CN104926309B - A kind of without boron or the preparation method of the compact silicon carbide ceramic of rare earth element - Google Patents
A kind of without boron or the preparation method of the compact silicon carbide ceramic of rare earth element Download PDFInfo
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Abstract
The present invention relates to a kind of without boron or the preparation method of the compact silicon carbide ceramic of rare earth element, including: 1) aluminum source, carbon source, silicon carbide powder and dehydrated alcohol uniformly mixed post-drying, grind sieve after obtain mixed powder, and use mixed powder compacting to obtain biscuit of ceramics；2) biscuit of ceramics is added thermal cracking at vacuum, 650 DEG C～1050 DEG C；3) ceramic body after thermal cracking is carried out carbothermic reduction reaction at nitrogen atmosphere, 1550 DEG C～1750 DEG C；4) biscuit of ceramics after carbothermic reduction reaction is sintered at inert atmosphere, 2050 DEG C～2300 DEG C obtain compact silicon carbide ceramic.Containing Si, Al, C, O and N element in silicon carbide ceramics prepared by employing the inventive method, it is the element that neutron absorption cross-section is little, the B big without neutron absorption cross-section or rare earth element.
Description
Technical field
The present invention relates to a kind of without boron or the preparation method of the compact silicon carbide ceramic of rare earth element, belong to structural ceramics technology
Field.
Background technology
Silicon carbide ceramics has high intensity, high rigidity, high heat conductance, high-wearing feature, high-temperature stability, corrosion resistance etc.
Excellent properties, is widely used in the field such as machinery, chemical industry.Carborundum has low neutron absorption cross-section and good high-temperature stable
Property, it is the most promising a kind of structural material in forth generation nuclear power system.Carborundum is covalent bond, sinters extremely difficult, logical
Often need to add a small amount of sintering aid and have B with acceleration of sintering densification, conventional sintering aid4C+C、AlN+B4C+C、
AlN+RE2O3(rare earth element such as RE=Y, Nd, Lu), Al2O3+RE2O3Deng.These sintering aids are after high temperature sintering
Remain in silicon carbide ceramics matrix, drastically influence anti-neutron irradiation performance and the high-temperature stability of silicon carbide ceramics.Such as,
Boron and rare earth element have the biggest neutron absorption cross-section, have a strong impact on the anti-neutron irradiation performance of silicon carbide ceramics；Al2O3、
RE2O3Deng oxide, there is relatively low fusing point, have a strong impact on the high-temperature stability of silicon carbide ceramics.
At present, in most research, the sintering aid of silicon carbide ceramics all contains boron or rare earth element, even if adopting
Aluminum and nitrogen element with low neutron absorption cross-section are as sintering aid, but in order to obtain high-compactness, the most still with the addition of
The B of few content4C or RE2O3As sintering aid, prepare fine and close SiC ceramic with aluminium nitride and carbon for sintering aid merely
Study the fewest.Only document 1 " Sintering of nano crystalline a silicon carbide doping with aluminum
Nitride, MS DATTA, AK BANDYOPADHYAY and B CHAUDHURI, Bull.Mater.Sci.,
2002,25 (2), 121-125. " simple use aluminium nitride and carbon as the sintering aid of silicon carbide powder, 2100 DEG C under vacuum
Insulation 15min, obtains the silicon carbide ceramics of consistency nearly 99% by normal pressure solid-phase sintering, and wherein aluminium nitride is with the shape of powder body
Formula introduces, and carbon introduces with the form of phenolic resin, and the mean diameter of the silicon carbide powder used is 37nm.
But, for the sintering of silicon carbide in submicro level powder body, simple employing aluminium nitride powder and carbon are as sintering aid
Time, it is difficulty with the densification of silicon carbide ceramics.Thus, how to realize preparing without boron or rare earth with silicon carbide in submicro level powder body
The compact silicon carbide ceramic of element, for one of one research direction of those skilled in the art.
