CN108409304A - A kind of preparation method of carbomer gel casting aluminium oxide biscuit - Google Patents
A kind of preparation method of carbomer gel casting aluminium oxide biscuit Download PDFInfo
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- CN108409304A CN108409304A CN201810181074.8A CN201810181074A CN108409304A CN 108409304 A CN108409304 A CN 108409304A CN 201810181074 A CN201810181074 A CN 201810181074A CN 108409304 A CN108409304 A CN 108409304A
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Abstract
The invention discloses a kind of preparation methods of carbomer gel casting aluminium oxide biscuit, which is characterized in that is pre-processed to alundum (Al2O3) powder using aconitic acid, obtains pretreatment alumina powder；Gel solution is prepared using carbomer；Then, in the ball mill, it is added by percent by volume, pre-processes alumina powder：50% ~ 55%, gel solution：42% ~ 46%, urea：2% ~ 5%, the sum of each component is absolutely, to grind 12 ~ 15h, and froth in vacuum processing obtains aluminium oxide ceramics slurry；Stage oxidation aluminium ceramic slurry is injected in mold, slow heating, temperature to 70 ± 3 DEG C of 8 ~ 10 h of constant temperature, after natural cooling, through drying, demoulding obtains aluminium oxide biscuit.Aluminium oxide biscuit prepared by this method has solid content high, and content of organics is low, environmental protection, and the aluminium oxide ceramics consistency of gained is high after sintering.
Description
Technical field
The invention belongs to ceramic forming materials and preparation field, and in particular to a kind of carbomer gel casting aluminium oxide
The preparation method of biscuit is a kind of easy to operate, environmentally friendly, high solids content, can near-net-shape complicated shape compact aluminum oxide
The preparation method of ceramic.
Background technology
In the early 1990s, Oak Ridge National Key Laboratory of U.S. Janney etc. proposes gel casting forming skill
Art（gelcasting）, conventional preparation techniques and polymer chemistry are combined for the first time, has started and has been molded work in ceramics
In skill molding technology is carried out using high polymer monomer polymerization.The technology can prepare even density, large scale, complexity with high accuracy
The ceramic component of shape, this method have many advantages, such as simple for process, at low cost.So far, domestic and international related gel casting forming
In the majority with ceramic materials such as aluminium oxide, silicon carbide, silicon nitride, titanium nitrides in research, traditional gel injection molding and forming technology uses
Toxicity has more by force the monomer polyacrylamide or N,N-DMAA of stimulation taste, crosslinking agent N, N- di-2-ethylhexylphosphine oxide
Acrylamide, initiator are ammonium persulfate, and dispersant is polyacrylic acid.Green body prepared by conventional colloidal moulding process is in drying
Shrink in the process it is usually bigger, to cause green body to deform in the drying process, problems of crack；And due to molding
The intensity of green body is relatively low, and green body is easily damaged during demoulding, especially for large scale, complicated shape molding blank sometimes
It can not even demould.Ceramic material is inevitably present green body dimensional contraction phenomenon in shaping and drying, sintering process.In order to
Overcome conventional gel casting disadvantage, study new gel injection-moulding system, finds excellent adhesive monomer, dispersant etc.,
The condition of research gel injection molded body system prepares biscuit of ceramics and attracts attention.
Aluminium oxide ceramics is one kind with aluminium oxide（Al2O3）Based on ceramic material, be used for thick film integrated circuit.Oxidation
Aluminium ceramics have preferable conductibility, mechanical strength and heat-resisting quantity.Such as ceramic bearing, ceramic seal and water valve plate, it is made molten
Melt glass to replace platinum crucible, the ceramic component of superhigh intensity using its translucency and to be resistant to alkali metal corrosivity as sodium vapor lamp
Pipe, can be used as ic substrate and high-frequency insulation material etc. in the electronics industry.Some high added value alumina ceramic products
Or defence and military need to special parts, such as speculum, nuclear fuel and gun barrel product, field use hot isostatic pressing firing side
Method.Because its superior performance, more and more extensive in the application of modern society, it is satisfied with daily and property need
It wants.
Carbomer（English name：Carbomer）For white loose sprills；There is characteristic micro- smelly；Have and draw moist, is medicinal
Auxiliary material.Carbomer is the high molecular polymer that acrylic acid is bonded allyl sucrose or pentaerythrite allyl ether.It is calculated by dry product,
Containing carboxylic acid group（—COOH）It should be 56.0%~68.0%.Carbopol940：Short rheological characteristic, high viscosity, high clarity, it is low it is resistance to from
Sub- property and endurance of cutting, suitable for gel and cream.Carbopol941：Long rheological characteristic, low viscosity, high clarity, it is medium resistance to
Ionic and resistant to shearing is suitable for gel and lotion.Carbopol934：Cross-linked polyacrylic resin, local medicine-applying system,
Stablize when high viscosity, for dense gelling agent, emulsion, suspension.Carbomer is non-toxic, is widely applied to cosmetics, excipient substance
In.
The present invention by aluminium oxide powder material by add dispersant, adhesive, initiator under suitable condition
Gel injection-moulding prepares the biscuit of aluminium oxide ceramics, and the application system can be that the volume ratio of solid content reaches 58%, formed precision
Height, biscuit intensity is high, and the consistency of prepared aluminium oxide ceramics reaches 99%, and structure is uniform, flawless.Preparation process is simple,
Environmental protection, it is at low cost.
Invention content
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of carbomer gel casting aluminium oxide biscuit, which is characterized in that this method has following
Processing step：
（1）Alumina powder pre-processes：In the ball mill, it is added by mass percentage, alundum (Al2O3)：90% ~ 94%, sintering helps
Agent：0.1% ~ 1.0%, aconitic acid：2% ~ 4%, open 0.5 h of ball mill grinding, the ammonium hydroxide that sprinkling mass percentage concentration is 10%：3%~
6%, the sum of each component is a hundred percent, then grinds 0.5h, dry, obtains pretreatment alumina powder, grain size is in 0.1 ~ 0.2 μ
Between m；
（2）Gel solution is prepared：In the reactor, it is added by mass percentage concentration, deionized water：95% ~ 98%, carbomer：
0.2% ~ 3.0%, triethanolamine：0.24 ~ 3.6%, the sum of each component is that absolutely, stirring and dissolving obtains gel solution；
（3）Aluminium oxide ceramics slurry preparation：In the ball mill, it is added by percent by volume, pre-processes alumina powder：50%~
55%, gel solution：42% ~ 46%, urea：2% ~ 5%, the sum of each component is absolutely, to grind 12 ~ 15h, and froth in vacuum is handled,
Obtain aluminium oxide ceramics slurry；
（4）The preparation of aluminium oxide biscuit：By step（3）Aluminium oxide ceramics slurry injects in mold, slow heating, and temperature to 70 ±
3 DEG C of 8 ~ 10 h of constant temperature, after natural cooling, through drying, demoulding obtains aluminium oxide biscuit.
In step（1）Described in alumina powder grain size in 0.05 ~ 0.12 μ m.
In step（1）Described in sintering aid be diboron trioxide, the mixing of one or both of lanthana.
In step（2）Described in carbomer and triethanolamine mass ratio be 1：1.2.
In step（5）Described in biscuit aluminium oxide ceramics is obtained after high temperature sintering.
The present invention compared with the prior art, has the following advantages that and advantageous effect：
（1）The present invention is to be decomposed into the pH value that ammonia improves system by heating urea, so that carbomer crosslinking is become gel, is homogeneous
Reaction can be very good the uniformity of control gel, and carbomer can improve solid content in the case that viscosity is small when pH value is low,
This method solid content volume ratio is up to 58%.
（2）It need not be heated when batch mixing, heating curing molding, prepared ceramics under urea decomposition after casting
Compactness up to 99%.
（3）Content of organics is few in prepared biscuit of ceramics, drying and moulding process will not crack, prepared biscuit
With certain intensity, can be processed before sintering.
（4）This method can prepare various complicated form parts, can prepare large-sized ceramic component, molding precision
It is high.
（5）This method be by dispersant first with the ceramic powder of solid is wear-resisting mixes, can be dispersant in this way in solid table
Face is formed when electric double layer is mixed with gel solution with excellent dispersibility.
Specific implementation mode
Embodiment 1
（1）Alumina powder pre-processes：In the ball mill, it is separately added into, alundum (Al2O3)：920g, lanthana：5g, aconitic acid：
30g opens 0.5 h of ball mill grinding, the ammonium hydroxide that sprinkling mass percentage concentration is 10%：45 mL, then 0.5h is ground, it is dry, it obtains
To pretreatment alumina powder, grain size is between 0.1 ~ 0.2 μm；
（2）Gel solution is prepared：In the reactor, it is separately added into, deionized water：960 mL, carbomer：18g, triethanolamine：
22g, stirring and dissolving obtain gel solution；
（3）Aluminium oxide ceramics slurry preparation：In the ball mill, it is separately added into, pre-processes alumina powder：520 mL, gel are molten
Liquid：440 mL, urea：40g, grinds 14h, and froth in vacuum processing obtains aluminium oxide ceramics slurry；
（4）The preparation of aluminium oxide biscuit：By step（3）Aluminium oxide ceramics slurry injects in mold, slow heating, and temperature to 70 ±
3 DEG C of constant temperature 9h, after natural cooling, through drying, demoulding obtains aluminium oxide biscuit.
Embodiment 2
（1）Alumina powder pre-processes：In the ball mill, it is separately added into, alundum (Al2O3)：900g, diboron trioxide：10g, crow
Head acid：40g opens 0.5 h of ball mill grinding, the ammonium hydroxide that sprinkling mass percentage concentration is 10%：50 mL, then 0.5h is ground, it does
It is dry, pretreatment alumina powder is obtained, grain size is between 0.1 ~ 0.2 μm；
（2）Gel solution is prepared：In the reactor, it is separately added into, deionized water：980 mL, carbomer：9g, triethanolamine：
11g, stirring and dissolving obtain gel solution；
（3）Aluminium oxide ceramics slurry preparation：In the ball mill, it is separately added into, pre-processes alumina powder：500 mL, gel are molten
Liquid：450 mL, urea：50g, grinds 12h, and froth in vacuum processing obtains aluminium oxide ceramics slurry；
（4）The preparation of aluminium oxide biscuit：By step（3）Aluminium oxide ceramics slurry injects in mold, slow heating, and temperature to 70 ±
3 DEG C of constant temperature 8h, after natural cooling, through drying, demoulding obtains aluminium oxide biscuit.
Embodiment 3
（1）Alumina powder pre-processes：In the ball mill, it is separately added into, alundum (Al2O3)：940g, lanthana：2g, aconitic acid：
28g opens 0.5 h of ball mill grinding, the ammonium hydroxide that sprinkling mass percentage concentration is 10%：30 mL, then 0.5h is ground, it is dry, it obtains
To pretreatment alumina powder, grain size is between 0.1 ~ 0.2 μm；
（2）Gel solution is prepared：In the reactor, it is separately added into, deionized water：950 mL, carbomer：23g, triethanolamine：
27g, stirring and dissolving obtain gel solution；
（3）Aluminium oxide ceramics slurry preparation：In the ball mill, it is separately added into, pre-processes alumina powder：550 mL, gel are molten
Liquid：420 mL, urea：30g, grinds 11h, and froth in vacuum processing obtains aluminium oxide ceramics slurry；
（4）The preparation of aluminium oxide biscuit：By step（3）Aluminium oxide ceramics slurry injects in mold, slow heating, and temperature to 70 ±
3 DEG C of constant temperature 10h, after natural cooling, through drying, demoulding obtains aluminium oxide biscuit.
Embodiment 4
（1）Alumina powder pre-processes：In the ball mill, it is separately added into, alundum (Al2O3)：930g, diboron trioxide：8g, crow
Head acid：22g opens 0.5 h of ball mill grinding, the ammonium hydroxide that sprinkling mass percentage concentration is 10%：40 mL, then 0.5h is ground, it does
It is dry, pretreatment alumina powder is obtained, grain size is between 0.1 ~ 0.2 μm；
（2）Gel solution is prepared：In the reactor, it is separately added into, deionized water：970 mL, carbomer：13g, triethanolamine：
17g, stirring and dissolving obtain gel solution；
（3）Aluminium oxide ceramics slurry preparation：In the ball mill, it is separately added into, pre-processes alumina powder：540 mL, gel are molten
Liquid：440 mL, urea：20g, grinds 13h, and froth in vacuum processing obtains aluminium oxide ceramics slurry；
（4）The preparation of aluminium oxide biscuit：By step（3）Aluminium oxide ceramics slurry injects in mold, slow heating, and temperature to 70 ±
3 DEG C of perseverance 9.5h, after natural cooling, through drying, demoulding obtains aluminium oxide biscuit.
Embodiment 5
（1）Alumina powder pre-processes：In the ball mill, it is separately added into, alundum (Al2O3)：910g, lanthana：5g, aconitic acid：
35g opens 0.5 h of ball mill grinding, the ammonium hydroxide that sprinkling mass percentage concentration is 10%：50 mL, then 0.5h is ground, it is dry, it obtains
To pretreatment alumina powder, grain size is between 0.1 ~ 0.2 μm；
（2）Gel solution is prepared：In the reactor, it is separately added into, deionized water：960 mL, carbomer：20g, triethanolamine：
20g, stirring and dissolving obtain gel solution；
（3）Aluminium oxide ceramics slurry preparation：In the ball mill, it is separately added into, pre-processes alumina powder：530 mL, gel are molten
Liquid：430 mL, urea：40g, grinds 14h, and froth in vacuum processing obtains aluminium oxide ceramics slurry；
（4）The preparation of aluminium oxide biscuit：By step（3）Aluminium oxide ceramics slurry injects in mold, slow heating, and temperature to 70 ±
3 DEG C of constant temperature 8.5h, after natural cooling, through drying, demoulding obtains aluminium oxide biscuit.
Aluminium oxide biscuit prepared by the application carries out high temperature sintering and can be obtained aluminium oxide ceramics by simple processing.
Claims (5)
1. a kind of preparation method of carbomer gel casting aluminium oxide biscuit, which is characterized in that this method has following work
Skill step：
（1）Alumina powder pre-processes：In the ball mill, it is added by mass percentage, alundum (Al2O3)：90% ~ 94%, sintering helps
Agent：0.1% ~ 1.0%, aconitic acid：2% ~ 4%, open 0.5 h of ball mill grinding, the ammonium hydroxide that sprinkling mass percentage concentration is 10%：3%~
6%, the sum of each component is a hundred percent, then grinds 0.5h, dry, obtains pretreatment alumina powder, grain size is in 0.1 ~ 0.2 μ
Between m；
（2）Gel solution is prepared：In the reactor, it is added by mass percentage concentration, deionized water：95% ~ 98%, carbomer：
0.2% ~ 3.0%, triethanolamine：0.24 ~ 3.6%, the sum of each component is that absolutely, stirring and dissolving obtains gel solution；
（3）Aluminium oxide ceramics slurry preparation：In the ball mill, it is added by percent by volume, pre-processes alumina powder：50%~
55%, gel solution：42% ~ 46%, urea：2% ~ 5%, the sum of each component is absolutely, to grind 12 ~ 15h, and froth in vacuum is handled,
Obtain aluminium oxide ceramics slurry；
（4）The preparation of aluminium oxide biscuit：By step（3）Aluminium oxide ceramics slurry injects in mold, slow heating, and temperature to 70 ±
3 DEG C of 8 ~ 10 h of constant temperature, after natural cooling, through drying, demoulding obtains aluminium oxide biscuit.
2. a kind of preparation method of carbomer gel casting aluminium oxide biscuit according to claim 1, feature exist
In step（1）Described in alumina powder grain size in 0.05 ~ 0.12 μ m.
3. a kind of preparation method of carbomer gel casting aluminium oxide biscuit according to claim 1, feature exist
In step（1）Described in sintering aid be diboron trioxide, the mixing of one or both of lanthana.
4. a kind of preparation method of carbomer gel casting aluminium oxide biscuit according to claim 1, feature exist
In step（2）Described in carbomer and triethanolamine mass ratio be 1：1.2.
5. a kind of preparation method of carbomer gel casting aluminium oxide biscuit according to claim 1, feature exist
In step（5）Described in biscuit aluminium oxide ceramics is obtained after high temperature sintering.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112811913A (en) * | 2021-03-11 | 2021-05-18 | 无锡辰海新材料科技有限公司 | Method for preparing silicon nitride ceramic biscuit by environment-friendly gel injection molding |
| CN113372101A (en) * | 2021-06-29 | 2021-09-10 | 西安理工大学 | Preparation method of alumina ceramic |
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| CN101117284A (en) * | 2007-07-13 | 2008-02-06 | 北京中材人工晶体有限公司 | Alumina ceramic and preparation method thereof |
| CN103360039A (en) * | 2013-07-16 | 2013-10-23 | 山东工业陶瓷研究设计院有限公司 | Large-size sheet-type electric-insulation heat-dissipation ceramic substrate and preparation method thereof |
| CN103553636A (en) * | 2013-10-16 | 2014-02-05 | 冷水江市明玉陶瓷工具有限责任公司 | Gel injection molding method of engineering ceramic |
| CN103553629A (en) * | 2013-10-18 | 2014-02-05 | 中国科学院上海硅酸盐研究所 | Method for preparing aluminum oxynitride transparent ceramic through gel casting |
| CN104829221A (en) * | 2015-04-14 | 2015-08-12 | 苏州工业园区晶冠瓷材料科技有限公司 | Method for preparing Re:YAG transparent ceramic through gel injection mold forming |
| CN105084874A (en) * | 2015-08-10 | 2015-11-25 | 南京工业大学 | Method for gel-casting alumina or ZTA ceramic |
| CN106495666A (en) * | 2015-09-06 | 2017-03-15 | 南京理工大学 | A kind of preparation method of high-purity aluminum oxide ceramic material |
| CN105218095A (en) * | 2015-09-22 | 2016-01-06 | 中国科学院上海硅酸盐研究所 | Gel casting forming reaction sintering is utilized to prepare the method for yttrium aluminum garnet transparent ceramic |
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| CN113372101A (en) * | 2021-06-29 | 2021-09-10 | 西安理工大学 | Preparation method of alumina ceramic |
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