CN109437919B - Method for preparing aluminum nitride ceramic powder based on urea/melamine nitrogen source - Google Patents
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Abstract
A method for preparing aluminum nitride ceramic powder based on a urea/melamine nitrogen source comprises the following steps: (1) preparing raw materials; (2) dissolving aluminum nitrate nonahydrate in water, adding a coupling agent and polyethylene glycol, and uniformly stirring; (3) adding a precipitant, and stirring to form gel; filtering after alcohol washing to obtain gel; (4) putting the gel into absolute ethyl alcohol, adding phenolic resin under the stirring condition, and stirring to form a paste; drying, calcining and grinding to obtain precursor powder; (5) grinding and mixing the nitrogen source and the mixture, placing the mixture in a heating furnace, and heating the mixture to 950-1500 ℃ under the atmospheric pressure in the heating furnace for nitration synthesis; cooling and grinding the mixture along with the furnace to prepare coarse powder; (6) heating to 550-650 ℃ for decarbonization. The method of the invention uses urea/melamine with higher activity to replace nitrogen as a nitrogen source, combines a surface modification dispersion technology, leads an aluminum source and a carbon source to be uniformly mixed at an atomic or molecular level, and reduces the temperature of the carbothermic reduction reaction.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a method for preparing aluminum nitride ceramic powder based on a urea/melamine nitrogen source.
Background
The aluminum nitride is a ceramic material with excellent comprehensive performance, and with the continuous deepening of research, the preparation process of the aluminum nitride is mature day by day, and the application range of the aluminum nitride is expanded; especially, since the 21 st century, with the rapid development of microelectronic technology, electronic complete machines and electronic components are developing towards miniaturization, lightening, integration, high reliability, high power output and the like, and more complex devices put higher demands on the heat dissipation of substrates and packaging materials; the traditional resin substrate and the alumina ceramic substrate have thermal conductivity below 30W/(m.K), and can not meet the development requirements of large-scale integrated circuits and complex devices; the theoretical thermal conductivity of the aluminum nitride ceramic is 320W/(m.K), and the aluminum nitride ceramic has the advantages of good electrical insulation, low dielectric constant and dielectric loss, good matching thermal expansion coefficient with silicon, good chemical stability, environmental protection, no toxicity and the like, and becomes the most ideal substrate material and electronic device packaging material at present.
Method for producing aluminum nitride ceramic powder at presentMainly comprises an aluminum powder direct nitriding method, a carbothermic reduction method and a high-energy ball milling method; in the direct aluminum powder nitriding method, because the aluminum powder nitriding reaction is a strong exothermic reaction, the reaction process is not easy to control, a large amount of heat emitted easily leads aluminum to form a molten mass, the diffusion of nitrogen is blocked, the reaction is incomplete, and reaction products are often crushed, so that high-purity and fine-grained products are difficult to synthesize; in the carbothermic process, a mixed powder of alumina and carbon is subjected to high temperature, flowing N2Carrying out reduction nitridation reaction in gas to generate AlN powder; the nitrogen source adopted by the method is flowing inert gas-nitrogen, and the carbothermic reduction reaction can be carried out only at a high temperature (1500-1800 ℃), so that the particles grow up and the sintering activity is reduced; impurities are easily introduced in the high-energy ball milling method, so that the purity of the powder is low, and the method is not widely popularized and used.
Disclosure of Invention
The invention aims to provide a method for preparing aluminum nitride ceramic powder based on a urea/melamine nitrogen source, which adopts urea or melamine with higher activity to replace flowing inert nitrogen as the nitrogen source, adopts a surface dispersant to uniformly mix an aluminum source and the nitrogen source, and obtains the aluminum nitride ceramic powder by low-temperature carbothermic reduction.
