CN109437913A - A kind of method that low temperature is synthetically prepared Silicon Carbide Powder - Google Patents
A kind of method that low temperature is synthetically prepared Silicon Carbide Powder Download PDFInfo
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- CN109437913A CN109437913A CN201811616833.5A CN201811616833A CN109437913A CN 109437913 A CN109437913 A CN 109437913A CN 201811616833 A CN201811616833 A CN 201811616833A CN 109437913 A CN109437913 A CN 109437913A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
A kind of method that low temperature is synthetically prepared Silicon Carbide Powder, comprising the following steps: (1) sequentially add waterglass, coupling agent, polyethylene glycol and hydrochloric acid in deionized water, gel is made in stirring；It is filtered after washing and alcohol is washed；(2) it is put into dehydrated alcohol, phenolic resin is added under agitation, stirring forms paste；It dries under the conditions of 65~200 DEG C, is ground after being cooled to；(3) it is put into heating furnace, is passed through argon gas and keeps circulating；It is warming up to 1400~1550 DEG C of progress carbothermic reduction reactions, furnace cooling；(4) it is placed in resistance furnace, heat preservation makes remaining carbon removal under the conditions of 550~650 DEG C, grinds after cooling to room temperature with the furnace.Raw material sources of the present invention are extensive, by modes such as catalytic modifications, silicon source and carbon source made to reach atom or the other uniform mixing of molecular level, to reduce carbothermic reduction reaction temperature, reduce production cost.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, in particular to a kind of low temperature is synthetically prepared Silicon Carbide Powder
Method.
Background technique
Silicon carbide (SiC) ceramics have the excellent properties such as high temperature resistant, corrosion-resistant, high rigidity, high intensity and receive much attention, with
The continuous development of high-technology field, thyrite is in high-techs such as refractory material, metallurgy, machinery, chemical industry and military projects
Skill field has extensive development prospect；But presently, there are main problem be that the production cost of silicon carbide ceramics is higher, sternly
Ghost image rings the commercialization promotion and application of thyrite；For this purpose, there is an urgent need to reduce the production of thyrite
Cost.
One of the effective way for reducing thyrite production cost is to reduce raw materials for production (silicon carbide ceramics powder
Body) production cost；Currently, the production method that most Silicon Carbide Powder is promoted in commercialization is wet chemistry method and carbon thermal reduction
The method combined, existing main problem are that carbothermic reduction reaction temperature is higher, generally at 1550~1650 DEG C or so, are reunited
Caking phenomenon is serious, and common silicon source is mainly ethyl orthosilicate, and price is higher；For this purpose, inhibiting to reunite, reducing carbothermic reduction reaction
The price of temperature and silicon source is imperative.
Summary of the invention
The object of the present invention is to provide a kind of methods that low temperature is synthetically prepared Silicon Carbide Powder, by selecting raw material to match
Process flow is closed, on the basis of low temperature synthesis, high-purity carborundum is prepared, improves production efficiency while reducing cost.
The method of the present invention includes the following steps:
1, it prepares gel: preparing silicon source waterglass, hydrochloric, surfactant coupling agent and polyethylene glycol, wherein
The mass concentration of hydrochloric acid is 5~35%；Hydrochloric acid accounts for the percent by volume 1~30% of waterglass, and coupling agent accounts for waterglass and hydrochloric acid
The 0.01~10.0% of total volume, polyethylene glycol are the 0.01~10.0% of waterglass and hydrochloric acid gross mass；By waterglass, coupling
Agent, polyethylene glycol and hydrochloric acid sequentially add in deionized water, stir evenly and gel is made；By gel after washing and alcohol is washed, mistake
Filter obtains aqueous precursor gel；
2, it prepares presoma powder: aqueous precursor gel is put into dehydrated alcohol, phenolic resin is added under agitation,
Dissolve phenolic resin in dehydrated alcohol, aqueous precursor gel is dispersed, until whole materials form paste；Paste is set
In baking oven, drying removal volatile ingredient, surplus material cool to room temperature with the furnace under the conditions of 65~200 DEG C, take out grinding system
At presoma powder；Wherein the molar ratio of phenolic resin and waterglass is 0.5~10；
3, it synthesizes: presoma powder being put into heating furnace, argon gas is passed through into heating furnace and drives away air, and keeps argon
Air-flow is logical；Then heating furnace is warming up to 1400~1550 DEG C, keeps the temperature 2~5 hours, carry out carbothermic reduction reaction, reaction is completed
After cool to room temperature with the furnace, obtain coarse dispersion；
4, decarburization: coarse dispersion is placed in resistance furnace, is kept the temperature 2~8 hours under the conditions of 550~650 DEG C, is made remaining carbon
Removal, the material after reaction cools to room temperature with the furnace, then grinds and Silicon Carbide Powder is made.
