CN102452125B - Gel casting method and preparation method of ceramic - Google Patents
Gel casting method and preparation method of ceramic Download PDFInfo
- Publication number
- CN102452125B CN102452125B CN201010516357.7A CN201010516357A CN102452125B CN 102452125 B CN102452125 B CN 102452125B CN 201010516357 A CN201010516357 A CN 201010516357A CN 102452125 B CN102452125 B CN 102452125B
- Authority
- CN
- China
- Prior art keywords
- gel
- casting method
- weight
- weight portion
- silicone oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Ceramic Products (AREA)
- Mold Materials And Core Materials (AREA)
Abstract
The invention provides a gel casting method, comprising the following steps of: firstly degassing and pre-polymerizing suspensoid containing ceramic powder and organic system to obtain ceramic size; pouring the ceramic size into a mould, drying and then curing in situ, and demoulding to obtain gel-cast wet blank, the organic system contains 100 parts by weight of vinyl-terminated polyorganosiloxane, 2-10 parts by weight of hydrogen-containing silicone oil, 1-10 parts by weight of vinyl silicone oil, 0.2-0.8 part by weight of platinum complex catalyst, 0.02-0.1 part by weight of crosslinking inhibitor, 0.02-0.1 part by weight of viscosifier and 100-1000 parts by weight of organic solvent. The invention also provides a method for preparing ceramic by adopting the gel casting method. The gel casting method provided by the invention has wide application fields, and the ceramic obtained by adopting the gel casting method provided by the invention has higher mechanical properties.
Description
Technical field
The present invention relates to the preparation method of a kind of gel-casting method and a kind of pottery.
Background technology
Gel casting forming (gel-casting) is a kind of dead size moulding process after injection forming, injection moulding, in conjunction with traditional ceramics technique and polymer chemistry, has been successfully applied at present Al
2o
3, TiN, SiC, Si
3n
4industrial production on various structures pottery.The basic principle of gel injection molding and forming technology is in the ceramic size of high solid loading (volume fraction >=50 %), low viscosity (< 1PaS), to mix the organic monomer of low concentration, add again initator cast, there is home position polymerization reaction under certain condition in the organic monomer in slurry, form firm cross-linked structure, by the original position of slurry, solidify and make ceramic body custom-molded in place; Finally by crossing the demoulding, dry, sintering obtains required pottery.
The solvent that gel casting forming adopts comprises water system and two kinds of forms of non-water system, wherein adopt water as solvent for water-soluable gel casting (Aqueous Gel-casting), that adopt organic solvent is water-insoluble gel casting forming (Nonaqueons Gel-casting).Water-soluable gel injection moulding forming method, when preparing cermet, easily reacts with active metal in pottery as the water of solvent, thereby has certain limitation preparing cermet.
In gel injection-moulding technique, according to the difference of the organic monomer adopting, can be divided into a plurality of gel rubber systems, for example, can be divided into: acrylates (ester) class, acrylic amide, vinyl-based and propylene base class.But the gel rubber system that above-mentioned organic monomer forms easily occurs to solidify at normal temperatures, degassed not exclusively the wet base surface of having solidified rear formation is prone to out-of-flatness, subsides, and mechanical performance a little less than; Thereby cause the ceramic mechanical performance that forms after sintering also poor.
Summary of the invention
The invention solves the technical problem of the wet base surface irregularity, bad mechanical property and the ceramic machinery poor performance that exist in existing gel injection molding and forming technology.
The invention provides a kind of gel-casting method, comprise the first suspended substance that contains ceramic powder and organic system is degassed, pre-polymerization, obtain ceramic size; Again ceramic size is poured in mould, dry rear in-situ solidifying, the demoulding obtains the wet base of gel casting forming; Wherein, the ethenyl blocking polysiloxanes that contains 100 weight portions in described organic system, the containing hydrogen silicone oil of 2-10 weight portion, the vinyl silicone oil of 1-10 weight portion, the platinum complex catalyst of 0.2-0.8 weight portion, the cross-linked inhibitor of 0.02-0.1 weight portion, the tackifier of 0.02-0.1 weight portion, the organic solvent of 100-1000 weight portion.
The present invention also provides a kind of preparation method of pottery, comprises ceramic powder and organic system are passed through to gel casting forming, obtains wet base, and then to wetting, base carries out binder removal, sintering obtains; Wherein, described gel casting forming is gel-casting method provided by the invention.
