CN104418608A - Low-temperature sintering method of silicon carbide porous ceramic - Google Patents
Low-temperature sintering method of silicon carbide porous ceramic Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 63
- 239000000919 ceramic Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 31
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000009766 low-temperature sintering Methods 0.000 title abstract 2
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 claims abstract description 29
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 229910052810 boron oxide Inorganic materials 0.000 claims abstract description 11
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000015895 biscuits Nutrition 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000748 compression moulding Methods 0.000 claims abstract description 3
- 239000002671 adjuvant Substances 0.000 claims description 34
- 238000002485 combustion reaction Methods 0.000 claims description 34
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 12
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000005245 sintering Methods 0.000 abstract description 14
- 239000002243 precursor Substances 0.000 abstract description 6
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000000654 additive Substances 0.000 abstract 2
- 230000000996 additive effect Effects 0.000 abstract 2
- 239000000843 powder Substances 0.000 description 22
- 239000000463 material Substances 0.000 description 14
- 238000010304 firing Methods 0.000 description 11
- 238000005452 bending Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 6
- 239000004327 boric acid Substances 0.000 description 6
- 238000007493 shaping process Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005382 thermal cycling Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910021418 black silicon Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229940084936 gonak Drugs 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- -1 silicon carbide compound Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
- Ceramic Products (AREA)
Abstract
The invention relates to a low-temperature sintering method of silicon carbide porous ceramic. The method includes following steps: mixing aluminum oxide or a precursor thereof and boron oxide or a precursor thereof which are used as main raw materials of a sintering additive and silicon carbide powder uniformly and performing compression moulding to obtain a biscuit; drying the biscuit; and sintering the biscuit through a programmed temperature-increasing operation to 1100-1400 DEG C to obtain the silicon carbide porous ceramic. In the invention the aluminum oxide or the precursor thereof and the boron oxide or the precursor thereof are used as the main raw materials and are mixed with the silicon carbide to sintering the silicon carbide porous ceramic. By means of in-situ generated aluminium borate during the sintering process as the sintering additive, the silicon carbide porous ceramic can be sintered at a low temperature. The silicon carbide porous ceramic is high in porosity and is high in strength.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, be specifically related to the easy fired method of carborundum porous ceramics.
Background technology
Silicon carbide ceramics has excellent mechanical behavior under high temperature, and thermal expansivity is little, thermal conductivity is large, hardness is high, there is certain chemical resistance and oxidation-resistance strong, be widely used in precision bearing, sealing member, gas-turbine rotor, nozzle heat exchanger component and atonic heat capacity reactor materials etc.Silicon carbide is covalent linkage compound, and carbon and the Siliciumatom rate of diffusion when sintering is very low, and the sintering processing be difficult to ionic linkage bond material is commonly used sinters.Although pure SiC powder can reach fine and close by hot pressing, need the temperature more than 2000 DEG C and the pressure more than 35MPa.Therefore, how to reduce firing temperature and burn till pressure, and keeping the premium properties of silicon carbide ceramics as far as possible, be the important theme of silicon carbide ceramics research always.
Except being used widely with the form of ceramic of compact, carborundum porous ceramics is also widely applied in high temperature air filtration, metallurgical filtration and sensor.Carborundum porous ceramics all has the feature of high porosity and high permeability usually, and has good thermal shock resistance and mechanical behavior under high temperature.Equally, process for calcining is also the emphasis of carborundum porous ceramics research and development.
Carborundum porous ceramics adopts the sintering processing of atmospheric low-temperature mostly, to ensure the high porosity after burning till.By adding adjuvant for combustion, especially can low-temp reaction or melting adjuvant for combustion, the firing temperature of carborundum porous ceramics can be made to be reduced to less than 1500 DEG C.Silicates mineral and category of glass material are conventional adjuvant for combustion.Such as, so that the raw mineral materials of trichroite and mullite can be generated as adjuvant for combustion, the carborundum porous ceramics of high porosity, high strength can be burnt till at about 1400 DEG C.In addition, utilizing the silicon oxide layer on carborundum powder surface to generate glass state material, is also a kind of mode that carborundum porous ceramics burns till.