The degree of polymerization of above-mentioned polyethylene glycol is 2000~20000.
In above-mentioned step 1, after the dosage of deionized water is with deionized water and mixed in hydrochloric acid, waterglass, idol are all dissolved
Join subject to agent and polyethylene glycol.
In above-mentioned step 2, the dosage of dehydrated alcohol, which is subject to, dissolves whole phenolic resin.
The partial size of above-mentioned Silicon Carbide Powder is 200~1000 nanometers.
The silicon source that the present invention uses is waterglass cheap, from a wealth of sources, instead of ethyl orthosilicate on the high side,
Carbon source phenolic resin higher using phosphorus content, cheap；Due to waterglass and phenolic resin objectionable intermingling, lean on completely
Mechanical mixture, be difficult to make to reach between waterglass and phenolic resin atom or molecular level it is other it is uniform mix, therefore pass through hydrochloric acid
Catalytic action promote waterglass to hydrolyze, in combination with the grafting of coupling agent and polyethylene glycol, surface is modified makees with dispersion
With making that colloidal particles obtain dispersion and surface is modified, even if silicon source and carbon source can be compatible, and reach atom or molecular level is other
Uniformly mixing reduces production cost to reduce carbothermic reduction reaction temperature.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of the Silicon Carbide Powder in the embodiment of the present invention 1；
Fig. 2 is the SEM photograph figure of the Silicon Carbide Powder in the embodiment of the present invention 1.
Specific embodiment
Waterglass, coupling agent, polyethylene glycol and the phenolic resin used in the embodiment of the present invention is commercial products.
X-ray diffractometer model PW3040/60 is used in the embodiment of the present invention.
Scanning electron microscope model SSX-550 is used in the embodiment of the present invention.
In the embodiment of the present invention, it is that gel is first placed in water to stirring at least 5min that washing and alcohol, which are washed, then takes out and is placed in
At least 5min is stirred in ethyl alcohol.
In the embodiment of the present invention, the time dried under the conditions of 65~200 DEG C is 2~24 hours.
Coupling agent selects KH-550, KH-560 or KH-570 in the embodiment of the present invention.
Phenolic resin selects FQ-9 in the embodiment of the present invention.
Embodiment 1
Prepare silicon source waterglass, hydrochloric, surfactant coupling agent and polyethylene glycol, wherein the quality of hydrochloric acid is dense
Degree is 35%；Hydrochloric acid accounts for the percent by volume 1% of waterglass, and coupling agent accounts for the 0.01% of waterglass and hydrochloric acid total volume, poly- second
Glycol is the 0.01% of waterglass and hydrochloric acid gross mass；Waterglass, coupling agent, polyethylene glycol and hydrochloric acid are sequentially added into deionization
In water, stirs evenly and gel is made；By gel after washing and alcohol is washed, the solid phase of acquisition is filtered as aqueous precursor gel；Wherein
The degree of polymerization of polyethylene glycol is 2000；After the dosage of deionized water is with deionized water and mixed in hydrochloric acid, waterglass, idol are all dissolved
Join subject to agent and polyethylene glycol；
Aqueous precursor gel is put into dehydrated alcohol, phenolic resin is added under agitation, makes phenolic resin anhydrous
It is dissolved in ethyl alcohol, aqueous precursor gel is dispersed, until whole materials form paste；Paste is placed in baking oven, at 65 DEG C
Under the conditions of drying removal volatile ingredient, surplus material cools to room temperature with the furnace, takes out grinding and presoma powder is made；Dehydrated alcohol
Dosage be subject to by whole phenolic resin dissolve；The molar ratio of phenolic resin and waterglass is 2；
Presoma powder is put into heating furnace, argon gas is passed through into heating furnace and drives away air, and argon gas is kept to circulate；
Then heating furnace is warming up to 1400 DEG C, keeps the temperature 5 hours, carried out carbothermic reduction reaction, cool to room temperature with the furnace after the reaction was completed,
Obtain coarse dispersion；
Coarse dispersion is placed in resistance furnace, 8 hours is kept the temperature under the conditions of 550 DEG C, makes remaining carbon removal, the object after reaction
Material cools to room temperature with the furnace, then grinds and Silicon Carbide Powder is made, and 100~350 nanometers of partial size, X-ray diffraction result such as Fig. 1
Shown, product does not have apparent impurity as seen from the figure, and silicon carbide powder SEM photograph is as shown in Figure 2.
Embodiment 2
With embodiment 1, difference is method:
(1) mass concentration of hydrochloric acid is 25%；Hydrochloric acid accounts for the percent by volume 10% of waterglass, coupling agent account for waterglass and
The 1% of hydrochloric acid total volume, polyethylene glycol are the 1% of waterglass and hydrochloric acid gross mass；The degree of polymerization of polyethylene glycol is 4000；
(2) molar ratio of phenolic resin and waterglass is 5, and paste dries removal volatile ingredient under the conditions of 80 DEG C；
(3) heating furnace is warming up to 1450 DEG C and keeps the temperature 4 hours, carry out carbothermic reduction reaction；
(4) coarse dispersion keeps the temperature 6 hours under the conditions of 600 DEG C, makes remaining carbon removal, the material after reaction cools to the furnace
Room temperature, then grind and Silicon Carbide Powder is made, 200~450 nanometers of partial size.
Embodiment 3
With embodiment 1, difference is method:
(1) mass concentration of hydrochloric acid is 15%；Hydrochloric acid accounts for the percent by volume 20% of waterglass, coupling agent account for waterglass and
The 5% of hydrochloric acid total volume, polyethylene glycol are the 10% of waterglass and hydrochloric acid gross mass；The degree of polymerization of polyethylene glycol is 6000；
(2) molar ratio of phenolic resin and waterglass is 8, and paste dries removal volatile ingredient under the conditions of 120 DEG C；
(3) heating furnace is warming up to 1500 DEG C and keeps the temperature 3 hours, carry out carbothermic reduction reaction；
(4) coarse dispersion keeps the temperature 4 hours under the conditions of 620 DEG C, makes remaining carbon removal, the material after reaction cools to the furnace
Room temperature, then grind and Silicon Carbide Powder is made, 300~700 nanometers of partial size.
Embodiment 4
With embodiment 1, difference is method:
(1) mass concentration of hydrochloric acid is 5%；Hydrochloric acid accounts for the percent by volume 30% of waterglass, coupling agent account for waterglass and
The 10.0% of hydrochloric acid total volume, polyethylene glycol are the 5% of waterglass and hydrochloric acid gross mass；The degree of polymerization of polyethylene glycol is 20000；
(2) molar ratio of phenolic resin and waterglass is 10, and paste dries removal volatile ingredient under the conditions of 200 DEG C；
(3) heating furnace is warming up to 1550 DEG C and keeps the temperature 2 hours, carry out carbothermic reduction reaction；
(4) coarse dispersion keeps the temperature 2 hours under the conditions of 650 DEG C, makes remaining carbon removal, the material after reaction cools to the furnace
Room temperature, then grind and Silicon Carbide Powder is made, 350~850 nanometers of partial size.
