CN104926310B - Silicon Carbide Powder that a kind of aluminium nitride is modified and preparation method thereof - Google Patents
Silicon Carbide Powder that a kind of aluminium nitride is modified and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to modified Silicon Carbide Powder of a kind of aluminium nitride and preparation method thereof, including: 1) aluminum source, carbon source, silicon carbide powder and dehydrated alcohol uniformly mixed post-drying, grinds and sieve and dry-pressing formed obtain biscuit of ceramics；2) biscuit of ceramics is added thermal cracking at vacuum condition, 600 DEG C～1050 DEG C；3) biscuit of ceramics after thermal cracking is carried out carbothermic reduction reaction at nitrogen atmosphere, 1500 DEG C～1750 DEG C；4) the biscuit of ceramics grinding after carbothermic reduction reaction is sieved, i.e. obtain aluminium nitride and the Silicon Carbide Powder of carbon modification.In the Silicon Carbide Powder of aluminium nitride modification prepared by employing the inventive method, aluminium nitride solid solution enters carborundum lattice, and later stage sintering experiment result shows that powder sintering activity is improved.
Description
Technical field
The present invention relates to modified Silicon Carbide Powder of a kind of aluminium nitride and preparation method thereof, belong to structural ceramics technology neck
Territory.
Background technology
Silicon carbide ceramics have high intensity, high rigidity, high heat conductance, high-wearing feature, high-temperature stability, corrosion resistance,
The excellent properties such as anti-neutron irradiation, are widely used in the field such as machinery, chemical industry.Carborundum is covalent bond, sinters extremely difficult,
Typically require a small amount of sintering aid of interpolation 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.
In most research, aluminium nitride sintering aid generally adds entrance silicon carbide powder with the form of powder granule
In, aluminum nitride particle can only carry out point cantact with the silicon dioxide layer of carborundum powder surface, the promotion played in sintering process
The limited use of sintering densification, carborundum mixed powder has relatively low sintering activity.If the method using fabricated in situ exists
Silicon carbide powder situ synthesis aluminium nitride and carbon sintering aid, the sintering activity that can well solve carborundum mixed powder is difficult
Topic, but the most relevant report does not occurs.
Summary of the invention
It is contemplated that overcome the technical barrier that existing Silicon Carbide Powder sintering activity is low, the invention provides a kind of nitrogen
Change modified Silicon Carbide Powder of aluminum and preparation method thereof.
The invention provides the preparation method of the modified Silicon Carbide Powder of a kind of aluminium nitride, including:
1) aluminum source, carbon source, silicon carbide powder and dehydrated alcohol are uniformly mixed post-drying, grinds and sieve and dry-pressing formed made pottery
Porcelain biscuit；
2) biscuit of ceramics is added thermal cracking at vacuum condition, 600 DEG C～1050 DEG C；
3) biscuit of ceramics after thermal cracking is carried out carbothermic reduction reaction at nitrogen atmosphere, 1500 DEG C～1750 DEG C；
4) the biscuit of ceramics grinding after carbothermic reduction reaction is sieved, i.e. obtain the Silicon Carbide Powder that aluminium nitride is modified.
It is preferred that source of aluminium includes Alumina gel or alumina powder jointed.
It is preferred that described carbon source includes phenolic resin or white carbon black.
It is preferred that the particle diameter of silicon carbide powder is micron order, preferably smaller than 2 microns.
It is preferred that in described biscuit of ceramics, count by weight percentage, aluminium oxide is 0.6 10wt%, and carbon source is
2.4 31.7wt% phenolic resin or 0.7 9.5wt% white carbon black.
It is preferred that the technological parameter adding thermal cracking includes: with heating rate 1 DEG C/min～5 DEG C/min be warmed up to 600 DEG C～
1050 DEG C, temperature retention time is 0.5～4 hour, and the atmosphere in thermal cracking processes is vacuum, and after insulation, Temperature fall is to room
Temperature, obtains the biscuit of ceramics after thermal cracking.