The chemical constitution of aluminum borate generally can be expressed as xAl
2o
3yB
2o
3.Its kind is more, common are 9Al
2o
32B
2o
3, 2Al
2o
3b
2o
3and Al
2o
3b
2o
3three kinds of forms.Al
2o
3b
2o
3be present in natural mineral, 9Al
2o
32B
2o
3and 2Al
2o
3b
2o
3be then manufactured products.Wherein 9Al
2o
32B
2o
3whisker has excellent performance, and industrial widely used aluminum borate is 9Al substantially
2o
32B
2o
3whisker.
Aluminium borate whisker has higher Young's modulus, and good physical strength, thermotolerance, chemical resistance, electrical insulating property and neutron-absorbing performance, is mainly used in metal matrix and plastics composite, plays enhancement.
The thermal expansivity of aluminum borate material is about 4.2 × 10
-6/ K is suitable with carbofrax material.Aluminum borate material is the same with carbofrax material has excellent physical strength, and has the Young's modulus higher than carbofrax material.But, the fusing point of aluminum borate is about 1420 DEG C, the greatly low silicon carbide of sintering temperature.Therefore, take aluminum borate as the agglutinant of silicon carbide, or by aluminum borate and silicon carbide compound, be expected to prepare the excellent material of high-temperature behavior with lower firing temperature.
Just had United States Patent (USP) introduction to be that adjuvant for combustion prepares silicon carbide ceramic of compact (US Patent4,487,734) with aluminum borate as far back as 1984, firing temperature is 1700 ~ 2300 DEG C.But this patent uses pre-synthesis boric acid aluminium powder to be raw material.And think with aluminum oxide and boron oxide for raw material can only obtain the lower silicon carbide ceramics of density.Within 2006, Chinese patent discloses " a kind of aluminium borate composite porous ceramics and preparation method thereof " (China Patent Publication No. CN1730427A).The starting raw material that this patent is aluminum borate with aluminum contained compound fine powder and boric acid powder, with one or more particulate matter in corundum, mullite, alumina, magnesia and magnesium-aluminium spinel for aggregate.
Summary of the invention
In the face of the problems referred to above that prior art exists, the invention provides a kind of new be the method that adjuvant for combustion prepares carborundum porous ceramics with aluminum borate, namely, the aluminum borate that generates while burning till silicon carbide using reaction in－situ is as adjuvant for combustion.This method can prepare carborundum porous ceramics at a lower temperature, and gained carborundum porous ceramics has porosity is large, intensity is high feature.
At this, the invention provides a kind of take aluminum borate as the method that adjuvant for combustion prepares carborundum porous ceramics, and described method comprises:
Mixed with silicon carbide powder by aluminum oxide or its presoma and boron oxide or its presoma main raw material as described adjuvant for combustion, compression moulding obtains biscuit; And
Burn till between temperature programming to 1100 ~ 1400 DEG C after described biscuit drying, obtained described carborundum porous ceramics.
Method of the present invention utilizes aluminum oxide or its presoma and boron oxide or its presoma as the main raw material of described adjuvant for combustion, burn till after it is mixed with silicon carbide, utilize aluminum borate that sintering process situ produces as adjuvant for combustion, can carry out burning till of silicon carbide in lower temperature, and obtained carborundum porous ceramics porosity is large, intensity is high.
Preferably, in described adjuvant for combustion, the mol ratio of aluminium element and boron can be 10 ~ 2:1, and especially preferably, in described adjuvant for combustion, the mol ratio of aluminium element and boron can be 9:2.
Preferably, described adjuvant for combustion also comprises Calcium Fluoride (Fluorspan), and the weight percentage of described Calcium Fluoride (Fluorspan) in described adjuvant for combustion is 0 ~ 20wt%.Add Calcium Fluoride (Fluorspan) as the submember of adjuvant for combustion, the intensity of carborundum porous ceramics can be improved.
Preferably, the consumption of described adjuvant for combustion is 0.5 ~ 30wt% of silicon carbide powder consumption.
Preferably, the atmosphere of burning till described in can be air, nitrogen or vacuum.
Preferably, described temperature programming can comprise:
Be warming up to 300 ~ 500 DEG C with 1 ~ 5 DEG C/min, be incubated 0.5 ~ 2 hour, then be warming up to 1100 ~ 1400 DEG C of insulations 0.5 ~ 3 hour with 4 ~ 50 DEG C/min.