The method of the invention is carried out according to the following steps:
1. preparing aluminum nitrate nonahydrate serving as an aluminum source, ammonium bicarbonate solution or ammonia water serving as a precipitator, a surfactant coupling agent, polyethylene glycol, carbon source phenolic resin and nitrogen source urea or melamine; wherein the coupling agent accounts for 0.01-10% of the total mass of the aluminum nitrate nonahydrate, the polyethylene glycol accounts for 0.01-10% of the total mass of the aluminum nitrate nonahydrate, the molar ratio of the phenolic resin to the aluminum nitrate nonahydrate is 0.5-10, the molar ratio of the nitrogen source to the aluminum nitrate nonahydrate is 5-60, and the dosage of the precipitator is ammonium bicarbonate or NH3·H2The molar ratio of O to aluminum nitrate nonahydrate is 2-8; wherein the concentration of the ammonium bicarbonate solution is 0.1-2M, and the concentration of the ammonia water is 0.1-5M;
2. dissolving aluminum nitrate nonahydrate in deionized water, adding a coupling agent and polyethylene glycol, and uniformly stirring to prepare a mixed solution;
3. adding a precipitant into the mixed solution, and then stirring until a gel is formed; washing the gel with alcohol, filtering, and removing water and a coupling agent in a free state to obtain precursor gel;
4. putting the precursor gel into absolute ethyl alcohol, adding phenolic resin under the stirring condition, dissolving the phenolic resin in the absolute ethyl alcohol, and dispersing the precursor gel until all materials form a paste; placing the paste body in an oven, drying to remove volatile components, placing in a resistance furnace, calcining to remove structural water, cooling to normal temperature along with the furnace, taking out, and grinding to obtain precursor powder;
5. grinding and uniformly mixing the precursor powder and a nitrogen source to prepare composite precursor powder; placing the composite precursor powder in a heating furnace, purging the interior of the heating furnace by using nitrogen, and discharging air; then under the condition that the air pressure in the heating furnace is higher than the atmospheric pressure, heating the heating furnace to 950-1500 ℃, preserving the heat for 1-5 hours, and carrying out a nitridation synthesis reaction; cooling to normal temperature along with the furnace after the reaction is finished, and grinding to prepare aluminum nitride coarse powder;
6. and (3) placing the aluminum nitride coarse powder into a resistance furnace, heating to 550-650 ℃, preserving heat for 2-5 hours to remove carbon, then cooling to normal temperature along with the furnace, and grinding to prepare the aluminum nitride ceramic powder.
In the step 2, the dosage of the deionized water is based on the complete dissolution of the aluminum nitrate nonahydrate, the coupling agent and the polyethylene glycol.
In the step 4, the amount of the absolute ethyl alcohol is based on the complete dissolution of the phenolic resin.
In the step 4, the drying temperature is 60-150 ℃ and the drying time is 1-48 hours.
In the step 4, the calcination temperature is 200-500 ℃ and the calcination time is 1-6 hours.
The particle size of the aluminum nitride ceramic powder is 200-1000 nm.
The polymerization degree of the polyethylene glycol is 2000-20000.
In the step 5, the pressure in the heating furnace is controlled to be higher than the atmospheric pressure in the heating furnace and the heat preservation process.
According to the method, urea/melamine with high activity replaces flowing inert nitrogen to serve as a nitrogen source, and a surface modification dispersion technology is combined, namely, a surfactant coupling agent and polyethylene glycol are used for surface grafting modification and dispersion, so that the compatibility of an aluminum source and a carbon source is improved, the aluminum source and the carbon source are uniformly mixed at an atomic or molecular level and undergo a carbothermic reduction reaction with high-activity ammonia generated by decomposition of urea or melamine in situ, the temperature of the carbothermic reduction reaction is reduced, and the aluminum nitride ceramic powder is finally obtained; the reason for using more urea/melamine and phenolic resin is to allow the aluminum source to react sufficiently without remaining.
Drawings
FIG. 1 is an X-ray diffraction chart of an aluminum nitride ceramic powder in example 1 of the present invention;
FIG. 2 is an SEM photograph of the aluminum nitride ceramic powder in example 1 of the present invention.
Detailed Description
Aluminum nitrate nonahydrate (Al (NO) used in examples of the present invention3)3·9H2O) is a commercially available product.
The urea, the polyethylene glycol and the ammonia water adopted in the embodiment of the invention are commercial products.
The phenolic resin adopted in the embodiment of the invention is FQ-9.
In the embodiment of the invention, the coupling agent is KH-550, KH-560 or KH-570.
The ammonium bicarbonate used in the examples of the present invention is a commercially available product.
The X-ray diffractometer adopted in the embodiment of the invention is PW 3040/60.
The scanning electron microscope adopted in the embodiment of the invention is SSX-550.
In the embodiment of the invention, the paste body is poured into the tray to be spread horizontally so as to increase the heat dissipation area, and then the tray is placed into the oven to be dried.
In the alcohol washing in the embodiment of the invention, the gel is placed in ethanol and stirred for at least 5 min.
When the heating furnace is heated and insulated, the air pressure in the heating furnace is increased due to the ammonia gas generated by the decomposition of urea or melamine, and when the air pressure in the heating furnace is higher than or equal to 0.4MPa, the air pressure in the heating furnace is reduced by opening an air release valve on the heating furnace.
In the embodiment of the invention, when the air release valve is opened, the air release valve leads gas into the closed container containing water through the exhaust pipeline, so that the released ammonia gas is dissolved in the water for recycling.