Summary of the invention
Prepare without boron or the skill of the compact silicon carbide ceramic of rare earth element it is contemplated that overcome with silicon carbide in submicro level powder body
An art difficult problem, the invention provides a kind of without boron or the preparation method of the compact silicon carbide ceramic of rare earth element.
The invention provides a kind of without boron or the preparation method of the compact silicon carbide ceramic of rare earth element, including:
1) aluminum source, carbon source, silicon carbide powder and dehydrated alcohol uniformly mix post-drying, grinding obtains mixed powder after sieving, and
Mixed powder compacting is used to obtain biscuit of ceramics；
2) biscuit of ceramics is added thermal cracking at vacuum, 650 DEG C～1050 DEG C；
3) ceramic body after thermal cracking is carried out carbothermic reduction reaction at nitrogen atmosphere, 1550 DEG C～1750 DEG C；
4) biscuit of ceramics after carbothermic reduction reaction is sintered at inert atmosphere, 2050 DEG C～2300 DEG C obtain compact silicon carbide pottery
Porcelain.
The reaction mechanism of the present invention: aluminum source, carbon source (phenolic resin or white carbon black), dehydrated alcohol uniformly mix with silicon carbide powder
After conjunction, phenolic resin is evenly coated at carborundum powder surface, and Alumina gel is generation aluminium oxide after its cracking of aluminum source, phenolic resin
Residual carbon after cracking, the carbon of excess can ensure that carbon is fully contacted with aluminium oxide, and aluminium oxide and carbon occur carbon heat also in a nitrogen atmosphere
Former reaction generates aluminium nitride and CO (carbon monoxide converter) gas, and carbon generates carbon with the silicon dioxide layer generation reduction reaction of carborundum powder surface
SiClx and CO (carbon monoxide converter) gas, unnecessary carbon left behind.In sintering process, aluminium nitride and fresh carborundum powder surface
Contact and occur solid solution reaction to enter carborundum lattice, thus reducing crystal boundary energy and acceleration of sintering densification, and the carbon poly collection of excess
The effect of inhibiting grain growth is played at triangle grain boundaries.
It is preferred that source of aluminium is Alumina gel or alumina powder jointed.
It is preferred that described carbon source is phenolic resin or white carbon black, in described biscuit of ceramics count by weight percentage, aluminium oxide
Being 0.6～10wt%, carbon source is 2.4～31.7wt% phenolic resin or 0.7～9.5wt% white carbon black.
It is preferred that the particle diameter of described silicon carbide powder is submicron order.
It is preferred that the technological parameter adding thermal cracking includes: with 1 DEG C/min～the heating rate of 4 DEG C/min, be warmed up to
650 DEG C～1050 DEG C, temperature retention time is 0.5 hour～4 hours, and the atmosphere in thermal cracking processes is vacuum.
It is preferred that the technological parameter of carbothermic reduction reaction includes: with 2 DEG C/min～the heating rate of 10 DEG C/min, heat up
To 1550 DEG C～1750 DEG C, temperature retention time is 3 hours～10 hours, and the atmosphere during carbothermic reduction reaction is nitrogen.
It is preferred that in sintering process, be warmed up to 2050 DEG C～2300 DEG C, temperature retention time is 0.5～4 hour.
It is preferred that the silicon carbide ceramics that described compact silicon carbide ceramic is aluminium nitride and carbon doping, wherein, with weight percent
Than calculating, aluminium nitride is 0.5～8wt%, and carbon is 0.5～6wt%, and remaining is carborundum.
It is preferred that aluminium nitride is solid-solution in carborundum.
It is preferred that the consistency of described compact silicon carbide ceramic can reach 94%～99.7%.
