CN102452125A - Gel casting method and preparation method of ceramic - Google Patents
Gel casting method and preparation method of ceramic Download PDFInfo
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- CN102452125A CN102452125A CN2010105163577A CN201010516357A CN102452125A CN 102452125 A CN102452125 A CN 102452125A CN 2010105163577 A CN2010105163577 A CN 2010105163577A CN 201010516357 A CN201010516357 A CN 201010516357A CN 102452125 A CN102452125 A CN 102452125A
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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 technology and polymer chemistry, has been successfully applied to Al at present
2O
3, TiN, SiC, Si
3N
4Commercial production etc. multiple structural ceramics.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 initator and cast again; Home position polymerization reaction takes place under certain condition in the organic monomer in the slurry; Form firm cross-linked structure, solidify through the original position of slurry and make the ceramic body custom-molded in place; Obtain required pottery through the demoulding, drying, sintering at last.
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).The water-soluable gel injection moulding forming method is in preparation during cermet, as the water of solvent be prone to pottery in the active metal reaction, thereby certain limitation is arranged at the preparation cermet.
According to the difference of the organic monomer that adopts, can be divided into a plurality of gel rubber systems in the gel injection-moulding technology, 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 solidifies easily at normal temperatures, and the degassing not exclusively solidifies that the wet base surface of formation is prone to out-of-flatness, subsides after accomplishing, and mechanical performance a little less than; Thereby the mechanical performance of the pottery that causes forming behind the sintering is also relatively 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 the existing gel injection molding and forming technology.
The invention provides a kind of gel-casting method, comprise the suspended substance degassing, the pre-polymerization that will contain ceramic powder and organic system earlier, obtain ceramic size; Again ceramic size is poured in the mould, dry back in-situ solidifying, the demoulding obtains the wet base of gel casting forming; Wherein, The ethenyl blocking polysiloxanes that contains 100 weight portions in the said organic system, the containing hydrogen silicone oil of 2-10 weight portion, the vinyl silicone oil of 1-10 weight portion; 0.2-0.8 the platinum complex catalyst of weight portion; 0.02-0.1 the cross-linked inhibitor of 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 gel casting forming, obtains wet base, and base carries out binder removal, sintering obtains to wetting then; Wherein, said gel casting forming is a 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 the silicon gel system, and gel time is controlled, can guarantee fully the time of the degassing, the wet base surfacing that therefore obtains do not have subside, pore-free; In addition, the silicon gel system can not produce the oxygen anti-coagulating action, and curing rate is very fast in the in-situ solidifying process, and required time is shorter, solidifies the crosslinking net system that forms after accomplishing and has higher draw tensile strength and hardness.Simultaneously, the pottery that adopts preparation method of the present invention to obtain has higher density and bending strength, has high thermal simultaneously.
The specific embodiment
The invention provides a kind of gel-casting method, comprise the suspended substance degassing, the pre-polymerization that will contain ceramic powder and organic system earlier, obtain ceramic size; Again ceramic size is poured in the mould, dry back in-situ solidifying, the demoulding obtains the wet base of gel casting forming; Wherein, The ethenyl blocking polysiloxanes that contains 100 weight portions in the said organic system, the containing hydrogen silicone oil of 2-10 weight portion, the vinyl silicone oil of 1-10 weight portion; 0.2-0.8 the platinum complex catalyst of weight portion; 0.02-0.1 the cross-linked inhibitor of 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, and therefore, the not restriction of selection to ceramic powder for example can be silicon carbide ceramics powder material.
In the method provided by the invention; The organic system that is adopted is the organosilicon system; Particularly, contain ethenyl blocking polysiloxanes, containing hydrogen silicone oil, vinyl silicone oil, platinum complex catalyst, cross-linked inhibitor, tackifier and organic solvent in the said organic system.Wherein, ethenyl blocking polysiloxanes and vinyl silicone oil are as base polymer, and containing hydrogen silicone oil forms siliceous cross-linked network as crosslinking agent, has higher mechanical properties; In addition, can control the time that begins to solidify, guarantee the degassing fully, make and solidify the wet base surfacing in back, and have higher intensity, the demoulding easily through cross-linked inhibitor.
