CN107336485B - The preparation method of composite ceramics aluminum substrate - Google Patents
The preparation method of composite ceramics aluminum substrate Download PDFInfo
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- CN107336485B CN107336485B CN201710543707.0A CN201710543707A CN107336485B CN 107336485 B CN107336485 B CN 107336485B CN 201710543707 A CN201710543707 A CN 201710543707A CN 107336485 B CN107336485 B CN 107336485B
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Abstract
The present invention provides a kind of preparation method of composite ceramics aluminum substrate comprising following steps: S1, preparing ceramic slurries: organic resin, ceramic powder and additive being carried out grinding and mixing, obtain ceramic slurries；S2, it prepares composite ceramic film: ceramic slurries being coated on PET plastic film by automatic coating machine and obtain composite ceramic film；S3, it prepares composite ceramics aluminum substrate: after composite ceramic film obtained in S2 is bonded with aluminum substrate, being put into hot press, hot pressing obtains composite ceramics aluminum substrate under certain temperature, pressure condition.The present invention first passes through automatic coating machine and prepares composite ceramic film, hot pressed sintering is carried out after ceramic membrane is bonded with aluminum substrate again and is obtained, the composite ceramics aluminium base panel products that binding force is strong, blibbing pin hole rate is low can be made in the preparation process, additionally due to the reason of hot pressing, ceramic dense is improved, other performances of product also get a promotion, and obtained composite ceramics aluminum substrate conducts electricity very well, and hot property is good.
Description
Technical field
The invention belongs to the preparation method fields of composite ceramics aluminum substrate, and in particular to a kind of composite ceramics aluminum substrate
Preparation method.
Background technique
The tape casting, curtain coating and roll coating process is usually used in the coating process of aluminium base plate surface.Wherein the tape casting is called
Scraper method is to put coating slurries to coating machine, and by control scraper gap will apply slurry and be applied to substrate and obtain between difference
The surface coating layer of gap is suitable for the higher aluminium base of flexibility, and such as 1 is aluminium foil, and hard aluminum substrate can not then be carried out
Rotate coiled material.Showering rule is that coating slurries are sprayed on aluminum substrate by spray gun, which will obtain the surface of even compact
Coating, the equipment requirement needed is higher, is coated with more suitable for the surface of three-dimensional structure part.Roll coating process be chiefly used in plate ink,
Painted surface treatment process has the characteristics that equipment is relatively easy, is chiefly used in ink, the paint of UV curing type, this method is to coating
The table solidity of liquid, levelability has higher requirement, thus limits the use scope of the method.
Summary of the invention
In order to overcome the drawbacks of the prior art, the present invention provides a kind of preparation method of composite ceramics aluminum substrate, first passes through
Automatic coating machine prepares composite ceramic film, then carries out hot pressed sintering after ceramic membrane is bonded with aluminum substrate and obtain, technique preparation
The composite ceramics aluminium base panel products that binding force is strong, blibbing pin hole rate is low can be made in method, additionally due to the reason of hot pressing,
Ceramic dense is improved, other correlated performances of product can also get a promotion.
The present invention is implemented as follows:
The present invention provides a kind of preparation method of composite ceramics aluminum substrate comprising following steps:
S1, ceramic slurries are prepared: organic resin, ceramic powder and additive is subjected to grinding and mixing, obtain a kind of ceramics
Slurries,
The constituent of the ceramics slurries is as follows:
40-70 parts of ceramic powder；10-30 parts of organic resin；1-2 parts of curing agent；0.1 part of levelling agent；0.1 part of defoaming agent；
3-10 parts of filler and 10-30 parts of diluent；
S2, it prepares composite ceramic film: the ceramic slurries in S1 is coated on PET plastic film simultaneously by automatic coating machine
Being dried ceramic slurries by drying unit is ceramic half dry plate, obtains composite ceramic film；
S3, it prepares composite ceramics aluminum substrate: composite ceramic film obtained in S2 is had to the one side and aluminum substrate of ceramic membrane
It after fitting, is put into hot press, hot pressing obtains composite ceramics aluminum substrate under certain temperature, pressure condition.
Preferably, the preparation method of ceramic slurries specifically comprises the following steps: in S1
Diluent is added in S11, the organic resin for weighing aforementioned proportion, under conditions of being quickly dispersed with stirring, by organic tree
Rouge dissolved dilution；
S12, the ceramic powder for weighing aforementioned proportion, levelling agent, defoaming agent and filler are slowly added under agitation
In oneself diluted organic resin solution, it is transferred in sand mill is sanded after mixing evenly, the slurries mistake being finally sanded
Sealed storage is spare after filter；
Curing agent is added before S13, coating in the slurries obtained in S12 and stirs 10- under the revolving speed of 100-300rpm
The ceramic slurries for step S2 are obtained by filtration through 100-200 mesh screen after 30 minutes.
Preferably, in step S2, the scraper gap of automatic coating machine is 50-120um, the temperature of the tunnel oven of drying unit
Spending gradient includes four sections:
The temperature of first segment is 60-70 DEG C；The temperature of second segment is 70-80 DEG C；The temperature of third section is 80-100 DEG C；The
Four sections of temperature is 100-140 DEG C；The transmission speed of drying unit conveying belt is 0.5-2 ms/min.
Preferably, composite ceramics aluminum substrate is prepared in S3 specifically includes the following steps:
S31, after composite ceramic film obtained in S2 be aligned with aluminum substrate being bonded, under the conditions of certain pressure, temperature into
The hot pressed sintering of row certain time, the certain pressure, temperature condition include three sections, and three sections of pressure, temperature condition are specific
It is as follows:
The temperature of first segment is 80-100 DEG C, pressure 0kg/cm2, the retention time is 5 minutes；
The temperature of second segment is 100-140 DEG C, pressure 5-20kg/cm2, the retention time is 10 minutes；
The temperature of third section is 160-200 DEG C, pressure 20-30kg/cm2, the retention time is 60 minutes；
After the completion of S32, hot pressed sintering, 100 DEG C are cooled to, and hot press pressure is shed, take out composite ceramics aluminum substrate.
Preferably, the ceramic powder is one or more of inorganic, metal oxide, nitride and carbide, described
The partial size of ceramic powder is 0.1-10um.
Preferably, the organic resin is in epoxy resin, organic siliconresin, polyurethane resin and propylene acid ester resin
It is one or more of.
Preferably, the curing agent is one of organic amine system curing agent, organic platinum group catalyst or acid anhydrides system.
Preferably, the levelling agent is heat-resistance type levelling agent.
Preferably, the defoaming agent is organic silicon-type heat-resistance type defoaming agent.
Preferably, the filler be mica powder, talcum powder, bortz powder, calcined kaolin, long phosphate stone powder, titanium dioxide or
One or more of White Carbon black, the partial size of the filler are 0.1-5um.
Preferably, the diluent is DBE liquid, ethyl acetate, butyl acetate, propylene glycol monomethyl ether, dipropylene glycol methyl ether, third
One or more of ketone or butanone.
Preferably, the inorganic, metal oxide ceramic powder is one in aluminium oxide, zirconium oxide, magnesia or titanium oxide
Kind is several, and the nitride ceramics powder is one or more of aluminium nitride, boron nitride or silicon nitride, the carbide pottery
Porcelain powder is one or more of silicon carbide, boron carbide, zirconium carbide.
Compared with prior art, the invention has the following advantages:
The present invention first passes through automatic coating machine and prepares composite ceramic film, then carries out hot pressing after ceramic membrane is bonded with aluminum substrate
Sintering and obtain, which can be made that binding force is strong, the low composite ceramics aluminium base panel products of blibbing pin hole rate.
Heat pressing process is used in the production process, and not only ceramic dense is improved, other correlated performances of product can also obtain
To promotion.The hot property of last obtained composite ceramics aluminum substrate, electrical property are good, composite ceramics aluminum substrate in double flat,
Do not occur ceramic layer removing, is a kind of composite ceramics alumina-base material of good performance.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Below with reference to the attached drawing exemplary embodiment that the present invention will be described in detail, feature and aspect.It is identical attached in attached drawing
Icon note indicates element functionally identical or similar.Although the various aspects of embodiment are shown in the attached drawings, unless special
It does not point out, it is not necessary to attached drawing drawn to scale.
The present invention provides a kind of preparation method of composite ceramics aluminum substrate, as shown in Figure 1, itself the following steps are included:
S1, ceramic slurries are prepared: organic resin, ceramic powder and additive is subjected to grinding and mixing, obtain a kind of ceramics
Slurries；
S2, it prepares composite ceramic film: the ceramic slurries in S1 is coated on PET plastic film simultaneously by automatic coating machine
Being dried ceramic slurries by drying unit is ceramic half dry plate, obtains composite ceramic film；
S3, it prepares composite ceramics aluminum substrate: after composite ceramic film obtained in S2 is bonded with aluminum substrate, being put into hot press
In, hot pressing obtains composite ceramics aluminum substrate under certain temperature, pressure condition.
Preferably, the preparation method of ceramic slurries specifically comprises the following steps: in S1
Diluent is added in S11, the organic resin for weighing aforementioned proportion, under conditions of being quickly dispersed with stirring, by organic tree
Rouge dissolved dilution；
S12, the ceramic powder for weighing aforementioned proportion, levelling agent, defoaming agent and filler are slowly added under agitation
In oneself diluted organic resin solution, it is transferred in sand mill is sanded after mixing evenly, the slurries mistake being finally sanded
Sealed storage is spare after filter；
Curing agent is added before S13, coating in the slurries obtained in S12 and stirs 10- under the revolving speed of 100-300rpm
The ceramic slurries for step S2 are obtained by filtration through 100-200 mesh screen after 30 minutes.
Preferably, composite ceramics aluminum substrate is prepared in S3 specifically includes the following steps:
S31, after composite ceramic film obtained in S2 be aligned with aluminum substrate being bonded, under the conditions of certain pressure, temperature into
The hot pressed sintering of row certain time, the certain pressure, temperature condition include three sections, and three sections of pressure, temperature condition are specific
It is as follows:
The temperature of first segment is 80-100 DEG C, pressure 0kg/cm2, the retention time is 5 minutes；
The temperature of second segment is 100-140 DEG C, pressure 5-20kg/cm2, the retention time is 10 minutes；
The temperature of third section is 160-200 DEG C, pressure 20-30kg/cm2, the retention time is 60 minutes；
After the completion of S32, hot pressed sintering, 100 DEG C are cooled to, and hot press pressure is shed, take out composite ceramics aluminum substrate.
Preferably, the coating machine scraper gap in S2 is 50-120um, and the temperature gradient of tunnel oven includes four sections:
The temperature of first segment is 60-70 DEG C, and tunnel is 3 meters long；The temperature of second segment is 70-80 DEG C, and tunnel is 3 meters long；Third
The temperature of section is 80-100 DEG C, a length of 3 meters of tunnel；4th section of temperature is 100-140 DEG C, a length of 3 meters of tunnel；The speed of conveying belt
Degree is 0.5-2 ms/min.The present invention is further explained combined with specific embodiments below:
Embodiment 1
A kind of constituent of ceramics slurries is as follows:
55 parts of Al2O3 ceramic powder；4 parts of BN ceramic powder (six sides)；E-3110 parts of bisphenol A epoxide resin；Trimellitic acid
1 part of acid anhydride；0.1 part of levelling agent；0.1 part of defoaming agent；5 parts of bortz powder and 25 parts of butanone；
Ceramic slurries preparation: weighing bisphenol A epoxide resin E-31 by mass ratio as shown above respectively, diluent be added,
Under conditions of being quickly dispersed with stirring, by bisphenol A epoxide resin E-31 dissolved dilution, the Al2O3 that granularity is 3um is then weighed again
The bortz powder that ceramic powder, BN ceramic powder (six sides), levelling agent, defoaming agent and the granularity that granularity is 1um are 3um, is being stirred
Under the conditions of mixing, it is slowly added in oneself diluted organic resin solution, is transferred in sand mill after mixing evenly, finally by milled
200rpm mixing speed is arranged in ceramic slurries, and curing agent is added and stirs 30 minutes.
Prepare ceramic membrane: adjustment automatic coating machine scraper gap is 80um, the temperature gradient of the tunnel oven of drying unit
Including four sections:
The temperature of first segment is 70 DEG C, a length of 3 meters of tunnel；The temperature of second segment is 80 DEG C, a length of 3 meters of tunnel；Third section
Temperature be 100 DEG C, a length of 3 meters of tunnel；4th section of temperature is 110 DEG C, a length of 3 meters of tunnel；Transferring tape speed is 1 m/min
Clock.
The compacting of composite ceramics aluminum substrate: the ceramic membrane one side of the composite ceramic film with PET film is aligned aluminum substrate, then
Compacting sintering is carried out under the conditions of certain pressure, temperature, temperature gradient is as follows:
The temperature of first segment is 100 DEG C, pressure 10kg/cm2, the retention time 5 minutes；
The temperature of second segment is 140 DEG C, pressure 20kg/cm2, the retention time 10 minutes；
The temperature of third section is 200 DEG C, pressure 30kg/cm2, the retention time 60 minutes.
After the completion of hot pressed sintering, 100 DEG C are cooled to, and hot press pressure is shed, take out composite ceramics aluminum substrate.
The ceramic film thickness for measuring composite ceramics aluminum substrate obtained is 40um, thermal coefficient 3W/ (mK), composite ceramics aluminium
Substrate proof voltage reaches 5kv, and composite ceramics aluminum substrate double flat does not occur ceramic layer removing.
Embodiment 2
A kind of constituent of ceramics slurries is as follows:
60 parts of zirconia ceramics powder；E-4210 parts of bisphenol A epoxide resin；1 part of trimellitic anhydride；0.1 part of levelling agent；Disappear
0.1 part of infusion；1 part of talcum powder；1 part of calcined kaolin powder；2 parts of mica powder and 25 parts of ethyl acetate；
Ceramic slurries preparation: organic resin is weighed respectively by mass ratio as shown above, diluent is added, is quickly stirring
Under conditions of dispersion, by resin dissolved dilution, the BN that zirconia ceramics powder, granularity that granularity is 1um are 1um is then weighed again
Ceramic powder (six sides) ceramic powder, levelling agent, defoaming agent and granularity are talcum powder, the calcined kaolin powder, mica of 0.1um
Powder is slowly added in oneself diluted organic resin solution, is transferred in sand mill after mixing evenly, finally under agitation
By the slurries of milled, 200rpm mixing speed is set, curing agent is added and stirs 30 minutes.
Prepare ceramic membrane: adjustment automatic coating machine scraper gap 120um, the temperature gradient of the tunnel oven of drying unit:
First segment is 65 DEG C of temperature, a length of 3 meters of tunnel；80 DEG C of the temperature of second segment, a length of 3 meters of tunnel；The temperature of third section
Degree: 100 DEG C, tunnel is long: 3 meters；4th section: temperature: 100 DEG C, tunnel is long: 3 meters；Transfer 1 m/min of tape speed.
The compacting of composite ceramics aluminum substrate: the ceramic membrane of the composite ceramic film with PET film is faced into neat aluminum substrate, is then existed
Compacting sintering is carried out under the conditions of certain pressure, temperature, temperature gradient is as follows:
The temperature of first segment is 100 DEG C, pressure 10kg/cm2, the retention time 5 minutes；
The temperature of second segment is 120 DEG C, pressure 20kg/cm2, the retention time 10 minutes；
The temperature of third section is 200 DEG C, pressure 30kg/cm2, the retention time 60 minutes.
After the completion of hot pressed sintering, 100 DEG C are cooled to, and hot press pressure is shed, taken out.
The ceramic film thickness for measuring composite ceramics aluminum substrate obtained is 80um, and composite ceramics aluminum substrate proof voltage reaches 6kv, table
For surface hardness up to 7, substrate double flat does not occur ceramic layer removing, is a kind of heatproof, the composite ceramics aluminium base of excellent in heat insulating performance
Material.
Embodiment 3
A kind of constituent of ceramics slurries is as follows:
44 parts of Al2O3 ceramic powder；10 parts of SiC ceramic powder；10 parts of epoxy modified silicone resin；Mellophanic acid acid anhydride 1
Part；0.1 part of levelling agent；0.1 part of defoaming agent；10 parts of diamond powder and 25 parts of propylene glycol monomethyl ether.
Ceramic slurries preparation: weighing epoxy modified silicone resin by mass ratio as shown above respectively, diluent be added,
Under conditions of being quickly dispersed with stirring, by resin dissolved dilution, Al2O3 ceramic powder, the SiC that granularity is 5um are then weighed again
Ceramic powder, levelling agent, defoaming agent and granularity are 0.1um's, under agitation, it is molten to be slowly added to oneself diluted organic resin
It in liquid, is transferred in sand mill after mixing evenly, finally by the slurries of milled, 300rpm mixing speed is set, curing agent is added
Stirring 30 minutes.
Prepare ceramic membrane: adjustment automatic coating machine scraper gap 100um, the temperature gradient of the tunnel oven of drying unit:
The temperature of first segment is 70 DEG C, a length of 3 meters of tunnel；The temperature of second segment is 80 DEG C, a length of 3 meters of tunnel；Third section
Temperature be 100 DEG C, a length of 3 meters of tunnel；4th section of temperature is 140 DEG C, a length of 3 meters of tunnel；Transfer tape speed be 0.5 meter/
Minute.
The compacting of composite ceramics aluminum substrate: the ceramic membrane of the composite ceramic film with PET film is faced into neat aluminum substrate, is then existed
Compacting sintering is carried out under the conditions of certain pressure, temperature, temperature gradient is as follows:
The temperature of first segment is 80 DEG C, pressure 10kg/cm2, the retention time 5 minutes；
The temperature of second segment is 140 DEG C, pressure 20kg/cm2, the retention time 10 minutes；
The temperature of third section is 180 DEG C, pressure 30kg/cm2, the retention time 60 minutes.
After the completion of hot pressed sintering, 100 DEG C are cooled to, and hot press pressure is shed, taken out.
The ceramic film thickness for measuring composite ceramics aluminum substrate is 70um, and composite ceramics aluminum substrate proof voltage reaches 8kv, thermal coefficient
Up to 6W/ (mK), double flat does not occur ceramic layer removing, is the composite ceramics aluminium base of a kind of heatproof, excellent thermal conductivity
Material.
Finally, it should be noted that above-described embodiments are merely to illustrate the technical scheme, rather than to it
Limitation；Although the present invention is described in detail referring to the foregoing embodiments, those skilled in the art should understand that:
It can still modify to technical solution documented by previous embodiment, or to part of or all technical features into
Row equivalent replacement；And these modifications or substitutions, it does not separate the essence of the corresponding technical solution various embodiments of the present invention technical side
The range of case.
Claims (7)
1. a kind of preparation method of composite ceramics aluminum substrate, it is characterised in that: itself the following steps are included:
S1, ceramic slurries are prepared: organic resin, ceramic powder and additive are subjected to grinding and mixing, obtain ceramic slurries,
The constituent example in mass ratio of the ceramics slurries is respectively as follows:
40-70 parts of ceramic powder；10-30 parts of organic resin；1-2 parts of curing agent；0.1 part of levelling agent；0.1 part of defoaming agent；Filler
3-10 parts and 10-30 parts of diluent；
Specifically comprise the following steps:
Diluent is added in S11, the organic resin for weighing aforementioned proportion, under conditions of being quickly dispersed with stirring, organic resin is molten
Solution dilution, obtains diluted organic resin solution；
S12, the ceramic powder for weighing aforementioned proportion, levelling agent, defoaming agent and filler are slowly added to dilute under agitation
In the organic resin solution released, it is transferred in sand mill is sanded after mixing evenly, it finally will be after the slurries that be sanded filtering
Sealed storage is spare；
Curing agent is added in the slurries obtained in S12 before S13, coating and stirs 10-30 points under the revolving speed of 100-300 rpm
The ceramic slurries for step S2 are obtained by filtration in Zhong Houjing 100-200 mesh screen；
S2, it prepares composite ceramic film: the ceramic slurries in S1 is coated on PET plastic film and is passed through by automatic coating machine
The drying of ceramic slurries is ceramic half dry plate by drying unit, and the scraper gap of automatic coating machine is 50-120 μm, drying unit
The temperature gradient of tunnel oven includes four sections: the temperature of first segment is 60-70 DEG C；The temperature of second segment is 70-80 DEG C；Third section
Temperature be 80-100 DEG C；4th section of temperature is 100-140 DEG C；The transmission speed of drying unit conveyer belt is 0.5-2 ms/min
Clock obtains composite ceramic film；
S3, composite ceramics aluminum substrate is prepared: after composite ceramic film obtained in S2 is bonded with the one side of ceramics with aluminum substrate,
It being put into hot press, hot pressing obtains composite ceramics aluminum substrate under certain temperature and pressure condition, specifically includes the following steps:
S31, after being aligned composite ceramic film obtained in S2 with aluminum substrate and being bonded, one is carried out under the conditions of certain pressure, temperature
The hot pressed sintering fixed time, the certain pressure, temperature condition include three sections, and three sections of pressure, temperature condition are specific as follows:
The temperature of first segment is 80-100 DEG C, and pressure is 0 kg/cm2, the retention time is 5 minutes；
The temperature of second segment is 100-140 DEG C, and pressure is 5-20 kg/cm2, the retention time is 10 minutes；
The temperature of third section is 160-200 DEG C, and pressure is 20-30 kg/cm2, the retention time is 60 minutes；
After the completion of S32, hot pressed sintering, 100 DEG C are cooled to, and hot press pressure is shed, take out composite ceramics aluminum substrate.
2. the preparation method of composite ceramics aluminum substrate according to claim 1, it is characterised in that: the ceramic powder is nothing
One or more of machine metal oxide, nitride and carbide, the partial size of the ceramic powder are 0.1-10 μm.
3. the preparation method of composite ceramics aluminum substrate according to claim 1, it is characterised in that: the organic resin is ring
One or more of oxygen resin, organic siliconresin, polyurethane resin and propylene acid ester resin.
4. the preparation method of composite ceramics aluminum substrate according to claim 1, it is characterised in that: the curing agent is organic
One of amine system curing agent, organic platinum group catalyst or acid anhydrides system；The levelling agent is heat-resistance type levelling agent；The defoaming agent
For organic silicon-type heat-resistance type defoaming agent.
5. the preparation method of composite ceramics aluminum substrate according to claim 1, it is characterised in that: the filler is mica
One or more of powder, talcum powder, bortz powder, calcined kaolin, long phosphate stone powder, titanium dioxide or White Carbon black, the filler
Partial size be 0.1-5 μm.
6. the preparation method of composite ceramics aluminum substrate according to claim 1, it is characterised in that: the diluent is DBE
One or more of liquid, ethyl acetate, butyl acetate, propylene glycol monomethyl ether, dipropylene glycol methyl ether, acetone or butanone.
7. the preparation method of composite ceramics aluminum substrate according to claim 2, it is characterised in that: the inorganic metal
Object ceramic powder is one or more of aluminium oxide, zirconium oxide, magnesia or titanium oxide, and the nitride ceramics powder is nitrogen
Change one or more of aluminium, boron nitride or silicon nitride, the carbide ceramics powder is silicon carbide, in boron carbide, zirconium carbide
One or more.
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