Beneficial effects of the present invention:
1, containing Si, Al, C, O and N element in silicon carbide ceramics prepared by employing the inventive method, it is neutron absorption cross-section
Little element, the B big without neutron absorption cross-section or rare earth element；
2, the silicon carbide ceramics using the inventive method to prepare is fine and close, and consistency can reach 94%～99.7%；
3, using in the silicon carbide ceramics prepared of the inventive method remaining second mutually few, aluminium nitride solid solution enters carborundum lattice, nitrogen-free
Changing aluminum to exist mutually, only a small amount of carbon remnants form the second phase and are uniformly distributed in silicon carbide substrate；
4, the silicon carbide ceramics microstructure uniform and delicate using the inventive method to prepare, has preferable mechanical property, bending strength
Being 300～460MPa, fracture toughness is 2.8～4.0MPam1/2；
5, the inventive method device therefor is simple, invests little, and can manufacture the compact silicon carbide ceramic without boron or rare earth element.
Accompanying drawing explanation
Fig. 1 shows in the embodiment of the present invention 3 carborundum preparing (with fabricated in situ aluminium nitride and carbon as sintering aid)
The SEM figure of pottery section；
Fig. 2 shows in the embodiment of the present invention 3 unit of the silicon carbide ceramics preparing (with fabricated in situ aluminium nitride and carbon as sintering aid)
Element analysis chart；
Fig. 3 shows in the embodiment of the present invention 3 that the silicon carbide ceramics preparing (with fabricated in situ aluminium nitride and carbon as sintering aid) is through table
SEM figure after mirror polish and caustic corrosion；
Fig. 4 shows in the embodiment of the present invention 3 silicon carbide ceramics preparing (with fabricated in situ aluminium nitride and carbon as sintering aid)
TEM schemes；
Fig. 5 shows that comparative example prepares the SEM figure of the silicon carbide ceramics of (with aluminium nitride powder and carbon as sintering aid).
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that accompanying drawing and following embodiment are only below in conjunction with accompanying drawing and following embodiment
For the present invention is described, and the unrestricted present invention.
The present invention is to solve to use without pottery difficulty when boron or rare earth element sintering aid sintering silicon carbide in submicro level powder body
With fine and close problem, and propose a kind of without boron or the preparation method of the compact silicon carbide ceramic of rare earth element.By add aluminum source and
Carbon source is at silicon carbide powder situ synthesis aluminium nitride and carbon sintering aid so that it is possesses high sintering activity, solves and adopt merely
The problem that when being sintering aid sintering silicon carbide in submicro level powder body with aluminium nitride powder and carbon, pottery is difficult to densification.
The invention provides a kind of without boron or the preparation method of the compact silicon carbide ceramic of rare earth element, enter according to the following steps
OK:
Step one: by aluminum source (AlOOH colloidal sol or Al2O3Powder body, is calculated as 0.5～8wt%AlN by Al), carbon source (phenolic aldehyde tree
Fat, is calculated as 0.5～6wt%C by residual carbon after adding thermal cracking and carbothermic reduction reaction), silicon carbide powder and dehydrated alcohol uniformly mix
Closing, ball milling 4 hours, 60 DEG C of drying, grinding is sieved；
Step 2: mixed powder is dry-pressing formed with 20～100MPa, 200MPa isostatic pressed pressurize 2 minutes, obtain pottery element
Base；
Step 3: be placed in the mould of open topped by biscuit of ceramics, carries out thermal cracking in sintering furnace, is 1 DEG C with heating rate
Sintering furnace is heated to 650 DEG C～1050 DEG C by/min～4 DEG C/min, and temperature retention time is 0.5h～4h, in thermal cracking processes
Atmosphere be vacuum；
Step 4: then carry out carbothermic reduction reaction in sintering furnace, with heating rate be 2 DEG C/min～sintering furnace is added by 10 DEG C/min
Heat is warmed up to 1550 DEG C～1750 DEG C, and temperature retention time is 3h～10h, and the atmosphere during carbothermic reduction reaction is nitrogen；
Step 5: then carry out high temperature sintering in sintering furnace, with heating rate be 1 DEG C/min～sintering furnace heating is risen by 3 DEG C/min
Temperature is to 2050 DEG C～2300 DEG C, and temperature retention time is 0.5h～4h, and the atmosphere in high-temperature sintering process is noble gas, then drops
Warm to room temperature, i.e. obtain SiC ceramic.
