CN105272266A - Preparation method of precursor converted silicon carbide foam ceramics - Google Patents
Preparation method of precursor converted silicon carbide foam ceramics Download PDFInfo
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- CN105272266A CN105272266A CN201510851884.6A CN201510851884A CN105272266A CN 105272266 A CN105272266 A CN 105272266A CN 201510851884 A CN201510851884 A CN 201510851884A CN 105272266 A CN105272266 A CN 105272266A
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Abstract
The invention discloses a preparation method of precursor converted silicon carbide foam ceramics, relating to silicon carbide foam ceramics. The preparation method comprises the steps of preparing solid polycarbosilane; mixing solid polycarbosilane and a dimethylbenzene solution to obtain slurry A; standing organic polyurethane foam into a sodium hydroxide solution, removing redundant a film among the organic foam, cleaning after taking out the foam to obtain a pretreated organic polyurethane foam template, then, placing the organic polyurethane foam template into the slurry A, rolling, soaking the foam template in the slurry A, and discharging the redundant slurry A to obtain a slurry-coated product A; adding dimethylbenzene into solid polycarbosilane to obtain slurry B; soaking the slurry-coated product into the slurry B, and centrifuging to obtain a slurry-coated product B; placing the slurry-coated product B into an air drying oven, and heating to 180-200 DEG C in flowing air to obtain a product G; and placing the product G into a high-temperature furnace, heating to 500 DEG C at the atmosphere of N2 and the speed of 2 DEG C/min, and heating to 800-1200 DEG C at the speed of 5 DEG C/min to obtain the precursor converted silicon carbide foam ceramics.
Description
Technical field
The present invention relates to foam silicon carbide ceramics, especially relate to a kind of preparation method of polymer pyrolysis foam silicon carbide ceramics.
Background technology
Silicon carbide (SiC) foamed ceramics is owing to having hypertonicity, high-specific surface area, low density, lower thermal conductivity, the characteristic such as high temperature resistant, corrosion-resistant, metallic filter, support of the catalyst, heat-insulating and energy-saving can be widely used in, abate the noise and the field (Zhu Xinwen such as biological implantation, the east of a river is bright, Foam dipping method-a kind of economical and practical porous ceramics preparation technology, silicate is circulated a notice of, 2000,3:45-51; Cai Hongyu, He Xiulan, Tang Lina. the microstructure of foam silicon carbide ceramics and mechanical property research [J]. Chinese pottery, 2013,5 (49): 22-24; KIMYW, JINYJ.EngineeringPorosityinSiliconCarbideCeramics [J] .JournalofMaterialsScience, 2010,45:2808-2815; Li Junfeng, Lin Hong, carborundum porous ceramics void content and intensity effect factor [J].Journal of Inorganic Materials, 2011,26 (9): 32-35).Adopting Polymeric sponge method to prepare foamed ceramics is the most popular method of current suitability for industrialized production.The Polymeric sponge method of current report is with SiC ceramic mud for raw material mostly, by its hanging in organic foam pattern plates such as urethane, then by some row operations such as the demoulding, sintering, finally obtains SiC foam pottery.
