CN104276815B - A kind of high heat conduction oxide ceramic material and preparation method thereof - Google Patents

A kind of high heat conduction oxide ceramic material and preparation method thereof Download PDF

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CN104276815B
CN104276815B CN201310285765.XA CN201310285765A CN104276815B CN 104276815 B CN104276815 B CN 104276815B CN 201310285765 A CN201310285765 A CN 201310285765A CN 104276815 B CN104276815 B CN 104276815B
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CN104276815A (en
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单喆恺
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Shanghai jingkaide Photoelectric Technology Co.,Ltd.
SHANGHAI JINGKAIDE PRECISION CERAMICS Co.,Ltd.
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SHANGHAI JINGKAIDE PRECISION CERAMICS CO Ltd
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Abstract

The present invention relates to new ceramic material technical field, and in particular to a kind of oxide ceramic material and preparation method thereof.A kind of high heat conduction oxide ceramic material, as follows including raw material components:Magnesia 70%~96%, aluminum oxide 2%~25%, silica 0.2%~1.2%, calcium oxide 0.2%~2.5%, iron oxide 0.1%~0.5%, zircon 0.5%~1.5%, prepares after repairing the processing steps such as stage, the stage of burning till, rear road process segment and end properties test phase by raw material preparatory stage, ball milling stage and wax stage, formative stage, first burning stage, base substrate.Due to adopting above-mentioned technical proposal, sintering temperature of the present invention is lower, reduces energy resource consumption, improve yield rate, reduce manufacturing cost, product in addition to intensity height, high temperature resistant, the superior function such as corrosion-resistant, with the more excellent thermal diffusion of more general oxide material and heat-conductive characteristic.

Description

A kind of high heat conduction oxide ceramic material and preparation method thereof
Technical field
The present invention relates to new ceramic material technical field, and in particular to a kind of oxide ceramic material and its preparation side Method.
Background technology
Common ceramic material typically has the performances such as preferable heat-and corrosion-resistant, but more thin on heat-conductive characteristic Weak, it is impossible to meet the use requirement of a lot of heat collection neutralization thermal components.And preferably material is very expensive, as aluminium nitride etc..
The useful aluminum oxide of existing frequently-used ceramic heat emission material, talcum etc..Talcum belongs to lower end material, as radiator When thermal conductivity bad;Although the thermal conductivity factor of aluminium oxide ceramics is preferably, 15W/m K~25W/m K are reached, comparatively Or it is relatively low.We know magnesia ceramics heat conduction than aluminum oxide well a lot, and cost is not high, but make to get up to be stranded very much Difficulty, one is the moisture in the easy absorption air of manufacturing process magnesia powder, easily reunites;Two is to sinter more difficult, traditional handicraft burning Oxygenerating magnesium wants more than 1700 DEG C of high temperature, and not only with energy high cost, and crystalline phase is difficult to control, and which part crystal can also be put Greatly.And having the process that Emission in Cubic inversion is Tetragonal, the blank structure that works it out is more loose, low intensity, the pottery that finally produces Porcelain heat conductivility is unsatisfactory.
Content of the invention
An object of the present invention is, there is provided a kind of high heat conduction oxide ceramic material, solves above technical problem.
Another object of the present invention is to, there is provided a kind of preparation method of high heat conduction oxide ceramic material, more than solution Technical problem.
Technical problem solved by the invention can employ the following technical solutions to realize:
A kind of high heat conduction oxide ceramic material, it is characterised in that including following materials by weight:Oxidation Magnesium 70%~96%, aluminum oxide 2%~25%, silica 0.2%~1.2%, calcium oxide 0.2%~2.5%, iron oxide 0.1%~ 0.5%, zircon 0.5%~1.5%.
In the present invention, magnesia and aluminum oxide account for leading composition in component, wherein mix a small amount of silica, oxidation , used as filling components, in order to strengthen other characteristics of product, wherein silica can reduce sintering temperature for calcium, iron oxide and zircon Degree, and with higher acid resistance, product opposing acid corrosion characteristic can be improved, while can increase as binding agent intermolecular Pulling force, increases glass phase, suppresses crystal grain excessive;Calcium oxide has to be reduced sintering temperature and plays a part of stabilizer;Zircon As acid refractory, the natural decomposition speed of magnesia can be reduced, increase the life-span, at the same with higher dielectric properties and Mechanical performance, can increase the associativity of molecule, can increase into the toughness after porcelain.