Example 1
Preparing aluminum nitrate nonahydrate serving as an aluminum source and ammonium bicarbonate solution serving as a precipitator, wherein the concentration of the aluminum nitrate nonahydrate and the ammonium bicarbonate solution is 0.1M; surfactant coupling agent, polyethylene glycol, carbon source phenolic resin and nitrogen source urea; wherein the coupling agent accounts for 0.01 percent of the total mass of the aluminum nitrate nonahydrate, the polyethylene glycol accounts for 0.011 percent of the total mass of the aluminum nitrate nonahydrate, the molar ratio of the phenolic resin to the aluminum nitrate nonahydrate is 1.2, the molar ratio of the urea to the aluminum nitrate nonahydrate is 3, and the dosage of the precipitator is 8 according to the molar ratio of the ammonium bicarbonate to the aluminum nitrate nonahydrate; the polymerization degree of the polyethylene glycol is 6000;
dissolving aluminum nitrate nonahydrate in deionized water, adding a coupling agent and polyethylene glycol, and uniformly stirring to prepare a mixed solution; the dosage of the deionized water is based on the complete dissolution of the aluminum nitrate nonahydrate, the coupling agent and the polyethylene glycol;
adding a precipitant into the mixed solution, and then stirring until a gel is formed; washing the gel with alcohol, filtering, and removing water and a coupling agent in a free state to obtain precursor gel;
putting the precursor gel into absolute ethyl alcohol, adding phenolic resin under the stirring condition, dissolving the phenolic resin in the absolute ethyl alcohol, and dispersing the precursor gel until all materials form a paste; placing the paste body in an oven, drying to remove volatile components, placing in a resistance furnace, calcining to remove structural water, cooling to normal temperature along with the furnace, taking out, and grinding to obtain precursor powder; the dosage of the absolute ethyl alcohol is based on the complete dissolution of the phenolic resin; wherein the drying temperature is 90 ℃ and the drying time is 8 hours; the calcination temperature is 200 ℃ and the calcination time is 6 hours;
grinding and uniformly mixing the precursor powder and urea to prepare composite precursor powder; placing the composite precursor powder in a heating furnace, purging the interior of the heating furnace by using nitrogen, and discharging air; then under the condition that the air pressure in the heating furnace is higher than the atmospheric pressure, the heating furnace is heated to 950 ℃, the temperature is preserved for 3 hours, and the nitridation synthesis reaction is carried out; cooling the mixture to normal temperature along with the furnace after the reaction is finished to obtain aluminum nitride coarse powder; controlling the pressure in the heating furnace to be higher than the atmospheric pressure in the heating and heat preservation processes of the heating furnace;
placing the aluminum nitride coarse powder in a resistance furnace, heating to 550 ℃, preserving heat for 5 hours, decarbonizing, cooling to normal temperature along with the furnace, and preparing the aluminum nitride ceramic powder, wherein the particle size is 250-400 nanometers, the X-ray diffraction is shown in figure 1, the figure shows that the product has no obvious impurities, and the scanning electron microscope SEM photo is shown in figure 2.
Example 2
The method is the same as example 1, except that:
(1) the precipitator is ammonia water with the concentration of 0.1M; the nitrogen source is melamine; the coupling agent accounts for 1 percent of the total mass of the aluminum nitrate nonahydrate, the polyethylene glycol accounts for 1 percent of the total mass of the aluminum nitrate nonahydrate, the molar ratio of the phenolic resin to the aluminum nitrate nonahydrate is 3, the molar ratio of the melamine to the aluminum nitrate nonahydrate is 6, and the dosage of the precipitator is NH3·H2The molar ratio of O to aluminum nitrate nonahydrate is 8; the polymerization degree of the polyethylene glycol is 8000;
(2) the drying temperature is 80 ℃, and the drying time is 10 hours; the calcination temperature is 400 ℃, and the calcination time is 2 hours;
(3) the temperature of the nitration synthesis reaction is 1000 ℃, and the time is 2 hours;
(4) keeping the temperature of the aluminum nitride coarse powder at 620 ℃ for 4 hours to remove carbon; the particle size of the aluminum nitride ceramic powder is 280-430 nanometers.
Example 3
The method is the same as example 1, except that:
(1) the concentration of the precipitant ammonium bicarbonate solution is 2M; the coupling agent accounts for 5 percent of the total mass of the aluminum nitrate nonahydrate, the polyethylene glycol accounts for 5 percent of the total mass of the aluminum nitrate nonahydrate, the molar ratio of the phenolic resin to the aluminum nitrate nonahydrate is 6, the molar ratio of the urea to the aluminum nitrate nonahydrate is 12, and the dosage of the precipitator is 2 according to the molar ratio of the ammonium bicarbonate to the aluminum nitrate nonahydrate; the polymerization degree of the polyethylene glycol is 20000;
(2) the drying temperature is 60 ℃, and the time is 48 hours; the calcining temperature is 300 ℃, and the time is 4 hours;
(3) the reaction temperature of the nitridation synthesis is 1050 ℃, and the time is 2 hours;
(4) keeping the temperature of the aluminum nitride coarse powder at 600 ℃ for 3 hours to remove carbon; the particle size of the aluminum nitride ceramic powder is 300-500 nm.
