CN104328478B - A kind of preparation method of SiC whisker - Google Patents
A kind of preparation method of SiC whisker Download PDFInfo
- Publication number
- CN104328478B CN104328478B CN201410401688.4A CN201410401688A CN104328478B CN 104328478 B CN104328478 B CN 104328478B CN 201410401688 A CN201410401688 A CN 201410401688A CN 104328478 B CN104328478 B CN 104328478B
- Authority
- CN
- China
- Prior art keywords
- sic whisker
- presoma
- preparation
- silicon
- carbon source
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 43
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 37
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 37
- 239000010703 silicon Substances 0.000 claims abstract description 36
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000009768 microwave sintering Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000006004 Quartz sand Substances 0.000 claims abstract description 12
- 239000012467 final product Substances 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000003245 coal Substances 0.000 claims description 15
- 230000033228 biological regulation Effects 0.000 claims description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 10
- 241001502050 Acis Species 0.000 claims description 9
- 150000002148 esters Chemical group 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 238000005245 sintering Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 8
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 2
- 230000001419 dependent effect Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 69
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 66
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- 238000000746 purification Methods 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 5
- 239000004567 concrete Substances 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000004576 sand Substances 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 238000005339 levitation Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011157 advanced composite material Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N carbon tetrachloride Substances ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- -1 silicon halide Chemical class 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses the preparation method of a kind of SiC whisker, comprise the following steps: 1) take carbon source and presoma is made in silicon source；2) by step 1) after gained presoma tabletted, in embedment quartz sand, carry out microwave sintering synthetic reaction, to obtain final product.The preparation method of the SiC whisker of the present invention, utilizes the absorbing property that carbon is excellent, uses direct microwave synthesis method, it is achieved that the Fast back-projection algorithm of SiC whisker, obtains the SiC whisker of well-crystallized；Microwave sintering is dependent on the dielectric loss of material self to complete material sintering, compared to industry conventional heating methods, have can realize volume heating, pollute less, the sintering period is short, low power consumption and other advantages；Gained SiC whisker size is uniform, and draw ratio is high, better crystallinity degree, and defect is few, and yield is high；The method technique is simple, and easy to operate, with short production cycle, sintering temperature is low, and energy consumption is low, pollution is few, is suitable for large-scale industrial production, has broad application prospects.
Description
Technical field
The invention belongs to SiC material technical field, be specifically related to the preparation method of a kind of SiC whisker.
Background technology
Carborundum is again corundum or fire sand, and stable chemical performance, heat conductivity are high, thermal coefficient of expansion is little, wearability
Can be good, it is widely used in function ceramics, high grade refractory, abrasive material and metallurgical raw material；Its highly purified monocrystalline, can be used for
Manufacture quasiconductor, silicon carbide fibre.Silicon carbide whisker is by the chopped fiber of high-purity carborundum crystal growth, its machinery
Intensity is equal to adjacent interatomic force.The height-oriented structure of silicon carbide whisker not only makes it have high intensity, high-modulus and height and stretches
Long rate, but also there is electricity, light, magnetic, dielectric, conduct electricity, superconduct character.Silicon carbide whisker and host material have good
The good compatibility, is the reinforcing agent of the advanced composite materials such as Metal Substrate, ceramic base and high polymer base, such as: the U.S. succeeds in developing
" SiC whisker and nano composite spraying " technology for wear resistant corrosion resistant high-temperaure coating.Silicon carbide whisker is at Stupalox
Tool, space shuttle, vapour vehicle component, chemical industry, machinery and production of energy obtain extensively application.
The method of traditional mode of production silicon carbide whisker can be generally divided into two kinds, and one is gas-phase reaction method, i.e. with carbonaceous gas with
Silicon-containing gas reacts, or the method decomposing the organic gas synthesis SiC whisker of a kind of carbon containing, silicon compound；Another kind is
Solid material method, i.e. utilizes carrier gas to pass through carbon containing and siliceous mixing material, at the space formation SiC separated with reaction material
The synthetic method of whisker.In both approaches, Si and C is necessary for gas phase or entrance liquid phase ingredient utilizes VLS method to close
Become SiC whisker.Reaction mechanism prepared by SiC whisker mainly has: take SiC whisker (" Vapor-liquid-solid phase " by VLS legal system
Method), and by VS mechanism synthesis SiC whisker (pertain only to solid, gas is biphase, whole generation process is not related to liquid phase and exists).
