CN109607540A - The technique for preparing nanometer silicon carbide using sol-gal process - Google Patents
The technique for preparing nanometer silicon carbide using sol-gal process Download PDFInfo
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- CN109607540A CN109607540A CN201910094856.2A CN201910094856A CN109607540A CN 109607540 A CN109607540 A CN 109607540A CN 201910094856 A CN201910094856 A CN 201910094856A CN 109607540 A CN109607540 A CN 109607540A
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- silicon carbide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
- C01B32/97—Preparation from SiO or SiO2
Abstract
The present invention provides a kind of technique that nanometer silicon carbide is prepared using sol-gal process, is related to the preparation technical field of silicon carbide.The following steps are included: S1: preparing silica by sol-gal process；The silica of S2: step S1 preparation and homogeneous agent, carbon source help and burn reducing agent progress homogeneous and mix；S3: high temperature reduction；S4: dispersion classification.The present invention prepares silica by sol-gal process, and the silica being prepared is scattered；Monodispersed silica carries out the silicon carbide good dispersion that high temperature reduction is prepared after homogeneous mixes with homogeneous agent, carbon source with burning reducing agent is helped, and solves the problems such as reunion in nanometer silicon carbide preparation process.Energy is reacted by helping to burn reducing agent and activated, reduces reaction energy barrier, to reduce reducing silica temperature, having to utilize prevents high-temperature carborundum particle growth.Since carbon source object is uniformly mixed with monodispersed silica, reduce reaction interval, to help to improve reduction reaction speed.
Description
Technical field
The present invention relates to the preparation technical fields of silicon carbide, and in particular to a kind of to prepare nano silicon carbide using sol-gal process
The technique of silicon.
Background technique
Silicon carbide has many excellent physical and chemical properties, as hardness is big, intensity is high, stable chemical performance, anti-height
Warm oxidisability is good etc..And also have preferable chemical compatibility with many metals and metal oxide, can be used to prepare Metal Substrate,
Ceramic base and polymer matrix composite are wherein playing the role of enhancing, toughening and hardening, can also be directly as grinding-material
Or it is prepared into the grinding tool of certain shapes, for the grinding of the surfaces such as metal, ceramics, glass, stone material and polishing.
In recent years, increasing to the demand of single-crystal silica piece with the development of electronics and computer industry, and it is high
The processing of quality single crystalline silicon wafer must just use the superfines of the high quality such as silicon carbide, and nanoscale silicon carbide obtains increasingly
More concerns.Nanometer silicon carbide makes it have more unique excellent properties and more due to itself microscopic appearance and crystal structure
Add broad application prospect, is generally considered to be expected to the important composition unit as third generation wide bandgap semiconductor materials.
The prior art mainly uses sand mill or airflow milling for the preparation of nanometer silicon carbide to carry out physico be crushed and add
Work there is technical issues that carbon source and silicon source are difficult to be uniformly mixed, be difficult to during preparing silicon carbide nano material.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of works that nanometer silicon carbide is prepared using sol-gal process
Skill solves during preparing silicon carbide nano material, and the technology for being difficult to be uniformly mixed, be difficult to disperse there are carbon source and silicon source is asked
Topic.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of technique preparing nanometer silicon carbide using sol-gal process, comprising the following steps:
S1: silica is prepared by sol-gal process；
The silica of S2: step S1 preparation and homogeneous agent, carbon source help and burn reducing agent progress homogeneous and mix；
S3: high temperature reduction；
S4: dispersion classification.
Preferably, specific step is as follows by the step S1:
S1-1:1 parts of ammonium hydroxide, 2 parts of ethyl alcohol, 10 parts of distilled water are mixed to get solution A；
S1-2:1 parts of tetraethoxysilances, 10 parts of ethyl alcohol, 5 parts of distilled water are mixed to get solution B；
S1-3:B solution, which is added in solution A, to react 12 hours；
S1-4: washing obtains silica.
Preferably, specific step is as follows by the step S2:
S2-1: the silica that the S1 is obtained is scattered in liquid phase medium, and dispersing agent is added, and ultrasonic agitation is dispersed
Liquid；
S2-2: the dispersion liquid that the step S2-1 is obtained is added homogeneous agent, carbon source and helps burning reducing agent；
S2-3: the S2-2 mixture rotary drying.