Gel-casting method provided by the invention, adopt organic solvent, so its application is wider; In addition, the present invention adopts silicon gel system, and gel time is controlled, can guarantee the completely degassed time, the wet base surfacing therefore obtaining without subsiding, pore-free; In addition, silicon gel system can not produce oxygen anti-coagulating action, and in in-situ solidifying process, curing rate is very fast, and required time is shorter, and the crosslinking net system of having solidified rear formation has higher hot strength and hardness.Meanwhile, the pottery that adopts preparation method of the present invention to obtain has higher density and bending strength, has higher thermal conductivity simultaneously.
The specific embodiment
The invention provides a kind of gel-casting method, comprise the first suspended substance that contains ceramic powder and organic system is degassed, pre-polymerization, obtain ceramic size; Again ceramic size is poured in mould, dry rear in-situ solidifying, the demoulding obtains the wet base of gel casting forming; Wherein, the ethenyl blocking polysiloxanes that contains 100 weight portions in described organic system, the containing hydrogen silicone oil of 2-10 weight portion, the vinyl silicone oil of 1-10 weight portion, the platinum complex catalyst of 0.2-0.8 weight portion, the cross-linked inhibitor of 0.02-0.1 weight portion, the tackifier of 0.02-0.1 weight portion, the organic solvent of 100-1000 weight portion.
Gel-casting method of the present invention can be used for the moulding of various potteries, therefore, to not restriction of the selection of ceramic powder, for example, can be Silicon Carbide Powder material.
In method provided by the invention, the organic system adopting is organosilicon system, particularly, in described organic system, contain ethenyl blocking polysiloxanes, containing hydrogen silicone oil, vinyl silicone oil, platinum complex catalyst, cross-linked inhibitor, tackifier and organic solvent.Wherein, ethenyl blocking polysiloxanes and vinyl silicone oil are as base polymer, and containing hydrogen silicone oil, as crosslinking agent, forms siliceous cross-linked network, has higher mechanical performance; In addition, by cross-linked inhibitor, can control and start the curing time, guarantee degassed completely, wet base surfacing after making to solidify, and there is higher intensity, the easily demoulding.
In the present invention, in described ethenyl blocking polysiloxanes, Me
2the molar content of SiO segment is 95%, MeSiO
1.5the molar content of segment is 3%, Me
2the molar content of ViSiO segment is 0.7%, Me
3the molar content of SiO segment is 1.3%; The viscosity of ethenyl blocking polysiloxanes is 1000mPaS.Described ethenyl blocking polysiloxanes, chamber is synthetic by experiment, also can directly adopt and be purchased product, for example, can adopt the VM-18 of Zhejiang Jian Cheng organosilicon Co., Ltd.Described Me is methyl (CH
3) abbreviation, Vi is vinyl (CH=CH
2) abbreviation.
The structural formula of described containing hydrogen silicone oil is Me
3siO (Me
2siO)
x(MeHSiO)
ysiMe
3; Wherein repeating unit unit is Me
2siO(is designated as unit I) and MeHSiO(be designated as unit II).In described containing hydrogen silicone oil, it is 81-84% that the value of x, y makes the molar content of unit I, and the molar content of unit II is 14-17%; Silicon Containing Hydrogen oil viscosity 25-35mPaS, molal weight 2000-2500g/mol.Described containing hydrogen silicone oil by experiment chamber is synthetic, also can directly adopt and be purchased product, for example, can adopt the VM-29 of Zhejiang Jian Cheng organosilicon Co., Ltd.
The structural formula of described vinyl silicone oil is Me
3siO (Me
2siO)
a(MeViSiO)
bsiMe
3; Wherein repeating unit is Me
2siO(is designated as unit III) and MeViSiO(be designated as unit IV).In described vinyl silicone oil, it is 83-84% that the value of a, b makes the molar content of unit III, and the molar content of unit IV is 14-15%, and the viscosity of vinyl silicone oil is 50mPaS, and molal weight is 900-1000g/mol.Described vinyl silicone oil by experiment chamber is synthetic, also can directly adopt and be purchased product, for example, can adopt the VM-26 of Zhejiang Jian Cheng organosilicon Co., Ltd.