At present, specifically prepare the method for SiC whisker and also has many: with rice husk synthesis, organo-silicon compound thermal decomposition, silicon halide and
CCl4SiC whisker etc. is prepared Deng mixed gas reaction, oxide containing silicon carbon thermal reduction.But prepare SiC whisker in order to top method
The most highly desirable, exist as big in environmental pollution, energy loss, preparation technology and equipment complicated etc. in terms of problem.As existing
In technology, patent CN1449994A discloses the preparation method of a kind of silicon carbide whisker and micropowder, is by graphite and other works
After industry carbonaceous and siliceous raw material mixing, carry out synthetic reaction in loading industry SiC smelting furnace, make conductive heating unit with graphite
Prepare silicon carbide whisker and micropowder.But, it is high to there is sintering temperature in this method, the shortcoming of sintering time length.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of SiC whisker, solve existing preparation method sintering time length, the energy
Consume big, technique and the problem of equipment needed thereby complexity.
In order to realize object above, the technical solution adopted in the present invention is: the preparation method of a kind of SiC whisker, including under
Row step:
1) take carbon source and presoma is made in silicon source；
2) by step 1) after gained presoma tabletted, in embedment quartz sand, carry out microwave sintering synthetic reaction, to obtain final product.
Step 1) in, according to the ratio that mol ratio is 3～7.5:1 of carbon Yu silicon, carbon source and silicon source are made presoma.
Step 1) in, by the method that carbon source and silicon source make presoma it is: silicon source is made unformed by sol-gal process
Silicon dioxide, then presoma directly it is mixed and made into carbon source；Or, carbon source and silicon source are prepared as nothing by sol-gal process
The presoma of sizing Silica-coated carbon source.
Step 1) in, described carbon source is coal；Described silicon source is esters of silicon acis.
Step 1) in, it is also possible to directly with amorphous silica for silicon source, it is mixed with presoma with carbon source.
Described amorphous silica is graininess, and particle size is 385～900 μm.
Described carbon source is graininess, and particle size is less than 50 μm.
Described esters of silicon acis is tetraethyl orthosilicate.
Amorphous silica is made by sol-gal process in silicon source, comprises the following steps:
I) take esters of silicon acis, ethanol mixes with water, and regulation pH is 3～4, and stirring obtains mixture A；
Ii) pH of regulation mixture A is 8～9, and stirring obtains mixture B；
Iii) mixture B is filtered, take filter cake, be dried, obtain amorphous silica.
In step i), esters of silicon acis, ethanol are 23:35:50 with the volume ratio of water.
In step i), using Fructus Citri Limoniae acid for adjusting pH is 3～4；Step ii) in, using ammonia regulation pH is 8～9.
In step i), described stirring is to stir 1～4h under the conditions of 30～40 DEG C；Step ii) in, the time of described stirring
It is 0.5～2h.
Step iii) described in be dried temperature be 25～35 DEG C.
Carbon source and silicon source are prepared as the presoma of amorphous silica parcel carbon source by sol-gal process, including following step
Rapid:
A) take esters of silicon acis, ethanol mixes with water, and regulation pH is 3～4, and stirring obtains mixture A；
B) adding carbon source in mixture A, stirring, regulation pH is 8～9, obtains mixture B；
C) mixture B is filtered, take filter cake, be dried, obtain Silica-coated carbon source presoma.
In step a), esters of silicon acis, ethanol are 23:35:50 with the volume ratio of water.
In step a), using Fructus Citri Limoniae acid for adjusting pH is 3～4；In step b), using ammonia regulation pH is 8～9.
In step a), described stirring is to stir 1～4h under the conditions of 30～40 DEG C；In step b), described stirring be
1～2h is stirred under the conditions of 30～40 DEG C.
The temperature being dried described in step c) is 25～35 DEG C.
Step 2) in, the pressure of described compacting is 4～200MPa.
Step 2) in, described tabletted refers to be pressed into a diameter of 28～32mm, and thickness is the cylinder of 10～25mm
Sheet.
