CN106478110A - A kind of ZrB2The preparation method of SiC composite ceramicses - Google Patents
A kind of ZrB2The preparation method of SiC composite ceramicses Download PDFInfo
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
- C04B35/58064—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
- C04B35/58078—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on zirconium or hafnium borides
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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Abstract
The invention discloses a kind of ZrB2The preparation method of SiC composite ceramicses, its step is as follows:First, batch mixing:By ZrB2Powder, SiC put in ball grinder and are sufficiently mixed, then calcined mixed powder body in a vacuum furnace, obtain ZrB2SiC mixed powder;2nd, molding and the demoulding:In ZrB2Add binding agent in SiC powder, stir, be then charged into carrying out pressure forming in mould, the demoulding from mould, obtain biscuit;3rd, sintering and post processing:Biscuit is lain on high-purity alumina ceramic piece, then puts into sintering, furnace cooling in vacuum sintering furnace together, obtain ZrB2SiC composite ceramicses.ZrB2The preparation of SiC composite ceramicses adopts vaccum sintering process, and ZrB2SiC does not have direct reaction, thus avoiding deviateing component ratio.The ZrB that the present invention prepares2The preparation of SiC composite ceramicses easily operates, and is so effectively improved ratio defective product.
Description
Technical field
The invention belongs to technical field, it is related to a kind of ZrB2The preparation method of-SiC composite ceramicses is and in particular to one kind is adopted
Prepare ZrB with high-temperature vacuum sintering process2The method of-SiC composite ceramicses.
Background technology
ZrB2- SiC composite ceramicses are as superhigh temperature ceramics(Ultra High Temperature Ceramics, referred to as
UHTCs)There iing the advanced ceramic remaining under the harsh environmental conditions such as oxygen atmosphere as usual use more than more than 2000 DEG C.ZrB2Pottery
(zirconium diboride ceramics)It is a kind of common superhigh temperature ceramics, but this material also has a lot of deficiencies
Part, such as:Hard-to-sinter becomes under fine and close sintered body, high temperature easily oxidation and the fragility of itself is easily caused the calamity of component and breaks
Bad.Research shows, adds SiC and can not only improve ZrB2The sintering character of pottery, and improve its antioxygenic property and power
Learn performance.
ZrB2- SiC composite ceramicses oxidation susceptibility more than 1200 DEG C is significantly better than single-phase ZrB2Material.This is because
1200 DEG C about, SiC can aoxidize the silicate forming glass phase, and the borate that on the one hand this can substitute volatilization rises to specimen surface
To protective effect, on the other hand can and boron oxide form that a kind of viscosity is bigger, can more effectively stop the oxygen in environment from entering matrix
Borosilicate.Additionally, adding SiC can also improve ZrB2Sintering character, suppression blapharoplast abnormal growth, thus changing
The mechanics of kind material and ablation, thermal shock resistance properties.ZrB2It is compounded under superhigh temperature excess oxygen with SiC, SiO can be formed on surface2
Glass phase, the passage that healing gas is spread to base material by coating to a certain extent, stop oxidizing gas to matrix material
Inside is spread further, has good antioxygenic property.
The oxidation behaviors of SiC will be converted into actively oxidation by passive oxidation, and its oxidation product will be by composite
There is the SiO of protective effect2It is converted into gaseous SiO.The addition of SiC can significantly improve ZrB2Antioxygenic property.ZrB2-
SiC composite ceramicses oxidation susceptibility more than 1200 DEG C is significantly better than single-phase ZrB2Material.Dominant mechanism is Surface Creation during high temperature
One layer of outer layer richness SiO2Glass and internal layer are rich ZrO2Oxide layer, the glass phase due to outer layer has good surface wettability
And healing properties, the borate that on the one hand this can substitute volatilization plays a protective role to specimen surface, and the rich ZrO generating2Oxygen
Change layer and be even more a kind of typical thermal barrier coatings, can effectively stop outside heat from spreading to material internal, improve high-temperature oxidation resistance
Can, on the other hand can and boron oxide form that a kind of viscosity is bigger, can more effectively stop the oxygen in environment from entering the borosilicic acid of matrix
Salt.Can be used above at 2200 DEG C.Additionally, adding SiC can also improve ZrB2Sintering character, suppression blapharoplast different
Often grow up, thus improving mechanics and ablation, the thermal shock resistance properties of material.Therefore, ZrB2The high-temperature heat-resistance punching of-SiC complex phase ceramic
Hitting property is to evaluate one of good and bad important indicator of its serviceability.
ZrB2- SiC composite ceramicses are current field of new primary study and a kind of new type high temperature heat structure material of exploitation
Material, due to having the advantages that fusing point is high, hardness is high, good conductivity and the preferable Aero-Space that become (aircraft nose cone cap and wing
Thermal protection system of leading edge etc.) and other industrial circles high-temperature material, these applications mainly make under high temperature and aerobic environment
With.
