CN103387214A - Microwave preparation method of high-quality aluminum nitride powder - Google Patents
Microwave preparation method of high-quality aluminum nitride powder Download PDFInfo
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Abstract
The invention discloses a microwave preparation method of high-quality aluminum nitride powder. The microwave preparation method comprises the following steps of: mixing an aluminum source with a carbon source in a C/AL molar ratio of (3-6):1; adding calcium carbonate with an Al/Ca molar ratio of 100:(1-5) for uniformly mixing; carrying out microwave synthesis in a microwave reaction device under a nitrogen-containing atmosphere, wherein the heating rate for the microwave synthesis is 3 DEG C/min-20 DEG C/min, the temperature is 1200 DEG C-1600 DEG C, and the thermal insulation time is 0-10 hours; and cooling the obtained product to obtain the high-quality finished product aluminum nitride powder. Different from a conventional heating way by convection, conduction or radiation, the microwave preparation method is used for generating heat by coupling a special wave band of the microwave with a base structure of the material, and used for heating in an integral material heating way by virtue of medium loss of the material; moreover, the microwave preparation method of the high-quality aluminum nitride powder has the advantages of good synthesis quality, low synthesis temperature, short synthesis time, low synthesis energy consumption and the like.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic aluminium nitride powder, particularly relate to a kind of microwave preparation of high quality aluminium nitride powder.
Background technology
The sintered compact of aluminium nitride is a kind of novel stupalith, it has a series of good characteristics such as high thermal conductivity, low thermal expansivity, low specific inductivity and dielectric loss, nontoxic, insulation, the ideal material that not only is considered to new generation of semiconductor substrate and semiconductor packages, application in electronic industry comes into one's own day by day, and again applicable to the member that uses in high temperature and corrosive atmosphere.Aluminium nitride ceramics has become one of study hotspot of modern field of new.
But high-quality aluminium nitride powder is the key factor that determines these application, and present traditional method is difficult to synthesize the aluminium nitride powder of high purity, fine granularity, narrow particle size distribution, stable performance, has limited greatly the application of aluminium nitride material.
At present, traditional aluminium nitride powder preparation method mainly contains following five kinds:
1, the metallic aluminium powder heats the method for Direct-Nitridation in nitrogen or ammonia.Direct nitridation method technique is simple, temperature of reaction is generally at 800～1200 ℃, be suitable for the requirement of industrial batch production, but because the reaction of aluminium powder Direct-Nitridation is strong exothermal reaction, reaction process is wayward, the amount of heat of emitting easily makes aluminium formation melt piece, hinder the diffusion of nitrogen, cause reaction not exclusively, reaction product often needs pulverization process, unavoidably can bring impurity into, so this traditional method is difficult to synthesize high purity, fine-grained product.
2, the method for precursor reacting by heating in nitrogen or ammonia of the mixture of alumina powder and carbon dust or aluminium salt and organic carbon source.The cardinal principle of the method is to utilize carbon at 1400～1800 ℃ of reduction-oxidation aluminium, and aluminium nitride is produced in the aluminium that is reduced out and nitrogen reaction, and the total reaction equation is as follows:
Al
2O
3+3C+N
2=2AlN+3CO
The method can be by controlling aluminium source and the quality of carbon source and the aluminium nitride powder of mixing uniformity synthesizing fine-granularity and even particle size distribution, but in order fully aluminum oxide to be changed into aluminium nitride, need to add excessive carbon, reaction must be incubated a few hours after completing and even carry out carbonization treatment in tens of hours in the dry air of 600～900 ℃, increased a large amount of production costs.And due to the difference of aluminium source and carbon source polarity and proportion, raw material be difficult to mix or mixing process too loaded down with trivial details.In addition because the reactive behavior in aluminium source is poor, usually need at high temperature (usually above 1500 ℃) long-time (usually greater than 3h) just can complete building-up reactions, so not only increased the cost of product but also promoted growing up of particle,, because temperature of reaction is high, make carbon, Sauerstoffatom enter the aluminium nitride lattice as the solid solution material and cause the decline of nitrogen content.Therefore raw material is difficult to mix, synthesis temperature is high, generated time is long, carbon content is high, power consumption is high, technology stability is poor etc. is the major obstacle that restricts this method production application.
