CN104418608B - The easy fired method of carborundum porous ceramics - Google Patents
The easy fired method of carborundum porous ceramics Download PDFInfo
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Abstract
The present invention relates to a kind of easy fired method of carborundum porous ceramics, described method includes: aluminium oxide or its presoma and boron oxide or its presoma mixed homogeneously as the primary raw material of described adjuvant for combustion with silicon carbide powder, compressing prepared biscuit；And the described dried temperature programming of biscuit burns till between 1100～1400 DEG C, prepare described carborundum porous ceramics.The method of the present invention utilizes aluminium oxide or its presoma and boron oxide or its presoma as the primary raw material of described adjuvant for combustion, burn till after it is mixed with carborundum, utilize the Alborex M 12 that sintering process situ produces as adjuvant for combustion, burning till of carborundum can be carried out in relatively low temperature, and the carborundum porous ceramics porosity prepared is big, intensity is high.
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 coefficient of expansion is little, thermal conductivity is big, hardness is high, tool
There are certain chemical resistance and non-oxidizability strong, are widely used in precision bearing, sealing member, gas-turbine rotor, nozzle
Heat exchanger component and atomic heat pile materials etc..Carborundum is the diffusion when sintering of covalent bond compound, carbon and silicon atom
Speed is the lowest, is difficult to the sintering processing with ionic bond bond material is conventional and is sintered.Although pure SiC powder can pass through hot pressing
Reach fine and close, but require more than the temperature of 2000 DEG C and the pressure more than 35MPa.Therefore, firing temperature and burning how are reduced
One-tenth pressure, and keep the premium properties of silicon carbide ceramics as far as possible, the always important theme of silicon carbide ceramics research.
In addition to being used widely with the form of ceramic of compact, carborundum porous ceramics is at high temperature air filtration, metallurgy
The aspects such as filtration and sensor are also widely applied.Carborundum porous ceramics the most all has the spy of high porosity and high permeability
Point, and there is good thermal shock resistance and mechanical behavior under high temperature.Equally, process for calcining is also that carborundum porous ceramics grinds
Study carefully and the emphasis of exploitation.
Carborundum porous ceramics uses the sintering processing of atmospheric low-temperature mostly, to ensure the high porosity after burning till.By adding
Add adjuvant for combustion, especially can low-temp reaction or melted adjuvant for combustion, it is possible to make the firing temperature of carborundum porous ceramics reduce
To less than 1500 DEG C.Silicates mineral and category of glass material are conventional adjuvant for combustion.Such as, with can generate cordierite and
The raw mineral materials of mullite, as adjuvant for combustion, can burn till the silicon carbide porous of high porosity, high intensity at about 1400 DEG C
Pottery.It addition, utilize carborundum powder surface silicon oxide layer generate glass state material, be also carborundum porous ceramics burn till one
The mode of kind.
The chemical composition of Alborex M 12 typically can be expressed as xAl2O3·yB2O3.Its kind is more, common are
9Al2O3·2B2O3、2Al2O3·B2O3And Al2O3·B2O3Three kinds of forms.Al2O3·B2O3It is present in natural minerals,
9Al2O3·2B2O3And 2Al2O3·B2O3It is then manufactured products.Wherein 9Al2O3·2B2O3Whisker has the performance of excellence, industry
Upper widely used Alborex M 12 is substantially 9Al2O3·2B2O3Whisker.
Aluminium borate whisker has a higher elastic modelling quantity, and good mechanical strength, thermostability, chemical resistance,
Electrical insulating property and neutron-absorbing performance, be mainly used in Metal Substrate and plastic composite, plays potentiation.
The thermal coefficient of expansion of Alborex M 12 material is about 4.2 × 10-6/ K is suitable with carbofrax material.Alborex M 12 material and carborundum
Material equally has the mechanical strength of excellence, and has the elastic modelling quantity higher than carbofrax material.But, the fusing point of Alborex M 12
It is about 1420 DEG C, the lowest carborundum of sintering temperature.Therefore, the agglutinant with Alborex M 12 as carborundum, or by boric acid
Aluminum and silicon carbide compound, it is expected to prepare the material that high-temperature behavior is excellent with relatively low firing temperature.
