CN106395787B - A method of porous silicon carbide silicon materials are prepared based on rice husk - Google Patents
A method of porous silicon carbide silicon materials are prepared based on rice husk Download PDFInfo
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Abstract
The invention discloses a kind of methods preparing porous silicon carbide silicon materials based on rice husk, belong to carbofrax material preparing technical field.The present invention takes rice husk to be impregnated in sodium hydroxide solution, nickel nitrate sonic oscillation is added, it is filtered after heating discharging, filter residue is mixed with pectase, is impregnated in hydrochloric acid solution, and filtering filter residue mixes carbonization with graphite, aluminium oxide is added, ammonium fluoride is milled, standing is mixed after heat preservation with liquid nitrogen, then is mixed with hydrochloric acid solution, filtering filter residue and drying, which crushes, is made porous silicon carbide silicon materials.The beneficial effects of the invention are as follows：Preparation process of the present invention is simple, at low cost, makes full use of rice husk porous silicon carbide silicon materials, with strong points；Product morphology is uniform, and purity is high, and yield is big, and luminous efficiency is high, and glow peak is 1.98~2.78eV（635nm）.
Description
Technical field
The present invention relates to a kind of methods preparing porous silicon carbide silicon materials based on rice husk, belong to carbofrax material technology of preparing
Field.
Background technology
Carbofrax material makes it have more unique excellent properties and more due to itself microscopic appearance and crystal structure
Add the foreground of being widely applied, is generally considered to be expected to the important composition unit as third generation wide bandgap semiconductor materials.Carbonization
Silicon nano material has high energy gap, high critical breakdown electric field and thermal conductivity, small dielectric constant and higher electronics
It is saturated mobility and capability of resistance to radiation is strong, the characteristics such as good mechanical property, become and make high frequency, high-power, low energy consumption, resistance to height
The ideal material of the electronics and opto-electronic device of mild radioresistance device.The room temperature photoluminescence that silicon carbide nanometer line is shown
Property, become the ideal material of manufacture blue light-emitting diode and laser diode.Recent studies indicate that：Micron order carbon
SiClx whisker has been applied to enhancing ceramic base, Metal Substrate and polymer matrix composite, these composite materials and has shown good
Good mechanical performance, it is envisaged that use the silicon carbide nano material of intensity hardness higher and draw ratio bigger as composite material
Reinforced phase, it will its performance is made to be further enhanced.Silicon carbide nano material has threshold field strength low, and current density is big, high
Well equal excellent characteristics are expected as electron field emission material temperature stability, can be made into third generation Novel electric sub-light using this characteristic
Source, and will play a great role in terms of image display technology.But silicon carbide is as third generation wide bandgap semiconductor, since it belongs to
In indirect band-gap semiconductor, thus luminous efficiency is relatively low, this significantly limits the application in luminescent device, and current method
The silicon carbide nano material consersion unit of preparation is of high cost, and reaction product pattern is inhomogenous, and purity is low, and yield is small.
Invention content
The technical problems to be solved by the invention：For silicon carbide as third generation wide bandgap semiconductor, since it belongs to
Indirect band-gap semiconductor, luminous efficiency is relatively low, and the carbofrax material consersion unit that at present prepared by method is of high cost, reaction production
Object pattern is inhomogenous, and purity is low, and the small drawback of yield provides one kind and rice husk is taken to be impregnated in sodium hydroxide solution, and nitre is added
Sour nickel sonic oscillation filters after heating discharging, and filter residue is mixed with pectase, is impregnated in hydrochloric acid solution, and filter residue and graphite are filtered
Mixing carbonization, addition aluminium oxide, ammonium fluoride are milled, and are mixed standing after heat preservation with liquid nitrogen, then mix with hydrochloric acid solution, are filtered filter residue
The method that porous silicon carbide silicon materials are made in drying and crushing.Preparation process of the present invention is simple, at low cost, and product morphology is uniform, shines
Efficient, it is low to efficiently solve purity, yield minor issue.