The particle diameter of described silicon carbide powder is submicron order.Drawing without big neutron absorption cross-section element in prepared pottery
Enter.Thermal cracking processes, carbothermic reduction reaction process and sintering densification process can be carried out in same sintering furnace.
The reaction mechanism of the present invention: aluminum source, carbon source (phenolic resin or white carbon black), dehydrated alcohol uniformly mix with silicon carbide powder
After conjunction, phenolic resin is evenly coated at carborundum powder surface, and Alumina gel is generation aluminium oxide after its cracking of aluminum source, phenolic resin
Residual carbon after cracking, the carbon of excess can ensure that carbon is fully contacted with aluminium oxide, and aluminium oxide and carbon occur carbon heat also in a nitrogen atmosphere
Former reaction generates aluminium nitride and CO (carbon monoxide converter) gas, and carbon generates carbon with the silicon dioxide layer generation reduction reaction of carborundum powder surface
SiClx and CO (carbon monoxide converter) gas, unnecessary carbon left behind.In sintering process, aluminium nitride and fresh carborundum powder surface
Contact and occur solid solution reaction to enter carborundum lattice, thus reducing crystal boundary energy and acceleration of sintering densification, and the carbon poly collection of excess
The effect of inhibiting grain growth is played at triangle grain boundaries.
The present invention includes following beneficial effect:
1, containing Si, Al, C, O and N element in silicon carbide ceramics prepared by employing the inventive method, it is neutron absorption cross-section
Little element, the B big without neutron absorption cross-section or rare earth element；
2, the silicon carbide ceramics using the inventive method to prepare is fine and close, and consistency can reach 94%～99.7%；
3, using in the silicon carbide ceramics prepared of the inventive method remaining second mutually few, aluminium nitride solid solution enters carborundum lattice, nitrogen-free
Changing aluminum to exist mutually, only a small amount of carbon remnants form the second phase and are uniformly distributed in silicon carbide substrate；
4, the silicon carbide ceramics microstructure uniform and delicate using the inventive method to prepare, has preferable mechanical property, bending strength
Being 300～460MPa, fracture toughness is 2.8～4.0MPam1/2；
5, the inventive method device therefor is simple, invests little, and can manufacture the compact silicon carbide ceramic without boron or rare earth element.
Enumerate embodiment further below to describe the present invention in detail.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.The technique ginseng that following example is concrete
Number etc. is the most only an example in OK range, in the range of i.e. those skilled in the art can be done suitably by explanation herein
Select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
A kind of without boron or the method for the compact silicon carbide ceramic of rare earth element, sequentially include the following steps:
Step one: by 12wt% Alumina gel (containing 20wt%AlOOH, be calculated as 2wt%AlN by Al), 10.5wt% phenolic resin
(being calculated as 3wt%C by residual carbon after adding thermal cracking and carbothermic reduction reaction), 77.5wt% silicon carbide powder (powder body mean diameter
Being 0.4 micron, after adding thermal cracking and carbothermic reduction reaction, content is 95wt%) and dehydrated alcohol uniformly mix, ball milling 4 is little
Time, 60 DEG C of drying, grinding is sieved；
Step 2: by mixed powder with in the dry-pressing formed mould being placed on open topped of 20MPa, carry out adding hot tearing in sintering furnace
Solving, be that sintering furnace is heated to 900 DEG C by 2 DEG C/min with heating rate, temperature retention time is 1h, adds in thermal cracking processes
Atmosphere is vacuum；
Step 3: then carry out carbothermic reduction reaction in sintering furnace, is that sintering furnace is continued heating liter by 10 DEG C/min with heating rate
Temperature is to 1700 DEG C, and temperature retention time is 5h, and the atmosphere during carbothermic reduction reaction is nitrogen；
Step 4: then sieved to room temperature, grinding by the biscuit of ceramics slow cooling after carbothermic reduction reaction, becomes with 20MPa dry-pressing
Type, 200MPa isostatic pressing are placed in the mould of open topped, carry out high temperature sintering in freezing of a furnace, first with heating rate
It is that sintering furnace is heated to 1200 DEG C by 10 DEG C/min, then is that sintering furnace is heated to by 3 DEG C/min with heating rate
2170 DEG C, temperature retention time is 2h, and the atmosphere in high-temperature sintering process is argon, and then slow cooling is to room temperature, i.e. obtains SiC
Pottery (consistency is 97%).
