CN104649677A - A method of preparing an aluminium nitride ceramic substrate by gel casting - Google Patents
A method of preparing an aluminium nitride ceramic substrate by gel casting Download PDFInfo
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Abstract
A method of preparing an aluminium nitride ceramic substrate by gel casting is provided. The method adopts a gel tap casting technique, combines advantages of gel casting and advantages of tap casting, and adopts an alcohol as a solvent. The method includes: adding a small amount of an organic monomer, a crosslinking agent, a dispersant and a plasticizer, ball milling, mixing to obtain slurry with a high solid content, low viscosity and good fluidity, adding an initiator and a catalyst, performing tap casting, and triggering monomer polymerization at a certain temperature, so that AlN powder is uniformly distributed in a three-dimensional net structure formed by polymer. AlN green bodies and ceramic, which are uniform in structure and high in efficiency of space filling, can be prepared by the method.
Description
Technical field
The present invention relates to a kind of method that gel curtain coating prepares aluminium nitride ceramic substrate, belong to forming process of ceramics technical field.
Background technology
AlN(aluminium nitride) pottery have excellent insulativity, thermal conductivity, high thermal resistance, erosion resistance and with the advantage such as the thermal expansivity of silicon matches, become ideal heat radiation and the packaged material of large-scale integrated circuit of new generation, semiconductor module circuit and high power device.
At present, the main method of preparation AlN ceramic substrate is flow casting molding, and great majority are organic solvent flow casting molding.Flow casting molding technology is proposed first by Glenn N.Howatt and is successfully applied to the preparation of microwave-medium ceramics multi-layer capacitor.Flow casting molding technical equipment is simple, and be conducive to continuity operation, substantially realize automatization, production efficiency is higher, and its cost preparing diaphragm is lower, is comparatively applicable to suitability for industrialized production; Common casting machine carries out the thin slice that flow casting molding prepares thickness 10 μm ~ 1mm.Although through the development of decades, flow casting molding technology is applied to industrial production, but still there is a lot of problem.What organic solvent flow casting molding adopted is the organic solvent (benzene,toluene,xylene, butanone etc.) with certain toxicity, comparatively serious to the pollution of environment, and endanger healthy, still have a large amount of organism in shaping rear base substrate, the binder removal process in later stage easily causes blank cracking and distortion; In drying process, ceramic powder generation sedimentation, base substrate upper and lower surface forms density gradient, and upper surface easily cracks, low in glossiness.Inject & congeal shaping, is also gel casting forming, is the stupalith wet-forming technique invented by Oak Ridge National Key Laboratory of the U.S..The method that high polymer monomer is polymerized, by traditional ceramic process and organic polymer Chemical bond, is guided in ceramic molding by this technology neatly.The ultimate principle of this technique adds organic monomer in low in viscosity, that solid load is high slip, under the effect of catalyzer and initiator, the organic monomer crosslinking polymerization in slip is made to form tridimensional network, make slip in-situ solidifying shaping, and then carry out the demoulding, drying, organics removal, sintering, required ceramic part can be obtained.Gel-casting technology has that molding blank intensity is high, the overall good uniformity of base substrate, can do nearly size shaping, be suitable for preparing complicated shape ceramic component and industrialization promotion, without binder removal difficulty, low cost and other advantages, having broad application prospects.Current Inject & congeal shaping is mainly based on water base Inject & congeal shaping, and the report about organic Inject & congeal shaping is less.
The advantage of gel-tape-casting combine with technique Inject & congeal shaping and flow casting molding, with alcohols (ethanol, propyl alcohol, Virahol etc.) for solvent, then a small amount of organic monomer, linking agent, dispersion agent and softening agent is added, ball milling is mixed to get that solid content is high, viscosity is low and the slurry of good fluidity, add initiator and catalyzer again, carry out flow casting molding, trigger monomer polymerization under 40 ~ 80 DEG C of conditions, AlN powder is evenly distributed in the three-dimensional net structure of superpolymer formation.Therefore, this method can prepare even structure, the AlN base substrate that density is high and pottery.
Summary of the invention
The object of the invention is: propose a kind of gel-tape-casting method being suitable for aluminium nitride ceramic substrate suitability for industrialized production, solve traditional curtain coating forming technique Problems existing, reduce environmental pollution, traditional flow casting molding and Inject & congeal shaping are combined, define the method that a kind of film forming is fast, fast drying, organic content are low, all even performance of blank structure is good gel casting technology prepares aluminium nitride ceramic substrate, be conducive to the suitability for industrialized production realizing aluminium nitride ceramic substrate.
Technical scheme of the present invention:
Gel curtain coating prepares a method for aluminium nitride ceramic substrate, its preparation technology following (see Fig. 2):
(1) batching and ball milling, add organic solvent by organic monomer and linking agent and be configured to premixed liquid, then by premixed liquid, dispersion agent and AlN ceramic powder mixing and ball milling; Ratio of grinding media to material is 0.5:1 ~ 3:1, and the add-on of organic solvent is 20% ~ 100% of AlN ceramic powder weight, and Ball-milling Time is 2 ~ 50h; Described organic monomer is acrylamide, Methacrylamide, sorbyl alcohol polyglycidyl ether or extra large mattress epoxy resin etc., described linking agent is N, N '-methylene-bisacrylamide (MBAM), described organic solvent is alcohols (as ethanol, propyl alcohol or Virahol etc.), and described dispersion agent is ammonium polymethacrylate, PEI, phosphoric acid ester or ammonium polyacrylate etc.;
(2) add softening agent, in the slurry obtained, add softening agent, to increase the snappiness of AlN thin slice, then carry out secondary ball milling; Ball-milling Time is 4h ~ 30h;
(3) froth in vacuum, the slurry obtained by secondary ball milling carries out froth in vacuum, adds initiator simultaneously and is stirred, and stirring velocity is 30 ~ 100 turns/min, and the vacuum defoamation time is 5 ~ 30min;
(4) gel curtain coating, slurry froth in vacuum obtained carries out tape casting operation;
(5) thin slice is dry, and thin slice has some strength and toughness after solidification certain hour, then carries out drying treatment; Body drying to a certain extent after, base substrate thin slice is peeled off from cast film, then carries out cutting and punching, obtain AlN ceramic blank.
Wherein, in step (1), thickness is less than or equal to the aluminium nitride green compact substrate of 1.5mm, total add-on of organic monomer and linking agent is 1% ~ 5% of AlN powder weight, the mass ratio of organic monomer and linking agent is 10:1 ~ 30:1, and the add-on of dispersion agent is 0.1% ~ 1% of AlN ceramic powder weight; Thickness is greater than to the aluminium nitride green compact substrate of 1.5mm, total add-on of organic monomer and linking agent is 3% ~ 10% of AlN powder weight, the mass ratio of organic monomer and linking agent is 5:1 ~ 20:1, and the add-on of dispersion agent is 0.5% ~ 2% of AlN ceramic powder weight.
In step (2), described softening agent is glycerine, polyoxyethylene glycol, phthalic ester, polyether glycol, oleic acid or their mixture; Thickness is less than or equal to the aluminium nitride green compact substrate of 1.5mm, the add-on of softening agent is 0.2% ~ 5% of AlN ceramic powder weight; Thickness is greater than to the aluminium nitride green compact substrate of 1.5mm, suitably need increases softening agent, to ensure the snappiness of aluminium nitride base substrate, the add-on of softening agent is 1% ~ 10% of AlN ceramic powder weight.
In step (3), described initiator is azo diisobutyl amidine dihydrochloride, tetraethylenepentamine or 3, and 3 '-diamino dipropyl amine etc., the add-on of initiator is 0.25% ~ 10% of organic monomer quality.
In step (4), thickness is less than or equal to the aluminium nitride green compact substrate of 1.5mm, casting belt speed is 2m/min ~ 5m/min, and casting belt heating interval temperature is 40 ~ 50 DEG C, and set time is 10min ~ 40min; Thickness is greater than to the aluminium nitride green compact substrate of 1.5mm, casting belt speed is 0.2m/min ~ 4m/min, and casting belt heating interval temperature is 45 ~ 60 DEG C, and set time is 30min ~ 1h.
In step (5), thickness is less than or equal to the aluminium nitride green compact substrate of 1.5mm, drying temperature is 30 ~ 45 DEG C, and the time is 30min ~ 2h; Thickness is greater than to the aluminium nitride green compact substrate of 1.5mm, drying temperature is 40 ~ 60 DEG C, and the time is 2h ~ 4h.
Compared with prior art, the present invention is not only the simple combination of curtain coating and gel casting process, material mainly used and proportioning difference thereof, concrete innovation is: first, this method can prepare the aluminium nitride ceramic substrate that thickness is 0.3 ~ 3mm, the different aluminium nitride ceramic substrate of thickness is prepared with dry-pressing formed (>1mm) without the need to using flow casting molding (<1mm) respectively, use a set of equipment, only need appropriate change formula, the aluminium nitride ceramic substrate of different thickness can be obtained, reduce costs; The second, because AlN powder is very easily hydrolyzed, Water-based Gel-casting Technology is difficult to apply in AlN ceramic field, and present method can be promoted rapidly in AlN ceramic field; 3rd, present method adopts alcohols (ethanol, propyl alcohol, Virahol etc.) to be solvent, success replaces traditional curtain coating and forms malicious solvent (benzene,toluene,xylene, butanone etc.), reduce environmental pollution, reduce production cost, and benzene class organic solvent is easy and organic monomer reacts, monomer is caused to form tridimensional network, affect slurry curing and green compact performance, therefore gel curtain coating can not adopt benzene class to do organic solvent, this and flow casting molding have essential distinction; 4th, stream of gel Yanzhong adds organic monomer and linking agent, and addition is less, without the need to adding the binding agent of flow casting molding, effectively reducing slurry viscosity, improving solid content, be conducive to obtaining finer and close AlN green compact and pottery, this is the maximum difference of gel curtain coating and flow casting molding; 5th, under initiator and thermogenic action, there is polymerization and be cross-linked, forming tridimensional network in organic monomer and linking agent, the distribution of AlN powder in the network architecture, avoids the settlement issues of AlN powder in flow casting molding, greatly improves the homogeneity of AlN base substrate; 6th, AlN blank strength prepared by Inject & congeal shaping is high, but snappiness is poor, and due to oxygen inhibition need increase inert gas protection device.Gel curtain coating is not the simple combination of gel injection and flow casting molding, adding of softening agent, the snappiness of AlN green chip can not only be increased, facilitate the later stage to punch and lamination operation, the more important thing is the oxygen inhibition that can reduce in polymerization process, this is the essential distinction with traditional Inject & congeal shaping.In traditional flow casting molding technology, softening agent is only the effect playing the former.Therefore, this method without the need to increasing inert gas protection device, reduces production cost in monomer polymerization process; 7th, because slurry solid content is high, organic solvent proportion is little, and solidification process heats up, and greatly accelerates the volatilization of solvent, shortens time of drying; 8th, adding of softening agent, make solvent under high evaporation rate, effectively can suppress the generation of billet surface crackle, enhance productivity.The method technique is simple, and product stability is higher, advances the suitability for industrialized production of AlN ceramic substrate.
Accompanying drawing explanation
The SEM picture of Fig. 1 gel curtain coating AlN thin slice
The process flow sheet of Fig. 2 making method of the present invention
Embodiment
The present invention utilizes gel casting technology, the advantage of comprehensive flow casting molding and gel casting forming, can improve homogeneity and the density of aluminium nitride green chip, realizes the preparation of high-performance aluminium nitride ceramics substrate (thickness 0.3 ~ 3mm).
Embodiment 1:
1) add in 55mL dehydrated alcohol: 1.5g acrylamide, 0.15g N, N '-methylene-bisacrylamide, is made into premixed liquid;
2) 1.5g dispersion agent PEI and 150g aluminum nitride ceramic powder is then added, ball milling 10h;
3) add softening agent glycerine 3g, again ball milling 10h, obtain AlN gel casting slurry;
4) add initiator azo diisobutyl amidine dihydrochloride 0.05g in the slurry, vacuum defoamation 20min under the stirring velocity of 40 turns/min, 40 DEG C of gel curtain coatings on casting machine, casting belt speed is 5m/min, then solidifies 40min;
5) under temperature is 30 DEG C of conditions, dry 1h, obtains the AlN green chip that thickness is 0.4mm ~ 0.8mm.The SEM figure of gained AlN green compact as shown in Figure 1.
Embodiment 2:
As described in Example 1, difference is:
(1) acrylamide is 14g, N, N '-methylene-bisacrylamide is 1g;
(2) phosphoric acid ester is dispersion agent, and its add-on is 3g;
(3) softening agent glycerine 15g;
(4) add initiator azo diisobutyl amidine dihydrochloride 0.45g in the slurry, vacuum defoamation 30min under the stirring velocity of 80 turns/min, 60 DEG C of gel curtain coatings on casting machine, casting belt speed is 1m/min, then solidifies 40min;
(5) under temperature is 50 DEG C of conditions, dry 4h, obtains the AlN green chip that thickness is 2mm ~ 3mm.
Embodiment 3:
As described in Example 1, difference is:
(1) extra large mattress epoxy resin is monomer, and its add-on is 3g;
(2) phosphoric acid ester is dispersion agent, and its add-on is 1g;
(3) softening agent glycerine 5g;
(4) initiator 3 is added in the slurry, 3 '-diamino dipropyl amine 0.1g, vacuum defoamation 15min under the stirring velocity of 60 turns/min;
(5) under temperature is 40 DEG C of conditions, dry 2h.
Embodiment 4:
As described in Example 1, difference is:
(1) sorbyl alcohol polyglycidyl ether is monomer, and its add-on is 10g;
(2) phosphoric acid ester is dispersion agent, and its add-on is 2g;
(3) softening agent glycerine 10g;
(4) add initiator tetraethylenepentamine 0.5g in the slurry, vacuum defoamation 20min under the stirring velocity of 100 turns/min, 45 DEG C of gel curtain coatings on casting machine, casting belt speed is 2m/min, then solidifies 30min;
(5) under temperature is 40 DEG C of conditions, dry 6h, obtains the AlN green chip that thickness is 2mm ~ 3mm.
Claims (7)
1. gel curtain coating prepares a method for aluminium nitride ceramic substrate, it is characterized in that, the preparation technology of the method is as follows:
(1) organic monomer and linking agent are added organic solvent and be configured to premixed liquid, then by premixed liquid, dispersion agent and AlN ceramic powder mixing and ball milling; Ratio of grinding media to material is 0.5:1 ~ 3:1, and the add-on of organic solvent is 20% ~ 100% of AlN ceramic powder weight, and Ball-milling Time is 2 ~ 50h; Described organic monomer is acrylamide, Methacrylamide, sorbyl alcohol polyglycidyl ether or extra large mattress epoxy resin, described linking agent is N, N '-methylene-bisacrylamide, described organic solvent is alcohols, and described dispersion agent is ammonium polymethacrylate, PEI, phosphoric acid ester or ammonium polyacrylate;
(2) in the slurry obtained, add softening agent, to increase the snappiness of AlN thin slice, then carry out secondary ball milling; Ball-milling Time is 4h ~ 30h;
(3) slurry obtained by secondary ball milling carries out froth in vacuum, adds initiator simultaneously and is stirred, and stirring velocity is 30 ~ 100 turns/min, and the vacuum defoamation time is 5 ~ 30min;
(4) slurry froth in vacuum obtained carries out tape casting operation;
(5) thin slice has some strength and toughness after solidification certain hour, then carries out drying treatment; Body drying to a certain extent after, base substrate thin slice is peeled off from cast film, then carries out cutting and punching, obtain AlN ceramic blank.
2. gel curtain coating as claimed in claim 1 prepares the method for aluminium nitride ceramic substrate, it is characterized in that, in step (1), thickness is less than or equal to the aluminium nitride green compact substrate of 1.5mm, total add-on of organic monomer and linking agent is 1% ~ 5% of AlN powder weight, the mass ratio of organic monomer and linking agent is 10:1 ~ 30:1, and the add-on of dispersion agent is 0.1% ~ 1% of AlN ceramic powder weight; Thickness is greater than to the aluminium nitride green compact substrate of 1.5mm, total add-on of organic monomer and linking agent is 3% ~ 10% of AlN powder weight, the mass ratio of organic monomer and linking agent is 5:1 ~ 20:1, and the add-on of dispersion agent is 0.5% ~ 2% of AlN ceramic powder weight.
3. gel curtain coating as claimed in claim 1 prepares the method for aluminium nitride ceramic substrate, and it is characterized in that, in step (2), described softening agent is glycerine, polyoxyethylene glycol, phthalic ester, polyether glycol, oleic acid or their mixture; Thickness is less than or equal to the aluminium nitride green compact substrate of 1.5mm, the add-on of softening agent is 0.2% ~ 5% of AlN ceramic powder weight; Thickness is greater than to the aluminium nitride green compact substrate of 1.5mm, suitably need increases softening agent, to ensure the snappiness of aluminium nitride base substrate, the add-on of softening agent is 1% ~ 10% of AlN ceramic powder weight.
4. gel curtain coating as claimed in claim 1 prepares the method for aluminium nitride ceramic substrate, it is characterized in that, in step (3), described initiator is azo diisobutyl amidine dihydrochloride, tetraethylenepentamine or 3,3 '-diamino dipropyl amine, the add-on of initiator is 0.25% ~ 10% of organic monomer quality.
5. gel curtain coating as claimed in claim 1 prepares the method for aluminium nitride ceramic substrate, it is characterized in that, in step (4), thickness is less than or equal to the aluminium nitride green compact substrate of 1.5mm, casting belt speed is 2m/min ~ 5m/min, casting belt heating interval temperature is 40 ~ 50 DEG C, and set time is 10min ~ 40min; Thickness is greater than to the aluminium nitride green compact substrate of 1.5mm, casting belt speed is 0.2m/min ~ 4m/min, and casting belt heating interval temperature is 45 ~ 60 DEG C, and set time is 30min ~ 1h.
6. gel curtain coating as claimed in claim 1 prepares the method for aluminium nitride ceramic substrate, and it is characterized in that, in step (5), thickness is less than or equal to the aluminium nitride green compact substrate of 1.5mm, drying temperature is 30 ~ 45 DEG C, and the time is 30min ~ 2h; Thickness is greater than to the aluminium nitride green compact substrate of 1.5mm, drying temperature is 40 ~ 60 DEG C, and the time is 2h ~ 4h.
7. gel curtain coating as claimed in claim 1 prepares the method for aluminium nitride ceramic substrate, and it is characterized in that, in step (1), described organic solvent is ethanol, propyl alcohol or Virahol.
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| CN107263671A (en) * | 2017-06-27 | 2017-10-20 | 江苏华友装饰工程有限公司 | Preparation method of double-whisker composite modified shrinkage-resistant aluminum nitride substrate |
| CN108640689A (en) * | 2018-05-22 | 2018-10-12 | 南京萨特科技发展有限公司 | A kind of ceramic tube preparation method of high breaking fuse |
| WO2019210568A1 (en) * | 2018-05-03 | 2019-11-07 | 苏州聚复高分子材料有限公司 | Photocurable composition |
| CN112142474A (en) * | 2020-09-28 | 2020-12-29 | 西华大学 | Preparation method of water-based tape casting high-thermal-conductivity aluminum nitride ceramic substrate |
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| CN114538935A (en) * | 2022-03-17 | 2022-05-27 | 天津硕科科技有限公司 | Forming method of high-thermal-conductivity silicon nitride substrate |
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| CN114149264A (en) * | 2021-12-14 | 2022-03-08 | 福建臻璟新材料科技有限公司 | Preparation process of in-situ polymerization formed silicon nitride ceramic sheet |
| CN114804890A (en) * | 2022-02-21 | 2022-07-29 | 郑州大学 | Method for preparing silicon nitride ceramic substrate by gel tape casting |
| CN114538935A (en) * | 2022-03-17 | 2022-05-27 | 天津硕科科技有限公司 | Forming method of high-thermal-conductivity silicon nitride substrate |
| CN116553934A (en) * | 2023-06-07 | 2023-08-08 | 湖南湘瓷科艺有限公司 | Aluminum nitride ceramic and preparation method thereof |
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