Preferably, the specific condition of the step S3 are as follows: carried out in protective atmosphere, be passed through hydrogen, sintering temperature is
800~1600 DEG C, the sintered heat insulating time is 4~10h.
Preferably, specific step is as follows by the step S4 are as follows: is handled by airflow milling shaping classification, in nitrogen protection gas
It is carried out in atmosphere.
Preferably, dispersing agent described in the step S2-1 is one of aqueous dispersion, oiliness dispersing agent or a variety of.
Preferably, in the step S2-2, the homogeneous agent is one of NaCl, KCl, ZnCl, LiCl or a variety of.
Preferably, described to help burning reducing agent are as follows: one of magnesium, carbon, potassium are a variety of in the step S2-2；Carbon source object
Matter are as follows: resin, glucose, carbohydrate, fatty acid, one of petroleum, peanut, muffin or a variety of.
Preferably, in the step S2-3, the condition of the rotary drying are as follows: drying temperature is 40~100 DEG C, and the time is
2~10h.
Preferably, in the step S3, protective atmosphere is nitrogen or argon gas, and pressure is micro-positive pressure, and hydrogen intake is 10
~200mL/min
(3) beneficial effect
The present invention provides a kind of techniques for preparing nanometer silicon carbide using sol-gal process.Compared with prior art, have
It is standby following the utility model has the advantages that
The present invention prepares silica by sol-gal process, and the silica being prepared is scattered；Monodispersed two
Silica carries out the silicon carbide dispersibility that high temperature reduction after homogeneous mixes is prepared with homogeneous agent, carbon source with burning reducing agent is helped
It is good, solve the problems such as reunion in nanometer silicon carbide preparation process.Energy is reacted by helping to burn reducing agent and activated, reduces reaction
Energy barrier, to reduce reducing silica temperature, having to utilize prevents high-temperature carborundum particle growth.Due to carbon source object and monodisperse
Silica be uniformly mixed, reduce reaction interval, to help to improve reduction reaction speed.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is silica dioxide granule schematic diagram prepared by sol-gal process.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, to the technology in the embodiment of the present invention
Scheme is clearly and completely described, it is clear that and described embodiments are some of the embodiments of the present invention, rather than whole
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
The every other embodiment obtained, shall fall within the protection scope of the present invention.
The embodiment of the present application solves solution by providing a kind of technique for preparing nanometer silicon carbide using sol-gal process
During preparing silicon carbide nano material, there is technical issues that carbon source and silicon source are difficult to be uniformly mixed, be difficult to.It realizes
Improve the degree of mixing of carbon source and silicon source.
Technical solution in the embodiment of the present application is to solve the problems, such as above-mentioned crosstalk, and general thought is as follows:
Using the preparation of sol-gal process silica, homogeneous mixing, high temperature reduction and dispersion classification, preparation are being carried out
Obtained silicon carbide powder particle diameter distribution is narrow, purity is high.
In order to better understand the above technical scheme, in conjunction with appended figures and specific embodiments to upper
Technical solution is stated to be described in detail.
The embodiment of the present invention provides a kind of technique for preparing nanometer silicon carbide using sol-gal process, comprising the following steps:
S1: silica is prepared by sol-gal process；
S2: the silica of the step S1 preparation is mixed with homogeneous agent, carbon source with burning reducing agent progress homogeneous is helped；
S3: high temperature reduction；
S4: dispersion classification.
The present invention prepares silica by sol-gal process, and the silica being prepared is scattered；Monodispersed two
Silica carries out the silicon carbide dispersibility that high temperature reduction after homogeneous mixes is prepared with homogeneous agent, carbon source with burning reducing agent is helped
It is good, solve the problems such as reunion in nanometer silicon carbide preparation process.Energy is reacted by helping to burn reducing agent and activated, reduces reaction
Energy barrier, to reduce reducing silica temperature, having to utilize prevents high-temperature carborundum particle growth.Due to carbon source object and monodisperse
Silica be uniformly mixed, reduce reaction interval, to help to improve reduction reaction speed.