Aluminum oxide and magnesia all have good fire-resistance property, and the thermal conductivity ratio aluminium oxide ceramics of magnesia ceramics is also high More than twice, and the composition weight proportioning of the magnesia in the present invention reaches more than 70%, then makes both by sintering curre fusion A certain proportion of spinel structure is combined to form, therefore product of the invention compares conventional aluminium oxide ceramic with more preferably Heat conductivility.
Zircon ingredient in the present invention is(ZrSiO4), i.e. zirconium silicate, zirconium silicate(ZrSiO4)Theoretical composition be 67.1% zirconium oxide(ZrO2)With 32.9% silica(SiO2), zirconium oxide(ZrO2)Prepare in part forming process in pottery, help In the formation of glass phase, bond strength is increased, when magnesia and aluminum oxide occur to change from tetragonal phase to cube crystalline phase, Shunk as zirconium oxide first can be expanded in phase transition process again, the change of the phase transition process volume between other materials is adapted, The dislocation and the porosity for making crystal is reduced, and is enhanced material and is prepared damage tolerance of the part in sintering, suppresses or prevent crackle Diffusion, increased overall compactness and fracture toughness.
A kind of preparation method of high heat conduction oxide ceramic material, it is characterised in that the component is through a manufacturing process Sintered moulded body is prepared, the manufacturing process includes raw material preparatory stage, ball milling stage and wax stage, formative stage, just burns rank Section, base substrate finishing stage, the stage of burning till, rear road process segment and end properties test phase.
The step of manufacturing process, is as follows:
1)The raw material preparatory stage:First then the component is pressed by magnesium oxide powder with 900 DEG C of -1100 DEG C of temperature calcinations Successively to import according to setting weight proportioning and original mixture is made after mixing in storage container, original mixture feeding drying box is done Dry, make powder depart from moisture, in case powder bonds in ball milling, be then stirred with planetary ball mill so as to which mixing is Even fully rear prepared material to be ground;
2)The ball milling stage:The ballstone of different-grain diameter is added in planetary ball mill, and is stirred after adding dispersant, Powder is derived after mixing time being set persistently, obtain superfine powder, superfine powder is imported in baking oven and is fully dried again, with Just and wax;
3)With the wax stage:Fully refined paraffin wax is dissolved, is added in the powder of milled, be then introduced in frame-type mixer After continuing setting time stirring, the slurry of a high plasticity is obtained;
4)Formative stage:By step 3)The slurry of generation is transported in hot-injection molding machine, installs mould, carries out pressure injection Shaping, forms preliminary base substrate;
5)Just burn the stage:By step 4)The material base substrate of generation is sent in middle temperature shuttle kiln, and according to just burning temperature control The operational factor of koji line centering temperature shuttle kiln is set, and is floated in design temperature scope by system control kiln temperature, Finally continue setting time insulation so that sizing, the more loose first base of prepared density is sintered to material base substrate;
6)Base substrate repairs the stage:Burned first base is repaired, unnecessary burr and base bits is removed, sand for surface skin Polishing is slided, and is polished where having plane, to improve yield rate;
7)Burn till the stage:First base after by finishing is sent in tunnel kiln and is sintered finished product again;By tunnel cave Stove carries out temperature control according to firing temperature controlling curve;
8)Road process segment afterwards:Porcelain piece after by cooling is put into polissoir and removes surface spikes and small attaching particles, Make fineness reach Ra0.8, then thermal conductive surface is polished with mechanical grinding machine, make it possible to hot face of fully fitting;
9)End properties are tested:Test block is done with standard disk, end properties are tested by laser determination instrument.
In the present invention, by magnesium oxide powder with high-temperature calcination, allows magnesia lose a part of activity, 60%- can be reduced 70% water absorption rate.
The step of manufacturing process 5)First burning temperature control curve by the stage be followed successively by the first temperature rise period, second liter Thermophase, the 3rd temperature rise period, constant temperature stage and natural cooling stage, specially:
First temperature rise period:Continue 19 hours, by room temperature to 300 DEG C;
Second temperature rise period:Continue 10 hours, 600 DEG C are warming up to by 300 DEG C;
3rd temperature rise period:Continue 8 hours, 1060 DEG C are warming up to by 600 DEG C;
The constant temperature stage:Continue 2 hours~3 hours, holding temperature is 1060 DEG C;
The natural cooling stage:Continue 9 hours~10 hours, be cooled to normal temperature scope.
Should ensure that product does not flow wax due to just burning de-waxing, ensure speed during volume production again, therefore preferably just burn temperature Controlling curve is:
First temperature rise period:Continue 19 hours, by room temperature to 300 DEG C;
Second temperature rise period:Continue 10 hours, 600 DEG C are warming up to by 300 DEG C;
3rd temperature rise period:Continue 8 hours, 1060 DEG C are warming up to by 600 DEG C;
The constant temperature stage:Continue 2 hours, holding temperature is 1060 DEG C;
The natural cooling stage:Continue 9 hours~10 hours, be cooled to normal temperature scope.
The step of manufacturing process 7)Firing temperature controlling curve by the stage be followed successively by the first temperature rise period, second liter Thermophase, the first constant temperature stage, the 3rd temperature rise period, the second constant temperature stage and natural cooling stage, specially:
First temperature rise period:Continue 5-7 hours, by room temperature to 1000 DEG C;
Second temperature rise period:Continue 4-6 hours, 1450 DEG C are warming up to by 1000 DEG C;
First constant temperature stage:Continue 1 hour, 1450 DEG C of holding temperature;
3rd temperature rise period:Continue 3-5 hours, 1650 DEG C are warming up to by 1450 DEG C;
Second constant temperature stage:Continue 2-4 hours, 1650 DEG C of holding temperature;
The natural cooling stage:Room temperature scope is persistently naturally cooled to.
It is preferred that firing temperature controlling curve is:
First temperature rise period:Continue 5 hours, by room temperature to 1000 DEG C;
Second temperature rise period:Continue 4 hours, 1450 DEG C are warming up to by 1000 DEG C;
First constant temperature stage:Continue 1 hour, 1450 DEG C of holding temperature;
3rd temperature rise period:Continue 3 hours, 1650 DEG C are warming up to by 1450 DEG C;
Second constant temperature stage:Continue 2 hours, 1650 DEG C of holding temperature;
The natural cooling stage:Room temperature scope is persistently naturally cooled to.
In the present invention, the temperature due to sintering reduces, and heating curve is improved, it is not necessary to dead roasting magnesia, and sinters Process time can be shortened, and save time and cost.And molecule can be crystallized at lower temperatures, stabilizer is added Effect, prevent reverse (cube->Four directions) crystalline phase change, make crystal boundary more consistent.With the help of zirconium oxide, between crystal boundary Space is reduced, and structure is tightr, increased bounce of the phonon between crystal boundary, increased heat-transfer rate, thin with feed particles Change, thermal conductivity may proceed to improve.
The step of concrete steps 2)Superfine powder in the particle containing more than 20% 1um particle diameters, more than 30% 5um grains The particle in footpath, the particle of less than 50% 6~20um particle diameters.
The step of manufacturing process 1)In planetary ball mill stir speed (S.S.) be 55rpm~75rpm, preferably 60rpm.
The step of manufacturing process 1)In planetary ball mill rotating ratio preferably 1:4.
The step of manufacturing process 1)In the mixing time of planetary ball mill be set as 10 minutes.
The step of manufacturing process 2)In ballstone preferably adopt zirconium oxide ballstone.
The step of manufacturing process 2)In ballstone particle size range be 20mm~40mm.
The step of manufacturing process 2)In dispersant preferably adopt stearic acid.
The step of manufacturing process 2)In planetary ball mill stir speed (S.S.) be 180rpm~250rpm, preferably 235rpm.
The step of manufacturing process 2)In the planetary drive ratio of planetary ball mill be preferably set to 1:6.
The step of manufacturing process 2)In ball milling duration of planetary ball mill be set as that 6 hours~12 is little When.
The step of manufacturing process 3)In wax ratio for powder 12.5%~15%.
The step of manufacturing process 3)In mixing time be preferably set to 2 hours.
The step of manufacturing process 3)In slurry mobility >=120mm
The hardness of the ceramic material obtained through the preparation technology is HRA82-HRA88.
The density of the ceramic material obtained through the preparation technology is 3.3g/cm3-3.6g/cm3.
The thermal conductivity factor of the ceramic material obtained through the preparation technology is 25W/m K-45W/m K.
The bending strength of the ceramic material obtained through the preparation technology is 300MPa-430MPa.
The ceramic material obtained through the preparation technology insoluble in organic solvent, due to the change of crystalline phase, chemically Matter is stable, normal using oxidized going bad, can be with the general acid and alkali corrosion of resistance to great majority.
Beneficial effect:Due to adopting above-mentioned technical proposal, the present invention make high fine and close, inexpensive new highly heat-conductive carbon/ceramic Ceramic material, sintering temperature are lower than magnesia, only 1650 DEG C, reduce energy resource consumption, can make of hot-press method, standard Heating curve is controlled, and improves yield rate, reduces manufacturing cost, and resulting product is except having intensity height, high temperature resistant, corrosion-resistant etc. Outside superior function, with the more excellent thermal diffusion of more general oxide material and heat-conductive characteristic;Can be used for LED illumination lamp Radiator, computer and chip for cell phone check piece radiating etc., more effectively reduce temperature, increase electronic devices and components service life.
Description of the drawings
Fig. 1 is the process flow diagram of the present invention;
Fig. 2 is the first burning temperature control curve figure of the present invention;
Fig. 3 is the firing temperature controlling curve figure of the present invention.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below Conjunction is specifically illustrating and the present invention is expanded on further.
With reference to Fig. 1, a kind of high heat conduction oxide ceramic material, including following materials by weight:Magnesia 70%~96%, aluminum oxide 2%~25%, silica 0.2%~1.2%, calcium oxide 0.2%~2.5%, iron oxide 0.1%~0.5%, Zircon 0.5%~1.5%.
In the present invention, magnesia and aluminum oxide account for leading composition in component, and magnesia determines that material has and preferably leads Hot, aluminum oxide and zirconium silicate determine that final finished has preferable compact structure and stability, and stronger hardness. A small amount of silica, calcium oxide, iron oxide and zircon are wherein mixed as filling components, in order to strengthen other spies of product Property, wherein silica has higher acid resistance, can improve product opposing acid corrosion characteristic, while can increase as binding agent Plus intermolecular pulling force, suppress crystal grain excessive;Calcium oxide has the thermodynamic stability better than other metal oxides, strengthens white Degree, reduces sintering temperature;Iron oxide has the effect for increasing heat conduction;Zircon can reduce magnesia as acid refractory Natural decomposition speed, increase the life-span, while with higher dielectric properties and mechanical performance, the associativity of molecule can be increased, The toughness after porcelain can be increased into.
Aluminum oxide and magnesia all have certain fire-resistance property, therefore using both components as key component material, So that product has more excellent hot-face insulation characteristic.Magnesia is a kind of powdery metal oxide of relatively lightweight, compares oxygen Change aluminium lighter, condensation of materials degree during mixing can be increased, by increasing the weight proportion of magnesia, while reducing aluminum oxide Weight proportion so that prepare part and aluminium oxide ceramic products have quality more using the part traditional ceramics that compares for preparing of this product Plus light the characteristics of.Magnesia as ceramic substrate when thermal conductivity ratio aluminum oxide as high twice during substrate more than, And the composition weight proportioning of the magnesia in the present invention reaches more than 70%, therefore product of the invention compares conventional aluminium oxide Ceramic has more preferable heat conductivility.
Zircon ingredient in the present invention is zirconium silicate(ZrSiO4), enhance material and prepare part in sinter molding Damage tolerance, suppress or prevent the diffusion of crackle.Zirconium silicate(ZrSiO4)Theoretical composition be 67.1% zirconium oxide(ZrO2) With 32.9% silica(SiO2), zirconium oxide(ZrO2)For external stress has stronger resistant property, part is prepared in pottery In sintering process, it helps the formation of glass phase, when magnesia is changed to a cube crystalline phase from tetragonal phase with aluminum oxide When, crystal can become big and produce local stress, easily produce cracking and crystal boundary staggered floor, and zirconium silicate crystal can now be formed necessarily Stress is resisted, and is hindered the formation of crackle, is improve the fracture toughness for preparing part.
Also include a manufacturing process, sintered moulded body to be prepared using said components, manufacturing process includes that raw material prepares Stage, ball milling stage and wax stage, formative stage, the first burning stage, base substrate finishing the stage, the stage of burning till, the rear road process segment and End properties test phase.The step of manufacturing process, is as follows:
1)The raw material preparatory stage:First then the component is pressed by magnesium oxide powder with 900 DEG C of -1100 DEG C of temperature calcinations Successively to import according to setting weight proportioning and original mixture is made after mixing in storage container, original mixture feeding drying box is done Dry, make powder depart from moisture, in case powder bonds in ball milling, be then stirred with planetary ball mill so as to which mixing is Even fully rear prepared material to be ground;
2)The ball milling stage:Particle diameter is added in planetary ball mill for the zirconium oxide ballstone of 20mm~40mm, and is added hard Used as dispersion machine, the stir speed (S.S.) for adjusting planetary ball mill is 235rpm to resin acid, and planetary drive ratio is 1:6, continue 6 hours~ Powder is derived after the stirring of 12 hours, obtain superfine powder, superfine powder is imported in baking oven and is fully dried again, so that and Wax;
3)With the wax stage:Fully refined paraffin wax is dissolved, is added in the powder of milled, wherein the proportioning of wax be 12.5%~ 15%, after being then introduced into continuing stirring in 2 hours in frame-type mixer, obtain the slurry of a high plasticity, the mobility of slurry ≥120mm;
4)Formative stage:By step 3)The slurry of generation is transported in hot-injection molding machine, installs mould, carries out pressure injection Shaping, forms preliminary base substrate;
5)Just burn the stage:By step 4)The material base substrate of generation is sent in middle temperature shuttle kiln, and according to just burning temperature control The operational factor of koji line centering temperature shuttle kiln is set, and is floated in design temperature scope by system control kiln temperature, Finally continue setting time insulation and natural cooling so that sizing is sintered to material base substrate, the more loose first base of prepared density, The temperature control curve of middle temperature shuttle kiln by the stage be followed successively by the first temperature rise period, the second temperature rise period, the 3rd temperature rise period, Constant temperature stage and natural cooling stage, concrete just burning temperature control curve are as shown in Figure 2:
First temperature rise period:Continue 19 hours, by room temperature to 300 DEG C;
Second temperature rise period:Continue 10 hours, 600 DEG C are warming up to by 300 DEG C;
3rd temperature rise period:Continue 8 hours, 1060 DEG C are warming up to by 600 DEG C;
The constant temperature stage:Continue 2 hours, holding temperature is 1060 DEG C;
The natural cooling stage:Continue 9 hours~10 hours, be cooled to normal temperature scope.
6)Base substrate repairs the stage:Burned first base is repaired, unnecessary burr and base bits is removed, sand for surface skin Polishing is slided, and is polished where having plane, to improve yield rate;
7)Burn till the stage:After first base after by finishing is sent in tunnel kiln, by tunnel kiln according to firing temperature control After curve carries out temperature control, finished product is sintered again to first base;, concrete firing temperature controlling curve such as Fig. 3 shows:
First temperature rise period:Continue 5 hours, by room temperature to 1000 DEG C;
Second temperature rise period:Continue 4 hours, 1450 DEG C are warming up to by 1000 DEG C;
First constant temperature stage:Continue 1 hour, 1450 DEG C of holding temperature;
3rd temperature rise period:Continue 3 hours, 1650 DEG C are warming up to by 1450 DEG C;
Second constant temperature stage:Continue 2 hours, 1650 DEG C of holding temperature;
The natural cooling stage:Continue natural cooling until room temperature scope;
8)Road process segment afterwards:Porcelain piece after by cooling is put into polissoir and removes surface spikes and small attaching particles, Make fineness reach Ra0.8, then thermal conductive surface is polished with mechanical grinding machine, make it possible to hot face of fully fitting;
9)End properties are tested:Test block is done with standard disk, end properties is tested by laser determination instrument,
The step of manufacturing process 2)Superfine powder be contained within the particle of more than 20% 1um particle diameters, more than 30% 5um particle diameters Particle, the particle of less than 50% 6~20um particle diameters.
Embodiment 1:Weigh magnesia 70%, aluminum oxide 25%, silica 1 .2%, calcium oxide 2.3%, iron oxide 0.5%, zirconium Diamond stone 1.0% is preparing raw material, by above-mentioned manufacturing technology steps finished product 1.
Embodiment 2:Weigh magnesia 82%, aluminum oxide 13%, silica 1 %, calcium oxide 2.5%, iron oxide 0.3%, zirconium English Stone 1.2% is preparing raw material, by above-mentioned manufacturing technology steps finished product 2.
Embodiment 3:Weigh magnesia 90%, aluminum oxide 6%, silica 1 %, calcium oxide 1.5%, iron oxide 0.3%, zirconium English Stone 1.2% is preparing raw material, by above-mentioned manufacturing technology steps finished product 3.
Embodiment 4:Weigh magnesia 95%, aluminum oxide 3%, silica 0.5%, calcium oxide 0.5%, iron oxide 0.1%, zirconium Diamond stone 0.9% is preparing raw material, by above-mentioned manufacturing technology steps finished product 4.
Said components final finished obtains following performance data after measured afterwards:
From above-mentioned performance data table, the thermal diffusivity and pyroconductivity of four kinds of formulas of the present invention are superior to typically Alumina material.
The hardness of the ceramic material obtained through preparation technology is HRA82-88, and bending strength is 300-430MPa.
The ceramic material obtained through preparation technology does not dissolve in organic solvent, and due to the change of crystalline phase, chemical property is steady Fixed, normal using oxidized going bad, can be with the general acid and alkali corrosion of resistance to great majority.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry Personnel it should be appreciated that the present invention is not restricted to the described embodiments, simply explanation described in above-described embodiment and specification this The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes Change and improvement is both fallen within scope of the claimed invention.The claimed scope of the invention by appending claims and its Equivalent thereof.

Claims (8)

1. a kind of high heat conduction oxide ceramic material, it is characterised in that including following materials by weight:Magnesia 70%~82%, aluminum oxide 2%~25%, silica 0.2%~1.2%, calcium oxide 0.2%~2.5%, iron oxide 0.1%~0.5%, zircon 0.5%~1.5%;
The raw material components prepare sintered moulded body through a manufacturing process, and the manufacturing process includes raw material preparatory stage, ball Mill stage and wax stage, formative stage, first burning stage, base substrate finishing stage, the stage of burning till, rear road process segment and into moral character Can test phase;
The step of manufacturing process, is as follows:
1) the raw material preparatory stage:First by magnesium oxide powder with 900 DEG C of -1100 DEG C of temperature calcinations, then by the component according to setting Determine original mixture to be made after weight proportion successively imports the interior mixing of storage container, original mixture is sent into drying box and is dried, Make powder depart from moisture, in case powder bonds in ball milling, be then stirred with planetary ball mill so as to be well mixed and fill Material to be ground is obtained after point;
2) the ball milling stage:The ballstone of different-grain diameter is added in planetary ball mill, and is stirred after adding dispersant, continue Powder is derived after setting mixing time, obtain superfine powder, superfine powder is imported in baking oven and is fully dried again, so that and Wax;
3) with the wax stage:Fully refined paraffin wax is dissolved, is added in the powder of milled, be then introduced into continuing in frame-type mixer After setting time stirring, the slurry of a high plasticity is obtained;
4) formative stage:By step 3) slurry that generates is transported in hot-injection molding machine, installs mould, carry out pressure injection into Type, forms preliminary base substrate;
5) just burn the stage:By step 4) the material base substrate that generates is sent in middle temperature shuttle kiln, and the fortune of centering temperature shuttle kiln Line parameter is set, and is floated in design temperature scope by system control kiln temperature, and finally persistently setting time is incubated and oneself So cooling to be sintered sizing, the more loose first base of prepared density to material base substrate;
6) the base substrate finishing stage:Burned first base is repaired, unnecessary burr and base bits is removed, sand for surface skin polishing Sliding, polish where having plane, to improve yield rate;
7) burn till the stage:First base after by finishing is sent in tunnel kiln, the temperature of tunnel kiln is controlled, is sintered again Finished product;
8) road process segment afterwards:Porcelain piece after by cooling is put into polissoir and removes surface spikes and small attaching particles, makes light Cleanliness reaches Ra0.8, then polishes thermal conductive surface with mechanical grinding machine;
9) end properties test:Test block is done with standard disk, end properties are tested by laser determination instrument.
2. a kind of preparation method of high heat conduction oxide ceramic material according to claim 1, it is characterised in that the system 5) the step of making technique is set according to the operational factor for just burning temperature control curve centering temperature shuttle kiln, the just burning temperature Degree controlling curve is followed successively by the first temperature rise period, the second temperature rise period, the 3rd temperature rise period, constant temperature stage and naturally cold by the stage But stage, specially:
First temperature rise period:Continue 19 hours, by room temperature to 300 DEG C;
Second temperature rise period:Continue 10 hours, 600 DEG C are warming up to by 300 DEG C;
3rd temperature rise period:Continue 8 hours, 1060 DEG C are warming up to by 600 DEG C;
The constant temperature stage:Continue 2 hours~3 hours, holding temperature is 1060 DEG C;
The natural cooling stage:Continue 9 hours~10 hours, be cooled to normal temperature scope.
3. a kind of preparation method of high heat conduction oxide ceramic material according to claim 1, it is characterised in that the system 7) the step of making technique is controlled to the temperature of tunnel kiln according to firing temperature controlling curve, and the firing temperature control is bent Line is followed successively by the first temperature rise period, the second temperature rise period, the first constant temperature stage, the 3rd temperature rise period, the second constant temperature rank by the stage Section and natural cooling stage, specially:
First temperature rise period:Continue 5-7 hours, by room temperature to 1000 DEG C;
Second temperature rise period:Continue 4-6 hours, 1450 DEG C are warming up to by 1000 DEG C;
First constant temperature stage:Continue 1 hour, 1450 DEG C of holding temperature;
3rd temperature rise period:Continue 3-5 hours, 1650 DEG C are warming up to by 1450 DEG C;
Second constant temperature stage:Continue 2-4 hours, 1650 DEG C of holding temperature;
The natural cooling stage:Room temperature scope is persistently naturally cooled to.
4. a kind of preparation method of high heat conduction oxide ceramic material according to claim 1, it is characterised in that the system The step of making technique superfine powder 2) is contained within the particle of more than 20% 1um particle diameters, the particle of more than 30% 5um particle diameters, The particle of less than 50% 6um~20um particle diameters.
5. a kind of preparation method of high heat conduction oxide ceramic material according to claim 1, it is characterised in that the system The step of making technique 1) in planetary ball mill stir speed (S.S.) be 55rpm~75rpm, rotating ratio is 1:4, mixing time sets It is set to 10 minutes.
6. a kind of preparation method of high heat conduction oxide ceramic material according to claim 1, it is characterised in that the system The step of making technique 2) in ballstone adopt zirconium oxide ballstone, the particle size range of ballstone is 20mm~40mm, and dispersant is using hard Resin acid, the stir speed (S.S.) of planetary ball mill are set as that the planetary drive ratio of 180rpm~250rpm planetary ball mills is set as 1:6, the ball milling duration is set as 6 hours~12 hours.
7. a kind of preparation method of high heat conduction oxide ceramic material according to claim 1, it is characterised in that the system The step of making technique 3) in wax ratio for powder 12.5%~15%, mixing time is set as 2 hours, the mobility of slurry ≥120mm.
8. the preparation method of a kind of high heat conduction oxide ceramic material according to any one of claim 1 to 7, its feature It is, the thermal conductivity factor of the ceramic material obtained through the preparation technology reaches 25W/m K-45W/m K, and hardness is HRA82-HRA88, bending strength are 300MPa-430MPa.
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CN108505715B (en) * 2018-04-16 2020-01-17 广东金意陶陶瓷集团有限公司 High-heat-conductivity long-service-life electric heating ceramic tile and manufacturing method thereof
CN110542702A (en) * 2019-09-21 2019-12-06 孟津青城古建制品有限公司 Method for controlling sintering curve of three-hole landscape archaized brick
CN112552048B (en) * 2020-12-25 2021-10-26 广东奥迪威传感科技股份有限公司 Preparation method of potassium-sodium niobate ceramic with high piezoelectric property and high remanent polarization
CN113121128B (en) * 2021-06-04 2023-03-17 嘉华特种水泥股份有限公司 High-strength toughened cementing material and preparation method and application thereof

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