Content of the invention
It is an object of the invention to provide one kind can obtain fully dense ZrB2The preparation method of-SiC composite ceramicses.
The purpose of the present invention is achieved through the following technical solutions:
A kind of ZrB2The preparation method of-SiC composite ceramicses, including material mixing, molding and the demoulding, sintering and three steps of post processing,
Specific implementation step is as follows:
First, batch mixing:By ZrB2Powder, SiC are 1 according to volume ratio:0.2~0.25 ratio is put in ball grinder and is fully mixed
Close, then calcined mixed powder body in a vacuum furnace, obtain ZrB2- SiC mixed powder;
2nd, molding and the demoulding:In ZrB2Add binding agent in-SiC mixed powder, stir, be then charged into carrying out in mould
Pressure forming, the demoulding from mould, obtain biscuit;
3rd, sintering and post processing:Biscuit is lain on high-purity alumina ceramic piece, then puts into together in vacuum sintering furnace and burn
Knot, furnace cooling, obtain ZrB2- SiC composite ceramicses.
As one kind preferably, in described mixing process, the particle diameter of two kinds of raw materials is respectively less than 10 m and the two particle diameter is different, leads to
The method crossing grain composition, obtains optimal mixed effect.
As a kind of preferred, described ZrB2The preparation method of powder is as follows:By ZrO2Powder, B4C powder and C powder according to mol ratio are
2:(1.00~1.10):(3.00 ~ 3.20) or ZrO2Powder, B2O3The mol ratio of powder and C powder is 1:(1.00~1.20):(5.00~
5.20) ratio is put in ball grinder and is sufficiently mixed, then calcined mixed powder body in a vacuum furnace, obtains ZrB2Powder body.
As a kind of preferred, described preparation ZrB2In the mixing process of powder body, the particle diameter of three kinds of raw materials be respectively less than 10 m and
Three's particle diameter is different, by the method for grain composition, obtains optimal mixed effect.
As one kind preferably, described mould is pressure forming die, and pressure forming die is all-metal material, using numerical control
Apparatus processing goes out the required mould of design.
As one kind preferably, described binding agent is PVA binding agent, and its addition is ZrB2- the 1 of SiC mixed powder weight ~
5%.
As a kind of preferred, during described pressure forming, make base to prevent on molding blank binding metal mould
Body ftractures, and all puts into the scraps of paper with depression bar same size in the upper and lower of pressing blank, plays the effect of isolation, mould inner wall table
Face paints stearic acid, Oleic acid etc. as releasing agent, and in the effect of forcing press, pressure is pressurized to 10 ~ 15MPa, and pressurize 5 ~
10min, fully pressurizes.If pressure is excessive, the elastic after effect effect producing during the demoulding easily makes blank cracking.
Preferably, after described biscuit takes out, in room temperature environment, keep 20min as a kind of, abundant release molding is follow-up
Residual pressure.
As one kind preferably, the specific requirement of described sintering is:Vacuum is 10 ~ 30Pa, is entered according to reaction-sintered curve
Row sintering, that is,:1.5 ~ 2h is increased to 1200 ~ 1250 DEG C from room temperature, is then warming up to 1600 DEG C of insulation 1 ~ 2h in 1 ~ 1.5h.
The invention has the advantages that:
1、ZrB2ZrB in-SiC composite ceramicses2Mutually adopt ZrO2Powder, B4C powder and C powder, the B suitably increasing4C powder and C powder mole
Ratio is due to B4C powder and the easy oxidation Decomposition in a vacuum furnace of C powder, thus improve B4C powder and C powder molar ratio, can hold
Obtain the ZrB of stoicheiometry2Powder body.This method is simple, and powder body married operation temperature is room temperature, can carry out more accurate
Control.
2、ZrB2The preparation of-SiC composite ceramicses adopts vaccum sintering process, and ZrB2- SiC does not have direct reaction, thus avoiding
Deviate component ratio.The ZrB that the present invention prepares2The preparation of-SiC composite ceramicses easily operates, and is so effectively improved product
Rate.
Brief description
Fig. 1 is ZrB in embodiment 12- SiC composite ceramicses preparation technology flow chart;
Fig. 2 is ZrB in embodiment 22- SiC composite ceramicses preparation technology flow chart;
Fig. 3 is ZrB2- 20Vol.%SiC composite ceramicses XRD diffracting spectrum(1800℃);
Fig. 4 is ZrB2- 20Vol.%SiC composite ceramicses;
Fig. 5 is ZrB2- 20Vol.%SiC composite ceramicses surface SEM microstructure(1800℃);
Fig. 6 is ZrB2- 20Vol.%SiC pottery fracture SEM microstructure(1800℃).