In specific implementation process, specific step is as follows by the step S1:
S1-1: following solvent stirs 1 part of ammonium hydroxide, 2 parts of ethyl alcohol in a container, and solution A is prepared in 10 parts of distillations；
S1-2: following solvent stirs in a container: 1 part of tetraethoxysilance, 10 parts of ethyl alcohol, and 5 parts of distilled water are prepared
B solution；
S1-3:B solution, which is added in solution A, to react 12 hours；
S1-4: washing obtains silica.
The raw material components of specific above-mentioned S1-1 and S1-2 are volume ratio.
It is as shown in Figure 1 silica dioxide granule schematic diagram prepared by sol-gal process, from figure it is found that silica is grain
Diameter is the individual particle of 200-500 nanometers of high dispersives, good dispersion.
In specific implementation process, specific step is as follows by the step S2:
S2-1: the silica that the S1 is obtained is scattered in liquid phase medium, and dispersing agent is added, and ultrasonic agitation is dispersed
Liquid；
S2-2: the dispersion liquid that the step S2-1 is obtained is added homogeneous agent, carbon source and helps burning reducing agent；
S2-3: the S2-2 mixture rotary drying.
In specific implementation process, the specific condition of the step S3 are as follows: carried out in protective atmosphere, be passed through hydrogen, burnt
Junction temperature is 800~1600 DEG C, and the sintered heat insulating time is 4~10h.
In specific implementation process, specific step is as follows by the step S4 are as follows: is handled by airflow milling shaping classification, in nitrogen
It is carried out in gas shielded atmosphere.
In specific implementation process, dispersing agent described in the step S2-1 is aqueous dispersion, one in oiliness dispersing agent
Kind is a variety of.It is specifically as follows macromolecule LBD-1 dispersing agent, dispersing agent NNO, Dispersant MF, sodium lignin sulfonate, acetone, wine
One of essence, PAN etc. or a variety of.
In specific implementation process, in the step S2-2, the homogeneous agent is one of NaCl, KCl, ZnCl, LiCl
Or it is a variety of.
It is described to help burning reducing agent in the step S2-2 are as follows: one of magnesium, carbon, potassium are more in specific implementation process
Kind；Carbon source material are as follows: resin, glucose, carbohydrate, fatty acid, one of petroleum, peanut, muffin or a variety of.
In specific implementation process, in the step S2-3, the condition of the rotary drying are as follows: drying temperature is 40~100
DEG C, the time is 2~10h.
In specific implementation process, in the step S3, protective atmosphere is nitrogen or argon gas, and pressure is micro-positive pressure, and hydrogen is logical
Entering amount is 10~200mL/min.
Below by specific embodiment, it is described in detail:
Embodiment 1:
A kind of technique preparing nanometer silicon carbide using sol-gal process, comprising the following steps:
S1: silica is prepared by sol-gal process；
S1-1:1 parts of ammonium hydroxide, 2 parts of ethyl alcohol, 10 parts of distilled water are mixed to get solution A；
S1-2:1 parts of tetraethoxysilances, 10 parts of ethyl alcohol, 5 parts of distilled water are mixed to get solution B；
S1-3:B solution, which is added in solution A, to react 12 hours；
S1-4: washing obtains silica.
The silica of S2: step S1 preparation and homogeneous agent, carbon source help and burn reducing agent progress homogeneous and mix；
S2-1: the silica that the S1 is obtained is scattered in liquid phase medium, and dispersing agent is added, and ultrasonic agitation is dispersed
Liquid；Dispersing agent is one of aqueous dispersion, oiliness dispersing agent or a variety of.The homogeneous agent is NaCl, KCl, ZnCl, LiCl
One of or it is a variety of.
S2-2: the dispersion liquid that the step S2-1 is obtained is added homogeneous agent, carbon source and helps burning reducing agent；It is described to help burning also
Former agent are as follows: one of magnesium, carbon, potassium are a variety of；Carbon source material are as follows: resin, glucose, carbohydrate, fatty acid, petroleum, peanut, powder
One of cake is a variety of.
