CN106187201A - A kind of flow casting molding without benzene prepares the method for aluminium nitride ceramics - Google Patents
A kind of flow casting molding without benzene prepares the method for aluminium nitride ceramics Download PDFInfo
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- CN106187201A CN106187201A CN201510220583.3A CN201510220583A CN106187201A CN 106187201 A CN106187201 A CN 106187201A CN 201510220583 A CN201510220583 A CN 201510220583A CN 106187201 A CN106187201 A CN 106187201A
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Abstract
The invention discloses a kind of method that flow casting molding without benzene prepares aluminium nitride ceramics.The present invention uses multiple alcohols solvent to be configured to mixed solvent, and the mixing of mixed solvent, dispersant, AlN ceramic powder and sintering aid is carried out first ball milling；It is subsequently adding plasticizer and binding agent carries out secondary ball milling；AlN slurry after secondary ball milling is carried out vacuum stirring de-bubble, carries out tape casting operation subsequently and be dried, peel off, obtain even structure, AlN base substrate thin slice that consistency is high.The method uses alcohols mixed solvent to replace traditional benzene class toxic solvent, decreases environmental pollution, reduces production cost, and technique is simply efficient, and product stability is higher, advances the industrialized production of AlN ceramic substrate.
Description
Technical field
The present invention relates to the preparation method of aluminium nitride ceramics, a kind of method preparing aluminium nitride ceramic substrate particularly to curtain coating without benzene,
Belong to pottery field shaping technique.
Background technology
AlN ceramic has excellent insulating properties, heat conductivity, heat-resisting quantity, corrosion resistance and the thermal coefficient of expansion phase with silicon
The advantage such as join, become preferable heat radiation and the encapsulation material of a new generation's large scale integrated circuit, semiconductor module circuit and high power device
Material.
At present, the main method of preparation AlN ceramic substrate is flow casting molding, and great majority are organic solvent flow casting molding.Curtain coating
Forming technique 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, beneficially seriality operation, substantially carries out automatization, and production efficiency is higher, and it is prepared
The cost of diaphragm is relatively low, is relatively suitable for industrialized production, carries out flow casting molding and prepare thickness 10 μm～1mm on common casting machine
Thin slice.Although through the development of decades, flow casting molding technology has been applied to commercial production, but still suffers from a lot of problem.
At present, in industrialized production, organic solvent flow casting molding uses the organic solvent with certain toxicity, as benzene, toluene,
The solvent that the toxicity such as dimethylbenzene, acetone, butanone are bigger, the pollution to environment is more serious, and endangers healthy.Later,
The combination properties such as surface tension and the relative dielectric constant due to mixed solvent are better than one-component, and the viscosity of slurry is the most on the low side,
And effectively increasing the dissolubility of binding agent PVB, it is to avoid be cast the cracking of thin slice in dry run, many researcheres are all adopted
With alcohols solvent and benzene,toluene,xylene, acetone, butanone etc. as mixed solvent, but still suffer from environmental pollution and harm.
Summary of the invention
The purpose of the present invention is to propose to a kind of flow casting molding method being suitable to aluminium nitride ceramic substrate industrialized production, solve conventional flow
Prolonging the problem that forming technique exists, reduce environmental pollution, reduce production cost, a kind of film forming of formation is fast, fast drying, Organic substance
The method that the casting technology that content is low, the most even performance of blank structure is good prepares aluminium nitride ceramic substrate, is advantageously implemented aluminium nitride
The industrialized production of ceramic substrate.
For achieving the above object, present invention employs following technical scheme:
A kind of flow casting molding prepares the method for aluminium nitride ceramic substrate, comprises the steps:
(1) first ball milling: two or more alcohols solvent is configured in proportion mixed solvent, then by mixed solvent,
Dispersant, AlN ceramic powder and sintering aid mixing carry out first ball milling.
The addition of ball material mass ratio preferably 0.5:1～the 3:1 mixed solvent of first ball milling is AlN ceramic powder volume
20%～80%, Ball-milling Time is preferably 4～24h.Wherein said alcohols solvent includes dehydrated alcohol, propanol, isopropanol, butanol
Deng；Dispersant such as ammonium polymethacrylate, polymine (PEI), phosphate ester, ammonium polyacrylate etc. or their mixing
Thing；Material or their mixture such as sintering aid such as yittrium oxide, dysprosia, boron oxide, calcium oxide, lithium oxide.Institute
State mixed solvent and be preferably dehydrated alcohol and the combination of the combination of propanol, dehydrated alcohol and isopropanol or dehydrated alcohol and butanol
Combination, in above-mentioned mixed solvent, the preferred volume ratio of each component is followed successively by 1:0.25～0.5:1,1:0.2～0.25:1,1:0.5～1:1,
Most preferably dehydrated alcohol and isopropanol volume ratio are the mixed solvent of 1:1.
(2) secondary ball milling: add plasticizer and binding agent in the AlN slurry that first ball milling obtains, to increase AlN thin slice
Pliability and hot strength, then carry out secondary ball milling.
The secondary ball milling time is preferably 4h～30h.Generally, the addition of plasticizer is the 0.2%～5% of AlN ceramic powder weight,
The addition of binding agent is the 0.5%～5% of AlN ceramic powder weight.Plasticizer such as dioctyl phthalate (DOP),
Dibutyl phthalate (DBP), BBP(Butyl Benzyl Phthalate (BBP), Polyethylene Glycol, glycerol, polyether polyol and oil
Acid or their mixture；Binding agent such as polyvinyl butyral resin (PVB), polymethyl methacrylate (PMMA) and third
Olefin(e) acid ester or their mixture.
(3) froth in vacuum: the AlN slurry obtained by secondary ball milling carries out vacuum stirring de-bubble.
The mixing speed of vacuum defoamation is preferably 30～100 turns/min, and the vacuum defoamation time is preferably 5～30min.
(4) flow casting molding: AlN slurry froth in vacuum obtained carries out tape casting operation, obtains AlN base substrate.
Casting temperature is preferably 20～40 DEG C；For the thickness aluminium nitride green compact substrate less than 1mm, curtain coating speed is
2m/min～5m/min；For the thickness aluminium nitride green compact substrate more than 1mm, curtain coating speed is 0.2m/min～4m/min.
(5) thin slice is dried: by AlN body drying, and strip down from cast film.
For the thickness AlN green compact substrate less than 1mm, preferably baking temperature is 30～45 DEG C, and the time is 30min～2h；Right
In the thickness AlN green compact substrate more than 1mm, preferably baking temperature is 40～70 DEG C, and the time is 1.5h～4h.Body drying arrives
To a certain degree, base substrate thin slice can be peeled off from cast film, then cut and punch.
Compared with prior art, the invention has the beneficial effects as follows: first, this method use cheap alcohols (ethanol, propanol,
Isopropanol etc.) it is mixed solvent, successfully replace tradition curtain coating and form poison solvent (benzene,toluene,xylene, butanone etc.), no
Only reduce environmental pollution, be also greatly reduced production cost.Second, due to satisfying of the alcohols solvent such as dehydrated alcohol and isopropanol
Bigger than the saturated vapor pressure of benzene kind solvent with vapour pressure, therefore, in dry run, by reasonably adjusting in mixed solvent not
With the ratio of alcohols solvent, being rapidly and efficiently dried of AlN curtain coating green compact can be realized, shorten drying time；3rd, dehydrated alcohol
Less than the surface tension of benzene class or ketones solvent with the surface tension of the alcohols solvents such as isopropanol, to the wetting effect of AlN granule relatively
Good, be conducive to obtaining the AlN casting slurry of high solids content, high homogeneity.The method technique is simple, can prepare even structure,
AlN base substrate that consistency is high and pottery, product stability is higher, advances the industrialized production of AlN ceramic substrate.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the AlN ceramic thin slice of embodiment one preparation.
Fig. 2 is the SEM figure of the AlN ceramic thin slice of embodiment two preparation.
Fig. 3 is the SEM figure of the AlN ceramic thin slice of embodiment three preparation.
Detailed description of the invention
Further illustrate the present invention below by embodiment, but limit the scope of the present invention never in any form.
Embodiment one
Dehydrated alcohol 30mL, isopropanol 30mL, dispersant phosphate ester 1.3g, AlN powder 124g and yittrium oxide 6g are mixed,
First ball milling 6h is carried out by ball material mass ratio 2:1.It is subsequently adding plasticizer glycerol 6.5g and binding agent PVB6.5g, ball milling again
10h, obtains AlN casting slurry.AlN slurry is vacuum defoamation 20min under the mixing speed of 40 turns/min, in casting machine temperature
Degree is to be cast when 45 DEG C, and curtain coating speed is 1m/min.After being dried 2h, obtain the AlN green chip that thickness is 1.1mm.
The SEM of gained AlN ceramic schemes as shown in Figure 1, it can be seen that prepared AlN ceramic even structure, and consistency is high.
Embodiment two
Dehydrated alcohol 45mL, propanol 15mL, dispersant phosphate ester 1.5g, AlN powder 100g and yittrium oxide 3g are mixed,
First ball milling 12h is carried out by ball material mass ratio 3:1.It is subsequently adding plasticizer phthalic acid dibutyl ester 3g and binding agent PVB 2g,
Ball milling 20h again, obtains AlN casting slurry.AlN slurry is vacuum defoamation 15min under the mixing speed of 80 turns/min,
Casting machine temperature is to be cast when 35 DEG C, and curtain coating speed is 2m/min.After being dried 1.5h, obtaining thickness is 0.85mm's
AlN green chip.The SEM figure of gained AlN ceramic is as in figure 2 it is shown, prepared AlN ceramic even structure, consistency
High.
Embodiment three
By dehydrated alcohol 55mL, butanol 30mL, polyethylene of dispersing agent imines 2g, AlN powder 120g, calcium oxide 2.4, oxygen
Change lithium 3.6g mixing, carry out first ball milling 20h by ball material mass ratio 1:1.It is subsequently adding plasticizer phthalic acid butyl benzyl 2.5g
With binding agent PVB 1.8g, ball milling 18h again, obtain AlN casting slurry.AlN slurry is in the mixing speed of 60 turns/min
Lower vacuum defoamation 25min, is cast when casting machine temperature is 30 DEG C, and curtain coating speed is 4m/min.After being dried 3h,
To the AlN green chip that thickness is 0.55mm.The SEM figure of gained AlN ceramic is as it is shown on figure 3, prepared AlN makes pottery
Porcelain even structure, consistency is high.
Claims (10)
1. the method that flow casting molding prepares aluminium nitride ceramic substrate, comprises the steps:
1) two or more alcohols solvent is configured to mixed solvent, then by mixed solvent, dispersant, AlN ceramic
Powder and sintering aid mixing carry out first ball milling；
2) in the AlN slurry that first ball milling obtains, add plasticizer and binding agent, then carry out secondary ball milling；
3) the AlN slurry obtained by secondary ball milling carries out vacuum stirring de-bubble；
4) AlN slurry froth in vacuum obtained carries out tape casting operation, obtains AlN base substrate；
5) by AlN body drying, and strip down from cast film.
2. the method for claim 1, it is characterised in that step 1) the ball material mass ratio of first ball milling is 0.5:1～3:1 ball milling
Time is 4～24h.
3. the method for claim 1, it is characterised in that step 1) described in alcohols solvent selected from following solvent: anhydrous second
Alcohol, propanol, isopropanol and butanol.
4. method as claimed in claim 3, it is characterised in that step 1) described mixed solvent be volume ratio be 1:0.25～0.5:1
Dehydrated alcohol and the mixed solvent of propanol, volume ratio is dehydrated alcohol and the mixed solvent of isopropanol of 1:0.2～0.25:1, or
Person be volume ratio be dehydrated alcohol and the mixed solvent of butanol of 1:0.5～1:1.
5. the method for claim 1, it is characterised in that step 1) addition of described mixed solvent is AlN ceramic powder
The 20%～80% of volume.
6. the method for claim 1, it is characterised in that step 1) described in dispersant selected from ammonium polymethacrylate, poly-
One or more in etherimide, phosphate ester and ammonium polyacrylate；Described sintering aid is selected from yittrium oxide, dysprosia, oxygen
Change one or more in boron, calcium oxide and lithium oxide；Step 2) described in plasticizer selected from dioctyl phthalate,
One in dibutyl phthalate, BBP(Butyl Benzyl Phthalate, Polyethylene Glycol, glycerol, polyether polyol and oleic acid or
Multiple；One or more in polyvinyl butyral resin, polymethyl methacrylate and acrylate of described binding agent.
7. the method for claim 1, it is characterised in that step 2) the secondary ball milling time is 4h～30h, the addition of plasticizer
Amount is the 0.2%～5% of AlN ceramic powder weight, and the addition of binding agent is the 0.5%～5% of AlN ceramic powder weight.
8. the method for claim 1, it is characterised in that step 3) mixing speed is 30～100 turns/min, during froth in vacuum
Between be 5～30min.
9. the method for claim 1, it is characterised in that step 4) casting temperature is 20～40 DEG C；For thickness less than 1mm
AlN green compact substrate, curtain coating speed be 2～5m/min；For the thickness AlN green compact substrate more than 1mm, curtain coating speed
Degree is 0.2～4m/min.
10. the method for claim 1, it is characterised in that step 5) for thickness less than the AlN green compact substrate of 1mm,
Baking temperature is 30～45 DEG C, and the time is 0.5～2h；For the thickness AlN green compact substrate more than 1mm, baking temperature is
40～70 DEG C, the time is 1.5～4h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324812A (en) * | 2017-07-14 | 2017-11-07 | 上海大学 | Behavior of Slurry for Aluminum Nitride Ceramics and preparation method thereof |
| CN107522495A (en) * | 2017-02-16 | 2017-12-29 | 李军廷 | It is a kind of to prepare the method for aluminium nitride electronic ceramics substrate using the tape casting and the tape casting prepares ceramics solvent |
| CN108484176A (en) * | 2018-05-24 | 2018-09-04 | 宁夏艾森达新材料科技有限公司 | A kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips |
| CN108706980A (en) * | 2018-06-27 | 2018-10-26 | 深圳市商德先进陶瓷股份有限公司 | Aluminium nitride ceramics and preparation method thereof, electrostatic chuck and application |
| 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 |
| 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 |
| CN114804841A (en) * | 2022-04-30 | 2022-07-29 | 北京智感度衡科技有限公司 | Alumina green ceramic chip for particulate matter sensor and preparation method thereof |
| CN114839212A (en) * | 2022-05-06 | 2022-08-02 | 江苏富乐华功率半导体研究院有限公司 | Ceramic slurry glue mixing uniformity pre-detection method |
| CN114933476A (en) * | 2022-06-10 | 2022-08-23 | 北京智感度衡科技有限公司 | Zirconia green ceramic chip for nitrogen-oxygen sensor and preparation method thereof |
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| CN107522495A (en) * | 2017-02-16 | 2017-12-29 | 李军廷 | It is a kind of to prepare the method for aluminium nitride electronic ceramics substrate using the tape casting and the tape casting prepares ceramics solvent |
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| CN107324812A (en) * | 2017-07-14 | 2017-11-07 | 上海大学 | Behavior of Slurry for Aluminum Nitride Ceramics and preparation method thereof |
| CN108484176A (en) * | 2018-05-24 | 2018-09-04 | 宁夏艾森达新材料科技有限公司 | A kind of preparation method of high-temperature co-fired ceramics aluminium nitride ceramic chips |
| CN108706980A (en) * | 2018-06-27 | 2018-10-26 | 深圳市商德先进陶瓷股份有限公司 | Aluminium nitride ceramics and preparation method thereof, electrostatic chuck and application |
| 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 |
| 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 |
| CN114804841A (en) * | 2022-04-30 | 2022-07-29 | 北京智感度衡科技有限公司 | Alumina green ceramic chip for particulate matter sensor and preparation method thereof |
| CN114839212A (en) * | 2022-05-06 | 2022-08-02 | 江苏富乐华功率半导体研究院有限公司 | Ceramic slurry glue mixing uniformity pre-detection method |
| CN114839212B (en) * | 2022-05-06 | 2023-11-10 | 江苏富乐华功率半导体研究院有限公司 | Ceramic slurry glue mixing uniformity pre-detection method |
| CN114933476A (en) * | 2022-06-10 | 2022-08-23 | 北京智感度衡科技有限公司 | Zirconia green ceramic chip for nitrogen-oxygen sensor and preparation method thereof |
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Application publication date: 20161207 |