Step 2) in, described quartz sand is placed in alumina crucible.
Step 2) in, described microwave sintering synthetic reaction is the mode using microwave sintering, first with the speed of 5～20 DEG C/min
Rate is warming up to 580～620 DEG C, regulates input power, then with the ramp of 20～200 DEG C/min to 1000～1700 DEG C,
Insulation 5～120min.
Described temperature retention time preferably 5～60min.
Step 2) in, described microwave sintering synthetic reaction products therefrom is subsphaeroidal nucleocapsid structure, and whisker grows in shell,
Shell has separated external crystal sand and has contacted with the direct of whisker.
Step 2) in, also can carry out microwave sintering synthetic reaction products therefrom purifying silicon carbide whisker；Concrete operations are:
In air atmosphere, products therefrom is calcined under the conditions of 700 DEG C 2h, to remove unnecessary carbon, recycle levitation method
Separate silicon carbide whisker and granule, obtain the silicon carbide whisker of purification.
Described microwave sintering synthetic reaction is carried out in the case of unprotect atmosphere.
In the preparation method of the SiC whisker of the present invention, the coal absorbing property as carbon source is good, the most just can be with microwave
Well coupling, so can realize the synthesis of SiC whisker under microwave action.Building-up process need to bury burning with quartz sand,
Main Function is: close to the quartz sand generation melting phenomenon of sample, and the nucleocapsid structure of formation serves the effect of isolation air；
The composition of quartz sand is SiO2, it is to avoid the infiltration of impurity.Before microwave sintering synthetic reaction, by presoma tabletted
Effect is: reduce intergranular air content, increases intergranular contact area, strengthens the bulk effect of microwave heating.
The preparation method of the SiC whisker of the present invention, makes presoma tabletted by carbon source and silicon source, in embedment quartz sand,
Carry out microwave sintering synthetic reaction again and prepare SiC whisker, utilize the absorbing property that carbon is excellent, use direct microwave synthesis method,
Achieve the Fast back-projection algorithm of SiC whisker, obtain the SiC whisker of well-crystallized；Microwave sintering is dependent on the dielectric of material self
Be lost material sintering, compared to industry conventional heating methods, have can realize volume heating, pollute less, sintering
Cycle is short, low power consumption and other advantages；Gained SiC whisker size is uniform, and draw ratio is high, and better crystallinity degree, defect is few, and whisker is long
Reaching tens microns, draw ratio is up to 45, and whisker yield is high, and about about 70%；The method technique is simple, easy to operate,
With short production cycle, sintering temperature is low, and energy consumption is low, pollution is few, is suitable for large-scale industrial production, before having wide application
Scape.
Accompanying drawing explanation
Fig. 1 is the pictorial diagram of microwave sintering synthetic reaction products therefrom (subsphaeroidal nucleocapsid structure) in embodiment 1；
Fig. 2 is the XRD figure of embodiment 1 gained SiC whisker；
Fig. 3 is the SEM figure of embodiment 1 gained SiC whisker；
Fig. 4 is the XRD figure of embodiment 2 gained SiC whisker；
Fig. 5 is the SEM figure of embodiment 2 gained SiC whisker；
Fig. 6 is the XRD figure of embodiment 3 gained SiC whisker；
Fig. 7 is the SEM figure of embodiment 4 gained SiC whisker.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further illustrated.
Embodiment 1
The preparation method of the SiC whisker of the present embodiment, comprises the following steps:
1) taking grain diameter less than the life coal of 50 μm is carbon source, and taking tetraethyl orthosilicate is silicon source, according to rubbing of carbon and silicon
That, than the ratio for 3:1, obtains unformed SiO by sol-gal process2The presoma of parcel coal particles；
2) under the pressure of 4MPa, by step 1) gained presoma is pressed into a diameter of 28mm, and thickness is 10mm's
Slice of cylinder, and imbed in the alumina crucible being placed with quartz sand, crucible is placed in the multimode cavity that frequency is 2.45GHz micro-
In ripple stove, add insulation construction, in the case of unprotect atmosphere, carry out microwave sintering synthetic reaction:
First turn on microwave source, regulate microwave input power, first with the ramp of 5 DEG C/min to 600 DEG C i.e. dehumidifying stage
Terminate, regulate input power, then with the ramp of 50 DEG C/min to 1000 DEG C, monitor reflection power simultaneously, be incubated 60min,
Products therefrom is subsphaeroidal nucleocapsid structure, concrete as it is shown in figure 1, whisker grow in shell, shell separated external crystal sand and
The directly contact of whisker；Silicon carbide whisker is taken out in shell, obtains silicon carbide whisker.
