CN106395787A - A method of preparing a porous silicon carbide material based on rice hulls - Google Patents
A method of preparing a porous silicon carbide material based on rice hulls Download PDFInfo
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Abstract
A method of preparing a porous silicon carbide material based on rice hulls is disclosed and belongs to the technical field of silicon carbide material preparation. The method includes weighing the rice hulls, soaking in a sodium hydroxide solution, adding nickel nitrate, performing ultrasonic vibration, heating, discharging, filtering, mixing filter residues with pectinase, soaking in a hydrochloric acid solution, mixing filter residues with graphite, carbonizing, adding alumina and ammonium fluoride, grinding, maintaining the temperature, mixing with liquid nitrogen, allowing the mixture to stand, mixing with a hydrochloric acid solution, drying filter residues and crushing to obtain the porous silicon carbide material. Beneficial effects of the method are that the method is simple in steps and low in cost, the rice hulls are fully utilized to produce the porous silicon carbide material so that the method is highly targeted, a product is uniform in morphology, high in purity, high in yield and high in luminescence efficiency, and a luminescent peak is 1.98-2.78 eV (635 nm).
Description
Technical field
The present invention relates to a kind of method that porous silicon carbide silicon materials are prepared based on rice husk, belong to carbofrax material preparing technical field.
Background technology
Carbofrax material, because itself microscopic appearance and crystal structure make it possess the excellent properties of more uniquenesses and are more widely applied prospect, is generally considered to be expected to become the important composition unit of third generation wide bandgap semiconductor materials.Silicon carbide nano material has high energy gap, high critical breakdown electric field and thermal conductivity, little dielectric constant and higher electronics saturation mobility, and capability of resistance to radiation is strong, the characteristics such as good mechanical property, become making high frequency, high-power, low energy consumption, the high temperature resistant and electronics of radioprotective device and the ideal material of opto-electronic device.The room temperature photoluminescence that silicon carbide nanometer line shows is so as to become the ideal material manufacturing blue light-emitting diode and laser diode.Recent studies indicate that:Micron order silicon carbide whisker has been applied to strengthen ceramic base, Metal Substrate and polymer matrix composite, these composites all show good mechanical performance, it is envisioned that with intensity hardness is higher and draw ratio is bigger silicon carbide nano material as composite enhancing phase, it will so that its performance is further enhanced.It is low that silicon carbide nano material has a threshold field strength, and electric current density is big, and high-temperature stability waits well excellent characteristics to be expected as electron field emission material, can be made into third generation novel electron light source using this characteristic, and will play a great role in terms of image display technology.But carborundum is as third generation wide bandgap semiconductor, because it belongs to indirect band-gap semiconductor, thus luminous efficiency is relatively low, this significantly limit the application in luminescent device, and the silicon carbide nano material consersion unit high cost of method preparation at present, product pattern heterogeneity, purity is low, and yield is little.
Content of the invention
The technical problem to be solved:For carborundum as third generation wide bandgap semiconductor, because it belongs to indirect band-gap semiconductor, its luminous efficiency is relatively low, and the carbofrax material consersion unit high cost of method preparation at present, product pattern heterogeneity, purity is low, the drawbacks of yield is little, providing one kind takes rice husk to soak in sodium hydroxide solution, add nickel nitrate sonic oscillation, filter after heating discharging, filtering residue is mixed with pectase, soak in hydrochloric acid solution, filter filtering residue and graphite mixing carbonization, add aluminium oxide, ammonium fluoride is milled, mix standing with liquid nitrogen after insulation, mix with hydrochloric acid solution again, filter filter residue and drying and pulverize the method that porous silicon carbide silicon materials are obtained.Preparation process of the present invention is simple, low cost, and product morphology is homogeneous, and luminous efficiency is high, and it is low to efficiently solve purity, yield minor issue.
For solving above-mentioned technical problem, the present invention using technical scheme as described below is:
(1)In take rice husk to be soaked in sodium hydroxide solution that mass fraction is 10%, add rice husk quality 0.2~0.5% nickel nitrate, it is placed in ultrasonator, after vibration 40~50min under 26~28KHz, mixture is put in autoclave, boosts to 1~2MPa, it is heated to 105~110 DEG C, 1~2h is stirred with 200r/min, naturally cools to room temperature, in 30~40s pressure release to normal atmosphere;
(2)After above-mentioned pressure release, carry out discharging and filter, filtering residue is mixed homogeneously with the pectase of its quality 0.8~1.1%, and be soaked in mass fraction be 1% hydrochloric acid solution in, at 28~32 DEG C, enzymolysis 2~3h is stirred with 130r/min, subsequently filter, collect filtering residue, filtering residue is mixed homogeneously with its quality 1.2~1.4% graphite, it is placed in tubular type retort, carbonization 1~2h at 430~470 DEG C;
(3)After above-mentioned carbonization terminates, by carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, put in grinder and be ground, cross 200 mesh sieves, the granule that will sieve is put in vacuum drying oven, design temperature is 230~260 DEG C, pressure is 70~80kPa, be incubated 2~3h, insulation takes out mixture after terminating, and by it with liquid nitrogen in mass ratio 12:1, mix homogeneously, stand 10~15min;
(4)After above-mentioned standing terminates, mixture and mass fraction are that 25% hydrochloric acid solution presses solid-to-liquid ratio 1:2, put in container, 30~40min is stirred with 160r/min, subsequently filter, using distilled water flushing filtering residue until flushing liquor pH is neutrality, then filtering residue is put in 90 DEG C of baking ovens 2~3h is dried, and pulverized, cross 200 mesh sieves, you can obtain porous silicon carbide silicon materials.
The porous silicon carbide material emission peak that the present invention is obtained is 1.98~2.78eV(635nm), energy gap is 2.56~2.86eV, and breakdown electric field is 0.78~1.56MV/cm, and electron mobility is 3200~4600cm2/ V s, thermal conductivity is 4.5~5.8W/cm K.
Compared with additive method, Advantageous Effects are the present invention:
(1)Preparation process of the present invention is simple, and low cost makes full use of rice husk porous silicon carbide silicon materials, with strong points;
(2)Product morphology is homogeneous, and purity is high, and yield is big, and luminous efficiency is high, and glow peak is 1.98~2.78eV(635nm).
Specific embodiment
In take rice husk to be soaked in first sodium hydroxide solution that mass fraction is 10%, add rice husk quality 0.2~0.5% nickel nitrate, it is placed in ultrasonator, after vibration 40~50min under 26~28KHz, mixture is put in autoclave, boosts to 1~2MPa, it is heated to 105~110 DEG C, 1~2h is stirred with 200r/min, naturally cools to room temperature, in 30~40s pressure release to normal atmosphere;Then after above-mentioned pressure release, carry out discharging and filter, filtering residue is mixed homogeneously with the pectase of its quality 0.8~1.1%, and be soaked in mass fraction be 1% hydrochloric acid solution in, at 28~32 DEG C, enzymolysis 2~3h is stirred with 130r/min, subsequently filter, collect filtering residue, filtering residue is mixed homogeneously with its quality 1.2~1.4% graphite, it is placed in tubular type retort, carbonization 1~2h at 430~470 DEG C;Again after above-mentioned carbonization terminates, by carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, put in grinder and be ground, cross 200 mesh sieves, the granule that will sieve is put in vacuum drying oven, design temperature is 230~260 DEG C, pressure is 70~80kPa, be incubated 2~3h, insulation takes out mixture after terminating, and by it with liquid nitrogen in mass ratio 12:1, mix homogeneously, stand 10~15min;Then, after above-mentioned standing terminates, mixture and mass fraction are that 25% hydrochloric acid solution presses solid-to-liquid ratio 1:2, put in container, 30~40min is stirred with 160r/min, subsequently filter, using distilled water flushing filtering residue until flushing liquor pH is neutrality, then filtering residue is put in 90 DEG C of baking ovens 2~3h is dried, and pulverized, cross 200 mesh sieves, you can obtain porous silicon carbide silicon materials.
Example 1
In take rice husk to be soaked in first sodium hydroxide solution that mass fraction is 10%, add rice husk quality 0.2% nickel nitrate, it is placed in ultrasonator, after vibration 40min under 26KHz, mixture is put in autoclave, boosts to 1MPa, it is heated to 105 DEG C, 1h is stirred with 200r/min, naturally cools to room temperature, in 30s pressure release to normal atmosphere;Then after above-mentioned pressure release, carry out discharging and filter, filtering residue is mixed homogeneously with the pectase of its quality 0.8%, and be soaked in mass fraction be 1% hydrochloric acid solution in, at 28 DEG C, enzymolysis 2h is stirred with 130r/min, subsequently filter, collect filtering residue, filtering residue is mixed homogeneously with its quality 1.2% graphite, it is placed in tubular type retort, carbonization 1h at 430 DEG C;Again after above-mentioned carbonization terminates, by carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, put in grinder and be ground, cross 200 mesh sieves, the granule that will sieve is put in vacuum drying oven, design temperature is 230 DEG C, pressure is 70kPa, be incubated 2h, insulation takes out mixture after terminating, and by it with liquid nitrogen in mass ratio 12:1, mix homogeneously, stand 10min;Then, after above-mentioned standing terminates, mixture and mass fraction are that 25% hydrochloric acid solution presses solid-to-liquid ratio 1:2, put in container, 30min is stirred with 160r/min, subsequently filter, using distilled water flushing filtering residue until flushing liquor pH is neutrality, then filtering residue is put in 90 DEG C of baking ovens 3h is dried, and pulverized, cross 200 mesh sieves, you can obtain porous silicon carbide silicon materials.
