CN107128924A - A kind of method that utilization microwave sintering prepares β SiC - Google Patents
A kind of method that utilization microwave sintering prepares β SiC Download PDFInfo
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- CN107128924A CN107128924A CN201710441360.9A CN201710441360A CN107128924A CN 107128924 A CN107128924 A CN 107128924A CN 201710441360 A CN201710441360 A CN 201710441360A CN 107128924 A CN107128924 A CN 107128924A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01—INORGANIC CHEMISTRY
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of method that utilization microwave sintering prepares β SiC, comprise the following steps that：By appropriate Na2SiO3·9H2O is dissolved in deionized water, and catalyst Fe (NO is added thereto3)3·9H2O and Tai Xi coals, stir, and magnetic agitation to mixture becomes sticky shape；Obtained thick liquid is dried in infrared drying oven, ground, silicon carbide precursor is obtained；Presoma is put into microwave agglomerating furnace and is sintered.The present invention has the advantages that overall heating, homogeneous heating, with short production cycle using microwave heating, using the higher nano beta SiC particulate of microwave sintering synthetic crystallization degree height, purity, significantly reduces energy consumption.Meanwhile, grain structure can be suppressed and grow up by being rapidly heated and being densified using microwave method, so as to prepare nano beta SiC particulate.
Description
Technical field
It is specifically that one kind prepares β-SiC using microwave sintering the present invention relates to semiconductor material performance studying technological domain
Method.
Background technology
β-SiC are due to electron mobility height (~800cm2V-1s-1), electronics saturation drift velocity it is big (~
2.5x107cms-1), the features such as dielectric constant is low, chemical stability is good, energy gap is big, be widely used in high frequency, anti-spoke
Penetrate, the field such as high temperature resistant, as the semi-conducting material for most having application prospect.The preparation technology of nano silicon carbide powder has a lot
Kind：Including pattern mnemonics, CNT limited reactions, vapour deposition process, sol-gal process and carbothermic method and electric arc
Electric discharge etc.；Purity is high, preparation technology is simpler because the silicon carbide powder of synthesis has for carbothermic method in numerous synthetic methods
The features such as, it is widely used in industrialized production.Sol-gel process and the powder granule obtained by vapour deposition process
Size is small, reunites few, but cost is high, low yield, is difficult to realize and produces in enormous quantities, is more suited to produce laboratory material and is used for
The product of particular/special requirement.Consider, in line with the principle of economic environmental protection, in the synthesis of silicon carbide powder, first have to reduce energy
The consumption in source, its secondary guarantee raw material is fully easily purchased, cheap；The microwave for being described as " 21 century a new generation's sintering technology " burns
Knot is that a kind of heating is quick, uniform, thermal efficiency height, environmental protection and the ceramic sintering new technology for having application prospect, and it utilizes microwave
The dielectric loss of ceramic material makes material integrally be heated to sintering temperature and realizes sintering and be densified in electromagnetic field.In addition, micro-
Ripple sintering process is without heat transfer, without thermal inertia, and thermal source can immediately generate heat or instantaneously stop, with short production cycle, single stove production
Amount amount is big, and piece-production cost is low.Since the advent of the world, Al has successfully been sintered using microwave2O3、ZrO2Deng oxide pottery
Porcelain, to Si3N4Feasibility study has also been carried out Deng non-oxide ceramicses, but using coal as carbon source, has been prepared and is carbonized using microwave sintering
Silicon is rarely reported.
The content of the invention
It is an object of the invention to provide a kind of method that utilization microwave sintering prepares β-SiC, to solve above-mentioned background skill
The problem of being proposed in art.
To achieve the above object, the present invention provides following technical scheme：
A kind of method that utilization microwave sintering prepares β-SiC, is comprised the following steps that：
(1) by appropriate Na2SiO3·9H2O is dissolved in deionized water, and catalyst Fe (NO is added thereto3)3·9H2O and
Too western coal, stirs, and then magnetic agitation to mixture becomes sticky shape under 90 DEG C of constant temperatures；
(2) obtained thick liquid is dried in infrared drying oven, ground, obtain silicon carbide precursor；
(3) using the temperature on infrared radiation thermometer direct measurement reaction mass surface, by manually adjusting microwave input power
Realize the control to microwave sintering；
(4) presoma no less than 20-30g is put into microwave agglomerating furnace and be sintered；Selected reaction temperature is 1300-
1600 DEG C, heating rate is 40 DEG C/min, and the reaction time is 30-90min.
It is used as further scheme of the invention：The too western coal crosses 200 mesh sieves.
It is used as further scheme of the invention：It is 1450 DEG C that reaction temperature is selected in the step (4), and heating rate is
40 DEG C/min, the reaction time is 60min.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention has the advantages that overall heating, homogeneous heating, with short production cycle using microwave heating, is burnt using microwave
Nano beta-SiC particulate that crystallinity is high, purity is higher is combined into, energy consumption is significantly reduced.Meanwhile, quickly risen using microwave method
Gentle densification can suppress grain structure and grow up, so as to prepare nano beta-SiC particulate.
Brief description of the drawings
Fig. 1 is the XRD spectrum of different soaking time products therefroms at 1600 DEG C in the embodiment of the present invention.
β-the SiC synthesized in Fig. 2 in A, B, C, D figure respectively embodiment of the present invention under 1600 DEG C, 60min SEM,
TEM and HR-TEM spectrograms.
The grain size distribution that Fig. 3 is β-SiC in the embodiment of the present invention.
Embodiment
The technical scheme of this patent is described in more detail with reference to embodiment.
Embodiment 1
A kind of method that utilization microwave sintering prepares β-SiC, is comprised the following steps that：
(1) by appropriate Na2SiO3·9H2O is dissolved in deionized water, and catalyst Fe (NO is added thereto3)3·9H2O and
The too western coal of 200 mesh sieves is crossed, is stirred, then magnetic agitation to mixture becomes sticky shape under 90 DEG C of constant temperatures；
(2) obtained thick liquid is dried in infrared drying oven, ground, obtain silicon carbide precursor；
(3) using the temperature on infrared radiation thermometer direct measurement reaction mass surface, by manually adjusting microwave input power
Realize the control to microwave sintering；
(4) 20g presoma is put into microwave agglomerating furnace and be sintered；Selected reaction temperature is 1300 DEG C, heating speed
Rate is 40 DEG C/min, and the reaction time is 30min.
Embodiment 2
A kind of method that utilization microwave sintering prepares β-SiC, is comprised the following steps that：
(1) by appropriate Na2SiO3·9H2O is dissolved in deionized water, and catalyst Fe (NO is added thereto3)3·9H2O and
The too western coal of 200 mesh sieves is crossed, is stirred, then magnetic agitation to mixture becomes sticky shape under 90 DEG C of constant temperatures；
(2) obtained thick liquid is dried in infrared drying oven, ground, obtain silicon carbide precursor；
(3) using the temperature on infrared radiation thermometer direct measurement reaction mass surface, by manually adjusting microwave input power
Realize the control to microwave sintering；
(4) 25g presoma is put into microwave agglomerating furnace and be sintered；Selected reaction temperature is 1450 DEG C, heating speed
Rate is 40 DEG C/min, and the reaction time is 60min.
Embodiment 3
A kind of method that utilization microwave sintering prepares β-SiC, is comprised the following steps that：
(1) by appropriate Na2SiO3·9H2O is dissolved in deionized water, and catalyst Fe (NO is added thereto3)3·9H2O and
The too western coal of 200 mesh sieves is crossed, is stirred, then magnetic agitation to mixture becomes sticky shape under 90 DEG C of constant temperatures；
(2) obtained thick liquid is dried in infrared drying oven, ground, obtain silicon carbide precursor；
(3) using the temperature on infrared radiation thermometer direct measurement reaction mass surface, by manually adjusting microwave input power
Realize the control to microwave sintering；
(4) 30g presoma is put into microwave agglomerating furnace and be sintered；Selected reaction temperature is 1600 DEG C, heating speed
Rate is 40 DEG C/min, and the reaction time is 90min.
Silicon source of the invention used is sodium metasilicate (analysis is pure), and carbon source used is high heating value, high-carbon, high chemism and low
Ash, low-sulfur, the too western coal of low volatile, as shown in table 1, catalyst is Fe (NO to its chemical analysis results3)3.By chemical reaction side
Formula SiO2(s)+3C (s)=SiC (s)+2CO (g), calculates and dispensing experiment is carried out after the mass fraction of reactant.
The chemical analysis results (mass fraction, %) of the too western coal of table 1
Implementation result is as follows：
1st, reaction temperature prepares β-SiC influence to microwave sintering
It is carbon source for the too western coal of 200 purposes to use granularity, identical with the sintering reaction time, and differential responses temperature is burnt to microwave
The result that knot prepares β-SiC is as follows：1300th, 1400 the XRD of 60min products therefroms, 1500, is incubated under 1600 DEG C of different temperatures
Spectrum confirms that the synthesized all β-SiC of carborundum of this experiment match with the standard diffraction card of β-SiC phases
(JCPDSCardNo.29-1129), lattice type is face-centered cubic.1300,1400 DEG C when, main thing mutually has SiO2With β-
SiC is present.At 1500 DEG C and 1600 DEG C, the main thing of product is mutually β-SiC, substantially without SiO2, react and be basically completed.
2nd, the time prepares β-SiC influence to microwave sintering
It is 1600 DEG C to select reaction temperature, and research 30,60,90min difference soaking times prepare β-SiC's to microwave sintering
Influence.Fig. 1 is the XRD spectrum of reaction different time products therefrom at 1600 DEG C.As shown in Figure 1, the reaction time be 30,60,
During 90min, main thing is mutually β-SiC in product, but all there is the unreacted SiO of very small amount2；With the extension of time, β-
SiC peak is remarkably reinforced, and illustrates that the extension of the crystallinity of product over time is improved.
3rd, the influence of reaction temperature and time to β-SiC yields
β-SiC yield under the conditions of the differential responses of table 2
Table 2 is listed under the conditions of same time, the influence of different reaction temperature to β-SiC yields；And same reaction
Under temperature conditionss, the yield impact of different soaking time to β-SiC.As shown in Table 2, during 60min, 1300 DEG C of yields are only
20.8%, illustrate that temperature is relatively low, reaction can not be carried out completely；Yield at 1400 DEG C rapidly increases to 56.4%, is 1300 DEG C
2.7 times；When temperature rises to 1500 DEG C, β-SiC content in product rises to 68.3%, is 1.2 times of 1400 DEG C；
Yield at 1600 DEG C is 75.7%, is 1.1 times of 1500 DEG C.Under the conditions of this explanation same time, with the rise of temperature, product
Yield gradually step up.1300 to 1400 DEG C of amplitudes improved to product yield are right more than 1400 to 1500 DEG C and 1500 to 1600 DEG C
The amplitude that product yield is improved.At 1600 DEG C of same reaction temperature, with the extension of soaking time, 30min, 60min, 90min couples
The yield answered is by 73.6% to 75.7%, then to 76.1%, and yield tends towards stability.When reaction temperature from 1500 DEG C rises to 1600
DEG C, the reaction time from 60min extend to 90min when, β-SiC amplification very little, illustrates at a lower temperature in reaction product
The comparison carried out is reacted in the shorter reaction time complete.Illustrate that microwave heating can significantly reduce reaction temperature, shortened
Into the time of reaction, energy consumption is significantly reduced.
Head product is put into ptfe plastic beaker, appropriate hydrochloric acid and hydrofluoric acid (volume ratio 1 is added:1), it is put into super
Ultrasound 2h under 100Hz, with neutrality is originally washed to, is put into baking oven and is dried to obtain pure products in sound washer.Production after purification
Thing only has the β-SiC of single-phase, and the intensity of diffraction maximum is very strong, illustrates that the β-SiC crystallinity of synthesis is high.Meanwhile, 2 θ=
At 33.6 °, occur in that weak diffraction maximum, represent β-SiC generated on (111) crystal face accumulation defect (stackingfault,
SF), it in the angle of diffraction is respectively the diffraction at 33.6 ° and 41.4 ° generally with β-SiC caused by the change of atom stacking sequence to be
The ratio between peak intensity come represent accumulate defect size.The ratio between peak intensity is smaller, shows that the accumulation defect produced is smaller.
Fig. 2 and Fig. 3 are SEM, TEM, HR-TEM spectrogram and particle diameter of the pure β-SiC powder synthesized under 1600 DEG C, 60min
Distribution map, can be seen that by Fig. 2 A, B figure and Fig. 3：Product β-SiC are the more uniform nano particle of size, and particle size exists
70-300nm, while in the presence of extremely a small amount of whisker.Sol-gel process makes silicon source fully be contacted with carbon source, obtained forerunner
Body has reached the uniform mixing on molecular level, is conducive to carborundum nucleation.It is right in order to further study the microstructure of product
Product carries out HR-TEM signs, and β-SiC have perfect crystal structure it can be seen from Fig. 2 C figures, and lattice fringe clearly may be used
See, and the distance between two neighboring parallel crystal face is 0.25nm, it is consistent with β-SiC (111) crystal face interplanar distance, illustrate [111]
It is the β-SiC direction of growth.In addition, being schemed from D, existing defects region in the β-SiC of synthesis, the defect for showing uniqueness is micro-
See structure.
β-SiC whole formation mainly have with growth course following ten set of equations into.(1)-(2) formula, due to Fe
(NO3)3·9H2O is to contain micro Fe in catalyst and too western coal in this experiment2O3, the Fe (NO in heating process3)3·
9H2O is decomposed to form Fe2O3, and it is reduced into Fe particles with C reactions.(3)-(7) formula, under complicated atmosphere, SiO (g) can dissolve
Liquid phase Fe-Si alloy liquid droplets are formed into Fe particles, favourable nucleation site is provided for reaction, and at high temperature with C and generation
CO gases further form Fe-Si-C-O eutectic drops, when Fe-Si-C-O drops reach supersaturation, Si and C start
Separate out, it then follows gas-liquid-solid (VLS) mechanism, synthesizing β-SiC particle.(8)-(10) formula, with the progress of reaction, Fe2O3Consumption
It is complete, gas-solid (VS) mechanism is followed in reactant part, between SiO and CO and is reacted, when reaching gas-solid reaction institute
During the dynamic conditions needed, reaction is smoothed out and generates a small amount of β-SiC whiskers.
(1)4Fe(NO3)3(s)→2Fe2O3(s)+12NO2(g)+3O2(g)
(2)3C(s)+2Fe2O3(s)→4Fe(s)+3CO2(g)
(3)SiO2(s)+2Fe(s)+2C(s)→Fe2Si(l)+2CO(g)
(4)3SiO2(s)+5Fe(s)+6C(s)→Fe5Si3(l)+6CO(g)
(5)Fe2Si(l)(Fe5Si3(l))+C(s)→SiC(s)+2Fe(s)
(6)SiO2(s)+C(s)→SiO(g)+CO(g)
(7)SiO2(s)+CO(g)→SiO(g)+CO2(g)
(8)CO2(g)+C(s)→2CO(g)
(9)SiO(g)+2C(s)→SiC(s)+CO(g)
(10)SiO(g)+3CO(g)→SiC(s)+2CO2(g)
The western coal of ether and sodium metasilicate of the present invention are raw material, Fe (NO3)3·9H2O is catalyst, is used in 1600 DEG C of x60min
Microwave sintering has prepared single-phase nano beta-SiC particulate that crystallinity is high, purity is higher, and yield reaches 75.7%, particle
Size is mainly distributed on 70-300nm；Microwave heating has the advantages that overall heating, homogeneous heating, with short production cycle, notable drop
Low energy consumption.Meanwhile, grain structure can be suppressed and grow up by being rapidly heated and being densified using microwave method, so as to prepare nanoscale
β-SiC particulate.
The better embodiment to this patent is explained in detail above, but this patent is not limited to above-mentioned embodiment party
, can also be on the premise of this patent objective not be departed from formula, the knowledge that one skilled in the relevant art possesses
Various changes can be made.
Claims (3)
1. a kind of method that utilization microwave sintering prepares β-SiC, it is characterised in that comprise the following steps that：
(1) by appropriate Na2SiO3·9H2O is dissolved in deionized water, and catalyst Fe (NO is added thereto3)3·9H2O and Tai Xi
Coal, stirs, and then magnetic agitation to mixture becomes sticky shape under 90 DEG C of constant temperatures；
(2) obtained thick liquid is dried in infrared drying oven, ground, obtain silicon carbide precursor；
(3) using the temperature on infrared radiation thermometer direct measurement reaction mass surface, realized by manually adjusting microwave input power
Control to microwave sintering；
(4) presoma no less than 20-30g is put into microwave agglomerating furnace and be sintered；Selected reaction temperature is 1300-1600
DEG C, heating rate is 40 DEG C/min, and the reaction time is 30-90min.
2. the method that utilization microwave sintering according to claim 1 prepares β-SiC, it is characterised in that the too western coal mistake
200 mesh sieves.
3. the method that utilization microwave sintering according to claim 1 prepares β-SiC, it is characterised in that in the step (4)
Selected reaction temperature is 1450 DEG C, and heating rate is 40 DEG C/min, and the reaction time is 60min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113718370A (en) * | 2021-09-14 | 2021-11-30 | 郑州航空工业管理学院 | Preparation method of hollow silicon carbide fiber |
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| CN102502640A (en) * | 2011-10-28 | 2012-06-20 | 东北大学 | Method for synthetizing silicon carbide through microwave heating of pulverized fuel ash and aluminium electrolysis of waste cathode carbon blocks |
| CN102897763A (en) * | 2012-10-08 | 2013-01-30 | 北京科技大学 | Low-temperature rapid synthesis method of alpha-SiC micropowder |
| CN103058192A (en) * | 2013-01-06 | 2013-04-24 | 保定科瑞晶体有限公司 | Preparation method of silicon carbide micro-powder used in silicon carbide crystal growth |
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Application publication date: 20170905 |