Just there is United States Patent (USP) introduction to prepare carborundum ceramic of compact (US Patent with Alborex M 12 for adjuvant for combustion as far back as 1984
4,487,734), firing temperature is 1700～2300 DEG C.But this patent uses pre-synthesis boric acid aluminium powder to be raw material.And
Think and can only obtain, for raw material, the silicon carbide ceramics that density is relatively low with aluminium oxide and boron oxide.Within 2006, Chinese patent discloses " one
Plant aluminium borate composite porous ceramics and preparation method thereof " (China Patent Publication No. CN1730427A).This patent is with aluminum contained compound
Fine powder and boric acid powder are the initiation material of Alborex M 12, with the one in corundum, mullite, Alumina, magnesia and magnesium aluminate spinel or
Multiple particulate matter is aggregate.
Summary of the invention
The problems referred to above existed in the face of prior art, the present invention provides a kind of and newly prepares carborundum with Alborex M 12 for adjuvant for combustion
The method of porous ceramics, i.e., while burning till carborundum using reaction in-situ generate Alborex M 12 as adjuvant for combustion.This side
Method can prepare carborundum porous ceramics at a lower temperature, and gained carborundum porous ceramics has, and porosity is big, intensity
High feature.
Here, the present invention provides a kind of method preparing carborundum porous ceramics for adjuvant for combustion with Alborex M 12, described method
Including:
Aluminium oxide or its presoma and boron oxide or its presoma are mixed as the primary raw material of described adjuvant for combustion with silicon carbide powder
Uniformly, compressing prepared biscuit；And
The dried temperature programming of described biscuit is burnt till between 1100～1400 DEG C, prepares described carborundum porous ceramics.
The method of the present invention utilizes main as described adjuvant for combustion of aluminium oxide or its presoma and boron oxide or its presoma
Raw material, burns till after it being mixed with carborundum, utilize the Alborex M 12 that sintering process situ produces as adjuvant for combustion, can
Carry out burning till of carborundum in relatively low temperature, and the carborundum porous ceramics porosity prepared is big, intensity is high.
It is preferred that the mol ratio of aluminium element and boron element can be 10～2:1, especially preferably, institute in described adjuvant for combustion
Stating the mol ratio of aluminium element and boron element in adjuvant for combustion can be 9:2.
It is preferred that described adjuvant for combustion also includes that calcium fluoride, described calcium fluoride weight percent in described adjuvant for combustion contain
Amount is 0～20wt%.Interpolation calcium fluoride, as the submember of adjuvant for combustion, can improve the intensity of carborundum porous ceramics.
It is preferred that the consumption of described adjuvant for combustion is silicon carbide powder consumption 0.5～30wt%.
The atmosphere burnt till described in it is preferred that can be air, nitrogen or vacuum.
It is preferred that described temperature programming comprises the steps that
Be warming up to 300～500 DEG C with 1～5 DEG C/min, be incubated 0.5～2 hour, then with 4～50 DEG C/min be warming up to 1100～
1400 DEG C are incubated 0.5～3 hour.
Accompanying drawing explanation
Fig. 1 illustrates XRD figure spectrum (* labelling belongs to Alborex M 12 diffraction maximum) of carborundum porous ceramics；
Fig. 2 illustrates that the apparent porosity of sample prepared by embodiment 1 and embodiment 2 and bending strength compare.
Detailed description of the invention
Further illustrate the present invention below in conjunction with accompanying drawing and following detailed description of the invention, it should be appreciated that following embodiment and/or
Accompanying drawing is merely to illustrate the present invention, and the unrestricted present invention.
The present invention introduces a kind of method preparing carborundum porous ceramics for adjuvant for combustion with Alborex M 12.This method can be
Burn till carborundum porous ceramics under lower temperature (lower temperatures of such as about 1200 DEG C), and gained silicon carbide porous is made pottery
Porcelain has the feature of high porosity and high intensity.
The technical solution used in the present invention:
1. material choice
Primary raw material with carborundum powder as carborundum porous ceramics, maybe can generate the compound (aluminium oxide of aluminium oxide with alumina powder
Presoma), boron oxide maybe can generate the main component that compound (boron oxide presoma) is adjuvant for combustion of boron oxide, root
The calcium fluoride submember as adjuvant for combustion can be added according to needs.