3, the synthetic method of self propagating high temperature.Concrete grammar is metallic aluminium powder is lighted by extraneous thermal source in high pressure nitrogen after, and the high chemical reaction heat between metallic aluminium and nitrogen makes reaction from keeping down, until aluminium powder transforms into aluminium nitride fully.Self propagating high temperature is synthetic the same with the aluminium powder Direct-Nitridation, and because the fusing point of metallic aluminium is low, under the high temperature of combustion synthesis reaction, the metallic aluminium of melting is easily reunited, and hinders nitrogen to the powder internal penetration, makes aluminium powder be difficult to nitrogenize complete.Because speed of response is exceedingly fast, reaction product is very easily lumpd, and is difficult to the loose powder that disposable acquisition is even, disperse, and generally will carry out ball milling and process to obtain the size distribution that needs, and so just inevitably will bring impurity into, reduces powder purity.Therefore, although the self propagating high temperature synthesis method has advantages of that production process is simple, speed of response is fast, energy consumption is low, synthetic product is active large, but exist spontaneous reaction heap to be difficult to the shortcomings such as controls, need further further investigation processing parameter on the impact of reacting with and synthesis mechanism.
4, the method for chemical vapour deposition.The method is based on the method for chemical reaction deposit aluminum nitride from gas phase of the volatile compound of aluminium and ammonia or nitrogen.The method have advantages of generate that product purity is high, fine size and distribution range little, but raw materials cost is high, output is little, reacts the shortcoming such as wayward, is difficult to apply in industrial reality.
5, the synthetic method of plasma chemistry.The method is used direct current-arc plasma producer or high-frequency plasma generator, and aluminium powder is transported in the plasma flame district, and in the flame high-temperature zone of temperature up to more than 10,000 degree, powder dissolves volatilization immediately, with nitrogen ion fast, synthesizes aluminium nitride.The major advantage of the method is that synthetic product fine size, specific surface area are large, has good sintering activity.But the main drawback that exists is that efficiency is low, equipment is complicated, reaction is incomplete, is difficult to production application.
Summary of the invention
Technical problem to be solved by this invention is to propose a kind ofly to reduce C/Al batching mol ratio, improve the raw material mixing uniformity or simplify mixing process, within lower temperature, shorter time, the microwave preparation of the high quality aluminium nitride powder of synthetic high quality aluminium nitride powder under normal pressure.
In order to solve the problems of the technologies described above, the microwave preparation of high quality aluminium nitride powder provided by the invention, mix as 3～6:1 by the C/Al molar ratio take aluminium source and carbon source as raw material, then adding the Al/Ca mol ratio is that the calcium carbonate of 100:1～5 mixes, carry out again microwave synthetic under nitrogen containing atmosphere in the microwave reaction device, the synthetic temperature rise rate of described microwave is 3～20 ℃/min, temperature is 1200～1600 ℃, soaking time is 0～10 hour, is high quality finished product aluminium nitride powder after products therefrom is cooling.
Described aluminium source is aluminum oxide, aluminium hydroxide or aluminum nitrate.
Described carbon source is simple substance, glucose or the sucrose of carbon.
Described nitrogen containing atmosphere is gas mixture or the ammonia that nitrogen, nitrogen add hydrogen, and pressure is normal pressure.
Described microwave reaction device is intermittent type industrial microwave oven or continous way industrial microwave oven.
Heat-treat in oxygen-containing atmosphere after described high quality aluminium nitride powder is cooling.
Described heat treated temperature is 600～800 ℃, and soaking time is 0～10 hour, and described heat treated purpose is that the microwave synthetic product is carried out carbon removal treatment.
