CN108129139A - A kind of preparation method of high-strength alumina ceramic substrate - Google Patents

A kind of preparation method of high-strength alumina ceramic substrate Download PDF

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CN108129139A
CN108129139A CN201711363239.5A CN201711363239A CN108129139A CN 108129139 A CN108129139 A CN 108129139A CN 201711363239 A CN201711363239 A CN 201711363239A CN 108129139 A CN108129139 A CN 108129139A
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ceramic substrate
alumina ceramic
obtains
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preparation
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龙仕冬
何少雄
陈可
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CHANGZHOU HAO LI LAI PHOTO-ELECTRICITY SCIENCE AND TECHNICAL Co Ltd
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CHANGZHOU HAO LI LAI PHOTO-ELECTRICITY SCIENCE AND TECHNICAL Co Ltd
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    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B2235/44Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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    • C04B2235/602Making the green bodies or pre-forms by moulding
    • C04B2235/6025Tape casting, e.g. with a doctor blade

Abstract

The invention discloses a kind of preparation methods of high-strength alumina ceramic substrate, belong to ceramic substrate preparing technical field.The present invention can form ultrafine aluminium hydroxide crystal grain after carbon dioxide is passed through sodium aluminate solution, incorporation precursor sol tape casting obtains the good curtain coating raw material band of caking property, since the coefficient of thermal expansion of colloidal sol is higher, cohesive toughening effect is played, so as to which craze and transfiguration occur when avoiding alumina ceramic substrate sinter molding;Colloidal sol can grow mullite crystal whisker through oversintering postcooling in the micro-drill(ing) of alumina ceramic substrate of the present invention, the aluminium oxide particles of alumina ceramic substrate is made to be wound by brilliant silk, brilliant silk is conducive to internal stress and is evenly distributed, reduce the relative displacement between aluminium oxide and crystalline silicates, and brilliant silk can inhibit crystal grain agglomeration, the stomata in ceramics can be effectively reduced, so as to improve the compactness of sintered body, make crystal grain distribution in alumina ceramic substrate uniform, crystal grain distribution is fine and close, mechanical strength enhances, and has a extensive future.

Description

A kind of preparation method of high-strength alumina ceramic substrate
Technical field
The invention discloses a kind of preparation methods of high-strength alumina ceramic substrate, belong to ceramic substrate technology of preparing neck Domain.
Background technology
Aluminium oxide ceramics is a kind of ceramic material based on aluminium oxide, for thick film integrated circuit.Aluminium oxide ceramics There are preferable conductibility, mechanical strength and heat-resisting quantity, it should be noted that need to be washed with ultrasonic wave.Aluminium oxide ceramics is A kind of widely used ceramics because its superior performance, more and more extensive in the application of modern society, are satisfied with daily With the needs of property.Aluminium oxide ceramics is divided into two kinds of high-purity type and plain edition.
Alumina ceramic substrate is widely used in electronics industry field, as electronic package material, substrate material, multilayer Capacitor material and materials of electronic components etc..Doctor-blade casting process is because its production efficiency is high, equipment is simple, easy to operate, it has also become Prepare the important forming method of alumina ceramic substrate.
In general, casting molding processes include the processes such as slurry preparation, molding, dry.It needs to add in ceramic powder molten Agent, dispersant, binding agent, plastic agent and defrother etc. prepare the slurry of stable uniform, are molded to obtain one by casting machine Determine the curtain coating raw material band of thickness, raw material band obtains required ceramic substrate after drying and sintering.
Aluminium oxide electronic package material has good electrical isolation for carrying electronic component and its connection circuit Property.Encapsulation has mechanical support and Environmental Role to chip, and hot property, reliability to device and circuit play important work With.Quad flat non-pin package is a kind of novel surface labeling type electronic packing forms, now also to be known as LCC encapsulation more. For LCC packing forms, back side surrounding is configured with electrode contacts, due to no lead, so conductive path is shorter, electric property It is excellent, at the same mount area than CQFP type encapsulate it is small, mounting height is relatively low, these performances for being all conducive to electronic component carry It rises, volume reduces, and reliability improves, and is the Main way of the product research of recent domestic Electronic Packaging and application.
There are craze and transfiguration and alumina ceramic-base easily occur during sinter molding for current alumina ceramic substrate The defects of piece intensity is relatively low.Therefore, inventing a kind of high-strength alumina ceramic substrate has ceramic substrate preparing technical field Positive effect.
Invention content
Present invention mainly solves the technical issues of, become for cracking easily occurs during alumina ceramic substrate sinter molding The defects of shape and relatively low alumina ceramic substrate intensity, provides a kind of preparation method of high-strength alumina ceramic substrate.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of high-strength alumina ceramic substrate, it is characterised in that specifically preparation process is:
(1)70~80g kyanite ores in sand form are placed in ball grinder, add in agate ball milling pearl, ball milling obtains aquamaine mountain flour, by aquamaine Mountain flour, which mixes to be put into ball grinder with aluminum fluoride trihydrate, continues ball milling, obtains mixed mineral powder, mixed mineral powder is put into corundum crucible In, heat temperature raising, heat preservation calcining obtains mullite;
(2)Mullite is put into mortar and is ground, sieving obtains Mullite Powder, 60~70g Mullite Powders are put into 200~ In 300mL Ludox, the shearing of high-speed shearing machine high speed is transferred to after being dispersed with stirring, 40~50mL is added in into high-speed shearing machine Aluminum nitrate solution adds pH in ammonium hydroxide regulation system, continues high speed shear, still aging, obtains precursor sol;
(3)Precursor sol is placed in supercentrifuge, high speed centrifugation processing removes supernatant liquor, obtains lower sediment, will Precipitation is washed 3~4 times, then the precipitation after washing is mixed dispersion with n-butanol successively with distilled water, absolute ethyl alcohol, is put into ventilation It is dry in drying box, obtain precursor powder;
(4)700~800mL sodium aluminate solutions are fitted into beaker, carbon dioxide gas is led into beaker, after ventilation, to 150~180g precursor powders and 8~10g ammonium polyacrylates are added in beaker, beaker is placed in water-bath, heat temperature raising, It is stirred, obtains mixed slurry;
(5)Mixed slurry is poured into tape casting machine and is cast, after slurry curtain coating to be mixed, standing and drying obtains curtain coating life Material strip;
(6)Curtain coating raw material band is placed in resistance furnace, is heated up, is kept the temperature, cooling obtains blank strip, and blank strip taking-up is put into presoma It impregnates, is placed into resistance furnace in colloidal sol, heat temperature raising, heat preservation sintering obtains alumina ceramic substrate.
Step(1)The grain size of the agate ball milling pearl be 6~8mm, Ball-milling Time be 30~45min, aquamaine mountain flour with The mass ratio of aluminum fluoride trihydrate mixing is 3 ︰ 1, and continuation Ball-milling Time is 1~2h, is to temperature after corundum crucible heat temperature raising 1550~1600 DEG C, heat preservation calcination time is 4~5h.
Step(2)The milling time is 3~4h, and specification of being sieved is 200 mesh, and the mass fraction of Ludox is 25%, The time is dispersed with stirring as 10~15min, high-speed shearing machine rotating speed is 4000~5000r/min, the mass fraction of aluminum nitrate solution It is 10%, the mass fraction of ammonium hydroxide is 50%, and pH is 9~10 in regulation system, and the continuation high speed shear time is 15~20min, quiet Put digestion time for 20~for 24 hours.
Step(3)The supercentrifuge centrifugal rotational speed is 7000~8000r/min, and high speed centrifugation processing time is 10 ~15min, the mass ratio that the precipitation after washing is mixed with n-butanol are 1 ︰ 5, and aeration cabinet set temperature is 100~110 DEG C, Drying time is 2~3h.
Step(4)The mass fraction of the sodium aluminate solution is 20%, and drop rate is 20~30mL/min, during ventilation Between for 40~45min, temperature is 70~80 DEG C after heat temperature raising, is stirred the time as 30~35min.
Step(5)The control scraper height is 0.5~2.0mm, curtain coating base band rate travel for 0.5cm/s~ 1.5cm/s, 2~3h of standing and drying.
Step(6)The heating rate is 5~7 DEG C/min, and temperature is 1100~1200 DEG C after heating, and soaking time is 40~50min, temperature is 70~75 DEG C after cooling, and it is 20~25min that blank strip, which is put into dip time in precursor sol, and heating rises Temperature is 1550~1650 DEG C after temperature, and the heat preservation sintering time is 4~5h.
The beneficial effects of the invention are as follows:
(1)Kyanite ore in sand form ball milling is obtained aquamaine mountain flour by the present invention, then by aquamaine mountain flour and aluminum fluoride trihydrate mixing and ball milling, forge Burning obtains mullite, continue by mullite pulverize it is last be scattered in Ludox, add in aluminum nitrate solution, by cutting at a high speed It cuts, be aged and obtain precursor sol, precursor sol centrifugal treating is precipitated, it is washed, dispersion is mixed with n-butanol, is dry It is dry to obtain mullite precursor powder, carbon dioxide is then passed through into sodium aluminate solution, adds in precursor powder and polypropylene Sour ammonium obtains mixed slurry, and mixed slurry is placed in curtain coating in tape casting machine obtains curtain coating raw material band, and curtain coating raw material band is put Enter and obtain blank strip in resistance furnace after isothermal holding, impregnate to continue to be put into resistance furnace high temperature after blank strip with precursor sol and be sintered To alumina ceramic substrate, carbon dioxide is passed through after sodium aluminate solution by the present invention can form ultrafine aluminium hydroxide crystal grain, mix Precursor sol tape casting obtains the good curtain coating raw material band of caking property, and curtain coating raw material band is under the decomposition temperature of aluminium hydroxide Isothermal holding can generate aluminium oxide, have micro-drill(ing) inside the blank strip obtained in decomposable process due to dehydration, impregnate presoma After colloidal sol, colloidal sol is inserted in perforation, since the coefficient of thermal expansion of colloidal sol is higher, can be played in sintering process to infiltration of ambient Toughening effect is bonded, so as to which craze and transfiguration occur when avoiding alumina ceramic substrate sinter molding;
(2)Colloidal sol can grow mullite crystal whisker through oversintering postcooling in the micro-drill(ing) of alumina ceramic substrate of the present invention, The coefficient of thermal expansion of whisker is high compared to individual aluminium silicate salt, thus whisker can expand slow merisis at normal temperatures, to The brilliant silk of surrounding diffusion growth, makes the aluminium oxide particles of alumina ceramic substrate be wound by brilliant silk, brilliant when being influenced by shock loading Silk can bear most of impact forces, and when impact force is converted into internal stress in alumina ceramic substrate, brilliant silk is conducive to internal stress It is evenly distributed, reduces the relative displacement between aluminium oxide and crystalline silicates, and brilliant silk can inhibit crystal grain agglomeration, energy The stomata in ceramics is enough effectively reduced, so as to improve the compactness of sintered body, makes crystal grain distribution in alumina ceramic substrate equal Even, crystal grain distribution is fine and close, and mechanical strength enhancing has a extensive future.
Specific embodiment
70~80g kyanite ores in sand form are placed in ball grinder, the agate ball milling pearl that addition grain size is 6~8mm, ball milling 30~ 45min obtains aquamaine mountain flour, and aquamaine mountain flour is mixed to be put into ball grinder for 3 ︰ 1 in mass ratio with aluminum fluoride trihydrate and continues ball 1~2h is ground, mixed mineral powder is obtained, mixed mineral powder is put into corundum crucible, is heated to 1550~1600 DEG C, heat preservation calcining 4~5h obtains mullite;Mullite is put into mortar 3~4h of grinding, 200 mesh is crossed and sieves to obtain Mullite Powder, by 60~ 70g Mullite Powders are put into the Ludox that 200~300mL mass fractions are 25%, are transferred to after being dispersed with stirring 10~15min With the rotating speed high speed shear of 4000~5000r/min in high-speed shearing machine, 40~50mL mass point is added in into high-speed shearing machine Number is 10% aluminum nitrate solution, and it is 9~10 to add pH in the ammonium hydroxide regulation system that mass fraction is 50%, continues high speed shear 15~20min, still aging 20~for 24 hours, obtain precursor sol;Precursor sol is placed in supercentrifuge, with 7000 The rotating speed high speed centrifugation of~8000r/min handles 10~15min, removes supernatant liquor, obtains lower sediment, and precipitation is used successively Distilled water, absolute ethyl alcohol wash 3~4 times, then the precipitation after washing is mixed dispersion for 1 ︰ 5 in mass ratio with n-butanol, are put into Set temperature is in 100~110 DEG C of aeration cabinet, and dry 2~3h obtains precursor powder;By 700~800mL mass The sodium aluminate solution that score is 20% is fitted into beaker, leads to carbon dioxide gas 40 into beaker with the rate of 20~30mL/min ~45min after ventilation, 150~180g precursor powders and 8~10g ammonium polyacrylates is added in into beaker, beaker is put In water-bath, 70~80 DEG C are heated to, is stirred 30~35min, obtains mixed slurry;Mixed slurry is poured into stream Prolong in molding machine and be cast, control scraper height is 0.5~2.0mm, and curtain coating base band rate travel is 0.5cm/s~1.5cm/s, is treated After mixed slurry is cast, 2~3h of standing and drying obtains curtain coating raw material band;Curtain coating raw material band is placed in resistance furnace, with 5~ The heating rate of 7 DEG C/min is warming up to 1100~1200 DEG C, keeps the temperature 40~50min, is cooled to 70~75 DEG C, obtains blank strip, will Blank strip taking-up is put into precursor sol after 20~25min of dipping, is placed into resistance furnace, is heated to 1550~1650 DEG C, 4~5h of heat preservation sintering obtains alumina ceramic substrate.
Example 1
70g kyanite ores in sand form are placed in ball grinder, add in the agate ball milling pearl that grain size is 6mm, ball milling 30min obtains aquamaine Aquamaine mountain flour with aluminum fluoride trihydrate for 3 ︰ 1 is mixed and is put into continuation ball milling 1h in ball grinder, obtains composite ore by mountain flour in mass ratio Mixed mineral powder is put into corundum crucible by powder, is heated to 1550 DEG C, and heat preservation calcining 4h obtains mullite;Mullite is put Enter and 3h is ground in mortar, cross 200 mesh and sieve to obtain Mullite Powder, it is 25% that 60g Mullite Powders are put into 200mL mass fractions Ludox in, be transferred in high-speed shearing machine with the rotating speed high speed shear of 4000r/min after being dispersed with stirring 10min, at a high speed The aluminum nitrate solution that 40mL mass fractions are 10% is added in cutter, is added in the ammonium hydroxide regulation system that mass fraction is 50% PH is 9, continues high speed shear 15min, still aging 20h and obtains precursor sol;Precursor sol is placed in supercentrifuge In, 10min is handled with the rotating speed high speed centrifugation of 7000r/min, supernatant liquor is removed, obtains lower sediment, precipitation is used successively Distilled water, absolute ethyl alcohol wash 3 times, then the precipitation after washing is mixed dispersion for 1 ︰ 5 in mass ratio with n-butanol, are put into setting Temperature is in 100 DEG C of aeration cabinet, and dry 2h obtains precursor powder;By the sodium aluminate that 700mL mass fractions are 20% Solution is fitted into beaker, leads to carbon dioxide gas 40min into beaker with the rate of 20mL/min, after ventilation, to beaker Middle addition 150g precursor powders and 8g ammonium polyacrylates, beaker is placed in water-bath, 70 DEG C is heated to, is stirred 30min obtains mixed slurry;Mixed slurry is poured into tape casting machine and is cast, control scraper height is 0.5mm, is cast base Band rate travel is 0.5cm/scm/s, and after slurry curtain coating to be mixed, standing and drying 2h obtains curtain coating raw material band;It will curtain coating Raw material band is placed in resistance furnace, is warming up to 1100 DEG C with the heating rate of 5 DEG C/min, is kept the temperature 40min, be cooled to 70 DEG C, obtain Blank strip taking-up is put into after impregnating 20min in precursor sol, places into resistance furnace, be heated to 1550 DEG C, protect by blank strip Temperature sintering 4h, obtains alumina ceramic substrate.
Example 2
75g kyanite ores in sand form are placed in ball grinder, add in the agate ball milling pearl that grain size is 7mm, ball milling 40min obtains aquamaine Aquamaine mountain flour with aluminum fluoride trihydrate for 3 ︰ 1 is mixed and is put into continuation ball milling 1.5h in ball grinder, mixed by mountain flour in mass ratio Mixed mineral powder is put into corundum crucible by miberal powder, is heated to 1570 DEG C, and heat preservation calcining 4.5h obtains mullite;To it not come Stone, which is put into mortar, grinds 3.5h, crosses 200 mesh and sieves to obtain Mullite Powder, 65g Mullite Powders are put into 250mL mass fractions It is transferred in high-speed shearing machine with the rotating speed high speed shear of 4500r/min in 25% Ludox, to be dispersed with stirring after 12min, to The aluminum nitrate solution that 45mL mass fractions are 10% is added in high-speed shearing machine, the ammonium hydroxide that mass fraction is 50% is added and adjusts body PH is 9 in system, continues high speed shear 17min, still aging 22h and obtains precursor sol;By precursor sol be placed at a high speed from In scheming, 12min is handled with the rotating speed high speed centrifugation of 7500r/min, supernatant liquor is removed, obtains lower sediment, will precipitation according to It is secondary to be washed 3 times with distilled water, absolute ethyl alcohol, then the precipitation after washing is mixed into dispersion for 1 ︰ 5 in mass ratio with n-butanol, it is put into Set temperature is in 105 DEG C of aeration cabinet, and dry 2.5h obtains precursor powder;It is 20% by 750mL mass fractions Sodium aluminate solution is fitted into beaker, leads to carbon dioxide gas 42min into beaker with the rate of 25mL/min, after ventilation, 170g precursor powders and 9g ammonium polyacrylates are added in into beaker, beaker is placed in water-bath, 75 DEG C is heated to, stirs Mixing 32min is mixed, obtains mixed slurry;Mixed slurry to be poured into tape casting machine and is cast, control scraper height is 0.7mm, It is 1.0cm/s to be cast base band rate travel, and after slurry curtain coating to be mixed, standing and drying 2.5h obtains curtain coating raw material band;It will Curtain coating raw material band is placed in resistance furnace, is warming up to 1150 DEG C with the heating rate of 6 DEG C/min, is kept the temperature 45min, be cooled to 72 DEG C, Blank strip is obtained, blank strip taking-up is put into after impregnating 22min in precursor sol, is placed into resistance furnace, be heated to 1600 DEG C, heat preservation sintering 4.5h obtains alumina ceramic substrate.
Example 3
80g kyanite ores in sand form are placed in ball grinder, add in the agate ball milling pearl that grain size is 8mm, ball milling 45min obtains aquamaine Aquamaine mountain flour with aluminum fluoride trihydrate for 3 ︰ 1 is mixed and is put into continuation ball milling 2h in ball grinder, obtains composite ore by mountain flour in mass ratio Mixed mineral powder is put into corundum crucible by powder, is heated to 1600 DEG C, and heat preservation calcining 5h obtains mullite;Mullite is put Enter and 4h is ground in mortar, cross 200 mesh and sieve to obtain Mullite Powder, it is 25% that 70g Mullite Powders are put into 300mL mass fractions Ludox in, be transferred in high-speed shearing machine with the rotating speed high speed shear of 5000r/min after being dispersed with stirring 15min, at a high speed The aluminum nitrate solution that 50mL mass fractions are 10% is added in cutter, is added in the ammonium hydroxide regulation system that mass fraction is 50% PH is 10, continues high speed shear 20min, it is still aging for 24 hours, obtain precursor sol;Precursor sol is placed in high speed centrifugation In machine, 15min is handled with the rotating speed high speed centrifugation of 8000r/min, supernatant liquor is removed, obtains lower sediment, will precipitated successively It is washed 4 times with distilled water, absolute ethyl alcohol, then the precipitation after washing is mixed into dispersion for 1 ︰ 5 in mass ratio with n-butanol, be put into and set Constant temperature degree is in 110 DEG C of aeration cabinet, and dry 3h obtains precursor powder;By the aluminic acid that 800mL mass fractions are 20% Sodium solution is fitted into beaker, leads to carbon dioxide gas 45min into beaker with the rate of 30mL/min, after ventilation, to burning 180g precursor powders and 10g ammonium polyacrylates are added in cup, beaker is placed in water-bath, is heated to 80 DEG C, stirring 35min is mixed, obtains mixed slurry;Mixed slurry is poured into tape casting machine and is cast, control scraper height is 2.0mm, is flowed Prolong base band rate travel as 1.5cm/s, after slurry curtain coating to be mixed, standing and drying 3h obtains curtain coating raw material band;It will curtain coating Raw material band is placed in resistance furnace, is warming up to 1200 DEG C with the heating rate of 7 DEG C/min, is kept the temperature 50min, be cooled to 75 DEG C, obtain Blank strip taking-up is put into after impregnating 25min in precursor sol, places into resistance furnace, be heated to 1650 DEG C, protect by blank strip Temperature sintering 5h, obtains alumina ceramic substrate.
Comparative example
High intensity produced by the present invention is aoxidized as a comparison case with the high-strength alumina ceramic substrate of Hebei company production High-strength alumina ceramic substrate in aluminium ceramic substrate and comparative example carries out performance detection, and testing result is as shown in table 1:
1st, test method:
The hardness of hardness test pencil represents;
Tensile strength test is detected by the standard of GB/T 23805-2009;
Impact strength test is detected using drop hammer type method.
Table 1
Test event Example 1 Example 2 Example 3 Comparative example
Pencil hardness(H) 4 5 5 1
Elongation percentage(%) 68.8 70.2 71.9 45.3
Viscosity number(Pa.s) 69 73 75 42
Impact strength (Nm) 49.8 50.7 51.6 20.4
The intensity of high-strength alumina ceramic substrate produced by the present invention is high according to above-mentioned middle data, and maximum elongation percentage reaches 71.9%, viscosity number is high, makes to be not susceptible to craze and transfiguration during alumina ceramic substrate sinter molding, mechanical strength is high, has Wide application prospect.

Claims (7)

1. a kind of preparation method of high-strength alumina ceramic substrate, it is characterised in that specifically preparation process is:
(1)70~80g kyanite ores in sand form are placed in ball grinder, add in agate ball milling pearl, ball milling obtains aquamaine mountain flour, by aquamaine Mountain flour, which mixes to be put into ball grinder with aluminum fluoride trihydrate, continues ball milling, obtains mixed mineral powder, mixed mineral powder is put into corundum crucible In, heat temperature raising, heat preservation calcining obtains mullite;
(2)Mullite is put into mortar and is ground, sieving obtains Mullite Powder, 60~70g Mullite Powders are put into 200~ In 300mL Ludox, the shearing of high-speed shearing machine high speed is transferred to after being dispersed with stirring, 40~50mL is added in into high-speed shearing machine Aluminum nitrate solution adds pH in ammonium hydroxide regulation system, continues high speed shear, still aging, obtains precursor sol;
(3)Precursor sol is placed in supercentrifuge, high speed centrifugation processing removes supernatant liquor, obtains lower sediment, will Precipitation is washed 3~4 times, then the precipitation after washing is mixed dispersion with n-butanol successively with distilled water, absolute ethyl alcohol, is put into ventilation It is dry in drying box, obtain precursor powder;
(4)700~800mL sodium aluminate solutions are fitted into beaker, carbon dioxide gas is led into beaker, after ventilation, to 150~180g precursor powders and 8~10g ammonium polyacrylates are added in beaker, beaker is placed in water-bath, heat temperature raising, It is stirred, obtains mixed slurry;
(5)Mixed slurry is poured into tape casting machine and is cast, after slurry curtain coating to be mixed, standing and drying obtains curtain coating life Material strip;
(6)Curtain coating raw material band is placed in resistance furnace, is heated up, is kept the temperature, cooling obtains blank strip, and blank strip taking-up is put into presoma It impregnates, is placed into resistance furnace in colloidal sol, heat temperature raising, heat preservation sintering obtains alumina ceramic substrate.
2. a kind of preparation method of high-strength alumina ceramic substrate according to claim 1, it is characterised in that:
Step(1)The grain size of the agate ball milling pearl is 6~8mm, and Ball-milling Time is 30~45min, aquamaine mountain flour and three water For the mass ratio of aluminum fluoride mixing for 3 ︰ 1, continuations Ball-milling Time is 1~2h, be 1550 to temperature after corundum crucible heat temperature raising~ 1600 DEG C, heat preservation calcination time is 4~5h.
3. a kind of preparation method of high-strength alumina ceramic substrate according to claim 1, it is characterised in that:
Step(2)The milling time is 3~4h, and specification of being sieved is 200 mesh, and the mass fraction of Ludox is 25%, stirring Jitter time is 10~15min, and high-speed shearing machine rotating speed is 4000~5000r/min, and the mass fraction of aluminum nitrate solution is 10%, the mass fraction of ammonium hydroxide is 50%, and pH is 9~10 in regulation system, and the continuation high speed shear time is 15~20min, is stood Digestion time for 20~for 24 hours.
4. a kind of preparation method of high-strength alumina ceramic substrate according to claim 1, it is characterised in that:
Step(3)The supercentrifuge centrifugal rotational speed is 7000~8000r/min, high speed centrifugation processing time for 10~ 15min, the mass ratio that the precipitation after washing is mixed with n-butanol are 1 ︰ 5, and aeration cabinet set temperature is 100~110 DEG C, is done The dry time is 2~3h.
5. a kind of preparation method of high-strength alumina ceramic substrate according to claim 1, it is characterised in that:
Step(4)The mass fraction of the sodium aluminate solution is 20%, and drop rate is 20~30mL/min, and duration of ventilation is 40~45min, temperature is 70~80 DEG C after heat temperature raising, is stirred the time as 30~35min.
6. a kind of preparation method of high-strength alumina ceramic substrate according to claim 1, it is characterised in that:
Step(5)The control scraper height is 0.5~2.0mm, and curtain coating base band rate travel is 0.5cm/s~1.5cm/s, 2~3h of standing and drying.
7. a kind of preparation method of high-strength alumina ceramic substrate according to claim 1, it is characterised in that:
Step(6)The heating rate is 5~7 DEG C/min, and temperature is 1100~1200 DEG C after heating, soaking time for 40~ 50min, temperature is 70~75 DEG C after cooling, and it is 20~25min that blank strip, which is put into precursor sol dip time, after heat temperature raising Temperature is 1550~1650 DEG C, and the heat preservation sintering time is 4~5h.
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CN109081949A (en) * 2018-07-19 2018-12-25 佛山市高明区爪和新材料科技有限公司 A kind of preparation method of resin clad metal composite heat-conducting filler
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CN112079630A (en) * 2020-09-28 2020-12-15 成都万士达瓷业有限公司 Sintering process of Al2O3 ceramic substrate
CN113004027A (en) * 2021-03-26 2021-06-22 福建安溪马斯特陶瓷有限公司 Wear-resistant high-performance ceramic roller and preparation method thereof
CN113004027B (en) * 2021-03-26 2022-05-17 福建安溪马斯特陶瓷有限公司 Wear-resistant high-performance ceramic roller and preparation method thereof
CN114656249A (en) * 2022-03-10 2022-06-24 蒙娜丽莎集团股份有限公司 High-strength tawnite-based thin ceramic plate and preparation method thereof
CN114656249B (en) * 2022-03-10 2023-02-21 蒙娜丽莎集团股份有限公司 High-strength tawnite-based thin ceramic plate and preparation method thereof
CN116768609A (en) * 2022-07-29 2023-09-19 苏州瑞瓷新材料科技有限公司 Application of tape casting formed firing-supporting raw porcelain in preparation of electronic ceramics
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CN116426149B (en) * 2023-04-28 2024-02-20 湖北工业大学 Quick-drying pearlescent paint and preparation method thereof

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Application publication date: 20180608