Gained silicon carbide whisker is carried out purification processes, and concrete operations are: in air atmosphere, by products therefrom at 700 DEG C
Under the conditions of calcine 2h, to remove unnecessary carbon, recycling levitation method separation silicon carbide whisker and granule, obtain high-quality,
The silicon carbide whisker of purification.
In the present embodiment, obtain unformed SiO by sol-gal process2The method of the presoma of parcel coal particles includes following
Step:
A) with the ratio that volume ratio is 23:35:50 of distilled water, three is mixed according to tetraethyl orthosilicate, ethanol, use Fructus Citri Limoniae
Acid for adjusting pH is 3, stirs 4h, obtain mixture A under the conditions of 30 DEG C；
B) in mixture A, add coal, under the conditions of 30 DEG C, stir 2h, be 8 with ammonia regulation pH, continue stirring
2h, obtains mixture B；
C) with sucking filtration machine, mixture B is carried out sucking filtration, take filter cake, be dried under the conditions of 30 DEG C, obtain unformed SiO2Bag
Wrap up in the presoma of coal particles.
The SiC whisker that the present embodiment gained is unpurified carries out XRD and SEM detection, and result is as shown in Figure 2,3.
From the XRD figure of Fig. 2 it can be seen that the present embodiment products therefrom is SiC.
It can be seen that gained silicon carbide whisker size a length of 5～10 μm, better crystallinity degree from the SEM figure of Fig. 3.
Embodiment 2
The preparation method of the SiC whisker of the present embodiment, comprises the following steps:
1) taking tetraethyl orthosilicate is silicon source, and by sol-gal process, tetraethyl orthosilicate is made amorphous silica；Take
Grain particle diameter is carbon source less than the life coal of 50 μm, according to the ratio that mol ratio is 7.5:1 of carbon Yu silicon, coal is fixed with nothing
Type SiO2Mechanical mixture is uniform obtains presoma；
2) under the pressure of 200MPa, by step 1) gained presoma is pressed into a diameter of 30mm, and thickness is 20mm
Slice of cylinder, and imbed and be placed with in the alumina crucible of quartz sand, crucible is placed in the multimode cavity that frequency is 2.45GHz
In microwave oven, add insulation construction, in the case of unprotect atmosphere, carry out microwave sintering synthetic reaction:
First turn on microwave source, regulate microwave input power, first with the ramp of 20 DEG C/min to 580 DEG C i.e. dehumidifying stage
Terminate, regulate input power, then with the ramp of 100 DEG C/min to 1200 DEG C, monitor reflection power simultaneously, be incubated 5min,
Products therefrom is subsphaeroidal nucleocapsid structure, and specifically with embodiment 1, whisker grows in shell, shell separated external crystal sand with
The directly contact of whisker；Silicon carbide whisker is taken out in shell, obtains silicon carbide whisker.
Gained silicon carbide whisker is carried out purification processes, and concrete operations are: in air atmosphere, by products therefrom at 700 DEG C
Under the conditions of calcine 2h, to remove unnecessary carbon, recycling levitation method separation silicon carbide whisker and granule, obtain purification
Silicon carbide whisker.
In the present embodiment, just tetraethyl orthosilicate makes amorphous silica by sol-gal process, comprises the following steps:
I) with the ratio that volume ratio is 23:35:50 of distilled water, three is mixed according to tetraethyl orthosilicate, ethanol, use citric acid
Regulation pH is 4, stirs 3h, obtain mixture A under the conditions of 30 DEG C；
Ii) pH with ammonia regulation mixture A is 8, stirs 2h, obtains mixture B；
Iii) with sucking filtration machine, mixture B is carried out sucking filtration, takes filter cake, be dried under the conditions of 30 DEG C, grind and cross 300 mesh sieves,
Obtain unformed SiO2。
SiC whisker unpurified to the present embodiment gained carries out XRD and SEM detection, and result is as shown in Figure 4,5.
From the XRD figure of Fig. 4 it can be seen that the present embodiment products therefrom is SiC.
It can be seen that gained silicon carbide whisker size a length of 7～10 μm, better crystallinity degree from the SEM figure of Fig. 5.
Embodiment 3
The preparation method of the SiC whisker of the present embodiment, comprises the following steps:
1) taking grain diameter less than the life coal of 50 μm is carbon source, and taking tetraethyl orthosilicate is silicon source, according to rubbing of carbon and silicon
That, than the ratio for 5:1, obtains unformed SiO by sol-gal process2The presoma of parcel coal particles；
2) under the pressure of 100MPa, by step 1) gained presoma is pressed into a diameter of 32mm, and thickness is 25mm
Slice of cylinder, and imbed and be placed with in the alumina crucible of quartz sand, crucible is placed in the multimode cavity that frequency is 2.45GHz
In microwave oven, add insulation construction, in the case of unprotect atmosphere, carry out microwave sintering synthetic reaction:
First turn on microwave source, regulate microwave input power, first with the ramp of 15 DEG C/min to 620 DEG C i.e. dehumidifying stage
Terminate, regulate input power, then with the ramp of 200 DEG C/min to 1700 DEG C, monitor reflection power simultaneously, be incubated 40min,
Products therefrom is subsphaeroidal nucleocapsid structure, and specifically with embodiment 1, whisker grows in shell, shell separated external crystal sand with
The directly contact of whisker；Silicon carbide whisker is taken out in shell, obtains silicon carbide whisker.
Gained silicon carbide whisker is carried out purification processes, and concrete operations are: in air atmosphere, by products therefrom at 700 DEG C
Under the conditions of calcine 2h, to remove unnecessary carbon, recycling levitation method separation silicon carbide whisker and granule, obtain high-quality,
The silicon carbide whisker of purification.
In the present embodiment, obtain unformed SiO by sol-gal process2The method of the presoma of parcel coal particles includes following
Step:
A) with the ratio that volume ratio is 23:35:50 of distilled water, three is mixed according to tetraethyl orthosilicate, ethanol, use Fructus Citri Limoniae
Acid for adjusting pH is 4, stirs 1h, obtain mixture A under the conditions of 40 DEG C；
B) in mixture A, add coal, under the conditions of 40 DEG C, stir 1h, be 9 with ammonia regulation pH, continue stirring
0.5h, obtains mixture B；
C) with sucking filtration machine, mixture B is carried out sucking filtration, take filter cake, be dried under the conditions of 30 DEG C, obtain unformed SiO2Bag
Wrap up in the presoma of coal particles.
SiC whisker unpurified to the present embodiment gained carries out XRD and SEM detection, and result is as shown in Figure 6,7.
From the XRD figure of Fig. 6 it can be seen that the present embodiment products therefrom is SiC.
It can be seen that gained silicon carbide whisker size a length of 10～20 μm from the SEM figure of Fig. 7, draw ratio is high, crystallization
Spend.
Claims (7)
1. the preparation method of a SiC whisker, it is characterised in that: comprise the following steps:
1) take carbon source and presoma is made in silicon source；
2) by step 1) after gained presoma tabletted, in embedment quartz sand, carry out microwave sintering synthetic reaction, to obtain final product；
Step 1) in, by the method that carbon source and silicon source make presoma it is: carbon source and silicon source are prepared by sol-gal process
Become the presoma of amorphous silica parcel carbon source；Described carbon source is coal；Described silicon source is esters of silicon acis；
Carbon source and silicon source are prepared as the presoma of amorphous silica parcel carbon source by sol-gal process, including following step
Rapid:
A) take esters of silicon acis, ethanol mixes with water, and regulation pH is 3～4, and stirring obtains mixture A；
B) adding carbon source in mixture A, stirring, regulation pH is 8～9, obtains mixture B；
C) mixture B is filtered, take filter cake, be dried, obtain Silica-coated carbon source presoma.
The preparation method of SiC whisker the most according to claim 1, it is characterised in that: step 1) in, according to carbon with
The mol ratio of silicon is the ratio of 3～7.5:1, and carbon source and silicon source are made presoma.
The preparation method of SiC whisker the most according to claim 1, it is characterised in that: in step a), esters of silicon acis,
Ethanol is 23:35:50 with the volume ratio of water.
The preparation method of SiC whisker the most according to claim 1, it is characterised in that: in step a), use Fructus Citri Limoniae
Acid for adjusting pH is 3～4；In step b), using ammonia regulation pH is 8～9.
The preparation method of SiC whisker the most according to claim 1, it is characterised in that: step 2) in, described compacting
Pressure be 4～200MPa.
The preparation method of SiC whisker the most according to claim 1, it is characterised in that: step 2) in, described quartz
Sand is placed in alumina crucible.
The preparation method of SiC whisker the most according to claim 1, it is characterised in that: step 2) in, described microwave
Sintering synthetic reaction is the mode using microwave sintering, first with the ramp of 5～20 DEG C/min to 580～620 DEG C, and regulation
Input power, then with the ramp of 20～200 DEG C/min to 1000～1700 DEG C, it is incubated 5～120min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410401688.4A CN104328478B (en) | 2014-08-14 | 2014-08-14 | A kind of preparation method of SiC whisker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410401688.4A CN104328478B (en) | 2014-08-14 | 2014-08-14 | A kind of preparation method of SiC whisker |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104328478A CN104328478A (en) | 2015-02-04 |
| CN104328478B true CN104328478B (en) | 2016-08-31 |
Family
ID=52403282
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410401688.4A Active CN104328478B (en) | 2014-08-14 | 2014-08-14 | A kind of preparation method of SiC whisker |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104328478B (en) |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105502400B (en) * | 2015-12-03 | 2017-08-22 | 郑州大学 | A kind of B4The preparation method of C whiskers |
| CN105859298B (en) * | 2016-03-29 | 2018-09-18 | 郑州大学 | A kind of polymer precursor ceramic microwave after-treatment modification method |
| 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 |
| CN110387583A (en) * | 2018-04-18 | 2019-10-29 | 郑州航空工业管理学院 | A kind of method and SiC whisker preparing SiC whisker using interfacial reaction |
| CN110745827B (en) * | 2018-07-24 | 2022-02-15 | 郑州航空工业管理学院 | Preparation method of two-dimensional flaky SiC material |
| CN110791810B (en) * | 2018-08-03 | 2021-03-16 | 郑州大学 | Preparation method of silicon carbide crystal |
| CN110483995A (en) * | 2019-09-05 | 2019-11-22 | 安徽省聚科石墨烯科技股份公司 | A kind of graphene heat-conducting plastic and preparation method thereof |
| CN111235636B (en) * | 2020-01-08 | 2021-06-04 | 黑龙江冠瓷科技有限公司 | Preparation method of dendritic SiC whisker |
| CN111392730B (en) * | 2020-04-22 | 2022-08-30 | 扬州市汀月科技有限公司 | Method for preparing silicon carbide whisker by combining fluidized bed with carbothermic reduction reaction and application thereof |
| CN113307611A (en) * | 2021-06-30 | 2021-08-27 | 中国建筑材料工业地质勘查中心宁夏总队 | Method for preparing SiC whiskers by adopting coal slime |
| CN113718370B (en) * | 2021-09-14 | 2023-08-18 | 郑州航空工业管理学院 | Preparation method of hollow silicon carbide fiber |
| CN114436674B (en) * | 2022-02-11 | 2023-04-11 | 洛阳理工学院 | Preparation method of network-like silicon carbide fiber |
| CN114804904B (en) * | 2022-05-09 | 2023-07-11 | 中国有色桂林矿产地质研究院有限公司 | Silicon carbide whisker modified boron nitride composite material, preparation method and application thereof, boron nitride composite body and preparation method thereof |
| CN115094287B (en) * | 2022-06-22 | 2023-05-05 | 齐鲁工业大学 | Laminated metal ceramic cutter material with self-generated micro-texture surface and preparation method thereof |
| CN115231572A (en) * | 2022-07-20 | 2022-10-25 | 郑州航空工业管理学院 | Preparation method of nano titanium carbide powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1449994A (en) * | 2003-05-09 | 2003-10-22 | 西安科技学院 | Industrial preparation method for silica carbide crystal whisker and micropowder |
