheet that is pressed into is placed vacuum annealing furnace, under room temperature, vacuumize, treat that vacuum tightness reaches 5 * 10 -3Behind the Pa, charge into the gas mixture (the argon gas volume percent is 95%, and hydrogen volume per-cent is 5%) of argon gas and hydrogen,,, with 20 ℃/minute speed of cooling it is cooled off at last, prepare Mg in 800 ℃ of constant temperature 3 hours with 30 ℃/minute temperature rise rate 6AlB 14Sheet.Mg with preparation 6AlB 14Sheet places vacuum annealing furnace with Nb sheet parcel.Treat that vacuum tightness reaches 5 * 10 -3Behind the Pa, with 35 ℃/minute temperature rise rate heating, in 900 ℃ of insulations 15 hours, last 20 ℃/minute speed of cooling was cooled off it, prepares purity and reaches 92% MgAlB 14Material.
Embodiment 2
With exsiccant magnesium (99%), aluminium (99%) and boron (99%) powder according to Mg: Al: B=6: 1: 14 ratio thorough mixing, briquetting.The piece that is pressed into is placed vacuum annealing furnace, under room temperature, vacuumize, treat that vacuum tightness reaches 5 * 10 -3Behind the Pa, charge into the gas mixture (the argon gas volume percent is 95%, and hydrogen volume per-cent is 5%) of argon gas and hydrogen,,, with 25 ℃/minute speed of cooling it is cooled off at last, prepare Mg in 800 ℃ of constant temperature 3 hours with 35 ℃/minute temperature rise rate 6AlB 14Sheet or piece.Mg with preparation 6AlB 14Sheet or piece place vacuum annealing furnace with Ta sheet parcel.Treat that vacuum tightness reaches 2 * 10 -3Behind the Pa,,, with 30 ℃/minute speed of cooling it is cooled off at last, prepare purity and reach 96% MgAlB in 1000 ℃ of insulations 20 hours with 40 ℃/minute temperature rise rate heating 14Material.
Embodiment 3
With exsiccant magnesium (99%), aluminium (99%) and boron (99%) powder according to Mg: Al: B=6: 1: 14 ratio thorough mixing, briquetting.The piece that is pressed into is placed vacuum annealing furnace, and vacuumize under the room temperature, treat that vacuum tightness reaches 5 * 10 -3Behind the Pa, charge into the gas mixture (the argon gas volume percent is 95%, and hydrogen volume per-cent is 5%) of argon gas and hydrogen,,, with 30 ℃/minute speed of cooling it is cooled off at last, prepare Mg in 900 ℃ of constant temperature 3 hours with 40 ℃/minute temperature rise rate 6AlB 14Sheet or piece.Mg with preparation 6AlB 14Sheet or piece place vacuum annealing furnace with Ta sheet parcel.Treat that vacuum tightness reaches 5 * 10 -3Behind the Pa,,, with 40 ℃/minute speed of cooling it is cooled off at last, prepare purity and reach 90% MgAlB in 700 ℃ of insulations 40 hours with 50 ℃/minute temperature rise rate heating 14Material.

Claims (1)

1, a kind of synthetic MgAlB 14The method of superhard material is characterized in that its preparation process is:
(1) with exsiccant magnesium powder, aluminium powder and boron powder according to Mg: Al: B=6: 1: 14 ratio thorough mixing, compacting in flakes or piece place vacuum annealing furnace with sheet or the piece that is pressed into, and vacuumize under room temperature, treat that vacuum tightness reaches 10 -3Pa, the gas mixture that charges into argon gas and hydrogen, cooled off it with 20-40 ℃/minute speed of cooling in 800-900 ℃ of constant temperature 3-6 hour with 30-50 ℃/minute temperature rise rate at last, prepared Mg 6AlB 14Sheet or piece, wherein the argon gas volume percent is 95%, hydrogen volume per-cent is 5%;
(2) with the Mg for preparing in the step (1) 6AlB 14Bulk or sheet material place vacuum annealing furnace with Nb or Ta sheet parcel, treat that vacuum tightness reaches 10 2-10 -3Behind the Pa,,, with 20-40 ℃/minute speed of cooling it is cooled off at last, prepare MgAlB in 700-1000 ℃ of insulation 10-50 hour with 30-50 ℃/minute temperature rise rate heating 14Material.
CNB2007100185968A 2007-09-05 2007-09-05 Method for synthesizing MgA1B14 superhard material Expired - Fee Related CN100485065C (en)

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Publication number Priority date Publication date Assignee Title
CN102942366B (en) * 2012-10-30 2014-07-02 太原科技大学 Preparation method of Al-Mg-B ceramic material
CN104529465B (en) * 2014-12-12 2016-08-31 仲恺农业工程学院 A kind of preparation method of magnalium boron titanium super hard abrasive
CN111471884A (en) * 2020-04-15 2020-07-31 中国人民解放军军事科学院防化研究院 Ternary alloy Mg0.5Al0.5B2Preparation method

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