Embodiment 2
Step one: by 12wt% Alumina gel (containing 20wt%AlOOH, be calculated as 2wt%AlN by Al), 3.8wt% white carbon black (by carbon heat
After reduction reaction, residual carbon is calculated as 3wt%C), (powder body mean diameter is 0.4 micron to 94.2wt% silicon carbide powder, adds thermal cracking
Be 95wt% with content after carbothermic reduction reaction) and dehydrated alcohol uniformly mix, ball milling 4 hours, 60 DEG C of drying, ground
Sieve；
Step 2: mixed powder is dry-pressing formed with 20MPa, 200MPa isostatic pressed pressurize 2 minutes, obtain biscuit of ceramics；
Step 3: be placed in the mould of open topped by biscuit of ceramics, carries out thermal cracking in sintering furnace, is 2 DEG C with heating rate
Sintering furnace is heated to 900 DEG C by/min, and temperature retention time is 1h, and the atmosphere in thermal cracking processes is vacuum；
Step 4: then carry out carbothermic reduction reaction in sintering furnace, is that sintering furnace is heated to by 5 DEG C/min with heating rate
1700 DEG C, temperature retention time is 5h, and the atmosphere during carbothermic reduction reaction is nitrogen；
Step 5: then carry out high temperature sintering in sintering furnace, first by the biscuit of ceramics slow cooling after carbothermic reduction reaction to 900 DEG C
Hereinafter, then it is passed through argon after evacuation, is that sintering furnace is heated to 1200 DEG C by 10 DEG C/min with heating rate, then with
Heating rate is that sintering furnace is heated to 2170 DEG C by 3 DEG C/min, and temperature retention time is 2h, and then slow cooling is to room temperature,
I.e. obtain SiC ceramic (consistency is 96.5%).
Embodiment 3
The present embodiment is unlike specific embodiment 1: the AlOOH colloidal sol in step one is changed to alumina powder jointed, and raw material composition depends on
Secondary for 2.2wt%Al2O3Powder body, 11.7wt% phenolic resin and 86.1wt%SiC powder body.Other step and parameter be embodied as
Example 1 is identical；
Fig. 1 is the SEM of the silicon carbide ceramics section as sintering aid with fabricated in situ aluminium nitride and carbon of specific embodiment 3 preparation
Figure, it can be seen that there is equally distributed second phase in silicon carbide ceramics；
Fig. 2 is the elementary analysis figure of the silicon carbide ceramics as sintering aid with fabricated in situ aluminium nitride and carbon of specific embodiment 3 preparation；
Figure it is seen that containing Si, Al, C and O element in silicon carbide ceramics, N element is not examined due to the reason of detection limit
Go out, be the element that neutron absorption cross-section is little；Al element and Si element are uniformly distributed in whole, illustrate that Al element solid solution enters
Enter carborundum lattice；The distribution of C element has preferable correspondence with the black region in SEM figure, and silicon carbide ceramics is described
In the second phase be carbon phase；
Fig. 3 is that the silicon carbide ceramics as sintering aid with fabricated in situ aluminium nitride and carbon of specific embodiment 3 preparation is through surface finish and strong
SEM figure after caustic corrosion.From figure 3, it can be seen that the uniform microstructure of silicon carbide ceramics is careful, crystal grain presents isometry
Shape, crystallite dimension about 1～10 μm；
Fig. 4 is the TEM figure of the silicon carbide ceramics as sintering aid with fabricated in situ aluminium nitride and carbon of specific embodiment 3 preparation.From
Fig. 4 is it can be seen that the crystal boundary in silicon carbide ceramics is clean；
The bulk density of the silicon carbide ceramics as sintering aid with fabricated in situ aluminium nitride and carbon of specific embodiment 3 preparation is
3.16g/cm3, it (is 3.17g/cm by solid density that consistency can reach 99.7%3Calculate), bending strength is 442MPa, disconnected
Splitting toughness is 3.27MPam1/2。
In Fig. 2, the elementary analysis result of silicon carbide ceramics is:
| Element (Element) | Percentage by weight (Weight%) | Atomic percent (Atomic%) |
| C | 25.07 | 43.86 |
| Al | 2.15 | 1.67 |
| Si | 72.78 | 54.46 |
| Add up to (Totals) | 100.00 | 99.99 |
Embodiment 4
The present embodiment is unlike specific embodiment 1: in step one by carbothermic reduction reaction completely after product (consist of:
0.5wt%AlN, 0.5wt%C and 99wt%SiC) calculate mixed powder composition be followed successively by 3.5wt% Alumina gel, 2.3wt% phenolic aldehyde
Resin and 94.2wt%SiC powder body.Other step and parameter are identical with specific embodiment 1.The consistency of silicon carbide ceramics is
94.6%.