Preparation process of the present invention is simple, and low cost makes full use of rice husk porous silicon carbide silicon materials, with strong points;Product morphology is homogeneous, and purity is high, and yield is big, and luminous efficiency is high;Prepared porous silicon carbide material emission peak is 1.98eV(635nm), energy gap is 2.56eV, and breakdown electric field is 0.78MV/cm, and electron mobility is 3200cm2/ V s, thermal conductivity is 4.5W/cm K.
Example 2
In take rice husk to be soaked in first sodium hydroxide solution that mass fraction is 10%, add rice husk quality 0.3% nickel nitrate, it is placed in ultrasonator, after vibration 45min under 27KHz, mixture is put in autoclave, boosts to 2MPa, it is heated to 108 DEG C, 2h is stirred with 200r/min, naturally cools to room temperature, in 35s pressure release to normal atmosphere;Then after above-mentioned pressure release, carry out discharging and filter, filtering residue is mixed homogeneously with the pectase of its quality 1.0%, and be soaked in mass fraction be 1% hydrochloric acid solution in, at 30 DEG C, enzymolysis 3h is stirred with 130r/min, subsequently filter, collect filtering residue, filtering residue is mixed homogeneously with its quality 1.3% graphite, it is placed in tubular type retort, carbonization 2h at 440 DEG C;Again after above-mentioned carbonization terminates, by carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, put in grinder and be ground, cross 200 mesh sieves, the granule that will sieve is put in vacuum drying oven, design temperature is 245 DEG C, pressure is 75kPa, be incubated 3h, insulation takes out mixture after terminating, and by it with liquid nitrogen in mass ratio 12:1, mix homogeneously, stand 13min;Then, after above-mentioned standing terminates, mixture and mass fraction are that 25% hydrochloric acid solution presses solid-to-liquid ratio 1:2, put in container, 35min is stirred with 160r/min, subsequently filter, using distilled water flushing filtering residue until flushing liquor pH is neutrality, then filtering residue is put in 90 DEG C of baking ovens 3h is dried, and pulverized, cross 200 mesh sieves, you can obtain porous silicon carbide silicon materials.
Preparation process of the present invention is simple, and low cost makes full use of rice husk porous silicon carbide silicon materials, with strong points;Product morphology is homogeneous, and purity is high, and yield is big, and luminous efficiency is high;Prepared porous silicon carbide material emission peak is 2.38eV(635nm), energy gap is 2.71eV, and breakdown electric field is 1.17MV/cm, and electron mobility is 3900cm2/ V s, thermal conductivity is 5.1W/cm K.
Example 3
In take rice husk to be soaked in first sodium hydroxide solution that mass fraction is 10%, add rice husk quality 0.5% nickel nitrate, it is placed in ultrasonator, after vibration 50min under 28KHz, mixture is put in autoclave, boosts to 2MPa, it is heated to 110 DEG C, 2h is stirred with 200r/min, naturally cools to room temperature, in 40s pressure release to normal atmosphere;Then after above-mentioned pressure release, carry out discharging and filter, filtering residue is mixed homogeneously with the pectase of its quality 1.1%, and be soaked in mass fraction be 1% hydrochloric acid solution in, at 32 DEG C, enzymolysis 3h is stirred with 130r/min, subsequently filter, collect filtering residue, filtering residue is mixed homogeneously with its quality 1.4% graphite, it is placed in tubular type retort, carbonization 2h at 470 DEG C;Again after above-mentioned carbonization terminates, by carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, put in grinder and be ground, cross 200 mesh sieves, the granule that will sieve is put in vacuum drying oven, design temperature is 260 DEG C, pressure is 80kPa, be incubated 3h, insulation takes out mixture after terminating, and by it with liquid nitrogen in mass ratio 12:1, mix homogeneously, stand 15min;Then, after above-mentioned standing terminates, mixture and mass fraction are that 25% hydrochloric acid solution presses solid-to-liquid ratio 1:2, put in container, 40min is stirred with 160r/min, subsequently filter, using distilled water flushing filtering residue until flushing liquor pH is neutrality, then filtering residue is put in 90 DEG C of baking ovens 3h is dried, and pulverized, cross 200 mesh sieves, you can obtain porous silicon carbide silicon materials.
Preparation process of the present invention is simple, and low cost makes full use of rice husk porous silicon carbide silicon materials, with strong points;Product morphology is homogeneous, and purity is high, and yield is big, and luminous efficiency is high;Prepared porous silicon carbide material emission peak is 2.78eV(635nm), energy gap is 2.86eV, and breakdown electric field is 1.56MV/cm, and electron mobility is 4600cm2/ V s, thermal conductivity is 5.8W/cm K.
Claims (1)
1. a kind of the method for porous silicon carbide silicon materials is prepared it is characterised in that concrete preparation process is based on rice husk:
(1)In take rice husk to be soaked in sodium hydroxide solution that mass fraction is 10%, add rice husk quality 0.2~0.5% nickel nitrate, it is placed in ultrasonator, after vibration 40~50min under 26~28KHz, mixture is put in autoclave, boosts to 1~2MPa, it is heated to 105~110 DEG C, 1~2h is stirred with 200r/min, naturally cools to room temperature, in 30~40s pressure release to normal atmosphere;
(2)After above-mentioned pressure release, carry out discharging and filter, filtering residue is mixed homogeneously with the pectase of its quality 0.8~1.1%, and be soaked in mass fraction be 1% hydrochloric acid solution in, at 28~32 DEG C, enzymolysis 2~3h is stirred with 130r/min, subsequently filter, collect filtering residue, filtering residue is mixed homogeneously with its quality 1.2~1.4% graphite, it is placed in tubular type retort, carbonization 1~2h at 430~470 DEG C;
(3)After above-mentioned carbonization terminates, by carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, put in grinder and be ground, cross 200 mesh sieves, the granule that will sieve is put in vacuum drying oven, design temperature is 230~260 DEG C, pressure is 70~80kPa, be incubated 2~3h, insulation takes out mixture after terminating, and by it with liquid nitrogen in mass ratio 12:1, mix homogeneously, stand 10~15min;
(4)After above-mentioned standing terminates, mixture and mass fraction are that 25% hydrochloric acid solution presses solid-to-liquid ratio 1:2, put in container, 30~40min is stirred with 160r/min, subsequently filter, using distilled water flushing filtering residue until flushing liquor pH is neutrality, then filtering residue is put in 90 DEG C of baking ovens 2~3h is dried, and pulverized, cross 200 mesh sieves, you can obtain porous silicon carbide silicon materials.
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Cited By (7)
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CN106986654A (en) * | 2017-03-28 | 2017-07-28 | 常州大学 | A kind of preparation method of slag corrosion resistance type refractory for continuous casting |
CN107723494A (en) * | 2017-09-19 | 2018-02-23 | 常州诺丁精密机械制造有限公司 | A kind of preparation method of high-toughness metal ceramics |
CN109824362A (en) * | 2019-03-28 | 2019-05-31 | 武汉科技大学 | Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing |
CN110544721A (en) * | 2019-08-21 | 2019-12-06 | 大同新成新材料股份有限公司 | Preparation method of semiconductor material |
CN113149000A (en) * | 2021-05-12 | 2021-07-23 | 长春工业大学 | Preparation method of rice husk carbon-based graphitized carbon material |
CN113816716A (en) * | 2021-09-24 | 2021-12-21 | 江苏润沃达环境科技有限公司 | Preparation method of silicon carbide honeycomb structural body splicing slurry |
CN115838290A (en) * | 2023-02-20 | 2023-03-24 | 南通三责精密陶瓷有限公司 | Pressureless liquid phase sintered silicon carbide ceramic and preparation method thereof |
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CN106986654A (en) * | 2017-03-28 | 2017-07-28 | 常州大学 | A kind of preparation method of slag corrosion resistance type refractory for continuous casting |
CN107723494A (en) * | 2017-09-19 | 2018-02-23 | 常州诺丁精密机械制造有限公司 | A kind of preparation method of high-toughness metal ceramics |
CN107723494B (en) * | 2017-09-19 | 2019-11-26 | 江苏英特耐机械制造有限公司 | A kind of preparation method of high-toughness metal ceramics |
CN109824362A (en) * | 2019-03-28 | 2019-05-31 | 武汉科技大学 | Biomass carbon SiClx/carbon composite and preparation method thereof of one step firing |
CN110544721A (en) * | 2019-08-21 | 2019-12-06 | 大同新成新材料股份有限公司 | Preparation method of semiconductor material |
CN113149000A (en) * | 2021-05-12 | 2021-07-23 | 长春工业大学 | Preparation method of rice husk carbon-based graphitized carbon material |
CN113816716A (en) * | 2021-09-24 | 2021-12-21 | 江苏润沃达环境科技有限公司 | Preparation method of silicon carbide honeycomb structural body splicing slurry |
CN115838290A (en) * | 2023-02-20 | 2023-03-24 | 南通三责精密陶瓷有限公司 | Pressureless liquid phase sintered silicon carbide ceramic and preparation method thereof |
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