Among the present invention, in the said 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.Said ethenyl blocking polysiloxanes can be synthetic through the laboratory, also can directly adopt and be purchased product, for example can adopt Zhejiang to build the VM-18 of orange organosilicon Co., Ltd.Said Me is methyl (CH
3) abbreviation, Vi is vinyl (CH=CH
2) abbreviation.
The structural formula of said containing hydrogen silicone oil is Me
3SiO (Me
2SiO)
x(MeHSiO)
ySiMe
3Wherein the repeating unit unit is Me
2SiO (being designated as unit I) and MeHSiO (being designated as unit II).In the said 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%; The viscosity 25-35mPaS of containing hydrogen silicone oil, molal weight 2000-2500g/mol.Said containing hydrogen silicone oil can be synthetic through the laboratory, also can directly adopt and be purchased product, for example can adopt Zhejiang to build the VM-29 of orange organosilicon Co., Ltd.
The structural formula of said vinyl silicone oil is Me
3SiO (Me
2SiO)
a(MeViSiO)
bSiMe
3Wherein repeating unit is Me
2SiO (being designated as unit III) and MeViSiO (being designated as unit IV).In the said 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.Said vinyl silicone oil can be synthetic through the laboratory, also can directly adopt and be purchased product, for example can adopt Zhejiang to build the VM-26 of orange organosilicon Co., Ltd.
Among the present invention, the catalyst that gel casting forming adopts is a platinum complex catalyst.Under the preferable case, said 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 under the situation, in the said platinum complex catalyst, the content of platinum element is 3000-4000ppm.
Among the present invention, cross-linked inhibitor is used to prolong the time of organic system in-situ solidifying, guarantees the degassing fully, thereby strengthens the intensity of pottery.Said cross-linked inhibitor is at least a in 1-ethynylcyclohexanol, 3-methyl isophthalic acid-butine-3-alcohol, 3-Phenyl-1-butyn-3-ol, 3-propyl group-1-butine-3-alcohol, the 3-octyl group-1-butine-3-alcohol.
Among the present invention, also contain tackifier in the said organic system, be used to improve the intensity of wet base.The various tackifier that tackifier are used always for those skilled in the art 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 an organic solvent, and in the time of therefore can avoiding water as solvent and active metal reacts, thereby makes that the application of gel casting forming of the present invention is wider.Said organic solvent can be in toluene, xylenes, chloroform, oxolane, the butyl acetate at least a.
According to the method for the invention, first ceramic powder is mixed with organic system obtains suspended substance.In the said suspended substance, be benchmark with the ceramic powder of 100 weight portions, the content of organic system is the 10-50 weight portion, is preferably the 20-40 weight portion.
Under the preferable case,, also contain dispersant in the said suspended substance for improving the even dispersion of ceramic powder in organic system.The various silane couplers that said dispersant is used always for those skilled in the art.Particularly, said dispersant can be selected from γ-glycidyl ether oxygen propyl trimethoxy silicane), γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxy silane and VTES.Among the present invention, said dispersant can directly adopt and be purchased product, for example can adopt KH560, KH570, A-171, A-151.Ceramic powder with 100 weight portions is a benchmark, and the content of dispersant is the 0.5-1 weight portion.
In the gel casting forming provided by the invention, the said degassing is used for removing suspended substance part bubble.The said degassing can be adopted various degas method of the prior art, for example can adopt the method for froth in vacuum or ultrasonic vibration.Said pre-polymerization is used for removing suspended substance part organic solvent, improves the concentration of crosslinking agent in the suspended substance, prevents that the wet base behind the in-situ solidifying from subsiding.In the pre-polymerization process, part vinyl silicone oil and containing hydrogen silicone oil cross-linking reaction, the 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 through the condition of controlling pre-polymerization.Particularly, the condition of pre-polymerization comprises: the pre-polymerization temperature is 40-80 ℃, and the pre-polymerization time is 30-90min.
Pre-polymerization obtains ceramic size after accomplishing.Ceramic size is poured in the mould, and drying is removed the most of organic solvent in the ceramic size, carries out in-situ solidifying then, can obtain the wet base of gel casting forming after the demoulding.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 the preparation of pottery.Therefore, the invention provides a kind of preparation method of pottery, comprise ceramic powder and organic system are passed through gel casting forming, obtain wet base, base carries out binder removal, sintering obtains to wetting then; Wherein, said gel casting forming is a gel-casting method provided by the invention.