Specific embodiment
With reference to embodiment, technical scheme is further described, but is not limited thereto, every right
Technical solution of the present invention is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should contain
Cover in protection scope of the present invention.
Embodiment 1:
As shown in figure 1, the present embodiment prepares ZrB in accordance with the following steps2- SiC composite ceramicses:
(1)Batch mixing:Using commercially available ZrO2、B4C, C powder is respectively less than 10 m and three as raw material, the particle diameter of these three raw materials
Particle diameter is different, ZrO2、B4The mol ratio of C, C powder is 2:1:3.Weighing finishes, and they is poured in ball grinder, using ZrO2Carry out
Ball milling mixing 8h, reaches mixed uniformly effect.Mixed powder body heat treatment in a vacuum furnace, the powder body mixing is loaded
In aluminium oxide ceramics cup, put into vacuum sintering furnace, be heated to 1600 DEG C of insulation 1h and calcined, to obtain ZrB2Powder body.
Reaction equation is as follows:
2ZrO2+B4C+3C→2ZrB2+4CO (1)
Using above-mentioned ZrO2-B4The synthetically prepared ZrB of C-C system2With SiC powder as raw material, the particle diameter of both raw materials is
4~10 m and the two particle diameter difference, ZrB2, SiC volume ratio be 1:0.2.Weighing finishes, and they is poured in ball grinder, adopts
Use ZrO2Carry out ball milling mixing 8h, reach mixed uniformly effect.Mixed powder body heat treatment in a vacuum furnace, will mix
Powder body load aluminium oxide ceramics cup in, put into vacuum sintering furnace, be heated to 1600 DEG C insulation 1h calcined, with obtain
ZrB2- SiC mixed powder.
(2)Prepared by mould:Using metal as mold materials, the method using machining prepares a uniaxial pressure gold
Belong to mould.
(3)Compacting:After the material powder mixing is mixed in proportion with PVA, put in metal die, using pressure
Machine loads to mould, and pressure is pressurized to 10MPa, and pressurize 5min, and the addition controlling PVA is ZrB2- SiC mixed powder weight
1%.
(4)Sintering:The demoulding from mould, obtains biscuit, the biscuit preparing is placed on aluminium oxide flat board, then will
Aluminium oxide flat board is put in vacuum sintering furnace together with biscuit, closes fire door, evacuation, vacuum is evacuated to 10 ~ 30Pa.Open
Vacuum-sintering stove heat, temperature process curve is:1.5h is increased to 1200 DEG C from room temperature, is then warming up to 1600 DEG C of insulations in 1h
1h, then 2h cooling, mode is furnace cooling.
(5)Post processing:After furnace temperature drops to room temperature, open vacuum hotpressing stove, take out ZrB2- SiC composite ceramicses.
Fig. 3 is ZrB2- 20Vol.%SiC composite ceramicses XRD diffracting spectrum is it can be seen that ZrB2Do not have in 2 kinds of mixture of-SiC
There is Newly born phase, illustrate do not have new thing phase to generate.Fig. 4 is ZrB2The macro morphology of -20Vol.%SiC composite ceramicses;Fig. 5 is ZrB2-
20Vol.%SiC composite ceramicses surface SEM microstructure(1800℃)Sintered density is higher;Fig. 6 is ZrB2-20Vol.%SiC
Ceramic fracture SEM microstructure(1800℃)It can be seen that the ZrB of sintering2- SiC composite ceramicses hole is less.
Embodiment 2:
As shown in Fig. 2 the present embodiment prepares ZrB in accordance with the following steps2- SiC composite ceramicses:
(1)Batch mixing:
Using commercially available ZrO2、B2O3, C powder as raw material, the particle diameter of these three raw materials is respectively less than 10 m and three's particle diameter not
With ZrO2、B2O3, C powder mol ratio be 1:1.10:5.00.Weighing finishes, and they is poured in ball grinder, using ZrO2Carry out
Ball milling mixing 8h, reaches mixed uniformly effect.
Mixed powder body heat treatment in a vacuum furnace, the powder body mixing is loaded in aluminium oxide ceramics cup, puts into true
Empty sintering furnace, is heated to 1600 DEG C of insulation 1h and is calcined, to obtain ZrB2Powder body.
Reaction equation is as follows:
ZrO2+B2O3+5C→ ZrB2+5CO (2)
Using above-mentioned ZrO2-B2O3The synthetically prepared ZrB of-C system2With SiC powder as raw material, the particle diameter of both raw materials is equal
For 4~10 m and the two particle diameter difference, ZrB2, SiC volume ratio be 1:0.25.Weighing finishes, and they are poured in ball grinder,
Using ZrO2Carry out ball milling mixing 8h, reach mixed uniformly effect.