Accompanying drawing explanation
Fig. 1 illustrates the XRD figure spectrum (* mark belongs to aluminum borate diffraction peak) of carborundum porous ceramics;
Fig. 2 illustrates that the open porosity of embodiment 1 and sample prepared by embodiment 2 and bending strength compare.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that following embodiment and/or accompanying drawing are only for illustration of the present invention, and unrestricted the present invention.
It take aluminum borate as the method that adjuvant for combustion prepares carborundum porous ceramics that the present invention introduces a kind of.This method can burn till carborundum porous ceramics under lesser temps (such as the lesser temps of about 1200 DEG C), and gained carborundum porous ceramics has the feature of high porosity and high strength.
The technical solution used in the present invention:
1. material choice
Take carborundum powder as the main raw material of carborundum porous ceramics, with the main component that the compound (boron oxide presoma) that aluminum oxide powder maybe can generate the compound (alumina precursor) of aluminum oxide, boron oxide maybe can generate boron oxide is adjuvant for combustion, the submember of Calcium Fluoride (Fluorspan) as adjuvant for combustion can be added as required.
Its particle size and its distribution is mainly considered in the selection of carborundum powder.The carborundum powder that granularity is larger and size-grade distribution is narrower is more conducive to the porous ceramics preparing wide aperture and high permeability.
Generating the raw material of aluminum borate can be aluminum oxide powder and boron oxide powder, also can be its precursor, namely, can generate the compound of aluminum oxide and boron oxide, as aluminium hydroxide, aluminum isopropylate, boric acid etc.The crystalline phase of aluminum oxide powder does not also limit.Different raw materials is used to have certain influence to the porosity of carborundum porous ceramics and intensity.The chemical constitution of aluminum borate is with 9Al
2o
32B
2o
3for good.But, the composition of aluminum borate is not limited to this, and in fact, the mol ratio of aluminium element and boron all can obtain good sintering effect at 10 ~ 2:1.
Add the sintering effect that Calcium Fluoride (Fluorspan) can significantly improve carborundum porous ceramics, therefore can burn till composition as auxiliary.Its consumption be can aluminum borate weight 0 ~ 20%.
The consumption of adjuvant for combustion requires to be as the criterion with the intensity and porosity that meet carborundum porous ceramics.General aluminum borate consumption is 0.5 ~ 30% of carborundum powder weight.Adjuvant for combustion should mix, and granularity more carefully is more conducive to burning till.
2. moulding process
Carborundum powder, sintering aid mix by a certain percentage, then add the shaping assistants such as appropriate Mierocrystalline cellulose or polyvinyl acetate, mix.Then according to forming requirements, in said mixture, add appropriate water, obtain blank through techniques such as mixing, old, mud refinings.
Blank by suppressing, the mode such as to extrude is shaping, prepares sheet, strip, tubulose and the shape meeting application requiring such as cellular.The pressure of compacting can be 0.1 ~ 150MPa.
When preparing blank, shaping assistant can add as raw material, or adds after pulverizing, or is mixed with solution/emulsion and adds.Shaping assistant adds through pulverizing or being mixed with solution/emulsion, is conducive to the blank obtaining stable in properties.
3. firing process
Base substrate, after super-dry, burns till according to certain temperature increasing schedule.Temperature increasing schedule mainly consider the decomposition of shaping assistant and pore-forming material and eliminating, blank cracking the situation such as to avoid.Firing temperature is between 1100 ~ 1400 DEG C.In a preferred example, following heating schedule can be adopted: be warming up to 300 ~ 500 DEG C with 1 ~ 5 DEG C/min, be incubated 0.5 ~ 2 hour, then be warming up to 1100 ~ 1400 DEG C of insulations 0.5 ~ 3 hour with 4 ~ 50 DEG C/min.Firing atmosphere can be air, nitrogen or vacuum.Experiment shows, uses the firing temperature of about 1200 DEG C just can obtain porosity and all good carborundum porous ceramics of intensity.Under this firing temperature, even if burn till in air atmosphere, the oxidized speed of carborundum powder is very low, and therefore in prepared carborundum porous ceramics, the content of silicon-dioxide greatly reduces, thus its premium properties is guaranteed.