The selection of carborundum powder mainly considers its particle size and its distribution.The carborundum powder that granularity is the biggest and particle size distribution is the narrowest
More be conducive to preparation large aperture and the porous ceramics of high permeability.
The raw material generating Alborex M 12 can be alumina powder and boron oxide powder, it is also possible to is its predecessor, i.e., can generate
Aluminium oxide and the compound of boron oxide, such as aluminium hydroxide, aluminum isopropylate., boric acid etc..The crystalline phase of alumina powder does not the most limit.
Use different raw materials that porosity and the intensity of carborundum porous ceramics are had certain impact.The chemical composition of Alborex M 12 with
9Al2O3·2B2O3It is preferred.But, the composition of Alborex M 12 is not limited to this, it is true that the mol ratio of aluminium element and boron element exists
10～2:1 all can obtain good sintering effect.
Add calcium fluoride and can significantly improve the sintering effect of carborundum porous ceramics, therefore can burn till into as auxiliary
Point.Its consumption be can Alborex M 12 weight 0～20%.
The consumption of adjuvant for combustion requires to be as the criterion with the intensity and porosity meeting carborundum porous ceramics.General Alborex M 12 consumption
For carborundum powder weight 0.5～30%.Adjuvant for combustion should mix homogeneously, and granularity is the thinnest more is conducive to burning till.
2. moulding process
Carborundum powder, sintering aid mix by a certain percentage, add the shaping assistants such as appropriate cellulose or polyvinyl acetate, mixing
Uniformly.Then according to forming requirements, in said mixture, add appropriate water, obtain through techniques such as mixing, old, mud refinings
To blank.
Blank, by mode molding such as compacting, extrusions, is prepared lamellar, strip, tubulose and the satisfied application such as cellular and is wanted
The shape asked.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 configured to solution/breast
Liquid adds.Shaping assistant adds through pulverizing or being configured to solution/emulsion, is conducive to obtaining the blank of stable in properties.
3. firing process
Base substrate, through dried, burns till according to certain temperature increasing schedule.Temperature increasing schedule mainly consider the decomposition of shaping assistant and pore creating material with
Get rid of, blank cracking the situation such as avoid.Firing temperature is between 1100～1400 DEG C.In a preferred example, can
Use following heating schedule: be warming up to 300～500 DEG C with 1～5 DEG C/min, be incubated 0.5～2 hour, then with 4～50 DEG C/minute
Clock is warming up to 1100～1400 DEG C and is incubated 0.5～3 hour.Firing atmosphere can be air, nitrogen or vacuum.Experiment shows,
The firing temperature using about 1200 DEG C can be obtained by porosity and all good carborundum porous ceramics of intensity.Temperature is burnt till at this
Under degree, even if burning till in air atmosphere, the oxidized speed of carborundum powder is the lowest, therefore in prepared carborundum porous ceramics two
The content of silicon oxide greatly reduces, so that its premium properties is guaranteed.
4. test analysis:
For the sample of test, 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 carborundum and Alborex M 12, illustrates under the firing condition of the present invention, boric acid
Aluminum can efficiently generate.
The percent opening of sample, bulk density use Archimedes method to measure, and mechanical strength three-point bending resistance intensity characterizes.
Seeing Fig. 2, the carborundum porous ceramics porosity that the present invention prepares is high, and apparent porosity is up to more than 40%；Bending strength
Height, up to 25Mpa, after adding calcium fluoride, bending strength can further improve to more than 40Map.
Thermal shock resistance test method: put into by sample in the electric furnace that temperature is 800 DEG C, is incubated 20min, puts immediately after taking-up
It is cooled to room temperature in room temperature water or in air, is a thermal cycle.Sample takes out from water, dries, and a part of sample is used
In bending strength test, another part sample repeats said process, carries out repeatedly thermal cycling test.With air as cooling medium
Time, sample is even across the thermal cycle of more than 7 times, and its bending strength also keeps constant.During with water for cooling medium, first
After secondary thermal cycle, the bending strength of sample is decreased obviously, such as, be reduced to 17MPa by 37MPa；Second time and more times
Thermal cycle after, the bending strength of sample do not continue to reduce.