(2)Prepared by mould:Using metal as mold materials, the method using machining prepares a uniaxial pressure gold
Belong to mould.
(3)Compacting:After the material powder mixing is mixed in proportion with PVA, put in metal die, using pressure
Machine loads to mould, and pressure is pressurized to 10MPa, and pressurize 5min, and the addition controlling PVA is ZrB2- SiC mixed powder weight
1%.
(4)Sintering:The demoulding from mould, obtains biscuit, the biscuit preparing is placed on aluminium oxide flat board, then will
Aluminium oxide flat board is put in vacuum sintering furnace together with biscuit, closes fire door, evacuation, vacuum is evacuated to 10 ~ 30Pa.Open
Vacuum-sintering stove heat, temperature process curve is:1.5h is increased to 1200 DEG C from room temperature, is then warming up to 1600 DEG C of insulations in 1h
1h, then 2h cooling, mode is furnace cooling.
(5)Post processing:After furnace temperature drops to room temperature, open vacuum hotpressing stove, take out ZrB2- SiC composite ceramicses.
Claims (9)
1. a kind of ZrB2The preparation method of-SiC composite ceramicses is it is characterised in that methods described step is as follows:
First, batch mixing:By ZrB2Powder, SiC are 1 according to volume ratio:0.2~0.25 ratio is put in ball grinder and is sufficiently mixed,
Then calcined mixed powder body in a vacuum furnace, obtains ZrB2- SiC mixed powder;
2nd, molding and the demoulding:In ZrB2Add binding agent in-SiC mixed powder, stir, be then charged into being pressed in mould
Power molding, the demoulding from mould, obtain biscuit;
3rd, sintering and post processing:Biscuit is lain on alumina ceramic plate, then puts into sintering in vacuum sintering furnace together,
Furnace cooling, obtains ZrB2- SiC composite ceramicses.
2. ZrB according to claim 12The preparation method of-SiC composite ceramicses is it is characterised in that described ZrB2The preparation of powder
Method is as follows:By ZrO2Powder, B4C powder and C powder are 2 according to mol ratio:(1.00~1.10):(3.00 ~ 3.20) or ZrO2Powder, B2O3
The mol ratio of powder and C powder is 1:(1.00~1.20):The ratio of (5.00 ~ 5.20) is put in ball grinder and is sufficiently mixed, so
Calcined mixed powder body in a vacuum furnace afterwards, obtains ZrB2Powder body.
3. ZrB according to claim 22The preparation method of-SiC composite ceramicses it is characterised in that in described mixing process,
The particle diameter of three kinds of raw materials is respectively less than 10 m and three's particle diameter is different.
4. ZrB according to claim 12The preparation method of-SiC composite ceramicses it is characterised in that in described mixing process,
The particle diameter of two kinds of raw materials is respectively less than 10 m and the two particle diameter is different.
5. ZrB according to claim 12The preparation method of-SiC composite ceramicses is it is characterised in that described mould becomes for pressure
Pattern has.
6. ZrB according to claim 52The preparation method of-SiC composite ceramicses is it is characterised in that described pressure forming die
For all-metal material.
7. ZrB according to claim 12The preparation method of-SiC composite ceramicses is it is characterised in that described binding agent is PVA
Binding agent, its addition is ZrB2The 1 ~ 5% of-SiC mixed powder weight.
8. ZrB according to claim 12The preparation method of-SiC composite ceramicses is it is characterised in that described pressure forming process
In, pressure is pressurized to 10 ~ 15MPa, and pressurize 5 ~ 10min.
9. ZrB according to claim 12The preparation method of-SiC composite ceramicses is it is characterised in that the concrete of described sintering will
Ask for:Vacuum is 10 ~ 30Pa, is sintered according to reaction-sintered curve, that is,:1.5 ~ 2h is increased to 1200 ~ 1250 from room temperature
DEG C, then it is warming up to 1600 DEG C of insulation 1 ~ 2h in 1 ~ 1.5h.
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CN107140988A (en) * | 2017-07-04 | 2017-09-08 | 黑龙江科技大学 | ZrB2SiC ceramic material injection forming sintering method |
CN107176839A (en) * | 2017-05-10 | 2017-09-19 | 黑龙江科技大学 | ZrB2SiC layer shape composite ceramics and preparation method thereof |
CN107311664A (en) * | 2017-07-04 | 2017-11-03 | 黑龙江科技大学 | ZrB2Base SiC strengthens the preparation method of phase ceramics |
CN107353023A (en) * | 2017-08-02 | 2017-11-17 | 武汉科技大学 | A kind of oxidation resistant silicon carbide castable of selfreparing and preparation method thereof |
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