Example 4
The method is the same as example 1, except that:
(1) the precipitator is ammonia water with the concentration of 5M; the nitrogen source is melamine; the coupling agent accounts for 10 percent of the total mass of the aluminum nitrate nonahydrate, the polyethylene glycol accounts for 10 percent of the total mass of the aluminum nitrate nonahydrate, the molar ratio of the phenolic resin to the aluminum nitrate nonahydrate is 10, the molar ratio of the melamine to the aluminum nitrate nonahydrate is 20, and the dosage of the precipitator is NH3·H2The molar ratio of O to aluminum nitrate nonahydrate is 2; the polymerization degree of the polyethylene glycol is 2000;
(2) drying at 100 deg.c for 1 hr; the calcining temperature is 500 ℃ and the time is 1 hour;
(3) the temperature of the nitridation synthesis reaction is 1100 ℃, and the time is 2 hours;
(4) keeping the temperature of the aluminum nitride coarse powder at 650 ℃ for 2 hours to remove carbon; the particle size of the aluminum nitride ceramic powder is 500-800 nanometers.
Claims (2)
1. A method for preparing aluminum nitride ceramic powder based on a urea/melamine nitrogen source is characterized by comprising the following steps:
(1) preparing aluminum nitrate nonahydrate serving as an aluminum source, ammonium bicarbonate solution or ammonia water serving as a precipitator, a surfactant coupling agent, polyethylene glycol, carbon source phenolic resin and nitrogen source urea or melamine; wherein the coupling agent accounts for 0.01-10% of the total mass of the aluminum nitrate nonahydrate, the polyethylene glycol accounts for 0.01-10% of the total mass of the aluminum nitrate nonahydrate, the molar ratio of the phenolic resin to the aluminum nitrate nonahydrate is 0.5-10, the molar ratio of the nitrogen source to the aluminum nitrate nonahydrate is 5-60, and the dosage of the precipitator is ammonium bicarbonate or NH3•H2The molar ratio of O to aluminum nitrate nonahydrate is 2-8; wherein the concentration of the ammonium bicarbonate solution is 0.1-2M, and the concentration of the ammonia water is 0.1-5M; the polymerization degree of the polyethylene glycol is 2000-20000;
(2) dissolving aluminum nitrate nonahydrate in deionized water, adding a coupling agent and polyethylene glycol, and uniformly stirring to prepare a mixed solution; the dosage of the deionized water is based on the complete dissolution of the aluminum nitrate nonahydrate, the coupling agent and the polyethylene glycol;
(3) adding a precipitant into the mixed solution, and then stirring until a gel is formed; washing the gel with alcohol, filtering, and removing water and a coupling agent in a free state to obtain precursor gel;
(4) putting the precursor gel into absolute ethyl alcohol, adding phenolic resin under the stirring condition, dissolving the phenolic resin in the absolute ethyl alcohol, and dispersing the precursor gel until all materials form a paste; the dosage of the absolute ethyl alcohol is based on the complete dissolution of the phenolic resin; placing the paste body in an oven, drying to remove volatile components, placing in a resistance furnace, calcining to remove structural water, cooling to normal temperature along with the furnace, taking out, and grinding to obtain precursor powder; wherein the calcining temperature is 200-500 ℃ and the time is 1-6 hours;
(5) grinding and uniformly mixing the precursor powder and a nitrogen source to prepare composite precursor powder; placing the composite precursor powder in a heating furnace, purging the interior of the heating furnace by using nitrogen, and discharging air; then under the condition that the air pressure in the heating furnace is higher than the atmospheric pressure, heating the heating furnace to 950-1500 ℃, preserving the heat for 1-5 hours, and carrying out a nitridation synthesis reaction; cooling to normal temperature along with the furnace after the reaction is finished, and grinding to prepare aluminum nitride coarse powder;
(6) placing the aluminum nitride coarse powder in a resistance furnace, heating to 550-650 ℃, preserving heat for 2-5 hours, decarbonizing, cooling to normal temperature along with the furnace, and grinding to prepare aluminum nitride ceramic powder, wherein the particle size of the aluminum nitride ceramic powder is 200-1000 nanometers.
2. The method for preparing aluminum nitride ceramic powder based on urea/melamine nitrogen source as claimed in claim 1, wherein in step (4), the drying temperature is 60-150 ℃ and the drying time is 1-48 hours.
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| CN112110732A (en) * | 2020-09-23 | 2020-12-22 | 航天特种材料及工艺技术研究所 | Method for preparing aluminum nitride powder by using soluble carbon source |
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