S2-3: the S2-2 mixture rotary drying.The condition of the rotary drying are as follows: drying temperature is 40 DEG C, the time
For 2h.
S3: high temperature reduction；
It is carried out in protective atmosphere, is passed through hydrogen, sintering temperature is 800 DEG C, and the sintered heat insulating time is 4h.Protective atmosphere is
Nitrogen or argon gas, pressure are micro-positive pressure, and hydrogen intake is 10mL/min.
S4: it is handled by airflow milling shaping classification, is carried out in nitrogen protection atmosphere.
Embodiment 2:
A kind of technique preparing nanometer silicon carbide using sol-gal process, comprising the following steps:
S1: silica is prepared by sol-gal process；
S1-1:1 parts of ammonium hydroxide, 2 parts of ethyl alcohol, 10 parts of distilled water are mixed to get solution A；
S1-2:1 parts of tetraethoxysilances, 10 parts of ethyl alcohol, 5 parts of distilled water are mixed to get solution B；
S1-3:B solution, which is added in solution A, to react 12 hours；
S1-4: washing obtains silica.
The silica of S2: step S1 preparation and homogeneous agent, carbon source help and burn reducing agent progress homogeneous and mix；
S2-1: the silica that the S1 is obtained is scattered in liquid phase medium, and dispersing agent is added, and ultrasonic agitation is dispersed
Liquid；Dispersing agent is one of aqueous dispersion, oiliness dispersing agent or a variety of.The homogeneous agent is NaCl, KCl, ZnCl, LiCl
One of or it is a variety of.
S2-2: the dispersion liquid that the step S2-1 is obtained is added homogeneous agent, carbon source and helps burning reducing agent；It is described to help burning also
Former agent are as follows: one of magnesium, carbon, potassium are a variety of；Carbon source material are as follows: resin, glucose, carbohydrate, fatty acid, petroleum, peanut, powder
One of cake is a variety of.
S2-3: the S2-2 mixture rotary drying.The condition of the rotary drying are as follows: drying temperature is 100 DEG C, the time
For 10h.
S3: high temperature reduction；
It is carried out in protective atmosphere, is passed through hydrogen, sintering temperature is 1600 DEG C, and the sintered heat insulating time is 10h.Protective atmosphere
For nitrogen or argon gas, pressure is micro-positive pressure, and hydrogen intake is 200mL/min.
S4: it is handled by airflow milling shaping classification, is carried out in nitrogen protection atmosphere.
Embodiment 3:
A kind of technique preparing nanometer silicon carbide using sol-gal process, comprising the following steps:
S1: silica is prepared by sol-gal process；
S1-1:1 parts of ammonium hydroxide, 2 parts of ethyl alcohol, 10 parts of distilled water are mixed to get solution A；
S1-2:1 parts of tetraethoxysilances, 10 parts of ethyl alcohol, 5 parts of distilled water are mixed to get solution B；
S1-3:B solution, which is added in solution A, to react 12 hours；
S1-4: washing obtains silica.
The silica of S2: step S1 preparation and homogeneous agent, carbon source help and burn reducing agent progress homogeneous and mix；
S2-1: the silica that the S1 is obtained is scattered in liquid phase medium, and dispersing agent is added, and ultrasonic agitation is dispersed
Liquid；Dispersing agent is one of aqueous dispersion, oiliness dispersing agent or a variety of.The homogeneous agent is NaCl, KCl, ZnCl, LiCl
One of or it is a variety of.
S2-2: the dispersion liquid that the step S2-1 is obtained is added homogeneous agent, carbon source and helps burning reducing agent；It is described to help burning also
Former agent are as follows: one of magnesium, carbon, potassium are a variety of；Carbon source material are as follows: resin, glucose, carbohydrate, fatty acid, petroleum, peanut, powder
One of cake is a variety of.
S2-3: the S2-2 mixture rotary drying.The condition of the rotary drying are as follows: drying temperature is 70 DEG C, the time
For 6h.
