CN108484176A - A kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips - Google Patents
A kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips Download PDFInfo
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Abstract
A kind of high-temperature co-fired ceramics preparation method of aluminium nitride ceramic chips, includes the following steps:1)It is packed into mill ball;2)Configure slurry;3)Primary grinding;4)Configure casting slurry;5)Secondary grinding;6)Vacuum defoamation;7)Tape casting:Casting slurry after vacuum defoamation is moved into casting machine and carries out tape casting operation, makes the control of green tape thickness within the scope of 0.05 1mm;8)It cuts.Raw materials for production of the present invention are free of benzene, ketone, the toxic components such as aldehyde, production process does not generate organic poisonous and harmful substance and waste liquid, it reduces environmental pollution, ceramic chips made of the present invention, intensity is high, thermal conductivity is good, even density, it is unlikely to deform in the manufacturing process of high-temperature co-fired ceramics, it is high to punch printing precision, flatness is good, it is good with the contraction matching of Metal slurry, manufacturing process does not need overlay film operation, it is partially soft to solve aluminium nitride ceramic chips, processing difficulties, easily there is filling perforation printing offset, the problems such as lamination dislocation, improve production efficiency, reduce production cost.
Description
Technical field
The present invention relates to microelectronics technical field of ceramic material more particularly to a kind of high-temperature co-fired ceramics aluminium nitride greens
The preparation method of piece.
Background technology
Aluminium nitride ceramics has the characteristics that good thermal conductivity, high mechanical strength, electrical insulating property be good and nonhazardous, is being permitted at present
More high-tech area extensive applications are to develop a kind of faster ceramic material in recent years.Because it is small with dielectric constant, with
The chip material coefficient of expansion relatively matches, is easily achieved the features such as multilayer wiring, in microelectronics, photoelectron, power electronics and big work(
The fields such as rate Electronic Packaging have broad application prospects, and gradually start to replace traditional ceramic materials such as beryllium oxide, aluminium oxide.
Constantly expand with the application field of device packaged by ceramic shell, from platinotron, high current power electronic device to
The electronic devices such as the indispensable sensor in the fields such as new and effective electricity generation system solid fuel cell and environmentally friendly vehicle, high temperature
Common burning porcelain technology is grown rapidly because its structural strength is high, chemical stability is good, electric heating property is excellent in electronics industry.
In actual industrial production, aluminium nitride ceramic chips obtained usually occur when carrying out high-temperature co-fired ceramics making
The problems such as aluminium nitride ceramic chips are partially soft, processing difficulties, big deflection, production cost is high, seriously constrains aluminium nitride pottery
The development of ceramic material.
As Chinese patent CN105481368A discloses one kind for ceramic casting slurry, ceramic substrate and preparation method thereof
And application, the casting slurry include mixed solvent, dispersant, aluminum nitride ceramic powder, sintering aid, plasticizer and binder its
In, the mixed solvent is selected from two or more, the addition of the mixed solvent of absolute ethyl alcohol, ethyl acetate and propyl acetate
For the 30%-50% of aluminum nitride ceramic powder quality, the sintering aid is selected from yttrium oxide, calcium oxide, yttrium fluoride, lithia, carbon
The one or more of sour calcium or lithium carbonate, the plasticizer are selected from epoxyoleic acid butyl ester, octyl epoxy stearate, epoxidation
One kind or two of four ester of the own ester of triglyceride, triacetin, trioctyl trimellitate (TOTM), tri trimellitate or pyromellitic acid
Kind or more, the binder is selected from the one or more of sodium carboxymethylcellulose, polyvinyl alcohol or POLYPROPYLENE GLYCOL, described viscous
The quality of knot agent accounts for the 2-5%, preferably 3-5% of aluminum nitride ceramic powder.
In patent as above, there are following defects:Using one kind in sodium carboxymethylcellulose, polyvinyl alcohol or POLYPROPYLENE GLYCOL
Or several binders as production aluminium nitride ceramic chips, but since sodium carboxymethylcellulose is a kind of salt, insoluble in organic molten
Agent is not suitable for in high-temperature co-fired ceramics, at the same sodium carboxymethylcellulose, polyvinyl alcohol and POLYPROPYLENE GLYCOL all have compared with
Strong water imbibition, very unfavorable for preparation easily hydrolysis aluminium nitride, unstable products are easy to decompose, and the ceramic chips of preparation add
Work performance is bad.
Green for multi-layer wire substrate is prepared as Chinese patent CN104193340A discloses a kind of doctor-blade casting process
The method of piece, including multilayer ceramic chips, slurry production method and casting technique are by powder, sintering aid, dispersant, glue
It ties agent, plasticizer and stirring solvent to be uniformly mixed, forms slurry, then ceramic chips, ceramic chips thickness are made by the method for curtain coating
In 0.3mm hereinafter, made ceramic chips can meet multi-layer wire substrate making, the sintering aid is rare earth metal for control
One or both of oxide, alkaline earth oxide, the dispersant are oleic acid, olein, fish oil, acrylic acid
One or both of resin, the binder are polymerized thylene carbonate the third fat resin, and the plasticizer is repefral
With one or two in dibutyl phthalate, the solvent is the Diversity body in isopropanol, acetone, butanone, ethyl alcohol
System.
As Chinese patent CN103121238A discloses a kind of method that tape casting prepares aluminium nitride raw embryo, including with
Lower step:(1)Prepare organic gel:It is uniform that binder, plasticizer and organic solvent are proportionally added into container for stirring;(2)
Prepare casting slurry:Aluminium nitride powder sintering aid is added sequentially in ball grinder in proportion, sequentially adds organic solvent
And dispersant, ball milling is carried out, step is added(1)The organic gel of middle preparation, then carry out ball milling;(3)Deaeration is aging:By step(2)
In the casting slurry handled well carry out vacuum defoamation and carry out aging processing, control viscosity is in 8000-13000cps;(4)Curtain coating
Molding:With casting machine to step(3)In the casting slurry handled well carry out tape casting, control scraper height is 2.4-2.8mm,
It is 0.1-0.3m/ points to be cast belt speed, and one area of drying temperature of casting machine is 70-90 DEG C, and two area's temperature are 120-150 DEG C, are used
The above method can directly prepare the aluminium nitride raw embryo that thickness reaches 1.3-1.6mm.Binder described in CN103121238A is poly- third
One or both of e pioic acid methyl ester and polyvinyl butyral, the Ι classes plasticizer are dibutyl phthalate or adjacent benzene
One or both of dioctyl phthalate butyl benzyl or dioctyl phthalate, the organic solvent are toluene, dimethylbenzene or anhydrous
Ethyl alcohol, the sintering aid are one or both of erbium oxide, dysprosia or yttrium oxide.
In above-mentioned three patents, using the tape casting produce aluminium nitride ceramic chips when, raw materials for production also all use benzene, ketone,
The Organic Ingredients that aldehyde etc. is more toxic, the organic liquid waste generated in production process will cause environment larger harm and pollution,
And the poisonous and harmful element in Organic Ingredients easily remains in aluminium nitride ceramic chips in process of production, to the producer, user
Health have certain harmfulness.
Invention content
In view of this, it is necessary to propose a kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips.
A kind of high-temperature co-fired ceramics preparation method of aluminium nitride ceramic chips, includes the following steps:
1)It is packed into mill ball:Clean alumina ceramic grinding ball, the quality of mill ball and aluminum nitride powder are packed into nanometer sand mill
Than being 5:1;
2)Configure slurry:Weigh aluminum nitride powder, solvent, dispersant, sintering aid, anti-settling agent respectively in mass ratio, it first will be anti-settling
Agent is added in solvent, is stirred 0.5-1 hours with 1500rpm/min in high speed dispersor, so that anti-settling agent is evenly spread to molten
In agent, then solvent, aluminum nitride powder, dispersant, sintering aid containing anti-settling agent be added in nanometer sand mill together, mixing is equal
It is even and form slurry, prepare primary grinding;
3)Primary grinding:Nanometer sand mill is opened, is ground, testing size granularity in process of lapping, when D50 ranges are in 0.5-
When 1.5um, shut down;
4)Configure casting slurry:After primary grinding, binder, plasticizer are weighed in mass ratio, after being added to primary grinding
Slurry in, be uniformly mixed form casting slurry;
5)Secondary grinding:Casting slurry continues to grind in nanometer sand mill, and grinding is shut down after 2-4 hours;
6)Vacuum defoamation:Casting slurry after secondary grinding is transferred to be stirred under vacuum in deaeration machine and carries out vacuum defoamation, vacuum
Inclined heated plate is 0.5-1 hours, and viscosity stops deaeration when reaching 3000-6000PaS;
7)Tape casting:Casting slurry after vacuum defoamation is transferred to casting machine and carries out tape casting operation, the green for making curtain coating go out
Tape thickness controls within the scope of 0.05-1mm;
8)It cuts:The green band of tape casting is cut into the ceramic chips of required size.
Preferably, in the configuration slurry stage, the solvent is absolute ethyl alcohol, and the dispersant is containing the affine base of pigment
The high molecular weight block copolymer solution D ISPERBYK190 of group, the sintering aid are nano lanthanum oxide, yttrium oxide mixing point
Dispersion liquid, the anti-settling agent are the mixture of one or both of polyolefin-wax, polyethylene wax substance, the aluminum nitride powder grain size
For 0.5-1.5um, pattern is spherical.
Preferably, the anti-settling agent can also one or both of enough polyamide waxes, modified hydrogenated castor oil substance
Mixture replaces.
Preferably, the mass ratio that the aluminum nitride powder accounts for casting slurry is 50-60%, and the solvent accounts for the matter of casting slurry
Amount is than being 32-42.8%, and the mass ratio that the dispersant accounts for casting slurry is 1-2%, and the sintering aid accounts for the matter of casting slurry
For amount than being 0.2-5%, the mass ratio that the anti-settling agent accounts for casting slurry is 1-2%.
Preferably, the mass ratio that the aluminum nitride powder accounts for casting slurry is 50%, and the solvent accounts for the mass ratio of casting slurry
It is 41.7%, the mass ratio that the dispersant accounts for casting slurry is 1%, and the mass ratio that the sintering aid accounts for casting slurry is
0.3%, the mass ratio that the anti-settling agent accounts for casting slurry is 1%.
Preferably, it in a grinding steps, when the slurry granularity D50 is not more than 1um, shuts down.
Preferably, in the casting slurry step, the binder is polyacrylic resin, and the plasticizer is hexamethylene
The different monooctyl ester of alkane -1,2- dicarboxylic acids.
Preferably, the mass ratio that the binder accounts for casting slurry is 5-8%, and the plasticizer accounts for the quality of casting slurry
Than for 1-2%.
Preferably, the mass ratio that the binder accounts for casting slurry is 5%, and the plasticizer accounts for the mass ratio of casting slurry
It is 1%.
Preferably, in the tape casting step, curtain coating speed is 0.2-0.5m/min.
Ceramic chips made of the present invention have the advantages that intensity is high, thermal conductivity is good, stability good, in high-temperature co-fired ceramics
Manufacturing process in be unlikely to deform, punch that printing precision is high, flatness is good, good with the contraction matching of Metal slurry, making
Process does not need overlay film operation, solves partially soft aluminium nitride ceramic chips, processing difficulties, filling perforation printing offset, lamination mistake easily occurs
The problems such as position, improve production efficiency, reduce production cost.
Ceramic chips made of the present invention, after being fabricated to high-temperature co-fired ceramics device, post-shrinkage ratio is small for sintering, flatness
Good, processing performance is good, is free of organic poisonous and harmful element.
The present invention is replaced using polyacrylic resin " from the one of sodium carboxymethylcellulose, polyvinyl alcohol or POLYPROPYLENE GLYCOL
Kind or it is two or more " binder of composition, solve the problems, such as that its product ceramic chips is unstable, facile hydrolysis, ceramic chips obtained
Have good stability, processing performance it is good.
The present invention uses the tape casting property produced by using the Organic Ingredients without poisonous and harmful elements such as benzene, ketone, aldehyde
The good ceramic chips of energy solve the prior art using the Organic Ingredients production ceramic chips containing poisonous and harmful elements such as benzene, ketone, aldehyde
Problem, ensure production process do not generate organic poisonous and harmful substance and organic liquid waste, keep the production of ceramic chips environmentally protective,
Harm of the production process to environment and contact personnel is greatly decreased.
Specific implementation mode
With reference to embodiment, the present invention is further described, and following embodiment is intended to illustrate invention rather than to this hair
Bright further limits, and should not be limited the scope of the invention with this.
A kind of high-temperature co-fired ceramics preparation method of aluminium nitride ceramic chips proposed by the present invention, includes the following steps:
1)It is packed into mill ball:Clean alumina ceramic grinding ball, the quality of mill ball and aluminum nitride powder are packed into nanometer sand mill
Than 5:1;
Nanometer sand mill can open powder reuniting completely, and grind size is thinner, and the dispersion for making sintering aid evenly, is conducive to
The sintering of high-temperature co-fired ceramics.
2)Configure slurry:It weighs aluminum nitride powder, solvent, dispersant, sintering aid, anti-settling agent respectively in mass ratio, first will
Anti-settling agent is added in solvent, is stirred 0.5-1 hours with 1500rpm/min in high speed dispersor, is kept anti-settling agent evenly dispersed
It is added in nanometer sand mill, mixes together into solvent, then by solvent, aluminum nitride powder, dispersant, sintering aid containing anti-settling agent
Slurry is closed uniformly and formed, primary grinding is prepared;
3)Primary grinding:Nanometer sand mill is opened, is ground, testing size granularity in process of lapping, when D50 ranges are in 0.5-
When 1.5um, shut down;
4)Configure casting slurry:After primary grinding, binder, plasticizer are weighed in mass ratio, after being added to primary grinding
Slurry in, be uniformly mixed form casting slurry;
5)Secondary grinding:Casting slurry continues to grind in nanometer sand mill, and grinding is shut down after 2 hours, and casting slurry is made to mix
More uniformly;
6)Vacuum defoamation:Casting slurry after secondary grinding is transferred to be stirred under vacuum in deaeration machine and carries out vacuum defoamation, vacuum
Inclined heated plate 0.5-1 hours, viscosity stops deaeration when reaching 3000-6000PaS, real to extract the gas in casting slurry
Existing bubble-free effect;
7)Tape casting:Casting slurry after vacuum defoamation is transferred to casting machine and carries out tape casting operation, is made pottery according to high temperature co-firing
The requirement of porcelain ceramic chips used can control the green tape thickness being cast out within the scope of 0.05-1mm.
Since the rate of volatilization of absolute ethyl alcohol is very fast, it is easy cracking in casting processes, therefore by each section of casting machine
Air inlet is closed, and the volatilization of absolute ethyl alcohol, curtain coating speed 0.2-0.5m/min are reduced.
Green band produced by the present invention can meet different microwave devices, big work(by thickness control within the scope of 0.05-1mm
The different-thickness needs of rate microwave tube, high current power electronic device.
8)It cuts:The green band of tape casting is cut into the ceramic chips of required size.
Further, in the configuration slurry stage, the solvent is absolute ethyl alcohol, and the dispersant is containing the affine base of pigment
The high molecular weight block copolymer solution D ISPERBYK190 of group, the sintering aid are nano lanthanum oxide, yttrium oxide mixing point
Dispersion liquid, the anti-settling agent are the mixture of one or both of polyolefin-wax, polyethylene wax substance, the aluminum nitride powder grain size
For 0.5-1.5um, pattern is spherical.
Solvent is absolute ethyl alcohol, commonly uses organic solvent, nontoxic.
Dispersant is the high molecular weight block copolymer solution D ISPERBYK190 of the affinity groups containing pigment, is organic molten
Liquid is free of harmful components.
Sintering aid is nano lanthanum oxide, yttrium oxide mixed dispersion liquid, is distributed in the slurry and casting slurry of configuration equal
Even, condition is good after sintering for manufactured ceramic chips, solves current ceramic chips and easily occurs poor flatness after sintering, has white point
The problems such as.
Anti-settling agent is the mixture of one or both of polyolefin-wax, polyethylene wax substance, ensure that casting slurry
Uniformity consistency plays the role of preventing sedimentation in casting processes, makes entire casting processes slurry viscosity uniformity always,
It ensure that the uniformity of ceramic chips density, simultaneously because the addition of anti-settling agent, makes to be evenly distributed before and after the sintering aid in formula,
Make the flexural strength of product evenly, bigger, the ceramic chips of preparation will not be partially soft, it is easier to process, drilling precision is high, unbiased
It moves.
Solvent, dispersant, anti-settling agent are environment-friendly type organic chemicals, without poisonous and harmful elements such as benzene, ketone, aldehyde, are protected
Barrier production process does not generate organic poisonous and harmful substance and organic liquid waste, reduces environmental pollution.
Further, the anti-settling agent can also one or both of enough polyamide waxes, modified hydrogenated castor oil substance
Mixture replaces.
Further, the mass ratio that the aluminum nitride powder accounts for casting slurry is 50-60%, and the solvent accounts for the matter of casting slurry
Amount is than being 32-42.8%, and the mass ratio that the dispersant accounts for casting slurry is 1-2%, and the sintering aid accounts for the matter of casting slurry
For amount than being 0.2-5%, the mass ratio that the anti-settling agent accounts for casting slurry is 1-2%.
Further, the mass ratio that the aluminum nitride powder accounts for casting slurry is 50%, and the solvent accounts for the mass ratio of casting slurry
It is 41.7%, the mass ratio that the dispersant accounts for casting slurry is 1%, and the mass ratio that the sintering aid accounts for casting slurry is
0.3%, the mass ratio that the anti-settling agent accounts for casting slurry is 1%.
Further, it in a grinding steps, when the slurry granularity D50 is not more than 1um, shuts down.
Further, in the casting slurry step, the binder is polyacrylic resin, and the plasticizer is hexamethylene
The different monooctyl ester of alkane -1,2- dicarboxylic acids.
Binder is polyacrylic resin, and decomposition temperature is 300 DEG C in a nitrogen atmosphere, and decomposition temperature exists under air atmosphere
230 DEG C, have decomposition temperature low, the few feature of carbon residue is easy dumping, meets high-temperature co-fired ceramics cofiring condition, and poly- third
Olefin(e) acid resin-soluble can be used absolute ethyl alcohol as solvent, reduce environmental pollution in alcohols solvent.
Plasticizer is the different monooctyl ester of hexamethylene -1,2- dicarboxylic acids, is environment-friendlyplasticizer plasticizer, reduces human injury, reduces environment
Pollution.
Binder, plasticizer are environment-friendly type organic chemicals, and without poisonous and harmful elements such as benzene, ketone, aldehyde, guarantee produced
Journey does not generate organic poisonous and harmful substance and organic liquid waste, reduces environmental pollution.
Further, the mass ratio that the binder accounts for casting slurry is 5-8%, and the plasticizer accounts for the quality of casting slurry
Than for 1-2%.
Further, the mass ratio that the binder accounts for casting slurry is 5%, and the plasticizer accounts for the mass ratio of casting slurry
It is 1%.
Further, in the tape casting step, curtain coating speed is 0.2-0.5m/min.
As described above, the raw material proportioning of the casting slurry is:
Raw material proportioning 1:The mass ratio that aluminum nitride powder accounts for casting slurry is 50-60%, and the mass ratio that solvent accounts for casting slurry is 32-
42.8%, the mass ratio that dispersant accounts for casting slurry is 1-2%, and the mass ratio that sintering aid accounts for casting slurry is 0.2-5%, anti-settling
The mass ratio that agent accounts for casting slurry is 1-2%, and the mass ratio that binder accounts for casting slurry is 5-8%, and plasticizer accounts for casting slurry
Mass ratio is 1-2%.
For example, the raw material proportioning of the casting slurry can be as follows:
Raw material proportioning 2:Aluminum nitride powder mass ratio is 50%, and solvent quality ratio is 41.7%, and dispersant mass ratio is 1%, sintering aid
Mass ratio is 0.3%, and anti-settling agent mass ratio is 1%, and binder mass ratio is 5%, and plasticizer mass ratio is 1%.
Raw material proportioning 3:Aluminum nitride powder mass ratio is 55%, and solvent quality ratio is 32.8%, and dispersant mass ratio is 2%, sintering
Auxiliary agent mass ratio is 0.5%, and anti-settling agent mass ratio is 1.2%, and binder mass ratio is 7%, and plasticizer mass ratio is 1.5%.
Raw material proportioning 4:Aluminum nitride powder mass ratio is 57%, and solvent quality ratio is 33.5%, and dispersant mass ratio is 2%, sintering
Auxiliary agent mass ratio is 0.5%, and anti-settling agent mass ratio is 1%, and binder mass ratio is 5%, and plasticizer mass ratio is 1%.
Raw material proportioning 5:Aluminum nitride powder mass ratio is 50%, and solvent quality ratio is 42.8%, and dispersant mass ratio is 1%, sintering
Auxiliary agent mass ratio is 0.2%, and anti-settling agent mass ratio is 1%, and binder mass ratio is 4%, and plasticizer mass ratio is 1%.
Raw material proportioning 6:Aluminum nitride powder mass ratio is 50%, and solvent quality ratio is 33%, and dispersant mass ratio is 2%, and sintering helps
Agent mass ratio is 5%, and anti-settling agent mass ratio is 2%, and binder mass ratio is 7%, and plasticizer mass ratio is 1%.
Raw material proportioning 7:Aluminum nitride powder mass ratio is 51%, and solvent quality ratio is 38%, and dispersant mass ratio is 1.5%, sintering
Auxiliary agent mass ratio is 2.5%, and anti-settling agent mass ratio is 2%, and binder mass ratio is 6%, and plasticizer mass ratio is 1%.
Aluminum nitride powder, solvent, dispersant, sintering aid, anti-settling agent, binder, plasticizer in above-mentioned raw materials proportioning
Mass ratio can be integer, can also carry decimal, and specific raw material proportioning can be adjusted according to actual needs.
Specific embodiment 1:
1)It is packed into mill ball:Clean alumina ceramic grinding ball, the quality of mill ball and aluminum nitride powder are packed into nanometer sand mill
Than 5:1;
2)Configure slurry:Aluminum nitride powder 50% is weighed by raw material proportioning 2, solvent 41.7%, dispersant 1%, sintering aid 0.3%, is prevented
Heavy agent 1% is added in nanometer sand mill, is uniformly mixed and is formed slurry, and primary grinding is prepared;
3)Primary grinding:Nanometer sand mill is opened, is ground, testing size granularity in process of lapping, when D50 ranges are not more than
When 1um, shut down;
4)Configure casting slurry:After primary grinding, binder 5%, plasticizer 1% are weighed by raw material proportioning 2, is added to primary
In slurry after grinding, it is uniformly mixed and forms casting slurry;
5)Secondary grinding:Casting slurry continues to grind in nanometer sand mill, and grinding is shut down after 2 hours;
6)Vacuum defoamation:Casting slurry after secondary grinding is transferred to be stirred under vacuum in deaeration machine and carries out vacuum defoamation, vacuum
Inclined heated plate 0.5-1 hours, viscosity stops deaeration when reaching 3000-6000PaS;
7)Tape casting:Casting slurry after vacuum defoamation is transferred to casting machine and carries out tape casting operation, curtain coating speed is 0.2-
0.5m/min makes the green tape thickness that curtain coating goes out control within the scope of 0.05-1mm;
8)It cuts:The green band of tape casting is cut into the ceramic chips of required size.
Specific embodiment 2:
1)It is packed into mill ball:Clean alumina ceramic grinding ball, the quality of mill ball and aluminum nitride powder are packed into nanometer sand mill
Than 5:1;
2)Configure slurry:Aluminum nitride powder 55% is weighed by raw material proportioning 3, solvent 32.8%, dispersant 2%, sintering aid 0.5%, is prevented
Heavy agent 1.2% is added in nanometer sand mill, is uniformly mixed and is formed slurry, and primary grinding is prepared;
3)Primary grinding:Nanometer sand mill is opened, is ground, testing size granularity in process of lapping, when D50 ranges are not more than
When 1um, shut down;
4)Configure casting slurry:After primary grinding, binder 7%, plasticizer 1.5% are weighed by raw material proportioning 3, is added to one
In slurry after secondary grinding, it is uniformly mixed and forms casting slurry;
5)Secondary grinding:Casting slurry continues to grind in nanometer sand mill, and grinding is shut down after 2 hours;
6)Vacuum defoamation:Casting slurry after secondary grinding is transferred to be stirred under vacuum in deaeration machine and carries out vacuum defoamation, vacuum
Inclined heated plate 0.5-1 hours, viscosity stops deaeration when reaching 3000-6000PaS;
7)Tape casting:Casting slurry after vacuum defoamation is transferred to casting machine and carries out tape casting operation, curtain coating speed is 0.2-
0.5m/min makes the green tape thickness that curtain coating goes out control within the scope of 0.05-1mm;
8)It cuts:The green band of tape casting is cut into the ceramic chips of required size.
Specific embodiment 3:
1)It is packed into mill ball:Clean alumina ceramic grinding ball, the quality of mill ball and aluminum nitride powder are packed into nanometer sand mill
Than 5:1;
2)Configure slurry:Aluminum nitride powder 57% is weighed by raw material proportioning 4, solvent 33.5%, dispersant 2%, sintering aid 0.5%, is prevented
Heavy agent 1% is added in nanometer sand mill, is uniformly mixed and is formed slurry, and primary grinding is prepared;
3)Primary grinding:Nanometer sand mill is opened, is ground, testing size granularity in process of lapping, when D50 ranges are not more than
When 1um, shut down;
4)Configure casting slurry:After primary grinding, binder 5%, plasticizer 1% are weighed by raw material proportioning 4, is added to primary
In slurry after grinding, it is uniformly mixed and forms casting slurry;
5)Secondary grinding:Casting slurry continues to grind in nanometer sand mill, and grinding is shut down after 2 hours;
6)Vacuum defoamation:Casting slurry after secondary grinding is transferred to be stirred under vacuum in deaeration machine and carries out vacuum defoamation, vacuum
Inclined heated plate 0.5-1 hours, viscosity stops deaeration when reaching 3000-6000PaS;
7)Tape casting:Casting slurry after vacuum defoamation is transferred to casting machine and carries out tape casting operation, curtain coating speed is 0.2-
0.5m/min makes the green tape thickness that curtain coating goes out control within the scope of 0.05-1mm;
8)It cuts:The green band of tape casting is cut into the ceramic chips of required size.
Ceramic chips obtained by embodiment 1-3 are detected, and are compared with ceramic chips made from the prior art, number
According to as follows:
Embodiment 1 | Embodiment 2 | Embodiment 3 | Prior art | |
Drilling precision | Without offset | Without offset | Without offset | 5-9% is deviated |
Bending strength MPa | 402/387/392 | 419/409/422 | 413/407/420 | 342/309/378 |
Thermal conductivity | 180.2 | 179.5 | 180.4 | 174.5 |
Density | 2.22/2.23/2.18 | 2.25/2.23/2.19 | 2.17/2.22/2.19 | 2.02/2.37/1.98 |
Density is very poor | 0.05 | 0.06 | 0.05 | 0.39 |
As can be seen from the table, ceramic chips drilling precision produced by the present invention is high, and no offset, bending strength is big, and density is equal
Even and its very poor density much smaller than prior art solves the difficulties such as partially soft current ceramic chips, processing difficulties, deflection be big
Topic.
Above disclosed is only present pre-ferred embodiments, and the interest field of the present invention, ability cannot be limited with this
Domain those of ordinary skill is appreciated that all or part of flow of realization above-described embodiment, and made according to the claims of the present invention
Equivalent variations still belong to the scope covered by the invention.
Claims (10)
1. a kind of high-temperature co-fired ceramics preparation method of aluminium nitride ceramic chips, which is characterized in that include the following steps:
It is packed into mill ball:Clean alumina ceramic grinding ball, the mass ratio of mill ball and aluminum nitride powder are packed into nanometer sand mill
It is 5:1;
Configure slurry:Aluminum nitride powder, solvent, dispersant, sintering aid, anti-settling agent are weighed respectively in mass ratio, first by anti-settling agent
It is added in solvent, is stirred 0.5-1 hours with 1500rpm/min in high speed dispersor, anti-settling agent is made to evenly spread to solvent
In, then solvent, aluminum nitride powder, dispersant, sintering aid containing anti-settling agent be added in nanometer sand mill together, it is uniformly mixed
And slurry is formed, prepare primary grinding;
Primary grinding:Nanometer sand mill is opened, is ground, testing size granularity in process of lapping, when D50 ranges are in 0.5-
When 1.5um, shut down;
Configure casting slurry:After primary grinding, binder, plasticizer are weighed in mass ratio, after being added to primary grinding
In slurry, it is uniformly mixed and forms casting slurry;
Secondary grinding:Casting slurry continues to grind in nanometer sand mill, and grinding is shut down after 2-4 hours;
Vacuum defoamation:Casting slurry after secondary grinding is transferred to be stirred under vacuum in deaeration machine and carries out vacuum defoamation, vacuum is de-
It is 0.5-1 hours to steep the time, and viscosity stops deaeration when reaching 3000-6000PaS;
Tape casting:Casting slurry after vacuum defoamation is transferred to casting machine and carries out tape casting operation, the green band for making curtain coating go out
Thickness control is within the scope of 0.05-1mm;
It cuts:The green band of tape casting is cut into the ceramic chips of required size.
2. a kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips as described in claim 1, which is characterized in that institute
It states in configuration slurry stage, the solvent is absolute ethyl alcohol, and the dispersant is the high molecular weight block of the affinity groups containing pigment
Copolymer solution DISPERBYK190, the sintering aid are nano lanthanum oxide, yttrium oxide mixed dispersion liquid, and the anti-settling agent is
The mixture of one or both of polyolefin-wax, polyethylene wax substance, the aluminum nitride powder grain size are 0.5-1.5um.
3. a kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips as claimed in claim 2, which is characterized in that institute
State anti-settling agent can also the mixture of one or both of enough polyamide waxes, modified hydrogenated castor oil substance replace.
4. a kind of high-temperature co-fired ceramics preparation method of aluminium nitride ceramic chips as described in one of claim 1-3, feature
It is, the mass ratio that the aluminum nitride powder accounts for casting slurry is 50-60%, and the mass ratio that the solvent accounts for casting slurry is 32-
42.8%, the mass ratio that the dispersant accounts for casting slurry is 1-2%, and the mass ratio that the sintering aid accounts for casting slurry is 0.2-
5%, the mass ratio that the anti-settling agent accounts for casting slurry is 1-2%.
5. a kind of high-temperature co-fired ceramics preparation method of aluminium nitride ceramic chips as described in one of claim 1-3, feature
It is, the mass ratio that the aluminum nitride powder accounts for casting slurry is 50%, and the mass ratio that the solvent accounts for casting slurry is 41.7%, institute
It is 1% to state dispersant and account for the mass ratio of casting slurry, and the mass ratio that the sintering aid accounts for casting slurry is 0.3%, described anti-settling
The mass ratio that agent accounts for casting slurry is 1%.
6. a kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips as described in claim 1, which is characterized in that institute
It states in a grinding steps, when the slurry granularity D50 is not more than 1um, shuts down.
7. a kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips as described in claim 1, which is characterized in that institute
It states in casting slurry step, the binder is polyacrylic resin, and the plasticizer is that hexamethylene -1,2- dicarboxylic acids is different pungent
Ester.
8. a kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips as claimed in claim 7, which is characterized in that institute
It is 5-8% to state binder and account for the mass ratio of casting slurry, and the mass ratio that the plasticizer accounts for casting slurry is 1-2%.
9. a kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips as claimed in claim 8, which is characterized in that institute
It is 5% to state binder and account for the mass ratio of casting slurry, and the mass ratio that the plasticizer accounts for casting slurry is 1%.
10. a kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips as described in claim 1, which is characterized in that
In the tape casting step, curtain coating speed is 0.2-0.5m/min.
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CN114014669A (en) * | 2021-12-16 | 2022-02-08 | 河北中瓷电子科技股份有限公司 | Preparation method of stretch-resistant aluminum nitride raw ceramic substrate |
CN115124351A (en) * | 2022-07-18 | 2022-09-30 | 合肥圣达电子科技实业有限公司 | High-temperature solder resist slurry for aluminum nitride multilayer and preparation method thereof |
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CN109761617B (en) * | 2019-02-22 | 2021-11-05 | 福建臻璟新材料科技有限公司 | F-Ca-Lu doped aluminum nitride complex phase ceramic green body and preparation process thereof |
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CN114014669A (en) * | 2021-12-16 | 2022-02-08 | 河北中瓷电子科技股份有限公司 | Preparation method of stretch-resistant aluminum nitride raw ceramic substrate |
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