In the present invention, the catalyst that gel casting forming adopts is platinum complex catalyst.Under preferable case, described platinum complex catalyst is chloroplatinic acid-divinyl tetraphenyl silica alkane complex compound or 3,3,3-trifluoro propyl ethene silicone oil chloroplatinic acid complex compound.More preferably in situation, in described platinum complex catalyst, the content of platinum element is 3000-4000ppm.
In the present invention, cross-linked inhibitor is for extending time of organic system in-situ solidifying, guarantee degassed completely, thereby strengthen ceramic intensity.Described cross-linked inhibitor is at least one in 1-ethynylcyclohexanol, 3-methyl isophthalic acid-butine-3-alcohol, 3-Phenyl-1-butyn-3-ol, 3-propyl group-1-butine-3-alcohol, 3-octyl group-1-butine-3-alcohol.
In the present invention, in described organic system, also contain tackifier, for improving the intensity of wet base.Tackifier are the various quaternary ammonium salt tackifier that those skilled in the art commonly use, for example, can be selected from tetramethyl amine bromide, four butyl bromation amine, dodecyl bromination amine, cetyl amine bromide.
The solvent that organic system of the present invention adopts is organic solvent, and in the time of therefore can avoiding water as solvent and active metal reacts, thereby makes the application of gel casting forming of the present invention wider.Described organic solvent can be at least one in toluene, dimethylbenzene, chloroform, oxolane, butyl acetate.
The method according to this invention, is first mixed to get suspended substance by ceramic powder and organic system.In described suspended substance, the ceramic powder of 100 weight portions of take is benchmark, and the content of organic system is 10-50 weight portion, is preferably 20-40 weight portion.
Under preferable case, for improving dispersed in organic system of ceramic powder, in described suspended substance, also contain dispersant.The various silane couplers that described dispersant is commonly used for those skilled in the art.Particularly, described dispersant can be selected from γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxy silane and VTES.In the present invention, described dispersant can directly adopt and be purchased product, for example, can adopt KH560, KH570, A-171, A-151.The ceramic powder of 100 weight portions of take is benchmark, and the content of dispersant is 0.5-1 weight portion.
In gel casting forming provided by the invention, described degassed for removing suspended substance part bubble.The described degassed various degas method of the prior art that adopts, for example, can adopt the method for froth in vacuum or ultrasonic vibration.Described pre-polymerization is used for removing suspended substance part organic solvent, improves the concentration of crosslinking agent in suspended substance, prevents that the wet base after in-situ solidifying from subsiding.In pre-collecting process, part vinyl silicone oil and containing hydrogen silicone oil cross-linking reaction, suspended substance system viscosity increases, and obtains ceramic size.As those skilled in the art's common practise, thus the general degree of controlling pre-polymerization by controlling the condition of pre-polymerization.Particularly, the condition of pre-polymerization comprises: pre-polymerization temperature is 40-80 ℃, and the pre-polymerization time is 30-90min.
After pre-polymerization completes, obtain ceramic size.Ceramic size is poured in mould, is dried and removes the majority of organic solvent in ceramic size, then carry out in-situ solidifying, after the demoulding, can obtain the wet base of gel casting forming.The condition of in-situ solidifying comprises: solidification temperature is 120-150 ℃, and be 30-90min hardening time.
Gel-casting method provided by the invention can be used for ceramic preparation.Therefore, the invention provides a kind of preparation method of pottery, comprise ceramic powder and organic system are passed through to gel casting forming, obtain wet base, then to wetting, base carries out binder removal, sintering obtains; Wherein, described gel casting forming is gel-casting method provided by the invention.
According to preparation method provided by the invention, first by gel casting forming, obtain wet base, then to wetting, base carries out binder removal, sintering can obtain pottery.The mode of described binder removal, sintering can adopt variety of way of the prior art, in the present invention, is not particularly limited.
Under preferable case, the condition of binder removal comprises: the temperature of binder removal is 200-800 ℃, and the binder removal time is 1-6h.The step of sintering is controlled by temperature programming, specifically comprises: first in 120min, be warming up to 1000 ℃, then in 25min, be warming up to 1250 ℃, insulation 20min; In 60min, be warming up to 1850 ℃, insulation 30min; In last 40min, be warming up to 2150 ℃, insulation 60min.