According to preparation method provided by the invention, obtain wet base through gel casting forming earlier, base carries out binder removal, sintering can obtain pottery to wetting then.The mode of said binder removal, sintering can adopt variety of way of the prior art, does not have particular determination among the present invention.
Under the 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 specifically comprises through temperature programming control: in 120min, be warming up to 1000 ℃ earlier, be warming up to 1250 ℃ then in the 25min, insulation 20min; Be warming up to 1850 ℃ in the 60min, insulation 30min; Be warming up to 2150 ℃ in the last 40min, 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 the Comparative Examples all be commercially available.
Embodiment 1
Ethenyl blocking polysiloxanes VM-18 with 50 weight portion viscosity 1000mPaS; 2.5 (molar content of unit I is 82% to weight portion viscosity 25mPaS containing hydrogen silicone oil VM-29; The molar content of unit II is 16%); 1 parts by weight of ethylene base silicone oil VM-26 (molar content of 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 again is 10 microns silicon carbide ceramics powder material, 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, obtain suspended substance after stirring; Behind suspended substance vacuum degassing 20min, be heated to 60 ℃ of pre-polymerization 1h after; Slurry is injected mould, dry back 140 ℃ of following in-situ solidifying 1h, the demoulding obtains wet base, is designated as S1.
To wet base S1 at 300 ℃ of following binder removal 5h.Adopt temperature programming to carry out sintering then: in 120min, to be warming up to 1000 ℃ earlier, to be warming up to 1250 ℃ then in the 25min, insulation 20min; Be warming up to 1850 ℃ in the 60min, insulation 30min; Be warming up to 2150 ℃ in the last 40min, insulation 60min.Cool off, obtain the pottery of present embodiment, be designated as S11.
Embodiment 2
Ethenyl blocking polysiloxanes VM-18 with 50 weight portion viscosity 1000mPaS; (molar content of unit I is 82% to 5 weight portion viscosity 25mPaS containing hydrogen silicone oil VM-29; The molar content of unit II is 16%); 1 parts by weight of ethylene base silicone oil VM-26 (molar content of 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 again is 10 microns silicon carbide ceramics powder material, 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, obtain suspended substance after stirring; Behind suspended substance vacuum degassing 20min, be heated to 60 ℃ of pre-polymerization 1h after; Slurry is injected mould, dry back 140 ℃ of following in-situ solidifying 1h, the demoulding obtains wet base, is designated as S2.
To wet base S2 at 650 ℃ of following binder removal 2h.Adopt temperature programming to carry out sintering then: in 120min, to be warming up to 1000 ℃ earlier, to be warming up to 1250 ℃ then in the 25min, insulation 20min; Be warming up to 1850 ℃ in the 60min, insulation 30min; Be warming up to 2150 ℃ in the last 40min, insulation 60min.Cool off, obtain the pottery of present embodiment, be designated as S22.
Comparative Examples 1
With 20 weight portion acrylamides (AM), 1 weight portion crosslinking agent methylene-bisacrylamide (MBAM), 0.2 weight portion dispersant polyacrylamide, 10 microns silicon carbide ceramics powders of 80 weight portions; 150 weight parts waters are mixed with suspension, add 0.4 weight portion initiator ammonium persulfate, 0.2 weight portion catalyst n, N; N, the N-tetramethylethylenediamine mixes final vacuum de-bubble 5min, injects mould; At 70 ℃ of isothermal curing 1h, obtain the wet base of this Comparative Examples after the demoulding, be designated as DS1.
The base DS1 that will wet removes glue 3h down at 500 ℃, adopts temperature programming to carry out sintering then: in 120min, be warming up to 1000 ℃ earlier, be warming up to 1250 ℃ then in the 25min, insulation 20min; Be warming up to 1850 ℃ in the 60min, insulation 30min; Be warming up to 2150 ℃ in the last 40min, insulation 60min.Cool off, obtain the pottery of this Comparative Examples, be designated as DS11.