S3: high temperature reduction；
It is carried out in protective atmosphere, is passed through hydrogen, sintering temperature is 1200 DEG C, and the sintered heat insulating time is 7h.Protective atmosphere
For nitrogen or argon gas, pressure is micro-positive pressure, and hydrogen intake is 110mL/min.
S4: it is handled by airflow milling shaping classification, is carried out in nitrogen protection atmosphere.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of technique for preparing nanometer silicon carbide using sol-gal process, which comprises the following steps:
S1: silica is prepared by sol-gal process；
The silica of S2: step S1 preparation and homogeneous agent, carbon source help and burn reducing agent progress homogeneous and mix；
S3: high temperature reduction；
S4: dispersion classification.
2. the technique for preparing nanometer silicon carbide using sol-gal process as described in claim 1, which is characterized in that the step
Specific step is as follows by S1:
S1-1:1 parts of ammonium hydroxide, 2 parts of ethyl alcohol, 10 parts of distilled water are mixed to get solution A；
S1-2:1 parts of tetraethoxysilances, 10 parts of ethyl alcohol, 5 parts of distilled water are mixed to get solution B；
S1-3:B solution, which is added in solution A, to react 12 hours；
S1-4: washing obtains silica.
3. the technique for preparing nanometer silicon carbide using sol-gal process as described in claim 1, which is characterized in that the step
Specific step is as follows by S2:
S2-1: the silica that the S1 is obtained is scattered in liquid phase medium, and dispersing agent is added, and ultrasonic agitation obtains dispersion liquid；
S2-2: the dispersion liquid that the step S2-1 is obtained is added homogeneous agent, carbon source and helps burning reducing agent；
S2-3: the S2-2 mixture rotary drying.
4. the technique for preparing nanometer silicon carbide using sol-gal process as described in claim 1, which is characterized in that the step
The specific condition of S3 are as follows: carried out in protective atmosphere, be passed through hydrogen, sintering temperature is 800~1600 DEG C, the sintered heat insulating time
For 4~10h.
5. the technique for preparing nanometer silicon carbide using sol-gal process as described in claim 1, which is characterized in that the step
Specific step is as follows by S4 are as follows: is handled by airflow milling shaping classification, is carried out in nitrogen protection atmosphere.
6. the technique for preparing nanometer silicon carbide using sol-gal process as claimed in claim 3, which is characterized in that the step
Dispersing agent described in S2-1 is one of aqueous dispersion, oiliness dispersing agent or a variety of.
7. the technique for preparing nanometer silicon carbide using sol-gal process as claimed in claim 4, which is characterized in that the step
In S2-2, the homogeneous agent is one of NaCl, KCl, ZnCl, LiCl or a variety of.
8. the technique for preparing nanometer silicon carbide using sol-gal process as claimed in claim 3, which is characterized in that the step
It is described to help burning reducing agent in S2-2 are as follows: one of magnesium, carbon, potassium are a variety of；The carbon source material are as follows: resin, glucose, sugar
One of class, fatty acid, petroleum, peanut, muffin are a variety of.
9. the technique for preparing nanometer silicon carbide using sol-gal process as claimed in claim 3, which is characterized in that the step
In S2-3, the condition of the rotary drying are as follows: drying temperature is 40~100 DEG C, and the time is 2~10h.
10. the technique for preparing nanometer silicon carbide using sol-gal process as claimed in claim 4, which is characterized in that the step
In rapid S3, protective atmosphere is nitrogen or argon gas, and pressure is micro-positive pressure, and hydrogen intake is 10~200mL/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115072723A (en) * | 2022-07-18 | 2022-09-20 | 陕西煤业化工技术研究院有限责任公司 | Method for preparing nano silicon carbide by sol-gel method |
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Effective date of registration: 20200925 Address after: 321100 Lanxi Economic Development Zone, Jinhua City, Zhejiang Province (No.17, Chengjiao West Road, Lanjiang Street) Applicant after: LANXI ZHIDE NEW ENERGY MATERIALS Co.,Ltd. Address before: 311300 301-308-14 1, 958 Garden Road, Qingshan Lake, Ling'an, Hangzhou, Zhejiang. Applicant before: HANGZHOU ZHIDE NEW MATERIAL Co.,Ltd. |
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