In order to solve the above technical problems, the present invention is using technical solution as described below：
（1）Take rice husk be soaked in mass fraction be 10% sodium hydroxide solution in, add rice husk quality 0.2~
0.5% nickel nitrate, is placed in ultrasonator, and after vibrating 40~50min at 26~28KHz, it is anti-that mixture is put into high pressure
It answers in kettle, boosts to 1~2MPa, be heated to 105~110 DEG C, 1~2h, cooled to room temperature, 30 are stirred with 200r/min
~40s pressure releases are to standard atmospheric pressure；
（2）It after above-mentioned pressure release, is discharged and is filtered, filter residue is mixed with the pectase of its quality 0.8~1.1%
It is even, and it is at 28~32 DEG C, to stir 2~3h of enzymolysis with 130r/min, then in 1% hydrochloric acid solution to be soaked in mass fraction
Filtering collects filter residue, filter residue is uniformly mixed with its 1.2~1.4% graphite of quality, is placed in tubular type retort, 430~
Be carbonized 1~2h at 470 DEG C；
（3）After above-mentioned carbonization, by carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, it is put into grinder
Be ground, cross 200 mesh sieve, will sieving particle be put into vacuum drying oven, set temperature be 230~260 DEG C, pressure be 70~
80kPa keeps the temperature 2~3h, takes out mixture after heat preservation, and by itself and liquid nitrogen in mass ratio 12:1, it is uniformly mixed, stands 10
~15min；
（4）It is that 25% hydrochloric acid solution presses solid-to-liquid ratio 1 by mixture and mass fraction after above-mentioned standing:2, it is put into
In container, 30~40min is stirred with 160r/min, is then filtered, using distilled water flushing filter residue until flushing liquor pH is neutrality,
Filter residue is put into 90 DEG C of baking ovens dry 2~3h again, and is crushed, crosses 200 mesh sieve, you can obtain porous silicon carbide silicon materials.
Porous silicon carbide material emission produced by the present invention peak is 1.98~2.78eV（635nm）, energy gap 2.56
~2.86eV, breakdown electric field are 0.78~1.56MV/cm, and electron mobility is 3200~4600cm2/ Vs, thermal conductivity 4.5
~5.8W/cmK.
Compared with other methods, advantageous effects are the present invention：
（1）Preparation process of the present invention is simple, at low cost, makes full use of rice husk porous silicon carbide silicon materials, with strong points；
（2）Product morphology is uniform, and purity is high, and yield is big, and luminous efficiency is high, and glow peak is 1.98~2.78eV（635nm）.
Specific implementation mode
Take first rice husk be soaked in mass fraction be 10% sodium hydroxide solution in, add rice husk quality 0.2~
0.5% nickel nitrate, is placed in ultrasonator, and after vibrating 40~50min at 26~28KHz, it is anti-that mixture is put into high pressure
It answers in kettle, boosts to 1~2MPa, be heated to 105~110 DEG C, 1~2h, cooled to room temperature, 30 are stirred with 200r/min
~40s pressure releases are to standard atmospheric pressure；Then after above-mentioned pressure release, discharged and filtered, by filter residue and its quality 0.8~
1.1% pectase is uniformly mixed, and it is in 1% hydrochloric acid solution, at 28~32 DEG C, with 130r/min to be soaked in mass fraction
Stirring 2~3h of enzymolysis, then filters, collects filter residue, filter residue is uniformly mixed with its 1.2~1.4% graphite of quality, is placed in pipe
In formula retort, be carbonized 1~2h at 430~470 DEG C；Again after above-mentioned carbonization, by carbide, aluminium oxide and ammonium fluoride
In mass ratio 7:1:2, it is put into grinder and is ground, cross 200 mesh sieve, sieving particle is put into vacuum drying oven, set temperature
It it is 230~260 DEG C, pressure is 70~80kPa, keeps the temperature 2~3h, mixture is taken out after heat preservation, and itself and liquid nitrogen are pressed matter
Measure ratio 12:1, it is uniformly mixed, stands 10~15min；Then it is 25% by mixture and mass fraction after above-mentioned standing
Hydrochloric acid solution presses solid-to-liquid ratio 1:2, it is put into container, 30~40min is stirred with 160r/min, then filters, is rushed using distilled water
Filter wash slag is neutrality up to flushing liquor pH, then filter residue is put into 90 DEG C of baking ovens dry 2~3h, and is crushed, and 200 mesh are crossed
Sieve, you can obtain porous silicon carbide silicon materials.