It is preferred that the technological parameter of carbothermic reduction reaction includes: be 1 DEG C/min～3 DEG C/min with heating rate and be warmed up to
1500 DEG C～1750 DEG C, temperature retention time is 1～10 hour, and the atmosphere during carbothermic reduction reaction is nitrogen, after insulation
Temperature fall, to room temperature, obtains the biscuit of ceramics after carbothermic reduction reaction.
Also, present invention also offers Silicon Carbide Powder prepared by said method, described Silicon Carbide Powder is nitridation
The Silicon Carbide Powder that aluminum is modified, wherein, count by weight percentage, aluminium nitride is 0.5 8wt%, and carbon is 0.5
6wt%, remaining as carborundum.
It is preferred that aluminium nitride is solid-solution in carborundum lattice.
Beneficial effects of the present invention:
In the Silicon Carbide Powder of the aluminium nitride modification that 1, prepared by employing the inventive method, aluminium nitride solid solution enters carborundum lattice,
Later stage sintering experiment result shows that powder sintering activity is improved；
In the Silicon Carbide Powder of the aluminium nitride modification that 2, prepared by employing the inventive method, carbon is uniformly dispersed, and soilless sticking phenomenon is sent out
Raw；
3, the inventive method device therefor is simple, invests little, and can manufacture the Silicon Carbide Powder that aluminium nitride is modified.
Accompanying drawing explanation
Fig. 1 shows the SEM figure of the silicon carbide powder after the thermal cracking that in the embodiment of the present invention 1, step 2 obtains；
Fig. 2 shows the SEM figure of the Silicon Carbide Powder that the aluminium nitride of preparation is modified in the embodiment of the present invention 2；
Fig. 3 shows the TEM figure of the Silicon Carbide Powder that the aluminium nitride of preparation is modified in the embodiment of the present invention 2；
Fig. 4 shows the EDS collection of illustrative plates of the Silicon Carbide Powder that the aluminium nitride of preparation is modified in the embodiment of the present invention 2.
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 a difficult problem low in order to solve the carborundum mixed powder sintering activity of existing nitrogen aluminum sinter auxiliary agent, and
Modified Silicon Carbide Powder of a kind of fabricated in situ aluminium nitride and preparation method thereof, sintering aid aluminium nitride and carbon are proposed by former
The method of position synthesis is incorporated in silicon carbide powder.
The invention provides modified Silicon Carbide Powder of a kind of fabricated in situ aluminium nitride and preparation method thereof, modified carbon
SiClx ceramic powder is prepared by the method for fabricated in situ aluminium nitride, specifically comprises the following steps that
Step one: aluminum source (Alumina gel or alumina powder jointed), carbon source (phenolic resin), silicon carbide powder and dehydrated alcohol are uniformly mixed
Closing, ball milling 4 hours, 60 DEG C of drying, grinding is sieved；
Step 2: mixed powder after sieving is dry-pressing formed obtains biscuit of ceramics, is subsequently placed in the mould of open topped, at sintering
Adding thermal cracking in stove, with heating rate be 1 DEG C/min～sintering furnace is heated to 600 DEG C～1050 DEG C by 5 DEG C/min, insulation
Time is 0.5h～4h, and the atmosphere in thermal cracking processes is vacuum, Temperature fall to room temperature, obtains the pottery element after thermal cracking
Base；
Step 3: be placed in the mould of open topped by the biscuit of ceramics after thermal cracking, carries out carbon thermal reduction in sintering furnace or tube furnace
Reaction, with heating rate be 1 DEG C/min～sintering furnace or diamond heating are warmed up to 1500 DEG C～1750 DEG C by 3 DEG C/min, protects
The temperature time is 1h～10h, and the atmosphere during carbothermic reduction reaction is nitrogen, and Temperature fall, to room temperature, obtains carbon thermal reduction anti-
Biscuit of ceramics after should；
Step 4: the biscuit of ceramics after carbothermic reduction reaction is ground and sieves, i.e. obtain the Silicon Carbide Powder that aluminium nitride is modified.
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, if Alumina gel is generation aluminium oxide after its cracking of aluminum source, and phenolic aldehyde tree
Residual carbon after fat cracking, aluminium oxide and carbon occurs carbothermic reduction reaction to generate aluminium nitride and CO (carbon monoxide converter) gas in a nitrogen atmosphere,
Carbon generates carborundum and CO (carbon monoxide converter) gas, unnecessary carbon residual with the silicon dioxide layer generation reduction reaction of carborundum powder surface
Get off.
The present invention includes following beneficial effect:
In the Silicon Carbide Powder of the aluminium nitride modification that 1, prepared by employing the inventive method, aluminium nitride solid solution enters carborundum lattice,
Later stage sintering experiment result shows that powder sintering activity is improved；
In the Silicon Carbide Powder of the aluminium nitride modification that 2, prepared by employing the inventive method, carbon is uniformly dispersed, and soilless sticking phenomenon is sent out
Raw；
3, the inventive method device therefor is simple, invests little, and can manufacture the Silicon Carbide Powder that aluminium nitride is modified.
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
Silicon Carbide Powder that a kind of aluminium nitride is modified and preparation method thereof, sequentially includes the following steps:
Step one: by 12wt% Alumina gel (containing 20wt%AlOOH), 10.5wt% phenolic resin, 77.5wt% silicon carbide powder (in
Position particle diameter about 0.4 micron) uniformly mix with dehydrated alcohol, ball milling 4 hours, 60 DEG C of drying, grinding is sieved, and carbon thermal reduction is anti-
Should completely after product consist of 2wt%AlN, 3wt%C and 95wt%SiC；
Step 2: in the dry-pressing formed mould being placed on open topped of mixed powder step one obtained, add hot tearing in sintering furnace
Solving, with about 3 DEG C/min of heating rate, sintering furnace is heated to 900 DEG C, temperature retention time is 1h, adds in thermal cracking processes
Atmosphere is vacuum, and Temperature fall to room temperature obtains the biscuit of ceramics after adding thermal cracking；
Step 3: step 2 is obtained add thermal cracking after biscuit of ceramics be placed in the mould of open topped, tube furnace carries out carbon
Thermal reduction reaction, is warmed up to 1600 DEG C with about 2 DEG C/min of heating rate by diamond heating, and temperature retention time is 4h, and carbon heat is also
Atmosphere in former course of reaction is nitrogen, and Temperature fall to room temperature obtains the biscuit of ceramics after carbothermic reduction reaction；
Step 4: the biscuit of ceramics after carbothermic reduction reaction step 3 obtained grinds and sieves, i.e. obtains the dense carbon that aluminium nitride is modified
SiClx ceramic powder；
Embodiment 1 step 2 is obtained add thermal cracking after biscuit of ceramics grind sieve, obtain the mixed powder after adding thermal cracking.Figure
The SEM that 1 is the mixed powder after adding thermal cracking schemes, it can be seen that carborundum powder surface exists nano level aluminium oxide granule
Grain, carbon is evenly coated at carborundum powder surface, illustrates that carbon is dispersed in silicon carbide powder.
Later stage sintering experiment:
The silicon carbide powder of preparation is pressed into ceramic body 2050 DEG C～2300 DEG C, sinter under inert atmosphere and obtain for 0.5-4 hour
Silicon carbide ceramics, the silicon carbide powder for example with embodiment 1 preparation is pressed into ceramic body, selects to sinter 2 at 2170 DEG C
Hour, the consistency of gained silicon carbide ceramics is 97.2%.
Embodiment 2
The present embodiment is unlike specific embodiment 1: step one is pressed carbothermic reduction reaction completely after product (4wt%AlN,
3wt%C and 93wt%SiC) calculate mixed powder composition respectively be: 21.2wt% Alumina gel, 11.5wt% phenolic resin and
67.3wt% silicon carbide powder.Other step and parameter are identical with specific embodiment 1；
Fig. 2 is the SEM figure of the Silicon Carbide Powder of the aluminium nitride modification of specific embodiment 2 preparation, it can be seen that silicon carbide powder
The nano-scale particle on surface disappears, and carborundum powder surface occurs in that step, illustrates that aluminium nitride solid solution enters carborundum lattice and leads
Cause the generation of stacking fault defects；
Fig. 3 is the TEM figure of the Silicon Carbide Powder of the aluminium nitride modification of specific embodiment 2 preparation, it can be seen that carborundum grain
There is more dislocation defects in inside, further illustrates aluminium nitride solid solution entrance carborundum lattice and result in the product of dislocation defects
Raw.
Later stage sintering experiment:
The silicon carbide powder of preparation is pressed into ceramic body 2050 DEG C～2300 DEG C, sinter under inert atmosphere and obtain for 0.5-4 hour
Silicon carbide ceramics, the silicon carbide powder for example with embodiment 2 preparation is pressed into ceramic body, selects to sinter 2 at 2170 DEG C
Hour, the consistency of gained silicon carbide ceramics is 97.2%.
Embodiment 3
The present embodiment is unlike specific embodiment 2: the Alumina gel in step one is changed to alumina powder jointed, prepares three kinds of proportionings simultaneously
Powder body, by carbothermic reduction reaction completely after product (product 1:2wt%AlN, 3wt%C and 95wt%SiC, product
2:4wt%AlN, 3wt%C and 93wt%SiC, product 3:6wt%AlN, 3wt%C and 91wt%SiC) calculate corresponding
Mixed powder composition respectively is: 2.2wt% is alumina powder jointed, 11.7wt% phenolic resin and 86.1wt% silicon carbide powder
(corresponding with product 1), 4.4wt% is alumina powder jointed, 13.9wt% phenolic resin and 81.7wt% silicon carbide powder be (with product 2
Corresponding), 6.4wt% is alumina powder jointed, 16wt% phenolic resin and 77.6wt% silicon carbide powder (corresponding with product 3).Other
Step and parameter are identical with specific embodiment 2.
Later stage sintering experiment:
The silicon carbide powder of preparation is pressed into ceramic body 2050 DEG C～2300 DEG C, sinter under inert atmosphere and obtain for 0.5-4 hour
Silicon carbide ceramics, such as, select the silicon carbide powder using embodiment 3 preparation to be pressed into ceramic body, sinter 2 at 2170 DEG C
Hour, the consistency of gained silicon carbide ceramics is followed successively by 96.8% (corresponding product 1), 99.7% (corresponding product 2), 99.7%
(corresponding product 3).
Table 1 below gives the elementary analysis result of the Silicon Carbide Powder of the aluminium nitride modification of specific embodiment 3 preparation,
Can be seen that and there is more nitrogen element in silicon carbide powder, if pressing nitrogen element to calculate carbothermic reduction reaction conversion ratio, conversion ratio is near
100%, owing to the reason of test error causes part data to exceed 100%.
Table 1
| The content of fabricated in situ auxiliary agent | 2wt%AlN+3wt%C | 4wt%AlN+3wt%C | 6wt%AlN+3wt%C |
| Nitrogen element in product | 0.77wt% | 1.46wt% | 1.96wt% |
| Nitrogen element theory value in product | 0.68wt% | 1.37wt% | 2.04wt% |
| Aluminium nitride conversion ratio | ＞ 100% (113%) | ＞ 100% (106%) | 96.1% |
Comparative example 1
Step one: by 2wt% aluminum nitride particle, 3wt% hydrocarbon black powder and 95wt% silicon carbide powder (median about 0.4 micron)
Biscuit of ceramics is obtained after the mixed powder that uniformly obtains after mixing is dry-pressing formed；
Step 2: be placed in the mould of open topped by biscuit of ceramics, is warmed up to diamond heating with about 2 DEG C/min of heating rate
1600 DEG C, temperature retention time is 4h, and atmosphere is nitrogen, and Temperature fall is to room temperature；
Step 3: biscuit of ceramics step 2 obtained grinds and sieves, i.e. obtains mixed powder (composition 2wt% aluminium nitride, 3wt%
Carbon, 95wt% carborundum).
Later stage sintering experiment:
The silicon carbide powder of preparation is pressed into ceramic body 2050 DEG C～2300 DEG C, sinter under inert atmosphere and obtain for 0.5-4 hour
Silicon carbide ceramics, such as, select the silicon carbide powder using comparative example 1 preparation to be pressed into ceramic body, sinter 2 at 2170 DEG C
Hour, the consistency of gained silicon carbide ceramics is 91.2%.
Claims (7)
1. the preparation method of the Silicon Carbide Powder of an aluminium nitride modification, it is characterised in that including:
1) aluminum source, carbon source, silicon carbide powder and dehydrated alcohol are uniformly mixed post-drying, grinds and sieve and dry-pressing formed obtain biscuit of ceramics；
2) biscuit of ceramics is added thermal cracking at vacuum condition, 600 DEG C～1050 DEG C；
3) biscuit of ceramics after thermal cracking is carried out carbothermic reduction reaction at nitrogen atmosphere, 1500 DEG C～1750 DEG C；
4) the biscuit of ceramics grinding after carbothermic reduction reaction is sieved, i.e. obtain the Silicon Carbide Powder that aluminium nitride is modified, in the Silicon Carbide Powder that gained aluminium nitride is modified, count by weight percentage, aluminium nitride is 0.5～8wt%, and carbon is 0.5～6wt%, remaining as carborundum.
Preparation method the most according to claim 1, it is characterised in that source of aluminium includes Alumina gel or alumina powder jointed.
Preparation method the most according to claim 1, it is characterised in that described carbon source includes phenolic resin or white carbon black.
Preparation method the most according to claim 1, it is characterised in that the median of silicon carbide powder is submicron order.
Preparation method the most according to claim 1, it is characterized in that, the technological parameter adding thermal cracking includes: be warmed up to 600 DEG C～1050 DEG C with heating rate 1 DEG C/min～5 DEG C/min, temperature retention time is 0.5～4 hour, atmosphere in thermal cracking processes is vacuum, after insulation, Temperature fall is to room temperature, obtains the biscuit of ceramics after thermal cracking.
6. according to described preparation method arbitrary in claim 1-5, it is characterized in that, the technological parameter of carbothermic reduction reaction includes: is 1 DEG C/min～3 DEG C/min with heating rate and is warmed up to 1500 DEG C～1750 DEG C, temperature retention time is 1～10 hour, atmosphere during carbothermic reduction reaction is nitrogen, after insulation, Temperature fall is to room temperature, obtains the biscuit of ceramics after carbothermic reduction reaction.
7. the Silicon Carbide Powder that in claim 1-6 prepared by arbitrary described method, it is characterised in that aluminium nitride is solid-solution in carborundum lattice.
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| CN107445624A (en) * | 2017-09-07 | 2017-12-08 | 张家港市山牧新材料技术开发有限公司 | A kind of preparation method of aluminum nitride silicon carbide composite ceramic material |
| CN113121252B (en) * | 2019-12-30 | 2022-06-07 | 海南大学 | Preparation method of high-thermal-conductivity SiC-AlN composite ceramic |
| CN112573896A (en) * | 2020-12-25 | 2021-03-30 | 唐山北方瓷都陶瓷集团卫生陶瓷有限责任公司 | High-strength ceramic biscuit 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 |
| CN115253950B (en) * | 2022-07-29 | 2024-02-13 | 氢源科技(江苏)有限公司 | Microreactor and preparation method and application thereof |
| CN116354735B (en) * | 2023-03-18 | 2024-02-23 | 西北工业大学 | Method for rapidly preparing AlN modified C/C-SiC friction material |
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| CN1654432A (en) * | 2004-10-11 | 2005-08-17 | 西安交通大学 | Method for preparing silicon nitride/silicon carbide porous ceramic |
| CN102010222A (en) * | 2010-10-29 | 2011-04-13 | 西安交通大学 | Silicon carbide porous ceramic and preparation method thereof |
| WO2012144638A1 (en) * | 2011-04-21 | 2012-10-26 | 株式会社ブリヂストン | Ceramic sintered body and method for producing ceramic sintered body |
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| CN1654432A (en) * | 2004-10-11 | 2005-08-17 | 西安交通大学 | Method for preparing silicon nitride/silicon carbide porous ceramic |
| CN102010222A (en) * | 2010-10-29 | 2011-04-13 | 西安交通大学 | Silicon carbide porous ceramic and preparation method thereof |
| WO2012144638A1 (en) * | 2011-04-21 | 2012-10-26 | 株式会社ブリヂストン | Ceramic sintered body and method for producing ceramic sintered body |
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