CN109133931B - Can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics - Google Patents
Can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics Download PDFInfo
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- CN109133931B CN109133931B CN201811076386.9A CN201811076386A CN109133931B CN 109133931 B CN109133931 B CN 109133931B CN 201811076386 A CN201811076386 A CN 201811076386A CN 109133931 B CN109133931 B CN 109133931B
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Abstract
The invention discloses a kind of can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics.After this method is fully ground mixing to can be thermally cured two kinds of materials of characteristic Polycarbosilane and polyurethane, it is added in mold, apply certain pressure, gas inside discharge powder obtains precast body, the foam preform is heat-treated again, the self-crosslinking solidification for realizing Polycarbosilane, high temperature pyrolysis is finally carried out in argon atmosphere, obtains foamed ceramics.The preparation method is simple, and process flow is few, at low cost, avoids the use of solvent, is conducive to environmental protection, and the foamed ceramics linear shrinkage ratio prepared is small by 10%, the small 0.6g/cm of bulk density3, between 60%~90%, flexural strength can use open porosity up to 1.0~2.6MPa in 1200 DEG C~1400 DEG C long-times.
Description
Technical field
The invention belongs to ceramic foam technical fields, and in particular to a kind of can be thermally cured Polycarbosilane and polyurethane preparation
The preparation method of foam silicon carbide ceramics.
Background technique
Traditional foam silicon carbide ceramics preparation process is complicated, mainly with silicon carbide powder and dispersing agent, sintering aid
Slurry is made in equal blendings, then impregnates to obtain precast body with organic foam template, and precast body is burnt through processes such as drying, exclusion organic matters
At obtaining foam silicon carbide ceramics.(liquid phase when Liang Hanqin, Yao Xiumin, Huang Zhengren, Liu Xuejian silicon carbide ceramics liquid-phase sintering
Generating process [J] mechanical engineering material, 2015,39 (02): 34-37.；) Liang Hanqin has studied SiC foam ceramic post sintering mechanism:
SiC foam ceramics are mainly that glass phase generates the cladding of SiC particulate, connection function and cenotype mullite.And sintering aid
Introducing is also unfavorable for preparing SiC amount of substance than similar foam silicon carbide ceramics.Excessively high sintering temperature can generate big ashlar
Ying Xiang influences the intensity of material to micro-crack occur in later cooling procedure.
In recent decades, polymer precursor, such as Polycarbosilane, polysilazane, as the forerunner for preparing ceramic material
Body causes the great interest of people in recent years, and in 105272266 A of patent CN, Li Siwei only uses Polycarbosilane as foam
The precursor of ceramics prepares slurry with solvent xylene, using processed polyurethane foam as template, hanging product is made, first
By pre-oxidation treatment in convection oven, then through being sintered to obtain sic foam in high temperature furnace.Contain in its foamed ceramics prepared
The oxygen of 8wt% or more, oxygen exist with SiOxCy phase., at 600 DEG C or more, violent decomposition reaction, such as following formula occur for SiOxCy for it
It is shown.
SiOxCy→SiC(s)+CO(g)+SiO(g)
The above decomposition reaction leads to the strength damage of foamed ceramics skeleton, and the use temperature for limiting foam silicon carbide ceramics exists
600 DEG C or less.
The prior art is summarized: being made into slurry with silicon-carbide particle and binder and solvent, is with the organic matter of foaming structure
Template after dipping, is sintered, but disadvantage is obvious at 1300 DEG C or so: the uniformity of slurry it is difficult to ensure that, preparation process has
The use of solvent, is unfavorable for environmental protection；Using organic silane compound Polycarbosilane as precursor, polymer-derived method prepares foam pottery
Porcelain, this part research is rare, and technology waits to develop.
Summary of the invention
Status in view of the above technology, the present invention is intended to provide a kind of can be thermally cured Polycarbosilane and polyurethane preparation carbonization
The preparation method of silicon foam ceramics.
In order to achieve the above technical purposes, at a certain temperature, be fully ground can be thermally cured Polycarbosilane and gathers the present invention
Two kinds of materials of urethane, obtain uniformly mixed powder.Powder is added in mold again, certain pressure is applied to mold, powder is discharged
The gas in internal portion obtains precast body, in argon atmosphere, is heat-treated to the precast body, in the process, polyurethane is not
Any chemical reaction and thawing, gasification etc. occurs, completes the self-crosslinking solidification of Polycarbosilane, obtains foam preform.Finally
High temperature pyrolysis is carried out to foam preform in argon atmosphere, in the process, foaming does not occur and serious volume contraction is existing
As.Polyurethane decomposes completely, and quality noresidue leaves volume, causes hole.It can be thermally cured Polycarbosilane and be changed into carbonization
Silicon ceramics, finally obtain foam silicon carbide ceramics.This foamed ceramics compact structure, can be in 1400 DEG C of long-time applications.
That is, the technical solution of the present invention is as follows: one kind can be thermally cured Polycarbosilane and polyurethane prepares foam silicon carbide ceramics
Preparation method, include the following steps:
(1) it under certain temperature, is fully ground and can be thermally cured Polycarbosilane and polyurethane, obtain powder；
(2) mold is added in powder, applies pressure, and the gas inside powder is discharged, foam preform is obtained, in argon atmosphere
In foam preform is heat-treated, realize that the self-crosslinking of heat cure Polycarbosilane solidify and the removing of solvent；
(3) in argon atmosphere, foam preform is heat-treated, realizes that the self-crosslinking of heat cure Polycarbosilane is solid
Change；
(4) in argon atmosphere, high temperature pyrolysis is carried out to the foam preform of crosslinking curing, obtains sic foam pottery
Porcelain；
Further, the step (1) is used as a kind of implementation, and detailed process is as follows: in the step (1), specific mistake
Journey is as follows:
It is mixed with can be thermally cured Polycarbosilane and polyurethane in ball grinder high speed cryogrinding, the powder being uniformly mixed
Body.
Preferably, the grinding temperature is not higher than 60 DEG C；
Preferably, the heat cure Polycarbosilane only contains three kinds of silicon, carbon, hydrogen elements；
Preferably, can be thermally cured Polycarbosilane is: Polycarbosilane (it is synthesized by the rearrangement of polydimethylsiloxane Pintsch process,
220~230 DEG C of softening point) and alkenyl silanes obtained by hydrosilylation.The amount of heat cure Polycarbosilane medium vinyl accounts for
The 20~50% of the si-h bond content of Polycarbosilane.
Further, the step (2) is used as a kind of implementation, and detailed process is as follows: mould is added in the powder mixed
In tool, apply pressure, after the gas inside powder is discharged, obtains precast body；
Preferably, the mould inside shape is unlimited, tubulose can be, rodlike, sheet or other geometrical morphologies；
Preferably, the pressure is 0.2~6MPa；
Further, a kind of implementation is used as in the step (3), detailed process is as follows: by precast body in argon atmosphere
In, 200 DEG C~300 DEG C are warming up to 1 DEG C/min~5 DEG C/min heating rate, keeps the temperature 1.5h~15h.
Further, in the step (4), as a kind of implementation, detailed process is as follows: by step (3), treated
Precast body under an argon atmosphere, with 1 DEG C/min~30 DEG C/min heating rate, is heated to 1100 DEG C~1200 DEG C, heat preservation
It 0.5h~5h hours, then cools to room temperature, obtains foamed ceramics.
Preferably, the foamed ceramics linear shrinkage ratio prepared is less than 10%, the small 0.6g/cm of bulk density3, open porosity
Between 20%~90%, flexural strength is up to 1.0~2.6Mpa.
The present invention is using heat cure Polycarbosilane (PVCS) and polyurethane as raw material, as shown in Figure 1, in order to realize above-mentioned technology
Purpose, the present invention at a certain temperature, are fully ground and can be thermally cured two kinds of materials of Polycarbosilane polyurethane, obtain uniformly mixed
Powder.Powder is added in mold again, certain pressure is applied to mold, the gas inside powder is discharged and obtains precast body, in argon
In gas atmosphere, which is heat-treated, in the process, any chemical reaction does not occur for polyurethane powder and polyurethane
With melt, gasification etc., complete Polycarbosilane self-crosslinking solidification, obtain foam preform.Finally to bubble in argon atmosphere
Foam precast body carries out high temperature pyrolysis, in the process, foaming and serious volume contraction phenomenon does not occur, polyurethane divides completely
Solution, quality noresidue leave volume, cause hole, can be thermally cured Polycarbosilane and be changed into silicon carbide ceramics and a small amount of carbon,
Finally obtain the foam silicon carbide ceramics of compact structure.
The present invention compared to the prior art the advantages of:
1, the present invention is simple using the raw material preparation process that is easy to get: Polycarbosilane commercial product, the preparation of heat cure Polycarbosilane
Process is simple, is easy to get, polyurethane, and commercial product is easy to get.
2, in preparation process of the present invention, solvent is not used, environmental protection is conducive to；
3, preparation process of the present invention is simple, can prepare the foamed ceramics structural member of different morphologies；
4, foam silicon carbide ceramics porosity of the present invention is controllable；
5, the foamed ceramics intensity that the present invention is prepared is high, and heat resistance is excellent.
Detailed description of the invention
Fig. 1 is the preparation flow signal that the present invention can be thermally cured Polycarbosilane and polyurethane prepares foam silicon carbide ceramics
Figure；
Fig. 2 is polyurethane and foamed ceramics porosity.
Specific embodiment
Below with reference to embodiment, present invention is further described in detail, it should be pointed out that embodiment described below purport
It is being convenient for the understanding of the present invention, and is not playing any restriction effect to it.
Embodiment 1:
With can be thermally cured Polycarbosilane and polyurethane prepare foam silicon carbide ceramics preparation process it is as follows:
(1) one of raw material can be thermally cured the preparation of Polycarbosilane
The preparation that can be thermally cured Polycarbosilane, with reference to (Gu Xishuan, Song Yongcai can be thermally cured the synthesis and property of Polycarbosilane
Can [J] organosilicon material, 2015,29 (6): 462-468.): by Polycarbosilane (commercially available, molecular weight 2800,220 DEG C of softening point,
Molecular weight 1700) be dissolved in dimethylbenzene with dimethyl divinyl silane (commercially available) l:l in mass ratio, be placed in autoclave, add
Enter platinum catalyst, vacuumizes displacement high pure nitrogen, plus-pressure to 12.5MPa；110 are heated under high pure nitrogen protection again
DEG C reaction 30h；Cooling, vacuum distillation obtains solid product PVCS.
Through characterizing, the amount of heat cure Polycarbosilane medium vinyl accounts for the 22% of the si-h bond content of Polycarbosilane, can thermosetting
The molecular weight for changing Polycarbosilane is that 1880, PVCS is handled to 400 DEG C in nitrogen atmosphere, it can be achieved that fully crosslinked solidification, gel
Content reaches 100%, and the Polycarbosilane after crosslinking curing turned Shi Bufa to silicon carbide ceramics in being pyrolyzed at 1100~1200 DEG C
Phenomena such as germ-vesicle, flowing, volume shrinkage phenomenon only occurs, finally obtain fine and close silicon carbide ceramics, ceramic yield is up to 78%.
(2) mixed raw material
Mass ratio, PVCS: polyurethane 1:0.3, at 30 DEG C, in argon atmosphere, it is sufficiently mixed and grinds both the above material, obtain
To uniformly mixed powder.
(3) plastotype
Powder is added in mold, and internal morphology is disc-shape, applies 0.3Mpa pressure, and the gas inside powder is discharged,
Obtain foam preform.
(4) it is heat-treated organic foam precast body
Organic foam precast body is put into furnace, after vacuumizing displacement high pure nitrogen three times, by organic foam in argon gas gas
In atmosphere, 220 DEG C are warming up to the heating rate of 3 DEG C/min, keeps the temperature 3h.
(5) high temperature pyrolysis prepares foamed ceramics
In argon atmosphere, under an argon atmosphere by step (3) treated precast body, with the heating speed of 1 DEG C/min
Rate is heated to 1100 DEG C, keeps the temperature 4h hours, then cools to room temperature, obtain black bright foamed ceramics.Bulk density 0.6g/
cm3, open porosity 68%, flexural strength reach 2.6MPa.
Embodiment 2:
With can be thermally cured Polycarbosilane and polyurethane prepare foam silicon carbide ceramics preparation process it is as follows:
(1) one of raw material can be thermally cured the preparation of Polycarbosilane
The preparation that can be thermally cured Polycarbosilane, with reference to (Gu Xishuan, Song Yongcai can be thermally cured the synthesis and property of Polycarbosilane
Can [J] organosilicon material, 2015,29 (6): 462-468.): by Polycarbosilane (commercially available, molecular weight 2800,240 DEG C of softening point,
Molecular weight 1900) be dissolved in dimethylbenzene with dimethyl divinyl silane (commercially available) l:l in mass ratio, be placed in autoclave, add
Enter platinum catalyst, vacuumizes displacement high pure nitrogen, plus-pressure to 12.5MPa；110 are heated under high pure nitrogen protection again
DEG C reaction 30h；Cooling, vacuum distillation obtains solid product PVCS.
Through characterizing, the amount of heat cure Polycarbosilane medium vinyl accounts for the 21% of the si-h bond content of Polycarbosilane, can thermosetting
The molecular weight for changing Polycarbosilane is that 2119, PVCS is handled to 400 DEG C in nitrogen atmosphere, it can be achieved that fully crosslinked solidification, gel
Content reaches 100%, and the Polycarbosilane after crosslinking curing turned Shi Bufa to silicon carbide ceramics in being pyrolyzed at 1100~1200 DEG C
Phenomena such as germ-vesicle, flowing, volume shrinkage phenomenon only occurs, finally obtain fine and close silicon carbide ceramics, ceramic yield is up to 79%.
(2) raw material is ground
Mass ratio, PVCS: polyurethane 1:0.3, at 30 DEG C, in argon atmosphere, it is sufficiently mixed and grinds with two kinds of materials, obtain
Uniformly mixed powder.
(3) plastotype
Powder is added in mold, and internal morphology is square shape, applies 0.5Mpa pressure, and the gas inside powder is discharged
Body obtains foam preform.
(4) it is heat-treated organic foam precast body
Organic foam precast body is put into furnace, after vacuumizing displacement high pure nitrogen three times, by organic foam in argon gas gas
In atmosphere, 220 DEG C are warming up to the heating rate of 2 DEG C/min, keeps the temperature 6h.
(5) high temperature pyrolysis prepares foamed ceramics
In argon atmosphere, under an argon atmosphere by step (3) treated precast body, with the heating speed of 3 DEG C/min
Rate is heated to 1150 DEG C, keeps the temperature 3h hours, then cools to room temperature, obtain black bright foamed ceramics.Bulk density 0.5g/
cm3, open porosity 81%, flexural strength reach 2.2MPa.
Embodiment 3:
With can be thermally cured Polycarbosilane and polyurethane prepare foam silicon carbide ceramics preparation process it is as follows:
(1) it can be thermally cured Polycarbosilane using prepared in embodiment one.
(2) raw material is ground
Mass ratio, PVCS: polyurethane 1:0.6, at 30 DEG C, in argon atmosphere, it is sufficiently mixed and grinds both the above material, obtain
To uniformly mixed powder.
(3) plastotype
Powder is added in mold, and internal morphology is cylindrical shape, applies 0.3Mpa pressure, and the gas inside powder is discharged,
Obtain foam preform.
(4) it is heat-treated organic foam precast body
Organic foam precast body is put into furnace, after vacuumizing displacement high pure nitrogen three times, by organic foam in argon gas gas
In atmosphere, 220 DEG C are warming up to the heating rate of 2 DEG C/min, keeps the temperature 6h.
(5) high temperature pyrolysis prepares silicon carbide-carbon aluminum foam ceramics
In argon atmosphere, under an argon atmosphere by step (3) treated precast body, with the heating speed of 5 DEG C/min
Rate is heated to 1200 DEG C, keeps the temperature 6h hours, then cools to room temperature, obtain black bright foamed ceramics.Bulk density 0.4g/
cm3, open porosity 89%, flexural strength reach 1.5MPa.
Claims (8)
1. it is a kind of can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics, it is characterized in that: including such as
Lower step:
Step 1 will can be thermally cured Polycarbosilane and polyurethane is ground, the powder being uniformly mixed；Described can thermosetting
Changing Polycarbosilane is: Polycarbosilane and vinyl silanes are obtained by hydrosilylation；Heat cure Polycarbosilane medium vinyl
Amount account for Polycarbosilane si-h bond content 20~50%；Polycarbosilane molecular weight 1700~1900, softening point 220~240
DEG C, it is synthesized by the rearrangement of polydimethylsiloxane Pintsch process；The heat cure Polycarbosilane only contains three kinds of silicon, carbon, hydrogen elements；
The powder mixed is added in mold step 2, applies pressure, the gas inside powder is discharged, obtains precast body；
Step 3 is heat-treated precast body in argon atmosphere, realizes the self-crosslinking solidification that can be thermally cured Polycarbosilane；
Step 4 carries out high temperature pyrolysis to the precast body after crosslinking curing in argon atmosphere, obtains foamed ceramics.
2. as described in claim 1 can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics,
Be characterized in: in the step 1, detailed process is as follows:
It is mixed with can be thermally cured Polycarbosilane and polyurethane in ball grinder high speed cryogrinding, the powder being uniformly mixed；
It can be thermally cured mass ratio 1:0.3~0.6 of Polycarbosilane and polyurethane；Grinding temperature is not higher than 60 DEG C.
3. as claimed in claim 1 or 2 can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics,
It is characterized in that: detailed process is as follows in the step 2: the powder mixed being added in mold, pressure is applied, powder is discharged
After internal gas, precast body is obtained, the pressure is 0.2~6MPa.
4. as described in claim 1 can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics,
Be characterized in: in the step 3, detailed process is as follows: by precast body in argon atmosphere, with 1 DEG C/min~5 DEG C/min heating
Rate is warming up to 200 DEG C~300 DEG C, keeps the temperature 1.5h~15h.
5. as described in claim 1 can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics,
Be characterized in: in the step 4, detailed process is as follows: under an argon atmosphere by step 3 treated precast body, with 1 DEG C/min~
The heating rate of 30 DEG C/min is heated to 1100 DEG C~1200 DEG C, keeps the temperature 0.5h~5h hours, then cools to room temperature, obtain
Foam silicon carbide ceramics.
6. as claimed in claim 5 can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics,
Be characterized in: in the step 4, the foamed ceramics linear shrinkage ratio prepared is less than 10%, the small 0.6g/cm of bulk density3, open pore
Rate is between 60%~90%, and flexural strength is up to 1.0~2.6MP a.
7. as claimed in claim 5 can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics,
Be characterized in: in the step 4, the foamed ceramics prepared is used in 1200 DEG C~1400 DEG C long-times.
8. a kind of foam silicon carbide ceramics, it is characterised in that: be made using method described in any one of claim 1-7.
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| CN103011887A (en) * | 2011-09-28 | 2013-04-03 | 贵州师范大学 | Silicon carbide foamed ceramics and preparation method thereof |
| CN105272266A (en) * | 2015-11-27 | 2016-01-27 | 厦门大学 | Preparation method of precursor converted silicon carbide foam ceramics |
| CN108069725A (en) * | 2016-11-09 | 2018-05-25 | 中国科学院金属研究所 | A kind of hollow foam material and its preparation method and application |
| CN107500732A (en) * | 2017-08-10 | 2017-12-22 | 浙江大学 | A kind of method for preparing three-D inorganic ceramics |
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