Example 1
It takes rice husk to be soaked in the sodium hydroxide solution that mass fraction is 10% first, adds 0.2% nitre of rice husk quality
Sour nickel, is placed in ultrasonator, after vibrating 40min at 26KHz, mixture is put into autoclave, is boosted to
1MPa is heated to 105 DEG C, and 1h, cooled to room temperature, in 30s pressure releases to standard atmospheric pressure are stirred with 200r/min；Then exist
It after above-mentioned pressure release, is discharged and is filtered, filter residue is uniformly mixed with the pectase of its quality 0.8%, and be soaked in quality point
Number is at 28 DEG C, to stir enzymolysis 2h in 1% hydrochloric acid solution with 130r/min, then filter, filter residue is collected, by filter residue and its
1.2% graphite of quality is uniformly mixed, and is placed in tubular type retort, be carbonized 1h at 430 DEG C；Again after above-mentioned carbonization,
By carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, it is put into grinder and is ground, cross 200 mesh sieve, by sieving
Grain is put into vacuum drying oven, and set temperature is 230 DEG C, pressure 70kPa, keeps the temperature 2h, takes out mixture after heat preservation, and by its
With liquid nitrogen in mass ratio 12:1, it is uniformly mixed, stands 10min；Then after above-mentioned standing, by mixture and mass fraction
Solid-to-liquid ratio 1 is pressed for 25% hydrochloric acid solution:2, it is put into container, 30min is stirred with 160r/min, then filters, uses distilled water
Filter residue is rinsed until flushing liquor pH is neutrality, then filter residue is put into 90 DEG C of baking ovens dry 3h, and is crushed, crosses 200 mesh sieve,
It can be obtained porous silicon carbide silicon materials.
Preparation process of the present invention is simple, at low cost, makes full use of rice husk porous silicon carbide silicon materials, with strong points；Product shape
Looks are uniform, and purity is high, and yield is big, and luminous efficiency is high；Porous silicon carbide material emission obtained peak is 1.98eV（635nm）, prohibit
Bandwidth is 2.56eV, breakdown electric field 0.78MV/cm, electron mobility 3200cm2/ Vs, thermal conductivity 4.5W/cm
K。
Example 2
It takes rice husk to be soaked in the sodium hydroxide solution that mass fraction is 10% first, adds 0.3% nitre of rice husk quality
Sour nickel, is placed in ultrasonator, after vibrating 45min at 27KHz, mixture is put into autoclave, is boosted to
2MPa is heated to 108 DEG C, and 2h, cooled to room temperature, in 35s pressure releases to standard atmospheric pressure are stirred with 200r/min；Then exist
It after above-mentioned pressure release, is discharged and is filtered, filter residue is uniformly mixed with the pectase of its quality 1.0%, and be soaked in quality point
Number is at 30 DEG C, to stir enzymolysis 3h in 1% hydrochloric acid solution with 130r/min, then filter, filter residue is collected, by filter residue and its
1.3% graphite of quality is uniformly mixed, and is placed in tubular type retort, be carbonized 2h at 440 DEG C；Again after above-mentioned carbonization,
By carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, it is put into grinder and is ground, cross 200 mesh sieve, by sieving
Grain is put into vacuum drying oven, and set temperature is 245 DEG C, pressure 75kPa, keeps the temperature 3h, takes out mixture after heat preservation, and by its
With liquid nitrogen in mass ratio 12:1, it is uniformly mixed, stands 13min；Then after above-mentioned standing, by mixture and mass fraction
Solid-to-liquid ratio 1 is pressed for 25% hydrochloric acid solution:2, it is put into container, 35min is stirred with 160r/min, then filters, uses distilled water
Filter residue is rinsed until flushing liquor pH is neutrality, then filter residue is put into 90 DEG C of baking ovens dry 3h, and is crushed, crosses 200 mesh sieve,
It can be obtained porous silicon carbide silicon materials.