Claims (5)
1. a kind of method that low temperature is synthetically prepared Silicon Carbide Powder, it is characterised in that the following steps are included:
(1) it prepares gel: preparing silicon source waterglass, hydrochloric, surfactant coupling agent and polyethylene glycol, wherein hydrochloric acid
Mass concentration be 5~35%；Hydrochloric acid accounts for the percent by volume 1~30% of waterglass, and coupling agent accounts for waterglass and hydrochloric acid is overall
Long-pending 0.01~10.0%, polyethylene glycol are the 0.01~10.0% of waterglass and hydrochloric acid gross mass；By waterglass, coupling agent,
Polyethylene glycol and hydrochloric acid sequentially add in deionized water, stir evenly and gel is made；By gel after washing and alcohol is washed, filtering is obtained
Obtain aqueous precursor gel；
(2) it prepares presoma powder: aqueous precursor gel is put into dehydrated alcohol, phenolic resin is added under agitation, make
Phenolic resin dissolves in dehydrated alcohol, and aqueous precursor gel is dispersed, until whole materials form paste；Paste is placed in
In baking oven, drying removal volatile ingredient, surplus material cool to room temperature with the furnace under the conditions of 65~200 DEG C, take out grinding and are made
Presoma powder；Wherein the molar ratio of phenolic resin and waterglass is 0.5~10；
(3) it synthesizes: presoma powder being put into heating furnace, argon gas is passed through into heating furnace and drives away air, and keeps argon gas
Circulation；Then heating furnace is warming up to 1400~1550 DEG C, keeps the temperature 2~5 hours, carry out carbothermic reduction reaction, after the reaction was completed
It cools to room temperature with the furnace, obtains coarse dispersion；
(4) decarburization: coarse dispersion is placed in resistance furnace, is kept the temperature 2~8 hours under the conditions of 550~650 DEG C, is removed remaining carbon
It removes, the material after reaction cools to room temperature with the furnace, then grinds and Silicon Carbide Powder is made.
2. the method that a kind of low temperature according to claim 1 is synthetically prepared Silicon Carbide Powder, it is characterised in that described
Polyethylene glycol the degree of polymerization be 2000~20000.
3. the method that a kind of low temperature according to claim 1 is synthetically prepared Silicon Carbide Powder, it is characterised in that step
(1) in, after the dosage of deionized water is with deionized water and mixed in hydrochloric acid, all dissolving waterglass, coupling agent and polyethylene glycol is
It is quasi-.
4. the method that a kind of low temperature according to claim 1 is synthetically prepared Silicon Carbide Powder, it is characterised in that step
(2) in, the dosage of dehydrated alcohol, which is subject to, dissolves whole phenolic resin.
5. the method that a kind of low temperature according to claim 1 is synthetically prepared Silicon Carbide Powder, it is characterised in that described
Silicon Carbide Powder partial size be 200~1000 nanometers.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56140079A (en) * | 1980-03-28 | 1981-11-02 | Nippon Steel Corp | Indefinite form refractory composition for vibration molding |
| CN101786622A (en) * | 2010-01-20 | 2010-07-28 | 中国科学院山西煤炭化学研究所 | Preparation method of silicon carbide nano-wire |
| CN101804981A (en) * | 2010-04-01 | 2010-08-18 | 中国科学院山西煤炭化学研究所 | Method for preparing hollow silicon carbide nano material |
| CN102432013A (en) * | 2011-10-08 | 2012-05-02 | 中国科学院山西煤炭化学研究所 | Preparation method of beta-nano-SiC |
| CN107963631A (en) * | 2017-12-12 | 2018-04-27 | 宁波爱克创威新材料科技有限公司 | Nanometer silicon carbide and preparation method thereof |
| CN108314050A (en) * | 2018-03-12 | 2018-07-24 | 鲁东大学 | A kind of preparation method of the nanometer silicon carbide particle of efficient absorption organic dyestuff |
-
2018
- 2018-12-27 CN CN201811616833.5A patent/CN109437913B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56140079A (en) * | 1980-03-28 | 1981-11-02 | Nippon Steel Corp | Indefinite form refractory composition for vibration molding |
| CN101786622A (en) * | 2010-01-20 | 2010-07-28 | 中国科学院山西煤炭化学研究所 | Preparation method of silicon carbide nano-wire |
| CN101804981A (en) * | 2010-04-01 | 2010-08-18 | 中国科学院山西煤炭化学研究所 | Method for preparing hollow silicon carbide nano material |
| CN102432013A (en) * | 2011-10-08 | 2012-05-02 | 中国科学院山西煤炭化学研究所 | Preparation method of beta-nano-SiC |
| CN107963631A (en) * | 2017-12-12 | 2018-04-27 | 宁波爱克创威新材料科技有限公司 | Nanometer silicon carbide and preparation method thereof |
| CN108314050A (en) * | 2018-03-12 | 2018-07-24 | 鲁东大学 | A kind of preparation method of the nanometer silicon carbide particle of efficient absorption organic dyestuff |
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