Embodiment 5
The present embodiment is unlike specific embodiment 3: in step one by carbothermic reduction reaction completely after product (consist of:
4wt%AlN, 4wt%C and 92wt%SiC) calculate mixed powder composition be followed successively by 4.3wt%Al2O3Powder body, 16.5wt% phenol
Urea formaldehyde and 79.2wt%SiC powder body.Other step and parameter are identical with specific embodiment 3.The consistency of silicon carbide ceramics is
99.5%.
Embodiment 6
The present embodiment is unlike specific embodiment 3: in step one by carbothermic reduction reaction completely after product (consist of:
8wt%AlN, 6wt%C and 86wt%SiC) calculate mixed powder composition be followed successively by 7.8wt%Al2O3Powder body, 24.8wt% phenol
Urea formaldehyde and 67.4wt%SiC powder body.Other step and parameter are identical with specific embodiment 3.The consistency of silicon carbide ceramics is
99.7%.
The consistency of SiC ceramic prepared by specific embodiment 1-6 is 94.6%～99.7%, bending strength be 300～
460MPa, fracture toughness is 2.8～4.0MPam1/2。
Comparative example
By aluminium nitride powder (0.5wt%, 2wt%, 5wt%, 10wt%, 15wt%), phenolic resin (by residual after carbothermic reduction reaction
Carbon amounts meter 0.5wt%～3wt%C), silicon carbide powder (powder body mean diameter is 0.4 micron) and dehydrated alcohol uniformly mix,
Ball milling 4 hours, 60 DEG C of drying, 200MPa isostatic pressing dry-pressing formed with 20MPa, obtain biscuit of ceramics.By pottery
Biscuit is placed in the mould of open topped, adds thermal cracking and sintering in sintering furnace, first will sinter with about 2 DEG C/min of heating rate
Stove heats to 900 DEG C, and temperature retention time is 1h, and adding the atmosphere in thermal cracking processes is vacuum, then passes to argon, to rise
Sintering furnace is heated to 2210 DEG C by temperature about 3 DEG C/min of speed, and temperature retention time is 2h, and then slow cooling is to room temperature, i.e.
Obtain SiC ceramic.
The bulk density maximum of the silicon carbide ceramics as sintering aid with aluminium nitride powder and carbon prepared by this comparative example is
2.89g/cm3, now the addition of aluminium nitride is 2wt%, and the consistency of silicon carbide ceramics is 91.2% (to be by solid density
3.17g/cm3Calculate).Fig. 5 is that (bulk density is for 2.89 for the silicon carbide ceramics prepared for sintering aid with aluminium nitride powder and carbon
g/cm3Sample) SEM figure, this silicon carbide ceramics consists of: 2wt%AlN, 3wt%C and 95wt%SiC, can see
Going out and there is more hole in silicon carbide ceramics, consistency is poor.