Below in conjunction with embodiment, the preparation method of gel-casting method provided by the invention and pottery is described further.Raw materials usedly in embodiment and comparative example be all commercially available.
Embodiment 1
By the ethenyl blocking polysiloxanes VM-18 of 50 weight portion viscosity 1000mPaS, the molar content of 2.5 weight portion viscosity 25mPaS containing hydrogen silicone oil VM-29(unit I is 82%, the molar content of unit II is 16%), the molar content of 1 parts by weight of ethylene base silicone oil VM-26(unit III is 84%, and the molar content of unit IV is 14%) and 300 parts by weight of toluene mix; Adding 950 weight portion average grain diameters is 10 microns of Silicon Carbide Powder material again, mixes; Add 0.2 weight portion platinum complex catalyst chloroplatinic acid-divinyl tetraphenyl silica alkane complex compound, 0.05 weight portion cross-linked inhibitor ethynylcyclohexanol, 0.05 weight portion tackifier four butyl bromation amine, after stirring, obtain suspended substance; By after suspended substance vacuum degassing 20min, be heated to after 60 ℃ of pre-polymerization 1h; Slurry is injected to mould, in-situ solidifying 1h at dry latter 140 ℃, the demoulding obtains wet base, is designated as S1.
Base S1 binder removal 5h at 300 ℃ will wet.Then adopt temperature programming to carry out sintering: first in 120min, to be warming up to 1000 ℃, then in 25min, to be warming up to 1250 ℃, insulation 20min; In 60min, be warming up to 1850 ℃, insulation 30min; In last 40min, be warming up to 2150 ℃, insulation 60min.Cooling, obtain the pottery of the present embodiment, be designated as S11.
Embodiment 2
By the ethenyl blocking polysiloxanes VM-18 of 50 weight portion viscosity 1000mPaS, the molar content of 5 weight portion viscosity 25mPaS containing hydrogen silicone oil VM-29(unit I is 82%, the molar content of unit II is 16%), the molar content of 1 parts by weight of ethylene base silicone oil VM-26(unit III is 84%, and the molar content of unit IV is 14%), 6 weight portion dispersant KH560 and 300 parts of toluene mix; Adding 950 weight portion average grain diameters is 10 microns of Silicon Carbide Powder material again, mixes; Add 0.2 weight portion platinum complex catalyst chloroplatinic acid-divinyl tetraphenyl silica alkane complex compound, 0.05 weight portion cross-linked inhibitor ethynylcyclohexanol, 0.05 weight portion tackifier four butyl bromation amine, after stirring, obtain suspended substance; By after suspended substance vacuum degassing 20min, be heated to after 60 ℃ of pre-polymerization 1h; Slurry is injected to mould, in-situ solidifying 1h at dry latter 140 ℃, the demoulding obtains wet base, is designated as S2.
Base S2 binder removal 2h at 650 ℃ will wet.Then adopt temperature programming to carry out sintering: first in 120min, to be warming up to 1000 ℃, then in 25min, to be warming up to 1250 ℃, insulation 20min; In 60min, be warming up to 1850 ℃, insulation 30min; In last 40min, be warming up to 2150 ℃, insulation 60min.Cooling, obtain the pottery of the present embodiment, be designated as S22.
Comparative example 1
By 20 weight portion acrylamides (AM), 1 weight portion crosslinking agent methylene-bisacrylamide (MBAM), 0.2 weight portion dispersant polyacrylamide, 80 10 microns of weight portions Silicon Carbide Powders, 150 weight parts waters are mixed with suspension, add 0.4 weight portion initiator ammonium persulfate, 0.2 weight portion catalyst n, N, N, N-tetramethylethylenediamine, mix final vacuum de-bubble 5min, inject mould, at 70 ℃ of isothermal curing 1h, the wet base that obtains this comparative example after the demoulding, is designated as DS1.
The base DS1 that will wet removes glue 3h at 500 ℃, then adopts temperature programming to carry out sintering: first in 120min, be warming up to 1000 ℃, then in 25min, be warming up to 1250 ℃, insulation 20min; In 60min, be warming up to 1850 ℃, insulation 30min; In last 40min, be warming up to 2150 ℃, insulation 60min.Cooling, obtain the pottery of this comparative example, be designated as DS11.