Because SiC is strong covalent bond structure, bond energy is high, and self-diffusion coefficient is low, makes SiC ceramic slurry be difficult at low temperatures sinter goods into, which limits the application that ceramic mud conversion method prepares foamed ceramics.In addition, some are had to the silicon carbide system foamed ceramics (PColombo of special chemical composition, MModesti, SiliconOxycarbideCeramicFoamsfromaPreceramicPolymer [J] .J.Am.Ceram.Soc., 1999, 82 (3): 573-578) as SiOC, SiOCN etc., they have good mechanical property usually, high-temperature stability, anti-oxidant and erosion resistance, a kind of potential thermal structure and function application material (Tian Hao, Hu Pingchun, horse pine, precursor pyrolysis and hot pressing prepares the current situation of foamed ceramics, silicate is circulated a notice of, 2011, 30 (2): 362-366), but ceramic mud conversion method traditionally cannot prepare the foamed ceramics of this metastable phase.Therefore, explore and develop the striving direction that new method for preparing foamed ceramics becomes domestic and international foamed ceramics investigator.It is a kind of novel process just occurred for 20 end of the centurys that precursor pyrolysis and hot pressing prepares foamed ceramics, and the advantages such as it has, and preparation temperature is low, pottery composition can design, plastic complex component, become a study hotspot in current method for preparing foamed ceramics.This method is for template with organic foam (as urethane), the mixed solution of ceramic precursor and ceramic is slurry, foamed ceramics preform is obtained through hanging, roll-in (or centrifugal), drying, last under certain temperature increasing schedule plastic removal, burn till, obtain foamed ceramics.(the NangrejoMR such as Nanggrejo, BaoX, EdirisingheMJ.Siliconcarbide-titaniumcarbidecompositefoa msproducedusingapolymericprecursor [J] .J.InorganicMater., 2001,3:37-45; NangrejoMR, BaoX, EdirisingheMJ.Preparationofsiliconcarbide – siliconnitridecompositefoamsfrompre-ceramicpolymers [J] .J.Eur.Ceram.Soc., 2000,20:1777-1785) take urethane as template, polysilane is precursor, TiC and Si
3n
4micro mist is filler, has prepared SiC-TiC and SiC-Si respectively
3n
4complex phase foamed ceramics.The foamed ceramics of preparation is obvious open-celled structure, without macroscopic defect in the muscle of hole.Controlling contraction, the void content of foams by controlling the concentration of precursor, filler content and sintering temperature, making the void content of gained foamed ceramics between 85% ~ 96%, and not changing lower than under the high temperature of 1600 DEG C.Domestic, (the Liu Hongli such as Liu Hongli, clock is civil and military, Gao Jing, Deng. nano-SiC filler is on the impact [J] of SiOC foamed ceramics performance. foundry engieering, 2008,29 (5): 597-600) different types of precursor (comprising filler) is chosen, prepare the silicon carbide-based foamed ceramics (SiOC, SiOC-SiC) of different composition according to the method described above, by the structure and the performance that control the cracking temperature of precursor, the processing parameter such as content, dipping-cracking enhancement process number of times of filler controls foamed ceramics.The foamed ceramics of preparation is tridimensional network, and hole muscle is fine and close, and connectivity is good, and porosity is between 80% ~ 88%, and pore diameter range is at 100 ~ 500 μm.
At present, polymer pyrolysis prepares the technological line that porous silicon carbide ceramic research relates to, although played the advantage that organic precursor method adhesive property is good, ceramming temperature is low to a certain extent, but slurry feedstock need comprise one or more ceramic powders as aggregate, and this certainly will add raw materials cost; In the process of configuration slurry, inorganic powder aggregate and organic precursor method be difficult to the mixed effect reaching high uniformity.In addition, the interface uncompatibility of ceramic size and organic formwork also significantly suppress the performance boost of foamed ceramics goods.
Summary of the invention
The object of this invention is to provide without the need to adding ceramic powder, technique is simple, with low cost, is applicable to the preparation method of a kind of polymer pyrolysis foam silicon carbide ceramics of high-performance silicon carbide foamed ceramics.
The present invention includes following steps:
1) solid-state Polycarbosilane is prepared;
2) solid-state Polycarbosilane is mixed with xylene solution, obtain slurry A;
3) urethane organic foam is placed in sodium hydroxide solution to leave standstill, removes film between unnecessary organic foam, then foam is taken out, clean, obtain pretreated urethane organic foam pattern plate;
4) by step 3) pretreated urethane organic foam pattern plate is placed in step 2) gained slurry A, flat plate mold is utilized repeatedly to roll, make slurry A infiltrate pretreated urethane organic foam pattern plate, then get rid of additional size A, form hanging product A;
5) continue to add dimethylbenzene in solid-state Polycarbosilane, obtain slurry B;
6) hanging product is placed in slurry B to flood, centrifugal, obtain hanging product B, complete secondary hanging;
7) hanging product B is put into convection oven, in fluidizing air, be warmed up to 180 ~ 200 DEG C, and be incubated 1 ~ 5h, make slurry crosslinking curing, obtain product G;
8) product G is put into High Temperature Furnaces Heating Apparatus, then at N
2be warming up to 500 DEG C with the speed of 2 DEG C/min under atmosphere, then be warming up to 800 ~ 1200 DEG C with the speed of 5 DEG C/min, insulation 0.5 ~ 5h, obtains polymer pyrolysis foam silicon carbide ceramics.
In step 1) in, the solid-state Polycarbosilane of described preparation can adopt Yajima (S.Yajima, J.HayashiandM.Omori, ChemicalLetters, method 1975:931) prepares solid-state Polycarbosilane, the number-average molecular weight Mn of described solid-state Polycarbosilane can be 900 ~ 1200, and softening temperature can be 180 ~ 250 DEG C.
In step 2) in, the viscosity of described slurry A can be 1 ~ 3PaS.
In step 3) in, described urethane organic foam can adopt aperture to be the urethane organic foam of 0.2 ~ 0.8mm; The mass percentage concentration of described sodium hydroxide solution can be 15%; The described standing time can be 2 ~ 5h.
In step 4) in, described eliminating additional size A can adopt to roll and get rid of additional size A, then left at room temperature 24h in atmosphere; Or
Adopt centrifugal eliminating additional size A, then dry more than 5h at 80 DEG C.
In step 5) in, the viscosity of described slurry B can be 0.3 ~ 2PaS.
In step 6) in, the time of described dipping can be more than 20min; Described complete secondary hanging can in atmosphere left at room temperature 24h or 80 DEG C dry more than 5h.
In step 7) in, the speed of described intensification can be 1 DEG C/min; Described PCS in slurry crosslinking curing is oxidized, Si-H key oxidized formation Si-O key, cause producing chemically crosslinked between different PCS molecule, make thermoplastic PCS become thermoset, avoid slurry to melt in follow-up high-temperature heat treatment process and the structure of not reproducible base body die plate.
Standard GB/T/T1966-1996 can be utilized to test its apparent porosity and unit weight.
The invention provides a kind of without the need to adding ceramic aggregate, by adjustment organic precursor method and solvent burden ratio, utilizing precursor and solvent directly to prepare slurry, preparing the novel method of foamed ceramics.The method technique is simple, cost is low, foamed ceramics product properties is good, can be used as metallic filter, support of the catalyst and sound-absorbing material etc., have the potentiality of commercial application.
By regulating the proportioning of organic precursor method and solvent, obtaining the slurry of suitable viscosity (solid content), by its hanging in organic foam pattern plate, then by slurry curing, the demoulding and easy fired operation, obtaining the foam silicon carbide ceramics that performance is controlled.
With existing foam silicon carbide ceramics technics comparing, the invention has the beneficial effects as follows:
(1) ceramic aggregate is not added, directly form the adjustable slurry of viscosity by the proportioning of the solid-state PCS precursor of regulation and control and xylene solvent, by follow-up hanging, solidification, the demoulding and thermal treatment, below 1000 DEG C, prepare even structure, high performance foamed ceramics, technique is simple, raw materials cost is low, technical risk is low;
(2) Polycarbosilane slurry is in atmosphere after solidification treatment, introduces the oxygen of more than 8wt% in the molecular structure.Thus after high-temperature heat treatment completes, also containing the oxygen of more than the 10wt% that has an appointment in foamed ceramics, ceramic structure is that RESEARCH OF PYROCARBON and the disperse of SiC crystallite are in the structure of amorphous Si-C-O.Compared with pure SiC structure, the homogeneity of this non-crystal structure is higher, has good mechanical property, and the Heat stability is good below 1000 DEG C, be a kind of novel high-temperature structural material.
(3) by adjustment crosslinking curing temperature and soaking time, the oxygen level of foamed ceramics can be changed, thus regulation and control foamed ceramics microtexture, finally realize the regulation and control to its conductivity, heat conductivility.
(4) at certain temperature and heat-retaining condition, steady phase SiC is pressed
xoy decomposes according to following reaction equation further:
SiC
xO
y→SiC+CO+SiO
The meeting then producing gas is formed nanometer level microporous in ceramic structure, by adjustment thermal treatment process (pyrolysis temperature in right amount low, soaking time is grown in right amount), can the nanometer level microporous of decomposing gas generation be retained in ceramic structure, and then form the complex construction that comprises across yardstick aperture, widen its application as porous ceramic film material further.
Accompanying drawing explanation
Fig. 1 prepares SiC foam pottery fracture SEM photo for utilizing polymer pyrolysis technique.In FIG, (a) is low power image; B () is high power image.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
(1) adopt Yajima route to prepare solid-state Polycarbosilane (A), the number-average molecular weight that gel permeation chromatograph (GPC) records is Mn=996, and the fusing point that melting point apparatus records is 191 DEG C.
(2) 30g (A) is placed in 30ml dimethylbenzene, ultrasonic 10min, then magnetic agitation 30min again, until the two mixes, namely forms the transparent slurry (B) of viscosity 1.5PaS.
(3) by aperture be the urethane organic foam of 0.5mm, cut out the sample for 10mm × 10mm × 10mm, be placed in the standing 2.5h of sodium hydroxide solution that concentration is 15%, then taken out, clean, obtain pretreated urethane organic foam pattern plate (C).
(4) (C) is placed in (B), utilizes dull and stereotyped grinding tool repeatedly to roll to make slurry to infiltrate organic formwork, then by rolling eliminating additional size, then left at room temperature 24h in atmosphere, forms hanging product (D).
(5) separately get (A) 30g, add 60ml dimethylbenzene wherein, form the slurry (E) that viscosity is 0.8PaS
(6) (D) is placed in (E), leaves standstill 20min, utilize centrifuging process, complete secondary hanging, then dry more than 5h at 80 DEG C, form hanging product (F).
(7) (F) is put into convection oven, in fluidizing air, be warmed up to 200 DEG C with the speed of 1 DEG C/min, and at 200 DEG C of insulation 3h, make slurry curing, obtain product (G).
(8) (G) is put into High Temperature Furnaces Heating Apparatus, then at N
2be warming up to 500 DEG C with 2 DEG C/min under atmosphere, be warming up to 900 DEG C with 5 DEG C/min, insulation 1h, obtains foamed ceramics (H).
As shown in Figure 1, the SiC foam pottery of gained is divided into millimeter grade hole, and (figure a) and nano grade pore (figure b), footpaths at different levels even aperture distribution for scanning electronic microscope (SEM) observations.
Apparent porosity test display, the apparent porosity of this foamed ceramics is 85%; Intensity test result shows, and the ultimate compression strength of this foamed ceramics is 1.6MPa.Fig. 1 is the fracture sample scans electron micrograph through compressive strength test.The SiC foam pottery of visible gained is divided into millimeter grade hole, and (figure a) and nano grade pore (figure b), the even aperture distribution in hole at different levels.
Embodiment 2
Step (1) ~ (7) are with embodiment 1.
(8) front 7 steps are obtained product and put into High Temperature Furnaces Heating Apparatus, then at N
2be warming up to 500 degree with 2 DEG C/min under atmosphere, be warming up to 800 DEG C with 5 DEG C/min, insulation 1h, obtains foamed ceramics (I).
Embodiment 3
Step (1) ~ (7) are with embodiment 1.
(8) front 7 steps are obtained product and put into High Temperature Furnaces Heating Apparatus, then at N
2be warming up to 500 degree with 2 DEG C/min under atmosphere, be warming up to 1200 DEG C with 5 DEG C/min, insulation 1h, obtains foamed ceramics (J).
Claims (10)
1. a preparation method for polymer pyrolysis foam silicon carbide ceramics, is characterized in that comprising the following steps:
1) solid-state Polycarbosilane is prepared;
2) solid-state Polycarbosilane is mixed with xylene solution, obtain slurry A;
3) urethane organic foam is placed in sodium hydroxide solution to leave standstill, removes film between unnecessary organic foam, then foam is taken out, clean, obtain pretreated urethane organic foam pattern plate;
4) by step 3) pretreated urethane organic foam pattern plate is placed in step 2) gained slurry A, flat plate mold is utilized repeatedly to roll, make slurry A infiltrate pretreated urethane organic foam pattern plate, then get rid of additional size A, form hanging product A;
5) continue to add dimethylbenzene in solid-state Polycarbosilane, obtain slurry B;
6) hanging product is placed in slurry B to flood, centrifugal, obtain hanging product B, complete secondary hanging;
7) hanging product B is put into convection oven, in fluidizing air, be warmed up to 180 ~ 200 DEG C, and be incubated 1 ~ 5h, make slurry crosslinking curing, obtain product G;
8) product G is put into High Temperature Furnaces Heating Apparatus, then at N
2be warming up to 500 DEG C with the speed of 2 DEG C/min under atmosphere, then be warming up to 800 ~ 1200 DEG C with the speed of 5 DEG C/min, insulation 0.5 ~ 5h, obtains polymer pyrolysis foam silicon carbide ceramics.
2. the preparation method of a kind of polymer pyrolysis foam silicon carbide ceramics as claimed in claim 1, is characterized in that in step 1) in, the number-average molecular weight Mn of described solid-state Polycarbosilane is 900 ~ 1200, and softening temperature is 180 ~ 250 DEG C.
3. the preparation method of a kind of polymer pyrolysis foam silicon carbide ceramics as claimed in claim 1, is characterized in that in step 2) in, the viscosity of described slurry A is 1 ~ 3PaS.
4. the preparation method of a kind of polymer pyrolysis foam silicon carbide ceramics as claimed in claim 1, is characterized in that in step 3) in, described urethane organic foam adopts aperture to be the urethane organic foam of 0.2 ~ 0.8mm.
5. the preparation method of a kind of polymer pyrolysis foam silicon carbide ceramics as claimed in claim 1, is characterized in that in step 3) in, the mass percentage concentration of described sodium hydroxide solution is 15%; The described standing time can be 2 ~ 5h.
6. the preparation method of a kind of polymer pyrolysis foam silicon carbide ceramics as claimed in claim 1, is characterized in that in step 4) in, described eliminating additional size A adopts to roll and gets rid of additional size A, then left at room temperature 24h in atmosphere; Or
Adopt centrifugal eliminating additional size A, then dry more than 5h at 80 DEG C.
7. the preparation method of a kind of polymer pyrolysis foam silicon carbide ceramics as claimed in claim 1, is characterized in that in step 5) in, the viscosity of described slurry B is 0.3 ~ 2PaS.
8. the preparation method of a kind of polymer pyrolysis foam silicon carbide ceramics as claimed in claim 1, is characterized in that in step 6) in, the time of described dipping is more than 20min.
9. the preparation method of a kind of polymer pyrolysis foam silicon carbide ceramics as claimed in claim 1, is characterized in that in step 6) in, described in complete secondary hanging be left at room temperature 24h or dry more than 5h at 80 DEG C in atmosphere.
10. the preparation method of a kind of polymer pyrolysis foam silicon carbide ceramics as claimed in claim 1, is characterized in that in step 7) in, the speed of described intensification is 1 DEG C/min.
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CN108558409A (en) * | 2018-07-09 | 2018-09-21 | 俞雪利 | A kind of foam silicon carbide ceramics and use the liquid metal filter that it is material |
CN108727059A (en) * | 2018-07-09 | 2018-11-02 | 宁波设会物联网科技有限公司 | It is a kind of can be thermally cured the preparation method that Polycarbosilane prepares foam silicon carbide ceramics |
CN108752038A (en) * | 2018-07-09 | 2018-11-06 | 宁波设会物联网科技有限公司 | It is a kind of with can be thermally cured Polycarbosilane preparation foam silicon carbide ceramics |
CN108794053A (en) * | 2018-07-09 | 2018-11-13 | 俞雪利 | A kind of material is the porous media combustor of foam silicon carbide ceramics |
CN108947578A (en) * | 2018-09-14 | 2018-12-07 | 宁波设会物联网科技有限公司 | A kind of preparation method of high-temperature resistant silicon carbide-hafnium carbide foamed ceramics |
CN109133931A (en) * | 2018-09-14 | 2019-01-04 | 宁波设会物联网科技有限公司 | Can be thermally cured the method that Polycarbosilane and polyurethane prepare foam silicon carbide ceramics |
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CN109913686A (en) * | 2019-01-07 | 2019-06-21 | 南京航空航天大学 | Modified SiC reinforced aluminum matrix composites in a kind of surface and preparation method thereof |
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