Adopt the microwave preparation of the high quality aluminium nitride powder of technique scheme, its principle of work is: utilize micro-wave energy to be converted into kinetic energy and the heat energy of molecule, with a kind of " mode of body heating " whole homogeneous heating,, to certain temperature, pass to nitrogen containing atmosphere, the insulation certain hour, realize synthetic.
The invention has the beneficial effects as follows, microwave is synthetic is to utilize microwave heating to synthesize material, it is different with traditional type of heating, traditional heating is to rely on heating that heat energy is passed to heated material by convection current, conduction or method of radiating to reach a certain temperature, heat transmits from outside to inside, generated time is long, and energy consumption is high; And microwave synthetic be basic structure coupling and the generation heat that utilizes special wave band that microwave has and material, the dielectric loss of material makes a kind of type of heating of its material monolithic heating, thereby it is low to have a synthesis temperature, and generated time is short, improve synthesis condition, a series of advantages such as energy consumption is low.Therefore the efficiency of microwave heating is high,, than traditional method power saving 30～70%, greatly reduce production cost, and industrial microwave oven is simple in structure, automatic operating, be easy to safeguard.
In sum, the present invention a kind ofly can reduce C/Al batching mol ratio, improves the raw material mixing uniformity or simplifies mixing process, within lower temperature, shorter time, the microwave preparation of the high quality aluminium nitride powder of synthetic high quality aluminium nitride powder under normal pressure, have heat-up rate fast, synthesis temperature is low, and soaking time is short, nitrogen content is high, save energy, the characteristics that production efficiency is high, be fit to scale operation.
Description of drawings
Fig. 1 is that to do the XRD analysis phase structure be the AlN schematic diagram for the aluminium nitride powder finished product that makes in embodiment 1.
Fig. 2 is that to do the XRD analysis phase structure be the AlN schematic diagram for the aluminium nitride powder finished product that makes in embodiment 2.
Embodiment
Take aluminium source and carbon source as raw material to carry out microwave under nitrogen containing atmosphere in microwave reaction device (intermittent type industrial microwave oven or continous way industrial microwave oven) synthetic.Be that 3～6:1 mix with carbon source by the C/Al molar ratio with the aluminium source, then adding the Al/Ca mol ratio is that the calcium carbonate of 100:1～5 mixes, again in the nitrogen containing atmosphere underlying enters the microwave reaction unit, pressure is normal pressure, temperature rise rate is 3～20 ℃/min, 1200～1600 ℃ of synthesis temperatures, passing into nitrogen containing atmosphere, to carry out microwave synthetic, be incubated 0～10 hour, the gained synthetics is heated to 600～800 ℃ in oxygen-containing atmosphere, carry out de-carbon thermal treatment, be incubated 0～10 hour, be high quality finished product aluminium nitride powder after products therefrom is cooling.
The aluminium source is the oxide compound of the aluminium such as aluminum oxide, aluminium hydroxide, aluminum nitrate and the salt compounds of aluminium.
Carbon source is the simple substance of carbon or the organic compound of the carbon containings such as glucose, sucrose.
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
Adopting granularity is γ-Al of 4.4 μ m
2O
3Powder and granularity are that the high-purity carbon black of the metallurgical grade of 1 μ m is made raw material, by the C/Al molar ratio, are that 3.57:1 takes the high-purity carbon black of metallurgical grade and γ-Al
2O
3Powder, be then that 100:3 adds calcium carbonate by the Al/Ca mol ratio, and take water as the medium mixing and ball milling 8 hours, drying and screening obtained the raw material that will synthesize.The raw material of preparation is placed in the microwave building-up reactions cavity of intermittent type industrial microwave oven to carry out microwave synthetic, pass into high pure nitrogen, pressure is normal pressure, temperature rise rate is 10 ℃/min, 1420 ℃ of synthesis temperatures, be incubated 2 hours, and the gained synthetics is 650 ℃ of thermal treatments in air, be incubated 10 hours, be the finished product aluminium nitride powder after products therefrom is cooling.Finished color is canescence.After measured, make the aluminium nitride powder finished product nitrogenous 33.5%, contain oxygen 0.6%, carbon containing 0.3%, doing the XRD analysis phase structure is AlN, as shown in Figure 1.