Claims (10)
1. one kind without boron or the preparation method of the compact silicon carbide ceramic of rare earth element, it is characterised in that including:
1) aluminum source, carbon source, silicon carbide powder and dehydrated alcohol are uniformly mixed post-drying, grinding and after sieving, obtains mixed powder, and use mixed powder compacting to obtain biscuit of ceramics；
2) biscuit of ceramics is added thermal cracking at vacuum, 650 DEG C～1050 DEG C；
3) ceramic body after thermal cracking is carried out carbothermic reduction reaction at nitrogen atmosphere, 1550 DEG C～1750 DEG C；
4) biscuit of ceramics after carbothermic reduction reaction is sintered at inert atmosphere, 2050 DEG C～2300 DEG C obtain compact silicon carbide ceramic；
The mean diameter of described silicon carbide powder is submicron order.
Preparation method the most according to claim 1, it is characterised in that source of aluminium is Alumina gel or alumina powder jointed.
Preparation method the most according to claim 1, it is characterised in that described carbon source is phenolic resin or white carbon black.
Preparation method the most according to claim 1, it is characterized in that, the technological parameter adding thermal cracking includes: with 1 DEG C/min～the heating rate of 4 DEG C/min, is warmed up to 650 DEG C～1050 DEG C, temperature retention time is 0.5 hour～4 hours, and the atmosphere in thermal cracking processes is vacuum.
Preparation method the most according to claim 1, it is characterized in that, the technological parameter of carbothermic reduction reaction includes: with 2 DEG C/min～the heating rate of 10 DEG C/min, is warmed up to 1550 DEG C～1750 DEG C, temperature retention time is 3 hours～10 hours, and the atmosphere during carbothermic reduction reaction is nitrogen.
Preparation method the most according to claim 1, it is characterised in that in sintering process, is warmed up to 2050 DEG C～2300 DEG C, and temperature retention time is 0.5 hour～4 hours.
Preparation method the most according to claim 1, it is characterised in that described compact silicon carbide ceramic is the silicon carbide ceramics of aluminium nitride and carbon doping, wherein, calculated in weight percent, aluminium nitride is 0.5～8wt%, and carbon is 0.5～6wt%, and remaining is carborundum.
Preparation method the most according to claim 7, it is characterised in that aluminium nitride is solid-solution in carborundum.
Preparation method the most according to claim 1, it is characterised in that the consistency of described compact silicon carbide ceramic reaches 94%～99.7%.
10. according to described preparation method arbitrary in claim 1-9, it is characterised in that described compact silicon carbide ceramic does not contains the big boron in neutron absorption cross-section or rare earth element.
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| CN109207783A (en) * | 2018-09-29 | 2019-01-15 | 陕西科技大学 | Low temperature in situ synthesis Al in a kind of alusil alloy4SiC4The method of ceramic particle |
| CN110935237B (en) * | 2019-11-18 | 2021-09-03 | 武汉科技大学 | Hierarchical pore silicon carbide porous ceramic for filtering high-temperature flue gas and preparation method thereof |
| CN114478014A (en) * | 2020-10-26 | 2022-05-13 | 深圳市万普拉斯科技有限公司 | Silicon carbide ceramic material, ceramic mold and preparation method thereof |
| CN114149269B (en) * | 2021-12-02 | 2022-11-04 | 北京科技大学 | AlN-SiC solid solution combined SiC composite refractory material for side wall of aluminum electrolytic cell and preparation method thereof |
| CN116375476A (en) * | 2021-12-22 | 2023-07-04 | 中国科学院上海硅酸盐研究所 | Silicon carbide ceramic material and preparation method thereof |
| CN114835492A (en) * | 2022-05-18 | 2022-08-02 | 厦门稀土材料研究所 | Rare earth-based zirconium-hafnium composite ceramic material and preparation method and application thereof |
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| US7939044B2 (en) * | 2008-02-11 | 2011-05-10 | Alexander Mukasyan | Method of manufacturing sub-micron silicon-carbide powder |
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