Performance test:
(1) wet base performance test:
The wet base S1-S2 of record and DS1 surface start the curing time;
Visually observe wet base S1-S2 and DS1, surfacing, without subsiding, without bubble, is designated as OK; Otherwise be NO;
Adopt Shenzhen to think carefully that the computer electronic universal testing machine of experimental facilities Co., Ltd carries out stretching experiment to wet base, loading speed is 10mm/min, records the hot strength of each wet base sample;
The needle penetration that adopts needle penetration tester to test each wet base sample.Test result is as shown in table 1.
(2) ceramic performance test:
According to the density of buoyancy drainage test S11-S22 and DS11;
Adopt microcomputer controlled electronic universal testing machine (Shenzhen Rui Geer Instrument Ltd.) to measure S11-S22 and DS11 by three-point bending beam method, pottery is of a size of 30mm * 3mm * 115mm, and span is 25mm, and loading speed is 1mm/min;
Adopt the thermal conductivity of DJR-1 type thermal conductance instrument (Xiang Tan instrument and meter Co., Ltd) test S11-S22 and DS11.Test result is as shown in table 2.
Table 1
| Wet base | Gel time (min) | Outward appearance | Hot strength (MPa) | Needle penetration (10 -1mm) |
| S1 | 30 | OK | 0.56 | 75 |
| S2 | 25 | OK | 0.68 | 60 |
| DS1 | 12 | NO | 0.42 | 56 |
Table 2
| Pottery | Density (g/cm 3) | Thermal conductivity (W/mk) | Bending strength (Mpa) |
| S11 | 3.2 | 130 | 440 |
| S22 | 3.12 | 130 | 440 |
| DS11 | 3.05 | 110 | 420 |
Test result by table 1 can be found out, when the present invention adopts silicon gel system to carry out gel casting forming, compares with acrylamide gel system of the prior art, gel time is controlled, ensure time enough make degassed completely, the wet base surfacing obtaining, without subsiding, without bubble; In silicon gel system in-situ solidifying process, anaerobic anti-coagulating action phenomenon, curing rate is fast, has solidified the hot strength of the wet base of rear formation and the wet base that needle penetration obtains apparently higher than prior art, illustrates that wet base has higher hot strength and hardness.
Test result by table 2 can find out, the pottery that adopts preparation method provided by the invention to obtain has higher density and bending strength, has higher thermal conductivity simultaneously.
Claims (10)
1. a gel-casting method, comprises the first suspended substance that contains ceramic powder and organic system is degassed, pre-polymerization, obtains ceramic size; Again ceramic size is poured in mould, dry rear in-situ solidifying, the demoulding obtains the wet base of gel casting forming; It is characterized in that, the ethenyl blocking polysiloxanes that contains 100 weight portions in described organic system, the containing hydrogen silicone oil of 2-10 weight portion, the vinyl silicone oil of 1-10 weight portion, the platinum complex catalyst of 0.2-0.8 weight portion, the cross-linked inhibitor of 0.02-0.1 weight portion, the tackifier of 0.02-0.1 weight portion, the organic solvent of 100-1000 weight portion;
Described containing hydrogen silicone oil is Me
3siO (Me
2siO)
x(MeHSiO)
ysiMe
3; The value of x, y makes Me
2the molar content of SiO segment is that the molar content of 81-84%, MeHSiO segment is 14-17%; Silicon Containing Hydrogen oil viscosity 25-35mPaS, molal weight is 2000-2500g/mol;
Cross-linked inhibitor is at least one in 1-ethynylcyclohexanol, 3-methyl isophthalic acid-butine-3-alcohol, 3-Phenyl-1-butyn-3-ol, 3-propyl group-1-butine-3-alcohol, 3-octyl group-1-butine-3-alcohol; Tackifier are selected from tetramethyl amine bromide, four butyl bromation amine, dodecyl bromination amine, cetyl amine bromide; Organic solvent is at least one in toluene, dimethylbenzene, chloroform, oxolane, butyl acetate.
2. gel-casting method according to claim 1, is characterized in that, in described ethenyl blocking polysiloxanes, and Me
2the molar content of SiO segment is 95%, MeSiO
1.5the molar content of segment is 3%, Me
2the molar content of ViSiO segment is 0.7%, Me
3the molar content of SiO segment is 1.3%; The viscosity of ethenyl blocking polysiloxanes is 1000mPaS.