4. test analysis:
For the sample tested, also prepare according to above-mentioned condition.Specimen size is long 32mm, wide 7mm, high 5mm.
Crystal phase analysis: smashed to pieces by sample, grinds to form fine powder; The XRD figure spectrum of fine powder is measured with x-ray diffractometer.See Fig. 1, XRD analysis shows, the principal crystalline phase of sample is silicon carbide and aluminum borate, illustrates that, under firing condition of the present invention, aluminum borate can effectively generate.
The percentage of open area of sample, volume density adopt Archimedes method to measure, and physical strength three-point bending resistance intensity characterizes.See Fig. 2, the carborundum porous ceramics porosity that the present invention obtains is high, and open porosity can reach more than 40%; Bending strength is high, can reach 25Mpa, and after adding Calcium Fluoride (Fluorspan), bending strength can further improve to more than 40Map.
Heat-shock resistance test method: sample is put into the electric furnace that temperature is 800 DEG C, insulation 20min, is placed in room temperature water after taking-up immediately or air is cooled to room temperature, is a thermal cycling.Sample takes out from water, oven dry, and a part of sample is used for bending strength test, and another part sample repeats said process, carries out repeatedly thermal cycling test.When taking air as heat-eliminating medium, even if sample is through the thermal cycling of more than 7 times, its bending strength also remains unchanged.When taking water as heat-eliminating medium, after first time thermal cycling, the bending strength of sample obviously declines, such as, be reduced to 17MPa by 37MPa; After second time and more thermal cycling, the bending strength of sample no longer continues to reduce.
Embodiment of illustrating further is below to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The temperature that following example is concrete, time etc. are also only examples in OK range, and namely, those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
With 320 order black silicon carbide powder for porous ceramics aggregate, be the starting raw material of aluminum borate with alpha-aluminium oxide powder (median 0.4 μm) and boric acid.First by aluminum oxide and boric acid according to the weight ratio co-grinding of 0.788:0.212, be mixed with adjuvant for combustion.Then 95g carborundum powder is mixed with 5g adjuvant for combustion, add appropriate 2% (weight) Gonak and, as shaping assistant, mix.The strip base substrate of (pressure is 60MPa) long 32mm, thick 5mm, wide about 7mm is suppressed with this mixture.After body drying, in electric furnace, be warming up to 400 DEG C with the speed of 2 DEG C/h, insulation 1h; Then 1300 DEG C are warming up to the speed of 4 DEG C/h, insulation 2h.Sample after burning till is for the test of properties.
XRD analysis shows, the principal crystalline phase of sample is silicon carbide and aluminum borate, as shown in Figure 1.Illustrate that, under this firing condition, aluminum borate can effectively generate.
Embodiment 2
Prepare carborundum porous ceramics by the method for example 1, just in adjuvant for combustion, add Calcium Fluoride (Fluorspan).The weight percent of Calcium Fluoride (Fluorspan) in adjuvant for combustion is 10%.Calcium fluoride crystal should grind to form fine powder in advance, then mixes with aluminum oxide powder, boric acid powder.
Fig. 2 is example 1 and the perforate void content of sample prepared by example 2 and comparing of bending strength.Test data shows, the open porosity of example 2 sample and example 1 sample is close, but its bending strength is much higher than the latter.Visible, add Calcium Fluoride (Fluorspan) component in adjuvant for combustion after, the sintering effect of carborundum porous ceramics significantly improves.
Embodiment 3
Prepare carborundum porous ceramics base substrate by the method for example 2, just process for calcining is: after body drying, in electric furnace, be warming up to 400 DEG C with the speed of 2 DEG C/h, insulation 30mim; Then open vacuum pump and the vacuum tightness of electric furnace is down to 90%, be then warming up to 1200 DEG C with the speed of 50 DEG C/min, insulation 30min.
Be 20.23MPa by the bending strength of sample prepared by example 3, density is 1.67g/cm
3, open porosity is 45.51%.
Industrial applicability: the low preparation cost of method of the present invention, quick, economic, the carborundum porous ceramics porosity of preparation is high, intensity is high, is expected at high temperature air filtration, metallurgically filters and be used widely in sensor.