Performance test:
(1) wet base performance test:
The time that wet base S1-S2 of record and DS1 surface begin to solidify;
Wet base S1-S2 of perusal and DS1, surfacing, nothing are subsided, no bubble, are designated as OK; Otherwise be NO;
Adopt the Shenzhen to think carefully that the microcomputer electronics universal testing machine of experimental facilities Co., Ltd carries out stretching experiment to wet base, loading speed is 10mm/min, writes down the hot strength of each wet base sample;
Adopt the needle penetration of each wet base sample of needle penetration tester test.Test result is as shown in table 1.
(2) ceramic performance test:
Density according to buoyancy drainage test S11-S22 and DS11;
Adopt system controlled by computer electronics universal testing machine (Rui Geer of Shenzhen Instr Ltd.) to measure S11-S22 and DS11 through the 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 appearance (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 the silicon gel system to carry out gel casting forming, compares with acrylamide gel system of the prior art; Gel time is controlled, guarantees to have time enough to make the degassing fully, the wet base surfacing that obtains; Nothing is subsided, no bubble; In the silicon gel system in-situ solidifying process, anaerobic anti-coagulating action phenomenon, curing rate is fast, and the hot strength of the wet base of formation and needle penetration explained that apparently higher than the wet base that prior art obtains wet base has higher draw tensile strength and hardness after curing was accomplished.
Test result by table 2 can find out that the pottery that adopts preparation method provided by the invention to obtain has higher density and bending strength, has high thermal simultaneously.
Claims (11)
1. a gel-casting method comprises the suspended substance degassing, the pre-polymerization that will contain ceramic powder and organic system earlier, obtains ceramic size; Again ceramic size is poured in the mould, dry back 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 the said organic system, the containing hydrogen silicone oil of 2-10 weight portion, the vinyl silicone oil of 1-10 weight portion; 0.2-0.8 the platinum complex catalyst of weight portion; 0.02-0.1 the cross-linked inhibitor of weight portion, the tackifier of 0.02-0.1 weight portion, the organic solvent of 100-1000 weight portion.
2. gel-casting method according to claim 1 is characterized in that, in the said 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, said containing hydrogen silicone oil is Me
3SiO (Me
2SiO)
x(MeHSiO)
ySiMe
3The 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%; The viscosity 25-35mPaS of containing hydrogen silicone oil, molal weight is 2000-2500g/mol.
4. gel-casting method according to claim 1 is characterized in that, said vinyl silicone oil is Me
3SiO (Me
2SiO)
a(MeViSiO)
bSiMe
3The 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 50mpa.S, and molal weight is 900-1000g/mol.
5. 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; Cross-linked inhibitor is at least a in 1-ethynylcyclohexanol, 3-methyl isophthalic acid-butine-3-alcohol, 3-Phenyl-1-butyn-3-ol, 3-propyl group-1-butine-3-alcohol, the 3-octyl group-1-butine-3-alcohol; Tackifier are quaternary ammonium salt, are selected from tetramethyl amine bromide, four butyl bromation amine, dodecyl bromination amine, cetyl amine bromide; Organic solvent is at least a in toluene, xylenes, chloroform, oxolane, the butyl acetate.
6. gel-casting method according to claim 1 is characterized in that, is benchmark with the ceramic powder of 100 weight portions, and the content of organic system is the 10-50 weight portion in the said suspended substance.
7. gel-casting method according to claim 1; It is characterized in that; Also contain dispersant in the said suspended substance, dispersant is selected from γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltrimethoxy silane and VTES; Ceramic powder with 100 weight portions is a benchmark, and the content of dispersant is the 0.5-1 weight portion.
8. gel-casting method according to claim 1 is characterized in that, froth in vacuum or ultrasonic vibration are adopted in the degassing; The condition of pre-polymerization comprises: the pre-polymerization temperature is 40-80 ℃, and the pre-polymerization time is 30-90min.
9. 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.
10. the preparation method of a pottery comprises ceramic powder and organic system is passed through gel casting forming, and obtain wet base, base carries out binder removal, sintering obtains to wetting then; It is characterized in that said gel casting forming is each described gel-casting method of claim 1-9.
11. preparation method according to claim 10 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 specifically comprises through temperature programming control: in 120min, be warming up to 1000 ℃ earlier, be warming up to 1250 ℃ then in the 25min, insulation 20min; Be warming up to 1850 ℃ in the 60min, insulation 30min; Be warming up to 2150 ℃ in the last 40min, insulation 60min.
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| 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 |
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