Embodiment 2:
Be that 4.2 ﹕ 1 are dissolved in the aqueous solution of analytically pure aluminum nitrate, calcium carbonate with analytically pure glucose by the C/Al mol ratio, the Al/Ca of aluminum nitrate and calcium carbonate mole proportioning is 100:5.The solution that then will prepare heats while stirring at 200 ℃, obtains finally a kind of fluffy powder as the precursor that reacts.Resulting precursor is placed in the microwave building-up reactions cavity of continous way industrial microwave oven that to carry out microwave synthetic, pass into high pure nitrogen, pressure is normal pressure, temperature rise rate is 8 ℃/min, synthesis temperature is 1350 ℃, is incubated 5 hours, and the gained synthetics is 680 ℃ of thermal treatments in air, be incubated 2 hours, be the finished product aluminium nitride powder after products therefrom is cooling.Finished color is canescence.After measured, make the aluminium nitride powder finished product nitrogenous 33.0%, contain oxygen 0.8%, carbon containing 1.2%, doing the XRD analysis phase structure is AlN, as shown in Figure 2.
Embodiment 3:
Adopting analytically pure aluminum nitrate and granularity is that the high-purity carbon black of metallurgical grade of 0.5 μ m is made raw material, be that 4.44:1 takes respectively the high-purity carbon black of metallurgical grade and aluminum nitrate by the C/Al molar ratio, then be that 100:2 adds calcium carbonate by the Al/Ca mol ratio, take water as the medium mixing and ball milling 5 hours, obtain the precursors that mixes after drying.The presoma of preparation is placed in the microwave building-up reactions cavity of intermittent type industrial microwave oven to carry out microwave synthetic, passes into N
2+ 5%H
2Mixed gas, pressure is normal pressure, temperature rise rate is 15 ℃/min, 1500 ℃ of synthesis temperatures are incubated 0.5 hour, the gained synthetics is 700 ℃ of thermal treatments in air, are incubated 2 hours, are the finished product aluminium nitride powder after products therefrom is cooling.Finished color is canescence.After measured, make the aluminium nitride powder finished product nitrogenous 33.2%, contain oxygen 1.0%, carbon containing 0.2%, granularity is 0.7 μ m.
Embodiment 4:
Be that 5 ﹕ 1 are dissolved in the aqueous solution of analytically pure aluminum nitrate and calcium carbonate with analytically pure glucose by the C/Al mol ratio, the Al/Ca of aluminum nitrate and calcium carbonate mole proportioning is 100:2.The solution that then will prepare heats while stirring at 130 ℃, obtains finally the precursor of a kind of foamed powder as reaction.Resulting precursor is placed in the microwave building-up reactions cavity of continous way industrial microwave oven that to carry out microwave synthetic, pass into high pure nitrogen, pressure is normal pressure, temperature rise rate is 3 ℃/min, synthesis temperature is 1450 ℃, is incubated 10 minutes, and the gained synthetics is 720 ℃ of thermal treatments in air, be incubated 2 hours, be the finished product aluminium nitride powder after products therefrom is cooling.Finished color is canescence.After measured, make the aluminium nitride powder finished product nitrogenous 33.1%, contain oxygen 0.6%, carbon containing 1.0%, granularity is 0.5 μ m.
Embodiment 5:
The employing granularity is that aluminium-hydroxide powder and the industrial acetylene carbon black of 5 μ m made raw material, be that 3.9:1 takes industrial acetylene carbon black and aluminium-hydroxide powder by the C/Al molar ratio, then be that 100:2.5 adds calcium carbonate by the Al/Ca mol ratio, take water as the medium mixing and ball milling 8 hours, drying and screening obtained the raw material that will synthesize.The raw material of preparation is placed in the microwave building-up reactions cavity of intermittent type industrial microwave oven to carry out microwave synthetic, passes into mobile NH
3Gas, pressure are normal pressure, and temperature rise rate is 20 ℃/min, and 1320 ℃ of synthesis temperatures are incubated 1 hour, and the gained synthetics is 680 ℃ of thermal treatments in air, are incubated 5 hours, are the finished product aluminium nitride powder after products therefrom is cooling.Finished color is canescence.After measured, make the aluminium nitride powder finished product nitrogenous 33.6%, contain oxygen 0.5%, carbon containing 0.3%, granularity is 200nm.
Embodiment 6:
Be that 4.5 ﹕ 1 are dissolved in analytically pure boehmite (in the aqueous solution of γ-AlOOH) and calcium carbonate with analytically pure sucrose by the C/Al mol ratio, the Al/Ca of boehmite and calcium carbonate mole proportioning is 100:3, the solution for preparing is heated while stirring at 150 ℃, obtain finally the presoma of a kind of loose powdered as reaction.Resulting presoma is placed in the microwave building-up reactions cavity of continous way industrial microwave oven that to carry out microwave synthetic, pass into high pure nitrogen, pressure is normal pressure, temperature rise rate is 5 ℃/min, synthesis temperature is 1480 ℃, is incubated 1 hour, and the gained synthetics is 700 ℃ of thermal treatments in air, be incubated 5 hours, be the finished product aluminium nitride powder after products therefrom is cooling.Finished color is canescence.After measured, make the aluminium nitride powder finished product nitrogenous 33.2%, contain oxygen 0.7%, carbon containing 1.1%, granularity is 150nm.
Embodiment 7:
Be that 3 ﹕ 1 are dissolved in the aqueous solution of analytically pure aluminum nitrate and calcium carbonate with analytically pure glucose by the C/Al mol ratio, the Al/Ca mol ratio proportioning of aluminum nitrate and calcium carbonate is 100:1.The solution that then will prepare heats while stirring at 130 ℃, obtains finally the precursor of a kind of foamed powder as reaction.Resulting precursor is placed in the microwave building-up reactions cavity of continous way industrial microwave oven that to carry out microwave synthetic, passes into mobile NH
3Gas, pressure are normal pressure, and temperature rise rate is 12 ℃/min, and 1200 ℃ of synthesis temperatures are incubated 10 hours, and the gained synthetics is 600 ℃ of thermal treatments in air, are incubated 5 hours, are the finished product aluminium nitride powder after products therefrom is cooling.Finished color is canescence.After measured, make the aluminium nitride powder finished product nitrogenous 33.6%, contain oxygen 0.5%, carbon containing 0.3%, granularity is 200nm.
Embodiment 8:
Be that 6 ﹕ 1 are dissolved in analytically pure boehmite (in the aqueous solution of γ-AlOOH) and calcium carbonate with analytically pure sucrose by the C/Al mol ratio, boehmite and calcium carbonate be 100:5 by Al/Ca mol ratio proportioning, the solution for preparing is heated while stirring at 150 ℃, obtain finally the presoma of a kind of loose powdered as reaction.Resulting presoma is placed in the microwave building-up reactions cavity of continous way industrial microwave oven that to carry out microwave synthetic, pass into high pure nitrogen, pressure is normal pressure, temperature rise rate is 18 ℃/min, synthesis temperature is 1600 ℃, the gained synthetics is 800 ℃ of thermal treatments in air, are the finished product aluminium nitride powder after products therefrom is cooling.Finished color is canescence.After measured, make the aluminium nitride powder finished product nitrogenous 33.2%, contain oxygen 0.7%, carbon containing 1.1%, granularity is 150nm.
Claims (7)
1. the microwave preparation of a high quality aluminium nitride powder, it is characterized in that: take aluminium source and carbon source as raw material, by the C/Al molar ratio, mix as 3～6:1, then adding the Al/Ca mol ratio is that the calcium carbonate of 100:1～5 mixes, carry out again microwave synthetic under nitrogen containing atmosphere in the microwave reaction device, the synthetic temperature rise rate of described microwave is 3～20 ℃/min, temperature is 1200～1600 ℃, and soaking time is 0～10 hour, is high quality finished product aluminium nitride powder after products therefrom is cooling.
2. the microwave preparation of high quality aluminium nitride powder according to claim 1, it is characterized in that: described aluminium source is aluminum oxide, aluminium hydroxide or aluminum nitrate.
3. the microwave preparation of high quality aluminium nitride powder according to claim 1 and 2, it is characterized in that: described carbon source is simple substance, glucose or the sucrose of carbon.
4. the microwave preparation of high quality aluminium nitride powder according to claim 1 and 2, it is characterized in that: described nitrogen containing atmosphere is gas mixture or the ammonia that nitrogen, nitrogen add hydrogen, and pressure is normal pressure.
5. the microwave preparation of high quality aluminium nitride powder according to claim 1 and 2, it is characterized in that: described microwave reaction device is intermittent type industrial microwave oven or continous way industrial microwave oven.
6. the microwave preparation of high quality aluminium nitride powder according to claim 1 and 2, is characterized in that: heat-treat in oxygen-containing atmosphere after described high quality aluminium nitride powder is cooling.
7. the microwave preparation of high quality aluminium nitride powder according to claim 6, it is characterized in that: described heat treated temperature is 600～800 ℃, soaking time is 0～10 hour.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629637A (en) * | 2016-12-30 | 2017-05-10 | 河北利福光电技术有限公司 | Method for preparing high-stability superfine aluminum nitride via low-temperature carbothermal reduction nitriding process |
| CN107354808A (en) * | 2017-06-28 | 2017-11-17 | 徐昌霞 | Aramid fiber/polyimide fiber composite-insulating paper of excellent performance and preparation method thereof is worn in a kind of resistance |
| CN108793102A (en) * | 2018-06-26 | 2018-11-13 | 宁夏艾森达新材料科技有限公司 | A kind of method that hyperbar prepares aluminium nitride powder |
| CN111302807A (en) * | 2020-04-02 | 2020-06-19 | 上海闻泰信息技术有限公司 | Preparation method of heat dissipation material for chip, heat dissipation chip and application |
| CN112759401A (en) * | 2020-12-02 | 2021-05-07 | 兆山科技（北京）有限公司 | Method for preparing high-entropy boron ceramic surface material by microwave sintering |
| CN113636581A (en) * | 2021-07-07 | 2021-11-12 | 中民驰远实业有限公司 | Method for synthesizing calcium aluminate composite powder by microwave induction heating |
-
2013
- 2013-07-23 CN CN2013103113187A patent/CN103387214A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 曾小锋等: "氮化工艺对微波碳热还原法合成AlN粉末的影响", 《硅酸盐通报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629637A (en) * | 2016-12-30 | 2017-05-10 | 河北利福光电技术有限公司 | Method for preparing high-stability superfine aluminum nitride via low-temperature carbothermal reduction nitriding process |
| CN107354808A (en) * | 2017-06-28 | 2017-11-17 | 徐昌霞 | Aramid fiber/polyimide fiber composite-insulating paper of excellent performance and preparation method thereof is worn in a kind of resistance |
| CN108793102A (en) * | 2018-06-26 | 2018-11-13 | 宁夏艾森达新材料科技有限公司 | A kind of method that hyperbar prepares aluminium nitride powder |
| CN111302807A (en) * | 2020-04-02 | 2020-06-19 | 上海闻泰信息技术有限公司 | Preparation method of heat dissipation material for chip, heat dissipation chip and application |
| CN112759401A (en) * | 2020-12-02 | 2021-05-07 | 兆山科技（北京）有限公司 | Method for preparing high-entropy boron ceramic surface material by microwave sintering |
| CN113636581A (en) * | 2021-07-07 | 2021-11-12 | 中民驰远实业有限公司 | Method for synthesizing calcium aluminate composite powder by microwave induction heating |
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