3. gel-casting method according to claim 1, is characterized in that, described vinyl silicone oil is Me
3siO (Me
2siO)
a(MeViSiO)
bsiMe
3; The value of a, b makes Me
2the molar content of SiO segment is that the molar content of 83-84%, MeViSiO segment is 14-15%; The viscosity of vinyl silicone oil is 50mPaS, and molal weight is 900-1000g/mol.
4. gel-casting method according to claim 1, is characterized in that, platinum complex catalyst is chloroplatinic acid-divinyl tetraphenyl silica alkane complex compound or 3,3,3-trifluoro propyl ethene silicone oil chloroplatinic acid complex compound.
5. gel-casting method according to claim 1, is characterized in that, the ceramic powder of 100 weight portions of take is benchmark, and in described suspended substance, the content of organic system is 10-50 weight portion.
6. gel-casting method according to claim 1, it is characterized in that, in described suspended substance, also contain dispersant, dispersant is selected from γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxy silane and VTES; The ceramic powder of 100 weight portions of take is benchmark, and the content of dispersant is 0.5-1 weight portion.
7. gel-casting method according to claim 1, is characterized in that, degassed employing froth in vacuum or ultrasonic vibration; The condition of pre-polymerization comprises: pre-polymerization temperature is 40-80 ℃, and the pre-polymerization time is 30-90min.
8. gel-casting method according to claim 1, is characterized in that, the condition of in-situ solidifying comprises: solidification temperature is 120-150 ℃, and be 30-90min hardening time.
9. a ceramic preparation method, comprises ceramic powder and organic system is passed through to gel casting forming, obtains wet base, and then to wetting, base carries out binder removal, sintering obtains; It is characterized in that, described gel casting forming is the gel-casting method described in claim 1-8 any one.
10. preparation method according to claim 9, is characterized in that, the condition of binder removal comprises: dump temperature is 200-800 ℃, and the binder removal time is 1-6h; The step of sintering is controlled by temperature programming, specifically comprises: first in 120min, be warming up to 1000 ℃, then in 25min, be warming up to 1250 ℃, insulation 20min; In 60min, be warming up to 1850 ℃, insulation 30min; In last 40min, be warming up to 2150 ℃, insulation 60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010516357.7A CN102452125B (en) | 2010-10-22 | 2010-10-22 | Gel casting method and preparation method of ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010516357.7A CN102452125B (en) | 2010-10-22 | 2010-10-22 | Gel casting method and preparation method of ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102452125A CN102452125A (en) | 2012-05-16 |
| CN102452125B true CN102452125B (en) | 2014-02-12 |
Family
ID=46036004
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010516357.7A Active CN102452125B (en) | 2010-10-22 | 2010-10-22 | Gel casting method and preparation method of ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102452125B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113087501A (en) * | 2021-03-05 | 2021-07-09 | 徐州亚苏尔高新材料有限公司 | High-strength quartz ceramic roller and preparation process thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020025520A (en) * | 2000-09-29 | 2002-04-04 | 김충섭 | A process for preparing ceramic gelbody |
| WO2002048206A1 (en) * | 2000-12-16 | 2002-06-20 | Samsung General Chemicals Co., Ltd. | Catalyst obtained by prepolymerization of polyolefin and olefin polymerization method using the same |
| CN101143790A (en) * | 2007-09-13 | 2008-03-19 | 中国海洋大学 | Gel injection moulding forming technique for boron carbide-metal composite material |
| CN101397210A (en) * | 2007-09-24 | 2009-04-01 | 深圳市金科特种材料股份有限公司 | Gel-casting moulding technique for preparing silicon nitride ceramics heating element |
| CN101608068A (en) * | 2009-07-10 | 2009-12-23 | 茂名市信翼化工有限公司 | A kind of organosilicon material and synthetic method thereof of power-type LED encapsulation usefulness |
| CN101624471A (en) * | 2009-03-06 | 2010-01-13 | 上海锐朗光电材料有限公司 | Heat curing in-situ forming high-conductivity silicon rubber composition and application thereof |