Preparation process of the present invention is simple, at low cost, makes full use of rice husk porous silicon carbide silicon materials, with strong points；Product shape
Looks are uniform, and purity is high, and yield is big, and luminous efficiency is high；Porous silicon carbide material emission obtained peak is 2.38eV（635nm）, prohibit
Bandwidth is 2.71eV, breakdown electric field 1.17MV/cm, electron mobility 3900cm2/ Vs, thermal conductivity 5.1W/cm
K。
Example 3
It takes rice husk to be soaked in the sodium hydroxide solution that mass fraction is 10% first, adds 0.5% nitre of rice husk quality
Sour nickel, is placed in ultrasonator, after vibrating 50min at 28KHz, mixture is put into autoclave, is boosted to
2MPa is heated to 110 DEG C, and 2h, cooled to room temperature, in 40s pressure releases to standard atmospheric pressure are stirred with 200r/min；Then exist
It after above-mentioned pressure release, is discharged and is filtered, filter residue is uniformly mixed with the pectase of its quality 1.1%, and be soaked in quality point
Number is at 32 DEG C, to stir enzymolysis 3h in 1% hydrochloric acid solution with 130r/min, then filter, filter residue is collected, by filter residue and its
1.4% graphite of quality is uniformly mixed, and is placed in tubular type retort, be carbonized 2h at 470 DEG C；Again after above-mentioned carbonization,
By carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, it is put into grinder and is ground, cross 200 mesh sieve, by sieving
Grain is put into vacuum drying oven, and set temperature is 260 DEG C, pressure 80kPa, keeps the temperature 3h, takes out mixture after heat preservation, and by its
With liquid nitrogen in mass ratio 12:1, it is uniformly mixed, stands 15min；Then after above-mentioned standing, by mixture and mass fraction
Solid-to-liquid ratio 1 is pressed for 25% hydrochloric acid solution:2, it is put into container, 40min is stirred with 160r/min, then filters, uses distilled water
Filter residue is rinsed until flushing liquor pH is neutrality, then filter residue is put into 90 DEG C of baking ovens dry 3h, and is crushed, crosses 200 mesh sieve,
It can be obtained porous silicon carbide silicon materials.
Preparation process of the present invention is simple, at low cost, makes full use of rice husk porous silicon carbide silicon materials, with strong points；Product shape
Looks are uniform, and purity is high, and yield is big, and luminous efficiency is high；Porous silicon carbide material emission obtained peak is 2.78eV（635nm）, prohibit
Bandwidth is 2.86eV, breakdown electric field 1.56MV/cm, electron mobility 4600cm2/ Vs, thermal conductivity 5.8W/cm
K。
Claims (1)
1. a kind of method preparing porous silicon carbide silicon materials based on rice husk, it is characterised in that specifically preparation process is：
（1）It takes rice husk to be soaked in the sodium hydroxide solution that mass fraction is 10%, adds 0.2~0.5% nitre of rice husk quality
Sour nickel, is placed in ultrasonator, and after vibrating 40~50min at 26~28KHz, mixture is put into autoclave,
1~2MPa is boosted to, is heated to 105~110 DEG C, 1~2h is stirred with 200r/min, cooled to room temperature is let out in 30~40s
It is depressed into standard atmospheric pressure；
（2）It after above-mentioned pressure release, is discharged and is filtered, filter residue is uniformly mixed with the pectase of its quality 0.8~1.1%,
And it is that at 28~32 DEG C, 2~3h of enzymolysis, subsequent mistake are stirred with 130r/min in 1% hydrochloric acid solution to be soaked in mass fraction
Filter collects filter residue, filter residue is uniformly mixed with its 1.2~1.4% graphite of quality, is placed in tubular type retort, 430~
Be carbonized 1~2h at 470 DEG C；
（3）After above-mentioned carbonization, by carbide, aluminium oxide and ammonium fluoride in mass ratio 7:1:2, it is put into grinder and carries out
200 mesh sieve is crossed in grinding, and sieving particle is put into vacuum drying oven, and set temperature is 230~260 DEG C, and pressure is 70~80kPa, is protected
2~3h of temperature, takes out mixture after heat preservation, and by itself and liquid nitrogen in mass ratio 12:1, it is uniformly mixed, stands 10~15min；
（4）It is that 25% hydrochloric acid solution presses solid-to-liquid ratio 1 by mixture and mass fraction after above-mentioned standing:2, it is put into container
In, 30~40min is stirred with 160r/min, is then filtered, using distilled water flushing filter residue until flushing liquor pH is neutrality, then will
Filter residue is put into 90 DEG C of baking ovens dry 2~3h, and crushes, and crosses 200 mesh sieve, you can obtain porous silicon carbide silicon materials.
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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 |
| 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 |
| CN113816716B (en) * | 2021-09-24 | 2022-11-29 | 江苏润沃达环境科技有限公司 | Preparation method of silicon carbide honeycomb structural body splicing slurry |
| CN115838290B (en) * | 2023-02-20 | 2023-06-20 | 南通三责精密陶瓷有限公司 | Pressureless liquid phase sintering silicon carbide ceramic and preparation method thereof |
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| CN102432011A (en) * | 2011-10-08 | 2012-05-02 | 江苏佳宇资源利用股份有限公司 | Method for synchronously removing iron and silicon impurities in silicon carbide micro-powder |
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