Citing embodiment is to describe the present invention in detail further below.It will similarly be understood that following example are served only for this
Bright it is further described, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential improvement and adjustment that foregoing is made belong to protection scope of the present invention.Temperature that following example is concrete,
Time etc. are the most only examples in OK range, i.e., those skilled in the art can do suitable model by explanation herein
Enclose interior selection, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
With 320 darkish eye carborundum powders for porous ceramics aggregate, the rising as Alborex M 12 with alpha-alumina (median 0.4 μm) and boric acid
Beginning raw material.First by aluminium oxide and boric acid according to the weight ratio co-grinding of 0.788:0.212, it is configured to adjuvant for combustion.Then will
95g carborundum powder is mixed homogeneously with 5g adjuvant for combustion, adds appropriate 2% (weight) Gonak as molding
Auxiliary agent, mix homogeneously.(pressure is 60MPa) long 32mm, thick 5mm, wide about 7mm is suppressed with this mixture
Strip base substrate.After body drying, in electric furnace, it is warming up to 400 DEG C with the speed of 2 DEG C/h, is incubated 1h；Then with 4 DEG C/h's
Speed is warming up to 1300 DEG C, is incubated 2h.Sample after burning till is for the test of properties.
XRD analysis shows, the principal crystalline phase of sample is carborundum and Alborex M 12, as shown in Figure 1.Illustrate at this firing condition
Under, Alborex M 12 can efficiently generate.
Embodiment 2
Prepare carborundum porous ceramics by the method for example 1, in adjuvant for combustion, simply add calcium fluoride.Calcium fluoride is in adjuvant for combustion
Percentage by weight be 10%.Calcium fluoride crystal should grind to form fine powder in advance, then mixs homogeneously with alumina powder, boric acid powder.
Fig. 2 is the perforate porosity and the comparison of bending strength of sample prepared by example 1 and example 2.Test tables of data
Bright, example 2 sample is close with the apparent porosity of example 1 sample, but its bending strength is much higher than the latter.It is visible,
After adding calcium fluoride component in adjuvant for combustion, the sintering effect of carborundum porous ceramics significantly improves.
Embodiment 3
Preparing carborundum porous ceramics base substrate by the method for example 2, simply process for calcining is: after body drying, with 2 DEG C in electric furnace
The speed of/h is warming up to 400 DEG C, is incubated 30mim；Then open vacuum pump and the vacuum of electric furnace be down to 90%, then with
The speed of 50 DEG C/min is warming up to 1200 DEG C, is incubated 30min.
The bending strength of sample as prepared by example 3 is 20.23MPa, and density is 1.67g/cm3, apparent porosity is
45.51%。
Industrial applicability: the low preparation cost of method of the present invention, quick, economic, the carborundum porous ceramics hole of preparation
Rate is high, intensity is high, is expected to be used widely at aspects such as high temperature air filtration, metallurgical filtration and sensors.
Claims (6)
1. the method preparing carborundum porous ceramics for adjuvant for combustion with Alborex M 12, it is characterised in that described method includes:
Aluminium oxide or its presoma and boron oxide or its presoma are mixed homogeneously as the primary raw material of described adjuvant for combustion with silicon carbide powder, compressing prepared biscuit；And
The dried temperature programming of described biscuit is burnt till between 1100～1400 DEG C, prepares described carborundum porous ceramics；Described adjuvant for combustion also includes that calcium fluoride, described calcium fluoride weight percentage in described adjuvant for combustion are 10 ~ 20wt%.
Method the most according to claim 1, it is characterised in that in described adjuvant for combustion, the mol ratio of aluminium element and boron element is 10～2: 1.
Method the most according to claim 2, it is characterised in that in described adjuvant for combustion, the mol ratio of aluminium element and boron element is 9:2.
Method the most according to claim 1, it is characterised in that the consumption of described adjuvant for combustion is the 0.5～30wt% of silicon carbide powder consumption.
Method the most according to claim 1, it is characterised in that described in the atmosphere burnt till be air, nitrogen or vacuum.
6. according to the method according to any one of Claims 1 to 5, it is characterised in that described temperature programming includes:
It is warming up to 300～500 DEG C with 1～5 DEG C/min, is 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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| 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 |
| 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 |
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| CN1323051C (en) * | 2005-06-20 | 2007-06-27 | 武汉科技大学 | Aluminium borate composite porous ceramics and its preparation method |
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