CN106699212A - Compound ceramic substrate and preparation method thereof - Google Patents

Compound ceramic substrate and preparation method thereof Download PDF

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Publication number
CN106699212A
CN106699212A CN201611239204.6A CN201611239204A CN106699212A CN 106699212 A CN106699212 A CN 106699212A CN 201611239204 A CN201611239204 A CN 201611239204A CN 106699212 A CN106699212 A CN 106699212A
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ceramic powder
powder
ceramics substrate
composite ceramics
substrate according
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董睿智
丁天昊
丁萍
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GUANGDONG REAL FAITH LIGHTING TECHNOLOGY Co Ltd
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GUANGDONG REAL FAITH LIGHTING TECHNOLOGY Co Ltd
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Abstract

The invention provides a compound ceramic substrate which is prepared from a sizing mixture and a base material, wherein the sizing mixture is prepared from the following materials in parts by weight: 50-85 parts of ceramic powder, 5-40 parts of an adhesive agent, 3-5 parts of an additive and 1-5 parts of a curing agent, wherein the particle size of the ceramic powder is 1-10 mu m; the ceramic powder is one or more of oxide ceramic powder, nitrogen ceramic powder, boride ceramic powder and carbide ceramic powder. The compound ceramic substrate is prepared by performing mixing, coating, pre-baking and hot pressed sintering processes on the mixture prepared from the ceramic powder, the adhesive agent, the additive and the curing agent, and the base material. The compound ceramic substrate has certain special properties of ceramic; furthermore, a preparation technology is simple, the sintering temperature in a preparation process is low, and basically no harmful gas overflows during the process, so that the compound ceramic substrate is a novel green ceramic material.

Description

A kind of composite ceramics substrate and preparation method thereof
Technical field
The invention belongs to composite ceramic material technical field, and in particular to a kind of composite ceramics substrate and preparation method thereof.
Background technology
Ceramic material has high temperature resistant, high pressure resistant, wear-resisting, corrosion resistance.Special ceramic material is even more to possess excellent Electric property, optical property even magnetic performance.Its product is widely used in Aero-Space, high-power structural element and function In property part.
Traditional ceramic objectses add the mixing of wax bonding agent using ceramic powder, and molded being put into stove of reheating is arranged Wax, being finally put into the semi-finished product that de-waxing is completed carries out high temperature sintering in high temperature furnace.This method needs to consume substantial amounts of energy, and Atmosphere pollution is produced during de-waxing.
The content of the invention
The present invention is intended to provide a kind of composite ceramics substrate and preparation method thereof, by ceramic powder, bonding agent, additive, The compound and matrix material of curing agent composition, a kind of ceramic material is obtained by mixing, coating, prebake conditions, hot pressed sintering process Material.The material has that intensity is high, hardness is high, the special property with ceramics, and manufacture craft is simple, and temperature is sintered in preparation process Degree it is low, during go out without pernicious gas benefit substantially, be a kind of novel green ceramic material.
What the present invention was realized in:
A kind of composite ceramics substrate, including mixed slurry and matrix material, the mixed slurry include following composition materials:
The ceramic powder of 50-85 weight portions,
The bonding agent of 5-40 weight portions,
The additive of 3-5 weight portions,
The curing agent of 1-5 weight portions,
Wherein:
The particle diameter of the ceramic powder is 1-10um,
The ceramic powder is oxide ceramic powder body, nitride ceramics powder, boride ceramics powder and carbide pottery One or more in porcelain powder.
Preferably, the oxide ceramic powder body is Al2O3、ZrO2, BeO, MgO and TiO2In one or more.
Preferably, the nitridation ceramic powder is AlN, BN, Si3N4, ZrN one or more.
Preferably, the boride ceramics powder is ZrB2And TiB2In one or two.
Preferably, the carbide ceramics powder is B4One or more in C, SiC, ZrC, TiC and WC.
Preferably, the bonding agent is thermosetting epoxy resin or heat curing-type modified epoxy.
Preferably, the additive be diatomite, talcum powder, calcined kaolin, silica flour and titanium dioxide in one kind or It is several.
Preferably, the curing agent is in m-phenylene diamine (MPD), diamino diphenyl sulfone, trimellitic anhydride and mellophanic acid acid anhydride One or more.
Preferably, described matrix material is one or more in carbon fiber, glass fibre, polyester fiber and metallic fiber Mixing, the metallic fiber is in aluminum fiber net, stainless steel fiber web, copper fiber net, titanium fleece and magnesium alloy fleece It is combined for one or more.
According to another aspect of the present invention, a kind of method for preparing above-mentioned composite ceramics substrate, comprises the following steps:
S1:Batch mixing:Ceramic powder, bonding agent, additive and the curing agent of dosage are weighed, is put into blender and is mixed 1-5 Hour, obtain batch mixing;
S2:Coating:Matrix material is tiled, then batch mixing is coated uniformly on the surface of stock;
S3:Prebake conditions:The matrix material that batch mixing will have been coated is put into baking oven, and 30-60 is toasted under the conditions of 80-140 DEG C Minute, obtain pre impregnated material;
S4:Hot pressed sintering:Pre impregnated material is taken out, is put into hot press, at 150-220 DEG C, pressure is 20- Hot pressing 1-5 hours under 100MPa;
S5:After the completion of hot pressing, room temperature is cooled to, obtains composite ceramics substrate.
Compared with prior art, composite ceramics substrate of the invention not only has the special property of ceramics, and manufacture craft Simply, sintering temperature is low in preparation process, during go out without pernicious gas benefit substantially, be a kind of novel green ceramic material.
Specific embodiment
Specific embodiment of the invention is described in detail below.It should be appreciated that described herein specific Implementation method is merely to illustrate and explain the present invention, and is not intended to limit the invention.
Embodiment 1
Al2O3Ceramic mixed slurry, including following composition materials:
80 weight portion particle diameter D50 are the Al of 1um2O3Ceramic powder,
The E-20 type epoxy resin of 15 weight portions,
The titanium dioxide of the talcum powder of 1 weight portion, the silica flour of 1 weight portion and 1 weight portion,
The m-phenylene diamine (MPD) of 2 weight portions.
The preparation technology of composite ceramics substrate is as follows:
S1:Batch mixing:Weigh the Al that 80 weight portion particle diameter D50 are 1um2O3The E-20 type asphalt mixtures modified by epoxy resin of ceramic powder, 15 weight portions Between the titanium white flour additive agent and 2 weight portions of fat bonding agent, the talcum powder of 1 weight portion, the silica flour of 1 weight portion and 1 weight portion Phenylenediamine curing agent, is put into V-arrangement batch mixer and mixes 5 hours, obtains batch mixing;
S2:Coating:Selection glass fabric is matrix material, and glass fibre is tiled, then batch mixing is uniformly coated On the surface of glass fibre;
S3:Prebake conditions:The glass fibre that batch mixing will have been coated is put into baking oven, is toasted 30 minutes under the conditions of 80 DEG C, is obtained To pre impregnated material;
S4:Hot pressed sintering:Pre-preg material is taken out, is put into hot press, at 150 DEG C, pressure is hot pressing 3 under 50MPa Hour;
S5:After the completion of hot pressing, room temperature is cooled to, obtains composite ceramics substrate.
Gained alumina ceramic composite material surface smoothness is good, and hardness is 6.5, and fracture toughness is 6.5Mpam1/2, tension Intensity is 50MPa, and bending strength is 150MPa, and heatproof is up to 180 DEG C of non yellowings, thermal conductivity 10W/mK, thermal coefficient of expansion 6.2×10-5/℃.Produced without pernicious gas in preparation process.
Embodiment 2
Zirconia ceramics mixed slurry, including following composition materials:
85 weight portion particle diameter D50 are the zirconia ceramics powder of 10um,
The E-03 type epoxy resin of 10 weight portions,
The calcined kaolin of the talcum powder of 1 weight portion, the silica flour of 1 weight portion and 1 weight portion,
The trimellitic anhydride of 2 weight portions.
The preparation technology of composite ceramics substrate is as follows:
S1:Batch mixing:Weigh zirconia ceramics powder, the E-03 type rings of 10 weight portions that 85 weight portion particle diameter D50 are 10um The calcined kaolin additive and 2 weights of oxygen resin adhesive, the talcum powder of 1 weight portion, the silica flour of 1 weight portion and 1 weight portion The trimellitic acid anhydride curing agents of part are measured, is put into V-arrangement batch mixer and is mixed 3 hours, obtain batch mixing;
S2:Coating:Selection glass fabric is matrix material, and glass fibre is tiled, then batch mixing is uniformly coated On the surface of glass fibre;
S3:Prebake conditions:The glass fibre that batch mixing will have been coated is put into baking oven, is toasted 30 minutes under the conditions of 140 DEG C, is obtained To pre impregnated material;
S4:Hot pressed sintering:Pre impregnated material is taken out, is put into hot press, at 180 DEG C, pressure is hot pressing under 30MPa 5 hours;
S5:After the completion of hot pressing, room temperature is cooled to, obtains composite ceramics substrate.
Gained Zirconium oxide ceramic composite material surface smoothness is good, and hardness is 7.5, and fracture toughness is 7.0Mpam1/2, tension Intensity is 65MPa, and bending strength is 130MPa, and up to 200 DEG C of non yellowings, thermal coefficient of expansion is 4.2 × 10 to resistance to temperature-5/℃.System Produced without pernicious gas during standby.
Embodiment 3
Boron nitride ceramics mixed slurry, including following composition materials:
85 weight portion particle diameter D50 are the hexagonal boron nitride ceramic powder of 10um,
The E-03 type epoxy resin of 10 weight portions,
The calcined kaolin of the talcum powder of 1 weight portion, the silica flour of 1 weight portion and 1 weight portion,
The trimellitic anhydride of 2 weight portions.
The preparation technology of composite ceramics substrate is as follows:
S1:Batch mixing:Weigh boron nitride ceramics powder, the E-03 type rings of 10 weight portions that 85 weight portion particle diameter D50 are 10um The calcined kaolin additive and 2 weights of oxygen resin adhesive, the talcum powder of 1 weight portion, the silica flour of 1 weight portion and 1 weight portion The trimellitic acid anhydride curing agents of part are measured, is put into V-arrangement batch mixer and is mixed 3 hours, obtain batch mixing;
S2:Coating:Selection glass fabric is matrix material, and glass fibre is tiled, then batch mixing is uniformly coated On the surface of glass fibre;
S3:Prebake conditions:The glass fibre that batch mixing will have been coated is put into baking oven, is toasted 30 minutes under the conditions of 140 DEG C, is obtained To pre impregnated material;
S4:Hot pressed sintering:Pre impregnated material is taken out, is put into hot press, at 180 DEG C, pressure is hot pressing under 30MPa 5 hours;
S5:After the completion of hot pressing, room temperature is cooled to, obtains composite ceramics substrate.
Gained boron nitride ceramics composite material surface smoothness is good, and hardness is 2, and fracture toughness is 4.0Mpam1/2, tension is strong It is 50MPa to spend, and bending strength is 100MPa, and up to 220 DEG C of non yellowings, thermal coefficient of expansion is 4.2 × 10 to resistance to temperature-5/℃.Prepare During without pernicious gas produce.
Embodiment 4
Silicon carbide ceramics mixed slurry, including following composition materials:
85 weight portion particle diameter D50 are the Silicon Carbide Powder of 10um,
The E-03 type epoxy resin of 10 weight portions,
The calcined kaolin of the talcum powder of 1 weight portion, the silica flour of 1 weight portion and 1 weight portion,
The trimellitic anhydride of 2 weight portions.
The preparation technology of composite ceramics substrate is as follows:
S1:Batch mixing:Weigh Silicon Carbide Powder, the E-03 type rings of 10 weight portions that 85 weight portion particle diameter D50 are 10um The calcined kaolin additive and 2 weights of oxygen resin adhesive, the talcum powder of 1 weight portion, the silica flour of 1 weight portion and 1 weight portion The trimellitic acid anhydride curing agents of part are measured, is put into V-arrangement batch mixer and is mixed 3 hours, obtain batch mixing;
S2:Coating:Selection glass fabric is matrix material, and glass fibre is tiled, then batch mixing is uniformly coated On the surface of glass fibre;
S3:Prebake conditions:The glass fibre that batch mixing will have been coated is put into baking oven, is toasted 30 minutes under the conditions of 140 DEG C, is obtained To pre impregnated material;
S4:Hot pressed sintering:Pre impregnated material is taken out, is put into hot press, at 180 DEG C, pressure is hot pressing under 30MPa 5 hours;
S5:After the completion of hot pressing, room temperature is cooled to, obtains composite ceramics substrate.
Gained composite silicon carbide ceramic material surface smoothness is good, and hardness is 7.2, and fracture toughness is 8.0Mpam1/2, resistance to compression Intensity is 200MPa, and bending strength is 10MPa, and up to 250 DEG C of non yellowings, thermal coefficient of expansion is 0.92 × 10 to resistance to temperature-5/℃。 Produced without pernicious gas in preparation process.
Compared with prior art, composite ceramics substrate of the invention not only has the special property of ceramics, and manufacture craft Simply, sintering temperature is low in preparation process, during go out without pernicious gas benefit substantially, be a kind of novel green ceramic material.
Finally it should be noted that:Above-described each embodiment is merely to illustrate technical scheme, rather than to it Limitation;Although being described in detail to the present invention with reference to the foregoing embodiments, it will be understood by those within the art that: It can still modify to the technical scheme described in previous embodiment, or which part or all technical characteristic are entered Row equivalent;And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technical side The scope of case.

Claims (10)

1. a kind of composite ceramics substrate, including mixed slurry and matrix material, it is characterised in that:The mixed slurry includes following Composition material:
The ceramic powder of 50-85 weight portions,
The bonding agent of 5-40 weight portions,
The additive of 3-5 weight portions,
The curing agent of 1-5 weight portions,
Wherein:
The particle diameter of the ceramic powder is 1-10um,
The ceramic powder is oxide ceramic powder body, nitride ceramics powder, boride ceramics powder and carbide ceramics powder One or more in body.
2. composite ceramics substrate according to claim 1, it is characterised in that:The oxide ceramic powder body is Al2O3、 ZrO2, BeO, MgO and TiO2In one or more.
3. composite ceramics substrate according to claim 1, it is characterised in that:It is described nitridation ceramic powder be AlN, BN, Si3N4With one or more in ZrN.
4. composite ceramics substrate according to claim 1, it is characterised in that:The boride ceramics powder is ZrB2With TiB2In one or two.
5. composite ceramics substrate according to claim 1, it is characterised in that:The carbide ceramics powder is B4C、SiC、 One or more in ZrC, TiC and WC.
6. composite ceramics substrate according to claim 1, it is characterised in that:The bonding agent be thermosetting epoxy resin or Heat curing-type modified epoxy.
7. composite ceramics substrate according to claim 1, it is characterised in that:The additive is diatomite, talcum powder, forging Burn one or more in kaolin, silica flour and titanium dioxide.
8. composite ceramics substrate according to claim 1, it is characterised in that:The curing agent is m-phenylene diamine (MPD), diaminourea One or more in diphenyl sulfone, trimellitic anhydride and mellophanic acid acid anhydride.
9. composite ceramics substrate according to claim 1, it is characterised in that:Described matrix material is carbon fiber, glass fibers One or more mixing in dimension, polyester fiber and metallic fiber, the metallic fiber be aluminum fiber net, stainless steel fiber web, It is combined for one or more in copper fiber net, titanium fleece and magnesium alloy fleece.
10. a kind of method for preparing the composite ceramics substrate described in claim any one of 1-9, it is characterised in that:Including following Step:
S1:Batch mixing:Ceramic powder, bonding agent, additive and the curing agent of dosage are weighed, are put into blender and are mixed 1-5 hours, Obtain batch mixing;
S2:Coating:Matrix material is tiled, then batch mixing is coated uniformly on the surface of stock;
S3:Prebake conditions:The matrix material that batch mixing will have been coated is put into baking oven, is toasted 30-60 minutes under the conditions of 80-140 DEG C, Obtain pre impregnated material;
S4:Hot pressed sintering:Pre impregnated material is taken out, is put into hot press, at 150-220 DEG C, pressure is under 20-100MPa Hot pressing 1-5 hours;
S5:After the completion of hot pressing, room temperature is cooled to, obtains composite ceramics substrate.
CN201611239204.6A 2016-12-28 2016-12-28 Compound ceramic substrate and preparation method thereof Pending CN106699212A (en)

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Application publication date: 20170524