| CN101654560A (en) * | 2009-07-10 | 2010-02-24 | 茂名市信翼化工有限公司 | Organic silicon material for power type LED encapsulation and synthetic method thereof |
-
2010
- 2010-10-22 CN CN201010516357.7A patent/CN102452125B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020025520A (en) * | 2000-09-29 | 2002-04-04 | 김충섭 | A process for preparing ceramic gelbody |
| WO2002048206A1 (en) * | 2000-12-16 | 2002-06-20 | Samsung General Chemicals Co., Ltd. | Catalyst obtained by prepolymerization of polyolefin and olefin polymerization method using the same |
| CN101143790A (en) * | 2007-09-13 | 2008-03-19 | 中国海洋大学 | Gel injection moulding forming technique for boron carbide-metal composite material |
| CN101397210A (en) * | 2007-09-24 | 2009-04-01 | 深圳市金科特种材料股份有限公司 | Gel-casting moulding technique for preparing silicon nitride ceramics heating element |
| CN101624471A (en) * | 2009-03-06 | 2010-01-13 | 上海锐朗光电材料有限公司 | Heat curing in-situ forming high-conductivity silicon rubber composition and application thereof |
| CN101608068A (en) * | 2009-07-10 | 2009-12-23 | 茂名市信翼化工有限公司 | A kind of organosilicon material and synthetic method thereof of power-type LED encapsulation usefulness |
| CN101654560A (en) * | 2009-07-10 | 2010-02-24 | 茂名市信翼化工有限公司 | Organic silicon material for power type LED encapsulation and synthetic method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 凝胶注模法制备多孔氧化铝陶瓷的研究;邵庄等;《中国陶瓷》;20071031;第43卷(第10期);第50-52页 * |
| 晏伯武等.锆钛酸铅压电陶瓷材料凝胶注模成型.《华中科技大学学报(自然科学版)》.2007,第35卷(第4期), * |
| 邵庄等.凝胶注模法制备多孔氧化铝陶瓷的研究.《中国陶瓷》.2007,第43卷(第10期), |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102452125A (en) | 2012-05-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105390461B (en) | Heat Insulation film and its manufacturing method | |
| CN104231798B (en) | Improved silica aerogel microball insulating moulding coating | |
| CN103708476B (en) | A kind of preparation method of flexible silica aerogel | |
| CN100482614C (en) | Collidal forming process for preparing high strength light ceramic material | |
| JP2016069272A (en) | Method for making ceramic matrix composite articles | |
| CN104086947B (en) | For the phenolaldehyde moulding compound of commutator | |
| CN102627448A (en) | Method for preparing ceramic fibers | |
| US20100316447A1 (en) | Inorganic-organic binder, method for the production thereof, and use thereof | |
| CN104230345A (en) | Preparation method of porous silicon nitride ceramic material | |
| CN105694370A (en) | Toughened-flame-retardant epoxy resin material and preparation method thereof | |
| CN101941231A (en) | Gel injection molding technology of large-sized and complicated-shape silicon carbide ceramic biscuit | |
| CN104673160A (en) | Filled surface modified silicon carbide isotropic thermal conduction adhesive and preparation method thereof | |
| CN105645967A (en) | Preparation method of porous silicon nitride ceramic material with highly oriented through holes | |
| CN105062085A (en) | Addition-type organosilicone mould rubber and preparation method thereof | |
| CN105778516A (en) | Addition type solidifiable polysiloxane composition | |
| CN102827479A (en) | Liquid silicone rubber | |
| CN102452125B (en) | Gel casting method and preparation method of ceramic | |
| CN101270220B (en) | Method for preparing polyalcohol-base light overpressure resistant floating force material and equipment thereof | |
| CN106977927A (en) | A kind of high intensity add-on type liquid silicon rubber maceration extract and its preparation and forming method | |
| CN106747267B (en) | A kind of Carbon Fiber Rigid thermal insulation tile and preparation method thereof | |
| CN109437959A (en) | A kind of method that environment-friendly type gel injection-moulding prepares mullite fiber base porous ceramics | |
| CN104072998A (en) | Base rubber material of high dielectric constant liquid silicone rubber and application thereof in composition | |
| CN105273680B (en) | A kind of two-component heat conductive silica gel sheet material and preparation method thereof and equipment | |
| CN104341548A (en) | Micron-grade copolymer microspheres and preparation method thereof | |
| JP4883308B2 (en) | Method for producing silicone rubber foam |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |