CN101791818A - Method for preparing aluminium oxide ceramics green ceramic chip by tape casting - Google Patents
Method for preparing aluminium oxide ceramics green ceramic chip by tape casting Download PDFInfo
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- CN101791818A CN101791818A CN 201010118620 CN201010118620A CN101791818A CN 101791818 A CN101791818 A CN 101791818A CN 201010118620 CN201010118620 CN 201010118620 CN 201010118620 A CN201010118620 A CN 201010118620A CN 101791818 A CN101791818 A CN 101791818A
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Abstract
The invention provides a method for preparing an aluminium oxide ceramic green ceramic chip by tape casting. The method comprises the following steps: evenly stirring ceramic powder, adhesives, plasticizer and solvent to form green ceramic slurry; and then casting the green ceramic slurry into the green ceramic chip by tape casting. The invention is characterized in that the solvent is ethanol, isopropanol and ethyl acetate. The invention adopts the solvent system of the ethanol, the isopropanol and the ethyl acetate to replace the traditional toluene to serve as the main solvent; the consistency and the stability of product quality are ensured; and compared with the traditional production method, the waste gas discharged by the method of the invention has less influence on the environment, thereby being favor of energy conversation and emission reduction and lowering cost.
Description
Technical field
The present invention relates to a kind of preparation method of aluminium oxide ceramics green ceramic chip, be specifically related to a kind of method of preparing aluminium oxide ceramics green ceramic chip by tape casting.
Background technology
Aluminium oxide ceramics is mainly used in high-frequency insulation material, multilayer co-firing ceramic substrate and digital integrated electronic circuit, the required ceramic package of microwave circuit device encapsulation.Aluminium oxide ceramics is divided into two kinds of high-purity type and plain editions.High-purity type aluminium oxide ceramics is Al
2O
3Content is at the ceramic material more than 99.9%, because its sintering temperature is up to 1650～1990 ℃, transmission peak wavelength is 1～6 μ m, generally fires the back to replace platinum crucible; Utilize its light transmission and can be used as the sodium vapor lamp pipe by alkaline-resisting metal protection; In electronics industry, can be used as ic substrate and high-frequency insulation material.Al presses in plain edition aluminium oxide ceramics system
2O
3The content difference is divided into kinds such as 99 porcelain, 95 porcelain, 90 porcelain, 85 porcelain and (refers to Al
2O
3Content is respectively 99%, 95%, 90%, 85% etc.), Al sometimes
2O
3Content also divides common aluminium oxide ceramics series into 80% or 75%.Wherein 99 alumina ceramics materials are used to make high-temperature crucibles, fire-resistant boiler tube and special high-abrasive material, as ceramic bearing, ceramic seal spare and water valve plate etc.; 95 alumina ceramics are mainly as corrosion-resistant, wear parts, electronic package material etc.; Owing to often mix the part talcum, improved electrical property and mechanical strength in 85 porcelain, can with metal sealings such as molybdenum, niobium, tantalum, have as electrovacuum device device.Multilayer co-firing is a stock with the aluminium oxide ceramics green ceramic chip between the general employing of aluminium oxide ceramics 90 porcelain～95 porcelain, makes the thick-film metalliz circuit through technologies such as printing, lamination, lamination, sintering.
The aluminium oxide ceramic products forming method has dry-pressing, slip casting, extruding, isostatic cool pressing, injects, rolls several different methods such as film, curtain coating, hot pressing and hip moulding.The basic composition material of multi-layer ceramics technology is a ceramics green ceramic chip, wherein only rolls the production that minority forming methods such as film, curtain coating are suitable for multilayer co-firing pottery flaky material.Roll the embrane method moulding because little, ceramics uniformity of production capacity and uniformity are bad, generally be not suitable for producing in batches.What employing was more now is that The tape casting is produced ceramic chips, and The tape casting is produced ceramic chips advantages such as consistency of thickness is good because of having, ceramics even and can produce continuously, relatively is fit to batch process.
The aluminium oxide ceramic chips is to adopt casting apparatus (as casting machine) the green slurry to be made the banded chip material of certain thickness and width.The green slurry is made up of ceramic powder (alumina powder and glass powder mix by a certain percentage), bonding agent, solvent and plasticizer, and ceramic powder is suspended in organic adhesive and the plasticizer.A kind of homogeneous mixture of process stirring composition system is fallen solvent evaporates wherein by the method for curtain coating again, thereby is met the ceramic chips of requirement.It is main solvent and to face dibatyl phithalate (DBP is hereinafter to be referred as DBP) be the system of plasticizer for bonding agent, toluene that traditional both at home and abroad casting method generally uses polyvinyl butyral resin (PVB is hereinafter to be referred as PVB).Adopt the system of toluene as primary solvent, in the curtain coating operating process, the steam that toluene evaporates can cause serious harm to operating personnel, needs to increase very high protective gear and the facility of cost.During curtain coating, mode by heating and exhausting is all volatilized away toluene, discharge capacity every day (conveyer belt is that 10 meters long, 0.5 meter wide casting machine is produced continuously) will reach more than the 20KG, annual discharge capacity is more than 6 tons, if directly will contain the curtain coating toxic emission of toluene, will cause serious pollution to the atmospheric environment in several kilometers on every side.The processing method commonly used of this type of waste gas has burning, condensation recovery or filtration treatment at present.Use the way floor space of burning big, also need to consume a large amount of electric power resources, only a small incinerator just need take about 200 square metres vacant lot, and its electrical power needs 160KW.The condensing unit will use highly energy-consuming is reclaimed in condensation, and filtration treatment is generally used filtration supports such as active carbon, need frequently to change, and the filtration supports of changing also needs further to handle just and can avoid secondary pollution.All these treating apparatus all need very big disposable input, and the expense of operation and maintenance is also very high, and these all do not meet the requirement of energy-saving and emission-reduction.
Summary of the invention
Goal of the invention: the objective of the invention is to overcome the weak point of prior art in environmental protection and highly energy-consuming, a kind of method of preparing aluminium oxide ceramics green ceramic chip by tape casting of energy-saving and environmental protection is provided.
Technical scheme: the method for a kind of preparing aluminium oxide ceramics green ceramic chip by tape casting of the present invention, ceramic powder, bonding agent, plasticizer and stirring solvent is even, form the green slurry, method by curtain coating obtains ceramic chips with green slurry curtain coating again, it is characterized in that: described solvent is ethanol, isopropyl alcohol and ethyl acetate.
Described ceramic powder, bonding agent, plasticizer and solvent can carry out proportioning as required, and the weight ratio of the comparative optimization that the inventor provides is 1: 0.04～0.2: 0.03～0.15: 0.45～2.1.
Proportioning as required between described etoh solvent, isopropyl alcohol and the ethyl acetate, its weight ratio comparative optimization is 0.15～0.70: 0.15～0.70: 0.15～0.70.
Described ceramic powders can dispose as required, mainly is made up of alumina powder 70%～99% and glass powder 1%～30%, by weight percentage; Described binding agent is PVB; Described plasticizer is DBP.
The method of above-mentioned preparing aluminium oxide ceramics green ceramic chip by tape casting, further specifically refinement comprises following steps:
(1) load weighted solvent and plasticizer are mixed, gradually bonding agent is joined wherein again, and stir at normal temperatures, bonding agent is dissolved fully, become mixed solution;
(2) load weighted ceramic powder is joined in the mixed solution, mix at normal temperatures again, form the green slurry;
(3) under rough vacuum, remove the green slurry bubble;
(4) open casting apparatus, subregion heating, air draft;
(5) gap between casting apparatus scraper and the conveyer belt is set;
(6) the green slurry of removing bubble is added in the slurry box of casting apparatus;
(7) open casting apparatus, the green slurry in the slurry box transmits through conveyer belt, the beginning curtain coating, and the green slurry obtains ceramic chips after by casting apparatus.
The heating of subregion described in the step (4) is to be divided into four districts, can heat according to common subregion heating means, but in order to ensure the ceramic chips stable performance that makes, quality is good, preferred temperature is: first district's temperature is 30～45 ℃, second district's temperature is 40～55 ℃, and the 3rd district's temperature is 55～75 ℃, and the 4th district's temperature is 60～80 ℃.
The specification of the ceramic chips that the gap described in the step (5) between casting apparatus scraper and the conveyer belt can prepare as required is provided with, and is set to 0.5～1.5mm usually.
Green slurry described in the step (7) in the slurry box can be common transfer rate through the speed that conveyer belt transmits, but in order to obtain the ceramic chips of better quality, speed is preferably 100～300mm/min.
Curtain coating is with pre-configured green slurry among the present invention, enters the thermal treatment zone of casting machine by scraper, the method for the solvent in the green slurry by subregion heating and exhausting is vapored away, thereby obtain the uniform ceramic chips of thickness.The composition of green slurry and characteristic directly influence the quality of ceramic chips, and it generally is made up of aluminium oxide and glass mixed powder, bonding agent, solvent, plasticizer etc.Aluminium oxide and glass mixed powder are most important compositions in the material system, after oversintering, have only this mixed powder to stay and form pottery, and other compositions have all been removed in pilot process.The effect of bonding agent is that the network that forms a kind of microcosmic keeps equally distributed state with whole system.The effect of solvent is the dissolving bonding agent, by fully mixing the various compositions of green slurry can be disperseed uniformly.The effect of plasticizer is the plasticity of ceramics after the increase curtain coating, makes ceramic chips be not easy fracture.
Beneficial effect of the present invention is:
1, the present invention uses ethanol, isopropyl alcohol and ethyl acetate solvent system to replace traditional toluene as primary solvent, in the time of the uniformity of assurance product quality and stability, its exhaust gas discharged reduces with respect to the traditional mode of production mode greatly to ambient influnence, be very beneficial for energy-saving and emission-reduction, and reduce cost;
2, the present invention uses ethanol, isopropyl alcohol and ethyl acetate to be solvent, because ethanol is limited to the solubility of PVB, if only use ethanol as solvent then be difficult to satisfy each composition and disperse uniformly, add the dissolution that has strengthened greatly behind a certain amount of isopropyl alcohol and the ethyl acetate PVB, thereby guaranteed the uniformity of green slurry;
3, the present invention has set the temperature of subregion heating and the transfer rate of driving-belt according to the characteristics of the solvent of newly selecting for use, the feasible ceramic chips good stability that makes, and quality meets the requirements;
4, the present invention uses PVB as bonding agent, whole system can satisfy the various machineries of green moulding in the follow-up multilayer co-firing aluminium oxide ceramics technology and the requirement of hot property, can produce complicated ceramic package constructed products, the product stability of moulding is good, the shrinkage factor unanimity behind the ceramic post sintering, stable;
5, the present invention uses solvent that each component material is fully mixed, and being evenly distributed of each component material of ceramic chips makes stable physical property behind the ceramic post sintering;
6, the ceramic chips surface smoothness of curtain coating of the present invention is good, and consistency of thickness is very suitable for the thick-film metalliz printing of multilayer co-firing pottery, and size can be cut out arbitrarily according to production requirement; Whole technology can be produced by the Continuous Flow ability of swimming, is suitable for producing in enormous quantities.
Description of drawings
Accompanying drawing is the inventive method process chart.
The specific embodiment
Below in conjunction with accompanying drawing, the mode by embodiment is elaborated to technical solution of the present invention, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1
Utilize the inventive method configuration 95%Al
2O
3Ceramic whiteware green slurry, and to obtain width with the casting machine curtain coating be 250mm, thickness is the ceramic chips of 0.2mm, technological process is as shown in drawings.
Processing step: (1) the ceramic powder 2500g that weighs with scale, wherein alumina powder accounts for 95%, and glass powder accounts for 5%; The PVB powder of weighing 250g; The ethanol of weighing 1000g (chemical pure), the isopropyl alcohol of weighing 250g (chemical pure), the ethyl acetate of weighing 250g (chemical pure); The DBP of weighing 150g (chemical pure).
(2) load weighted ethanol, isopropyl alcohol, ethyl acetate and DBP are joined in the bulk container.
(3) add load weighted PVB powder gradually, and stirring makes PVB be dissolved in the solvent fully.
(4) with load weighted Al
2O
3Powder and glass powder join in the ball grinder, pour the mixed solution that has dissolved PVB into ball grinder and lid is fastened, and open ball mill, at normal temperatures ball milling 24 hours (mixing and stirring).
(5) ball milling is good green slurry is poured clean stainless steel cask into, and puts into vacuum tank, degasification 30min under the vacuum of 150 torrs.
(6) the casting machine heating is set as follows respectively: 45 ℃ in first district; 55 ℃ in second district; 55 ℃ in the 3rd district;
60 ℃ in the 4th district.Open heater and air draft.
(7) scraper is installed on the casting machine, and the gap that is provided with between scraper and the conveyer belt is 0.65mm.
(8) the good green slurry of degasification is added in the wide green slurry box of 250mm.
(9) conveyer belt of operation casting machine is adjusted to 100mm/min with the speed of conveyer belt, the beginning curtain coating, and all green slurries promptly obtain ceramic chips after by casting machine.
Embodiment 2
Utilize the inventive method configuration Al
2O
3Black porcelain green slurry, and to obtain width with the casting machine curtain coating be 250mm, thickness is the ceramic chips of 0.3mm.
Processing step: technical process is with embodiment 1, but gets 2450g ceramic powder and 50g ceramic coloring powder, wherein Al in the 1st step
2O
3Powder accounts for 95%, and glass powder accounts for 5%.The temperature setting changes in the 6th step: 30 ℃ in first district; 40 ℃ in second district; 75 ℃ in the 3rd district; 80 ℃ in the 4th district.Scraper gap is set to 0.85mm in the 7th step.The speed of conveyer belt is 300mm/min in the 9th step.
Embodiment 3
Utilize the inventive method configuration 99%Al
2O
3Ceramic whiteware green slurry, and to obtain width with the casting machine curtain coating be 350mm, thickness is the ceramic chips of 0.15mm.
Processing step: technical process is with embodiment 1, but weigh with scale in the 1st step ceramic powder 2500g, wherein Al
2O
3Powder accounts for 99%, and glass powder accounts for 1%; The PVB powder of weighing 100g; The ethanol of weighing 375g (chemical pure), the isopropyl alcohol of weighing 375g (chemical pure), the ethyl acetate of weighing 375g (chemical pure); The DBP of weighing 75g (chemical pure).The temperature setting changes in the 6th step: 37 ℃ in first district; 47 ℃ in second district; 65 ℃ in the 3rd district; 70 ℃ in the 4th district.Scraper gap is set to 0.50mm in the 7th step.Use the wide green slurry box of 350mm in the 8th step.The speed of conveyer belt is 150mm/min in the 9th step.
Embodiment 4
Utilize the inventive method configuration 70%Al
2O
3Ceramic whiteware green slurry, and to obtain width with the casting machine curtain coating be 450mm, thickness is the ceramic chips of 0.7mm.
Processing step: technical process is with embodiment 1, but weigh with scale in the 1st step ceramic powder 2500g, wherein Al
2O
3Powder accounts for 70%, and glass powder accounts for 30%; The PVB powder of weighing 500g; The ethanol of weighing 1750g (chemical pure), the isopropyl alcohol of weighing 1750g (chemical pure), the ethyl acetate of weighing 1750g (chemical pure); The DBP of weighing 375g (chemical pure).Scraper gap is set to 1.50mm in the 7th step.Use the wide green slurry box of 450mm in the 8th step.The speed of conveyer belt is 300mm/min in the 9th step.
Claims (10)
1. the method for a preparing aluminium oxide ceramics green ceramic chip by tape casting, ceramic powder, bonding agent, plasticizer and stirring solvent is even, form the green slurry, method by curtain coating obtains ceramic chips with green slurry curtain coating again, it is characterized in that: described solvent is ethanol, isopropyl alcohol and ethyl acetate.
2. the method for preparing aluminium oxide ceramics green ceramic chip by tape casting according to claim 1, it is characterized in that: the weight ratio of described ceramic powder, bonding agent, plasticizer and solvent is 1: 0.04～0.2: 0.03～0.15: 0.45～2.1.
3. the method for preparing aluminium oxide ceramics green ceramic chip by tape casting according to claim 2, it is characterized in that: the weight ratio between described etoh solvent, isopropyl alcohol and the ethyl acetate is 0.15～0.70: 0.15～0.70: 0.15～0.70.
4. the method for preparing aluminium oxide ceramics green ceramic chip by tape casting according to claim 2, it is characterized in that: described ceramic powder mainly is made up of alumina powder 70%～99% and glass powder 1%～30%, by weight percentage.
5. the method for preparing aluminium oxide ceramics green ceramic chip by tape casting according to claim 2, it is characterized in that: described binding agent is a polyvinyl butyral resin.
6. the method for preparing aluminium oxide ceramics green ceramic chip by tape casting according to claim 2, it is characterized in that: described plasticizer is for facing dibatyl phithalate.
7. according to the method for the described preparing aluminium oxide ceramics green ceramic chip by tape casting of arbitrary claim in the claim 1～6, it is characterized in that it comprises following steps:
(1) load weighted solvent and plasticizer are mixed, gradually bonding agent is joined wherein again, and stir at normal temperatures, bonding agent is dissolved fully, become mixed solution;
(2) load weighted ceramic powder is joined in the mixed solution, mix at normal temperatures again, form the green slurry;
(3) under rough vacuum, remove the green slurry bubble;
(4) open casting apparatus, subregion heating, air draft;
(5) gap between casting apparatus scraper and the conveyer belt is set;
(6) the green slurry of removing bubble is added in the slurry box of casting apparatus;
(7) open casting apparatus, the green slurry in the slurry box transmits through conveyer belt, the beginning curtain coating, and the green slurry obtains ceramic chips after by casting apparatus.
8. the method for preparing aluminium oxide ceramics green ceramic chip by tape casting according to claim 7, it is characterized in that: the heating of subregion described in the step (4) is to be divided into four districts: first district's temperature is 30～45 ℃, second district's temperature is 40～55 ℃, the 3rd district's temperature is 55～75 ℃, and the 4th district's temperature is 60～80 ℃.
9. the method for preparing aluminium oxide ceramics green ceramic chip by tape casting according to claim 7, it is characterized in that: the gap described in the step (5) between casting apparatus scraper and the conveyer belt is 0.5～1.5mm.
10. the method for preparing aluminium oxide ceramics green ceramic chip by tape casting according to claim 7 is characterized in that: the green slurry described in the step (7) in the slurry box is 100～300mm/min through the speed that conveyer belt transmits.
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| CN102699986A (en) * | 2012-04-25 | 2012-10-03 | 中国电子科技集团公司第五十五研究所 | Molding method of complicated two-side cavity structure with multilayer ceramics |
| CN102862367A (en) * | 2012-09-11 | 2013-01-09 | 中国兵器工业集团第二一四研究所苏州研发中心 | Cavity forming method of multi-layered ceramic element |
| CN104098323A (en) * | 2013-04-12 | 2014-10-15 | 成都慧成科技有限责任公司 | Multilayer composite [beta]"-Al2O3 flat-plate-type solid electrolyte and preparation method thereof |
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| CN116751034A (en) * | 2023-05-24 | 2023-09-15 | 浙江东瓷科技有限公司 | Preparation method of high-strength alumina ceramic substrate |
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| CN102699986A (en) * | 2012-04-25 | 2012-10-03 | 中国电子科技集团公司第五十五研究所 | Molding method of complicated two-side cavity structure with multilayer ceramics |
| CN102699986B (en) * | 2012-04-25 | 2014-06-11 | 中国电子科技集团公司第五十五研究所 | Molding method of complicated two-side cavity structure with multilayer ceramics |
| CN102862367A (en) * | 2012-09-11 | 2013-01-09 | 中国兵器工业集团第二一四研究所苏州研发中心 | Cavity forming method of multi-layered ceramic element |
| CN102862367B (en) * | 2012-09-11 | 2015-01-14 | 中国兵器工业集团第二一四研究所苏州研发中心 | Cavity forming method of multi-layered ceramic element |
| CN104098323A (en) * | 2013-04-12 | 2014-10-15 | 成都慧成科技有限责任公司 | Multilayer composite [beta]"-Al2O3 flat-plate-type solid electrolyte and preparation method thereof |
| CN104261808A (en) * | 2014-09-09 | 2015-01-07 | 登封福中特种电器元件有限公司 | High-temperature conductor paste for printing electronic ceramic cast slice |
| CN107619285A (en) * | 2017-09-26 | 2018-01-23 | 南方科技大学 | Laminated sheet type electronic component casting slurry and preparation method thereof |
| CN108055712A (en) * | 2017-12-11 | 2018-05-18 | 东莞佐佑电子科技有限公司 | Dielectric paste and its preparation method and application |
| CN110436897A (en) * | 2019-09-04 | 2019-11-12 | 福建华清电子材料科技有限公司 | A kind of preparation method of ultrathin alumina ceramic substrate |
| 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 |
| CN114920567A (en) * | 2022-04-21 | 2022-08-19 | 苏州瑞瓷新材料科技有限公司 | Preparation method of alumina slurry and prepared alumina slurry |
| CN114920567B (en) * | 2022-04-21 | 2023-05-26 | 苏州瑞瓷新材料科技有限公司 | Preparation method of alumina slurry and prepared alumina slurry |
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| CN116003166A (en) * | 2022-12-05 | 2023-04-25 | 中国电子科技集团公司第五十五研究所 | Medium-temperature ceramic suitable for microwave power device packaging shell and preparation method |
| CN116003166B (en) * | 2022-12-05 | 2024-04-12 | 中国电子科技集团公司第五十五研究所 | Medium-temperature ceramic suitable for microwave power device packaging shell and preparation method |
| CN116313833A (en) * | 2023-05-19 | 2023-06-23 | 苏州晶晟微纳半导体科技有限公司 | Ceramic substrate and preparation method and application thereof |
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| CN116751034A (en) * | 2023-05-24 | 2023-09-15 | 浙江东瓷科技有限公司 | Preparation method of high-strength alumina ceramic substrate |
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