Claims (7)
1. be the method that adjuvant for combustion prepares carborundum porous ceramics with aluminum borate, it is characterized in that, described method comprises:
Mixed with silicon carbide powder by aluminum oxide or its presoma and boron oxide or its presoma main raw material as described adjuvant for combustion, compression moulding obtains biscuit; And
Burn till between temperature programming to 1100 ~ 1400 DEG C after described biscuit drying, obtained described carborundum porous ceramics.
2. method according to claim 1, is characterized in that, in described adjuvant for combustion, the mol ratio of aluminium element and boron is 10 ~ 2: 1.
3. method according to claim 2, is characterized in that, in described adjuvant for combustion, the mol ratio of aluminium element and boron is 9:2.
4. the method according to any one of claims 1 to 3, is characterized in that, described adjuvant for combustion also comprises Calcium Fluoride (Fluorspan), and the weight percentage of described Calcium Fluoride (Fluorspan) in described adjuvant for combustion is 0 ~ 20wt%.
5. the method according to any one of Claims 1 to 4, is characterized in that, the consumption of described adjuvant for combustion is 0.5 ~ 30wt% of silicon carbide powder consumption.
6. the method according to any one of Claims 1 to 5, is characterized in that, described in the atmosphere of burning till be air, nitrogen or vacuum.
7. the method according to any one of claim 1 ~ 6, is characterized in that, described temperature programming comprises:
Be warming up to 300 ~ 500 DEG C with 1 ~ 5 DEG C/min, be incubated 0.5 ~ 2 hour, then be warming up to 1100 ~ 1400 DEG C of insulations 0.5 ~ 3 hour with 4 ~ 50 DEG C/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104860698A (en) * | 2015-05-04 | 2015-08-26 | 安徽省亚欧陶瓷有限责任公司 | Impact-resisting ceramic tile and preparation method thereof |
| CN105367108A (en) * | 2015-10-27 | 2016-03-02 | 合肥龙多电子科技有限公司 | Tough and high-elastic composite silicon-carbide-based ceramic circuit board base board material and preparation method thereof |
| CN114956828A (en) * | 2022-05-17 | 2022-08-30 | 合肥商德应用材料有限公司 | Silicon carbide ceramic and preparation method and application thereof |
| CN115745619A (en) * | 2022-11-23 | 2023-03-07 | 广东昊陶科技有限公司 | Silicon carbide composite powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4487734A (en) * | 1983-05-10 | 1984-12-11 | Tdk Corporation | Method for the preparation of a high density sintered body of silicon carbide |
| CN1730427A (en) * | 2005-06-20 | 2006-02-08 | 武汉科技大学 | Aluminium borate composite porous ceramics and its preparation method |
| CN102503538A (en) * | 2011-11-02 | 2012-06-20 | 浙江大学 | Continuously pore-forming silicon carbide ceramic material and preparation method for same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4487734A (en) * | 1983-05-10 | 1984-12-11 | Tdk Corporation | Method for the preparation of a high density sintered body of silicon carbide |
| CN1730427A (en) * | 2005-06-20 | 2006-02-08 | 武汉科技大学 | Aluminium borate composite porous ceramics and its preparation method |
| CN102503538A (en) * | 2011-11-02 | 2012-06-20 | 浙江大学 | Continuously pore-forming silicon carbide ceramic material and preparation method for same |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104860698A (en) * | 2015-05-04 | 2015-08-26 | 安徽省亚欧陶瓷有限责任公司 | Impact-resisting ceramic tile and preparation method thereof |
| CN105367108A (en) * | 2015-10-27 | 2016-03-02 | 合肥龙多电子科技有限公司 | Tough and high-elastic composite silicon-carbide-based ceramic circuit board base board material and preparation method thereof |
| CN114956828A (en) * | 2022-05-17 | 2022-08-30 | 合肥商德应用材料有限公司 | Silicon carbide ceramic and preparation method and application thereof |
| CN114956828B (en) * | 2022-05-17 | 2023-08-15 | 合肥商德应用材料有限公司 | Silicon carbide ceramic and preparation method and application thereof |
| CN115745619A (en) * | 2022-11-23 | 2023-03-07 | 广东昊陶科技有限公司 | Silicon carbide composite powder and preparation method thereof |
| CN115745619B (en) * | 2022-11-23 | 2023-11-17 | 广东昊陶科技有限公司 | Silicon carbide composite powder and preparation method thereof |
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