| CN102373505A (en) * | 2010-08-17 | 2012-03-14 | 深圳大学 | Microwave preparation method of silicon carbide nano wire |
| CN102897763A (en) * | 2012-10-08 | 2013-01-30 | 北京科技大学 | Low-temperature rapid synthesis method of alpha-SiC micropowder |
-
2014
- 2014-08-14 CN CN201410401688.4A patent/CN104328478B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1449994A (en) * | 2003-05-09 | 2003-10-22 | 西安科技学院 | Industrial preparation method for silica carbide crystal whisker and micropowder |
| CN102373505A (en) * | 2010-08-17 | 2012-03-14 | 深圳大学 | Microwave preparation method of silicon carbide nano wire |
| CN102897763A (en) * | 2012-10-08 | 2013-01-30 | 北京科技大学 | Low-temperature rapid synthesis method of alpha-SiC micropowder |
Non-Patent Citations (6)
| Title |
|---|
| F. J. GARZA-MENDEZ,et al..Síntesis de whiskers de SiC asistida por microondas.《Boletín de la Sociedad Españ * |
| ola de Cerámica y Vidrio》.2013,第52卷(第3期), * |
| Silicon Carbide Whiskers: Preparation and High Dielectric Permittivity;Jianlei Kuang，et al.;《J. Am. Ceram. Soc.》;20131231;第96卷(第9期);第2877-2880页 * |
| 微波加热焦碳与石英砂合成SiC粉体;王福等;《材料工程》;20091231(第7期);第32-35页 * |
| 微波烧结制备碳化硅晶须的影响因素;郝斌等;《材料热处理学报》;20130831;第1-5页 * |
| 碳化硅纳米晶须的微波合成;戴长红等;《物理化学学报》;19970430;第13卷(第4期);第380-384页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104328478A (en) | 2015-02-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104328478B (en) | A kind of preparation method of SiC whisker | |
| Wang et al. | Effects of different aluminum sources on morphologies and properties of ceramic floor tiles from red mud | |
| CN103013442B (en) | Alpha-alumina-based abrasive and preparation method thereof | |
| CN1210204C (en) | Method for preparing silicon-carbide | |
| CN102583411B (en) | Method for producing mullite by using fly ash | |
| CN101348324A (en) | Non-transparent quartz crucible for polysilicon crystallization and manufacturing method thereof | |
| CN102674381A (en) | Method for preparing nano mullite powder from coal-based kaolin | |
| CN106276960A (en) | A kind of method of flyash microwave alkali fusion Hydrothermal Synthesis faujasite | |
| CN104947179A (en) | Method for preparing calcium sulfate whiskers | |
| CN108866678A (en) | A method of continuous alumina fiber is prepared by gangue | |
| CN102304750A (en) | Method for synthesizing mullite whiskers | |
| CN101045557A (en) | Preparation method of zirconium tetrachloride | |
| Liu et al. | Recycling photovoltaic silicon waste for fabricating porous mullite ceramics by low-temperature reaction sintering | |
| CN104894636A (en) | Preparation method of potassium octatitanate whisker | |
| CN110387583A (en) | A kind of method and SiC whisker preparing SiC whisker using interfacial reaction | |
| CN107487785A (en) | A kind of preparation technology of zirconium chloride | |
| CN102230223B (en) | Method for preparing magnesium potassium titanate by directly utilizing magnesium oxide | |
| CN105088345A (en) | Preparation method for utilizing desert sand to synthesize mullite whiskers at low temperature | |
| CN106064936A (en) | A kind of preparation method of high-purity mullite ceramic material | |
| CN113233877A (en) | Sodium removal method for calcining alpha alumina | |
| CN101486490B (en) | Preparation of refined zirconium tetrachloride | |
| CN105036136B (en) | A kind of preparation method of nanometer silicon carbide porous material | |
| CN103979787A (en) | Method for preparing mineral wool by using high-calcium coal ash | |
| CN106518035A (en) | Method for preparing high-purity mullite powder through modified fly ash at high yield | |
| Li et al. | Densification behavior of mullite-Al2TiO5 composites by reaction sintering of natural andalusite and TiO2 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |