CN109305815A - A kind of high intensity, porous ceramic and its preparation process - Google Patents
A kind of high intensity, porous ceramic and its preparation process Download PDFInfo
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Abstract
The present invention provides a kind of high intensity, porous ceramics and its preparation processes.First mixed powder is made in silicon carbide powder and polyvinyl alcohol tiny balloon by the present invention, then covering body raw material is made in chemical vapor deposition nano zircite, then covering body raw material is introduced into cellulose acetate-dimethyl sulfoxide-aqueous systems, successively heated through inert atmosphere heating, oxygen-containing atmosphere heating, inert atmosphere sintering and oxygen-containing atmosphere, polyvinyl alcohol tiny balloon and cellulose acetate decompose evolution system to form hole, so that product porosity with higher, the hole of specific distribution rule assigns the enough mechanical strengths of product;Nano zircite further functions as booster action, enhances the mechanical strength of product.
Description
Technical field
The present invention relates to ceramic technology fields, more particularly to a kind of high intensity, porous ceramics and its preparation process.
Background technique
Traditional ceramics are kneaded, form and calcine by crushing using natural clay and various natural minerals as primary raw material
It is made.With the development of modern science technology, occurs many new ceramic kinds again in the last hundred years, do not use clay, length
The traditional ceramics raw material such as stone, quartz, but other special materials are used, or even be expanded to the range of non-silicate, non-oxidized substance,
Therefore the meaning of ceramics actually much surmounts traditional concept narrow in the past.
Porous ceramics is one kind of ceramics, is to have the ceramic material for largely communicating with each other or being closed stomata through high temperature firing
Material.Porous ceramics has the characteristics that corrosion-resistant, large specific surface area, through performance be good and good biocompatibility, is widely used in
The technical fields such as chemical industry, petroleum, weaving, pharmacy, cement.In order to adapt to the high standards of special dimension, to porous ceramics
Mechanical strength and porosity propose requirements at the higher level.Usually, mechanical strength is the increase with porosity and reduces, together
When guarantee porous ceramics mechanical strength and porosity have certain difficulty.
Patent CN106007777B discloses a kind of porous ceramics, utilizes di-iron trioxide, manganese dioxide and three oxidations
Two cobalts play impurity effect, adjust the electronics and ion concentration ratio of product, so that the porosity of product is improved to 44%, it is pressure-resistant
Intensity is not less than 28MPa, and either porosity or compressive resistance is still not ideal enough, and be greatly improved space.
Summary of the invention
Present invention aim to provide a kind of high intensity, porous ceramic and its preparation process, porosity is high, and has
Higher mechanical strength.
To achieve the above object, the present invention is achieved by the following scheme:
A kind of preparation process of high intensity, porous ceramics, the specific steps are as follows:
(1) silicon carbide powder is made with polyvinyl alcohol tiny balloon with the ball milling mixing of mass ratio 1:0.1~0.2 and is mixed
Powder, then chemical vapor deposition nano zircite, obtains the covering body raw material of 1.1~1.2 times of mixed powder weight;
(2) cellulose acetate is dissolved in dimethyl sulfoxide, covering body raw material is added, supersonic oscillations are uniform, formed outstanding
Supernatant liquid;
(3) water is added into suspension, stirs and evenly mixs and is heated under inert atmosphere, cellulose acetate is decomposed to form Carbon deposition
Object, then heating removes a part of carbon deposits, the evolution of polyvinyl alcohol tiny balloon decomposed under an oxygen-containing atmosphere;
(4) it is sintered under inert atmosphere, then heating removes remaining carbon deposits under an oxygen-containing atmosphere, and polyvinyl alcohol is hollow
Microballoon sufficiently escapes to get a kind of high intensity, porous ceramics;
Wherein, cellulose acetate, dimethyl sulfoxide, covering body raw material, water mass ratio be 0.3~0.4:15~20:1:8
~10.
Preferably, in step (1), the ball milling mixing time is 10~15 hours.
Preferably, in step (1), the specific method of chemical vapor deposition is: it is anti-that mixed powder is put into chemical vapor deposition
Answer in room, carry out chemical vapour deposition reaction: using zirconium chloride as raw material, control material temperature is 350~370 DEG C, is passed through hydrogen
Gas and argon gas, the gas flow of hydrogen are 400~600ml/ minutes, and the gas flow of argon gas is 100~300ml/ minutes, adjustment
Reaction chamber temperature is to 800~1000 DEG C, the reaction chamber speed of rotation 30~60r/ minutes, the time 20~40 minutes, to the end of reacting,
It is cooled to room temperature taking-up.
Preferably, the oxygen-containing atmosphere is air, and the inert atmosphere is selected from nitrogen or argon gas.
Preferably, in step (3), heating condition under inert atmosphere are as follows: 1200~1300 DEG C are heated 2~3 hours;It is oxygenous
Heating condition is 1300~1400 DEG C of heating 10~15 minutes under atmosphere.
Preferably, in step (4), under inert atmosphere, sintering condition are as follows: 1300~1400 DEG C are sintered 3~5 hours.
Preferably, in step (4), under oxygen-containing atmosphere, heating condition are as follows: 1200~1300 DEG C are heated 2~3 hours.
It is further preferred that being heated to the temperature under oxygen-containing atmosphere with 20~25 DEG C/min of heating rate.Heating
The slow polyvinyl alcohol tiny balloon of speed can not shake off system constraint in a short time, and porosity is lower, but also can not be too fast, may
Cause Micro porosity to bang to collapse, influences product mechanical strength.
A kind of high intensity, porous ceramics obtained using above-mentioned preparation process.
The beneficial effects of the present invention are:
First mixed powder is made in silicon carbide powder and polyvinyl alcohol tiny balloon by the present invention, then chemical vapor deposition nanometer
Covering body raw material is made in zirconium oxide, and then covering body raw material is introduced into cellulose acetate-dimethyl sulfoxide-aqueous systems, according to
It is secondary to be heated through inert atmosphere heating, oxygen-containing atmosphere heating, inert atmosphere sintering and oxygen-containing atmosphere, polyvinyl alcohol tiny balloon and second
Acid cellulose decomposes evolution system to form hole, so that product porosity with higher, the hole of specific distribution rule
Assign the enough mechanical strengths of product;Nano zircite further functions as booster action, enhances the mechanical strength of product.
Due to polyvinyl alcohol tiny balloon is distributed between silicon carbide powder, between silicon carbide powder and nano zircite,
It makes between silicon carbide powder after escaping, forms lesser hole between silicon carbide powder and nano zircite.Acetate fiber
Element is distributed in the outside of covering body raw material, after decomposing disengaging system, can form biggish hole, two kinds of different scales on surface
Hole combine, both obtained higher porosity, in turn ensured higher mechanical strength.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Polyvinyl alcohol tiny balloon of the present invention is according to the document " preparation of polyvinyl alcohol tiny balloon and its to urea
Slow releasing function " (Shao Bing etc., Agriculture of Anhui science, 2008,36 (33), 14383-14385,14395) in method be prepared into
It arrives.
Embodiment 1
A kind of preparation process of high intensity, porous ceramics, the specific steps are as follows:
(1) mixed powder is made with mass ratio 1:0.1 ball milling mixing in silicon carbide powder and polyvinyl alcohol tiny balloon, then
Chemical vapor deposition nano zircite obtains the covering body raw material of 1.1 times of mixed powder weight;
(2) cellulose acetate is dissolved in dimethyl sulfoxide, covering body raw material is added, supersonic oscillations are uniform, formed outstanding
Supernatant liquid;
(3) water is added into suspension, stirs and evenly mixs and is heated under inert atmosphere, cellulose acetate is decomposed to form Carbon deposition
Object, then heating removes a part of carbon deposits, the evolution of polyvinyl alcohol tiny balloon decomposed under an oxygen-containing atmosphere;
(4) it is sintered under inert atmosphere, then heating removes remaining carbon deposits under an oxygen-containing atmosphere, and polyvinyl alcohol is hollow
Microballoon sufficiently escapes to get a kind of high intensity, porous ceramics;
Wherein, cellulose acetate, dimethyl sulfoxide, covering body raw material, water mass ratio be 0.3:15:1:8.
In step (1), the ball milling mixing time is 10 hours.
In step (1), the specific method of chemical vapor deposition is: mixed powder is put into chemical vapor deposition reaction chamber,
Carry out chemical vapour deposition reaction: using zirconium chloride as raw material, control material temperature is 350 DEG C, is passed through hydrogen and argon gas, hydrogen
Gas flow be 400ml/ minute, the gas flow of argon gas is 100ml/ minute, and adjustment reaction chamber temperature is reacted to 800 DEG C
Room speed of rotation 30r/ minutes the time 20 minutes, to the end of reacting, is cooled to room temperature taking-up.
Oxygen-containing atmosphere is air, and inert atmosphere is nitrogen.
In step (3), heating condition under inert atmosphere are as follows: 1200 DEG C are heated 2 hours;Heating condition is under oxygen-containing atmosphere
1300 DEG C are heated 10 minutes.
In step (4), under inert atmosphere, sintering condition are as follows: 1300 DEG C are sintered 3 hours.
In step (4), under oxygen-containing atmosphere, heating condition are as follows: 1200 DEG C are heated to 20 DEG C/min of heating rate,
It is heated 2 hours at a temperature of this.
A kind of high intensity, porous ceramics obtained using above-mentioned preparation process.
Embodiment 2
A kind of preparation process of high intensity, porous ceramics, the specific steps are as follows:
(1) mixed powder is made with mass ratio 1:0.2 ball milling mixing in silicon carbide powder and polyvinyl alcohol tiny balloon, then
Chemical vapor deposition nano zircite obtains the covering body raw material of 1.2 times of mixed powder weight;
(2) cellulose acetate is dissolved in dimethyl sulfoxide, covering body raw material is added, supersonic oscillations are uniform, formed outstanding
Supernatant liquid;
(3) water is added into suspension, stirs and evenly mixs and is heated under inert atmosphere, cellulose acetate is decomposed to form Carbon deposition
Object, then heating removes a part of carbon deposits, the evolution of polyvinyl alcohol tiny balloon decomposed under an oxygen-containing atmosphere;
(4) it is sintered under inert atmosphere, then heating removes remaining carbon deposits under an oxygen-containing atmosphere, and polyvinyl alcohol is hollow
Microballoon sufficiently escapes to get a kind of high intensity, porous ceramics;
Wherein, cellulose acetate, dimethyl sulfoxide, covering body raw material, water mass ratio be 0.4:20:1:10.
In step (1), the ball milling mixing time is 15 hours.
In step (1), the specific method of chemical vapor deposition is: mixed powder is put into chemical vapor deposition reaction chamber,
Carry out chemical vapour deposition reaction: using zirconium chloride as raw material, control material temperature is 370 DEG C, is passed through hydrogen and argon gas, hydrogen
Gas flow be 600ml/ minute, the gas flow of argon gas is 300ml/ minute, and adjustment reaction chamber temperature is reacted to 1000 DEG C
Room speed of rotation 60r/ minutes the time 40 minutes, to the end of reacting, is cooled to room temperature taking-up.
Oxygen-containing atmosphere is air, and inert atmosphere is argon gas.
In step (3), heating condition under inert atmosphere are as follows: 1300 DEG C are heated 3 hours;Heating condition is under oxygen-containing atmosphere
1400 DEG C are heated 15 minutes.
In step (4), under inert atmosphere, sintering condition are as follows: 1400 DEG C are sintered 5 hours.
In step (4), under oxygen-containing atmosphere, heating condition are as follows: 1300 DEG C are heated to 25 DEG C/min of heating rate,
It is heated 3 hours at a temperature of this.
A kind of high intensity, porous ceramics obtained using above-mentioned preparation process.
Embodiment 3
A kind of preparation process of high intensity, porous ceramics, the specific steps are as follows:
(1) mixed powder is made with mass ratio 1:0.1 ball milling mixing in silicon carbide powder and polyvinyl alcohol tiny balloon, then
Chemical vapor deposition nano zircite obtains the covering body raw material of 1.2 times of mixed powder weight;
(2) cellulose acetate is dissolved in dimethyl sulfoxide, covering body raw material is added, supersonic oscillations are uniform, formed outstanding
Supernatant liquid;
(3) water is added into suspension, stirs and evenly mixs and is heated under inert atmosphere, cellulose acetate is decomposed to form Carbon deposition
Object, then heating removes a part of carbon deposits, the evolution of polyvinyl alcohol tiny balloon decomposed under an oxygen-containing atmosphere;
(4) it is sintered under inert atmosphere, then heating removes remaining carbon deposits under an oxygen-containing atmosphere, and polyvinyl alcohol is hollow
Microballoon sufficiently escapes to get a kind of high intensity, porous ceramics;
Wherein, cellulose acetate, dimethyl sulfoxide, covering body raw material, water mass ratio be 0.3:20:1:8.
In step (1), the ball milling mixing time is 15 hours.
In step (1), the specific method of chemical vapor deposition is: mixed powder is put into chemical vapor deposition reaction chamber,
Carry out chemical vapour deposition reaction: using zirconium chloride as raw material, control material temperature is 350 DEG C, is passed through hydrogen and argon gas, hydrogen
Gas flow be 600ml/ minute, the gas flow of argon gas is 100ml/ minute, and adjustment reaction chamber temperature is reacted to 1000 DEG C
Room speed of rotation 30r/ minutes the time 40 minutes, to the end of reacting, is cooled to room temperature taking-up.
Oxygen-containing atmosphere is air, and inert atmosphere is nitrogen.
In step (3), heating condition under inert atmosphere are as follows: 1200 DEG C are heated 3 hours;Heating condition is under oxygen-containing atmosphere
1300 DEG C are heated 15 minutes.
In step (4), under inert atmosphere, sintering condition are as follows: 1300 DEG C are sintered 5 hours.
In step (4), under oxygen-containing atmosphere, heating condition are as follows: 1300 DEG C are heated to 20 DEG C/min of heating rate,
It is heated 2 hours at a temperature of this.
A kind of high intensity, porous ceramics obtained using above-mentioned preparation process.
Embodiment 4
A kind of preparation process of high intensity, porous ceramics, the specific steps are as follows:
(1) mixed powder is made with mass ratio 1:0.2 ball milling mixing in silicon carbide powder and polyvinyl alcohol tiny balloon, then
Chemical vapor deposition nano zircite obtains the covering body raw material of 1.1 times of mixed powder weight;
(2) cellulose acetate is dissolved in dimethyl sulfoxide, covering body raw material is added, supersonic oscillations are uniform, formed outstanding
Supernatant liquid;
(3) water is added into suspension, stirs and evenly mixs and is heated under inert atmosphere, cellulose acetate is decomposed to form Carbon deposition
Object, then heating removes a part of carbon deposits, the evolution of polyvinyl alcohol tiny balloon decomposed under an oxygen-containing atmosphere;
(4) it is sintered under inert atmosphere, then heating removes remaining carbon deposits under an oxygen-containing atmosphere, and polyvinyl alcohol is hollow
Microballoon sufficiently escapes to get a kind of high intensity, porous ceramics;
Wherein, cellulose acetate, dimethyl sulfoxide, covering body raw material, water mass ratio be 0.4:15:1:10.
In step (1), the ball milling mixing time is 10 hours.
In step (1), the specific method of chemical vapor deposition is: mixed powder is put into chemical vapor deposition reaction chamber,
Carry out chemical vapour deposition reaction: using zirconium chloride as raw material, control material temperature is 370 DEG C, is passed through hydrogen and argon gas, hydrogen
Gas flow be 400ml/ minute, the gas flow of argon gas is 300ml/ minute, and adjustment reaction chamber temperature is reacted to 800 DEG C
Room speed of rotation 60r/ minutes the time 20 minutes, to the end of reacting, is cooled to room temperature taking-up.
Oxygen-containing atmosphere is air, and inert atmosphere is argon gas.
In step (3), heating condition under inert atmosphere are as follows: 1300 DEG C are heated 2 hours;Heating condition is under oxygen-containing atmosphere
1400 DEG C are heated 10 minutes.
In step (4), under inert atmosphere, sintering condition are as follows: 1400 DEG C are sintered 3 hours.
In step (4), under oxygen-containing atmosphere, heating condition are as follows: 1200 DEG C are heated to 25 DEG C/min of heating rate,
It is heated 3 hours at a temperature of this.
A kind of high intensity, porous ceramics obtained using above-mentioned preparation process.
Embodiment 5
A kind of preparation process of high intensity, porous ceramics, the specific steps are as follows:
(1) mixed powder is made with mass ratio 1:0.15 ball milling mixing in silicon carbide powder and polyvinyl alcohol tiny balloon, so
Chemical vapor deposition nano zircite afterwards obtains the covering body raw material of 1.15 times of mixed powder weight;
(2) cellulose acetate is dissolved in dimethyl sulfoxide, covering body raw material is added, supersonic oscillations are uniform, formed outstanding
Supernatant liquid;
(3) water is added into suspension, stirs and evenly mixs and is heated under inert atmosphere, cellulose acetate is decomposed to form Carbon deposition
Object, then heating removes a part of carbon deposits, the evolution of polyvinyl alcohol tiny balloon decomposed under an oxygen-containing atmosphere;
(4) it is sintered under inert atmosphere, then heating removes remaining carbon deposits under an oxygen-containing atmosphere, and polyvinyl alcohol is hollow
Microballoon sufficiently escapes to get a kind of high intensity, porous ceramics;
Wherein, cellulose acetate, dimethyl sulfoxide, covering body raw material, water mass ratio be 0.35:18:1:9.
In step (1), the ball milling mixing time is 12 hours.
In step (1), the specific method of chemical vapor deposition is: mixed powder is put into chemical vapor deposition reaction chamber,
Carry out chemical vapour deposition reaction: using zirconium chloride as raw material, control material temperature is 360 DEG C, is passed through hydrogen and argon gas, hydrogen
Gas flow be 500ml/ minute, the gas flow of argon gas is 200ml/ minute, and adjustment reaction chamber temperature is reacted to 900 DEG C
Room speed of rotation 50r/ minutes the time 30 minutes, to the end of reacting, is cooled to room temperature taking-up.
Oxygen-containing atmosphere is air, and inert atmosphere is argon gas.
In step (3), heating condition under inert atmosphere are as follows: 1250 DEG C are heated 3 hours;Heating condition is under oxygen-containing atmosphere
1350 DEG C are heated 12 minutes.
In step (4), under inert atmosphere, sintering condition are as follows: 1350 DEG C are sintered 4 hours.
In step (4), under oxygen-containing atmosphere, heating condition are as follows: 1250 DEG C are heated to 22 DEG C/min of heating rate,
It is heated 3 hours at a temperature of this.
A kind of high intensity, porous ceramics obtained using above-mentioned preparation process.
Comparative example 1
A kind of preparation process of porous ceramics, the specific steps are as follows:
(1) in silicon carbide powder surface chemistry vapor deposition nano zircite, 1.15 times of carborundum powder body weights are obtained
Covering body raw material;
(2) cellulose acetate is dissolved in dimethyl sulfoxide, covering body raw material is added, supersonic oscillations are uniform, formed outstanding
Supernatant liquid;
(3) water is added into suspension, stirs and evenly mixs and is heated under inert atmosphere, cellulose acetate is decomposed to form Carbon deposition
Object, then heating removes a part of carbon deposits under an oxygen-containing atmosphere;
(4) it is sintered under inert atmosphere, then heating removes remaining carbon deposits to get a kind of porous under an oxygen-containing atmosphere
Ceramics;
Wherein, cellulose acetate, dimethyl sulfoxide, covering body raw material, water mass ratio be 0.35:18:1:9.
In step (1), the specific method of chemical vapor deposition is: silicon carbide powder is put into chemical vapor deposition reaction chamber
In, carry out chemical vapour deposition reaction: using zirconium chloride as raw material, control material temperature is 360 DEG C, is passed through hydrogen and argon gas,
The gas flow of hydrogen is 500ml/ minute, and the gas flow of argon gas is 200ml/ minutes, adjustment reaction chamber temperature to 900 DEG C,
The reaction chamber speed of rotation 50r/ minutes, the time 30 minutes, to the end of reacting, it is cooled to room temperature taking-up.
Oxygen-containing atmosphere is air, and inert atmosphere is argon gas.
In step (3), heating condition under inert atmosphere are as follows: 1250 DEG C are heated 3 hours;Heating condition is under oxygen-containing atmosphere
1350 DEG C are heated 12 minutes.
In step (4), under inert atmosphere, sintering condition are as follows: 1350 DEG C are sintered 4 hours.
In step (4), under oxygen-containing atmosphere, heating condition are as follows: 1250 DEG C are heated to 22 DEG C/min of heating rate,
It is heated 3 hours at a temperature of this.
A kind of porous ceramics obtained using above-mentioned preparation process.
Comparative example 2
A kind of preparation process of porous ceramics, the specific steps are as follows:
(1) mixed powder is made with mass ratio 1:0.15 ball milling mixing in silicon carbide powder and polyvinyl alcohol tiny balloon;
(2) cellulose acetate is dissolved in dimethyl sulfoxide, mixed powder is added, supersonic oscillations are uniform, form suspension;
(3) water is added into suspension, stirs and evenly mixs and is heated under inert atmosphere, cellulose acetate is decomposed to form Carbon deposition
Object, then heating removes a part of carbon deposits, the evolution of polyvinyl alcohol tiny balloon decomposed under an oxygen-containing atmosphere;
(4) it is sintered under inert atmosphere, then heating removes remaining carbon deposits under an oxygen-containing atmosphere, and polyvinyl alcohol is hollow
Microballoon sufficiently escapes to get a kind of porous ceramics;
Wherein, cellulose acetate, dimethyl sulfoxide, mixed powder, water mass ratio be 0.35:18:1:9.
In step (1), the ball milling mixing time is 12 hours.
Oxygen-containing atmosphere is air, and inert atmosphere is argon gas.
In step (3), heating condition under inert atmosphere are as follows: 1250 DEG C are heated 3 hours;Heating condition is under oxygen-containing atmosphere
1350 DEG C are heated 12 minutes.
In step (4), under inert atmosphere, sintering condition are as follows: 1350 DEG C are sintered 4 hours.
In step (4), under oxygen-containing atmosphere, heating condition are as follows: 1250 DEG C are heated to 22 DEG C/min of heating rate,
It is heated 3 hours at a temperature of this.
A kind of porous ceramics obtained using above-mentioned preparation process.
Test example
The porosity of detection Examples 1 to 5 and 1~2 porous ceramics of comparative example is tested using nitrogen adsorption.
According to GBT 6569-2006, using 1~2 porous ceramics of three-point bending resistance method testing example 1~5 and comparative example
Bending strength.
According to GBT 4740-1999, the compression strength of 1~2 porous ceramics of testing example 1~5 and comparative example.
Testing result is shown in Table 1.
The performance of 1. porous ceramics of table compares
Porosity (%) | Bending strength (MPa) | Compression strength (MPa) | |
Embodiment 1 | 72 | 560 | 820 |
Embodiment 2 | 71 | 565 | 820 |
Embodiment 3 | 72 | 570 | 823 |
Embodiment 4 | 72 | 570 | 825 |
Embodiment 5 | 72 | 573 | 830 |
Comparative example 1 | 41 | 560 | 820 |
Comparative example 2 | 71 | 315 | 402 |
By table 1, it could be assumed that, the porous ceramics hole rate of Examples 1 to 5 is high, high mechanical strength.Comparative example 1 is not introduced into
Polyvinyl alcohol tiny balloon, product porosity are obviously lower, and comparative example 2 is not introduced into nano zircite, and mechanical strength is obviously deteriorated.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (9)
1. a kind of preparation process of high intensity, porous ceramics, which is characterized in that specific step is as follows:
(1) mixed powder is made with the ball milling mixing of mass ratio 1:0.1~0.2 in silicon carbide powder and polyvinyl alcohol tiny balloon, so
Chemical vapor deposition nano zircite afterwards obtains the covering body raw material of 1.1~1.2 times of mixed powder weight;
(2) cellulose acetate is dissolved in dimethyl sulfoxide, covering body raw material is added, supersonic oscillations are uniform, form suspension;
(3) water is added into suspension, stirs and evenly mixs, is heated under inert atmosphere, cellulose acetate is decomposed to form carbon deposits, connects
Under an oxygen-containing atmosphere heating remove a part of carbon deposits, the evolution of polyvinyl alcohol tiny balloon decomposed.
(4) it is sintered under inert atmosphere, then heating removes remaining carbon deposits, polyvinyl alcohol tiny balloon under an oxygen-containing atmosphere
Sufficiently evolution is to get a kind of high intensity, porous ceramics.
Wherein, cellulose acetate, dimethyl sulfoxide, covering body raw material, water mass ratio about 0.3~0.4:15~20:1:8~
10。
2. preparation process according to claim 1, which is characterized in that in step (1), the ball milling mixing time is 10~15 small
When.
3. preparation process according to claim 1, which is characterized in that in step (1), the specific method of chemical vapor deposition
It is: mixed powder is put into chemical vapor deposition reaction chamber, carries out chemical vapour deposition reaction: using zirconium chloride as raw material, control
Material temperature processed is 350~370 DEG C, is passed through hydrogen and argon gas, and the gas flow of hydrogen is 400~600ml/ minutes, argon gas
Gas flow is 100~300ml/ minute, adjusts reaction chamber temperature to 800~1000 DEG C, 30~60r/ of the reaction chamber speed of rotation
Minute, the time 20~40 minutes, to the end of reacting, it is cooled to room temperature taking-up.
4. preparation process according to claim 1, which is characterized in that the oxygen-containing atmosphere is air, the inert atmosphere
Selected from nitrogen or argon gas.
5. preparation process according to claim 1, which is characterized in that in step (3), heating condition under inert atmosphere are as follows:
1200~1300 DEG C are heated 2~3 hours;Heating condition is 1300~1400 DEG C of heating 10~15 minutes under oxygen-containing atmosphere.
6. preparation process according to claim 1, which is characterized in that in step (4), under inert atmosphere, sintering condition are as follows:
1300~1400 DEG C are sintered 3~5 hours.
7. preparation process according to claim 1, which is characterized in that in step (4), under oxygen-containing atmosphere, heating condition are as follows:
1200~1300 DEG C are heated 2~3 hours.
8. preparation process according to claim 1, which is characterized in that under oxygen-containing atmosphere, with 20~25 DEG C/min of heating
Rate is heated to the temperature.
9. a kind of high intensity, porous ceramics obtained using preparation process described in any one of claim 1~8.
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