CN108298992A - A kind of method that environment-friendly type gel casting forming prepares silicon nitride ceramics biscuit - Google Patents
A kind of method that environment-friendly type gel casting forming prepares silicon nitride ceramics biscuit Download PDFInfo
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Abstract
The invention discloses a kind of methods that environment-friendly type gel casting forming prepares silicon nitride ceramics biscuit, which is characterized in that is pre-processed to beta-silicon nitride powder using edible oil, obtains pretreatment beta-silicon nitride powder；Using Carbopol 941 as adhesive, lemon acid amide, ethylenediamine prepare gel solution as acidity regulator and dispersant；Then, in the ball mill, it is added by percent by volume, pre-processes beta-silicon nitride powder：48% ~ 53%, gel solution：43% ~ 48%, ammonium oxalate：3% ~ 6%, the sum of each component is absolutely, to grind 10 ~ 12h, and froth in vacuum processing obtains silicon nitride ceramics slurry；Silicon nitride ceramics slurry is injected in mold, slow heating, temperature to 85 ± 3 DEG C of 16 ~ 18 h of constant temperature, after natural cooling, through drying, demoulding obtains silicon nitride biscuit.Silicon nitride biscuit prepared by this method has solid content high, and content of organics is low, environmental protection, and the silicon nitride 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 environment-friendly type gel casting forming prepares nitrogen
The method of SiClx biscuit of ceramics is a kind of easy to operate, environmentally friendly, high solids content, can near-net-shape complicated shape densification nitrogen
The preparation method of SiClx ceramic.
Background technology
Silicon nitride ceramics, non-shrinking inorganic material ceramics when being a kind of sintering.The intensity of silicon nitride is very high, especially hot
Silicon nitride is pressed, is most hard in the world one of substance.It is good, hard with high intensity, low-density, high temperature resistant, chemical resistance
Degree is high, the advantages such as wear-resisting property is good, friction coefficient is small, and density is low, no matter all has as structural material or functional material and answers
With foreground, receive more and more attention in recent years.Silicon nitride ceramics oil, chemical industry, microelectronics, space flight, aviation, papermaking,
The industrial circles such as laser, automobile, mining industry and atomic energy have been widely used.The preparation method of silicon nitride ceramics is main at present
Have：Powder compacting sintering method, sol-gal process and reaction sintering etc., when using gel casting forming, due to there is the presence of water,
Silicon nitride can hydrolyze, and influence the purity of silicon nitride, while generate gas, and prepared silicon nitride ceramics consistency is made to drop
Low, the application, which pre-processes beta-silicon nitride powder using grease, can successfully solve the problems, such as this.
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.
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 silicon nitride powder powder material by add dispersant, adhesive, initiator under suitable condition
Gel injection-moulding prepares the biscuit of silicon nitride ceramics, and the application system can be that the volume ratio of solid content reaches 55%, formed precision
Height, biscuit intensity is high, and the consistency of prepared silicon nitride 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 method that environment-friendly type gel casting forming prepares silicon nitride ceramics biscuit, which is characterized in that this method has
Following processing step：
（1）Beta-silicon nitride powder pre-processes：In the ball mill, it is added by mass percentage, silicon nitride：95% ~ 97%, sintering aid：
0.1% ~ 2.0%, edible oil：2% ~ 4%, the sum of each component is absolutely, to open ball mill grinding 2h, dry, is pre-processed
Beta-silicon nitride powder, grain size is between 0.15 ~ 0.25 μm；
（2）Gel solution is prepared：In the reactor, it is added by mass percentage concentration, deionized water：94% ~ 98%, Carbopol 941：
0.5% ~ 2.0%, lemon acid amide：0.5 ~ 4.0%, ethylenediamine：0.5 ~ 2.0%, the sum of each component is that absolutely, stirring and dissolving obtains
To gel solution；
（3）Silicon nitride ceramics slurry preparation：In the ball mill, it is added by percent by volume, pre-processes beta-silicon nitride powder：48%~
53%, gel solution：43% ~ 48%, ammonium oxalate：3% ~ 6%, the sum of each component is absolutely, 10 ~ 12h to be ground, at froth in vacuum
Reason, obtains silicon nitride ceramics slurry；
（4）The preparation of silicon nitride biscuit：By step（3）Silicon nitride ceramics slurry injects in mold, slow heating, and temperature to 85 ±
3 DEG C of 16 ~ 18 h of constant temperature, after natural cooling, through drying, demoulding obtains silicon nitride biscuit.
In step（1）Described in edible oil be soya-bean oil, it is peanut oil, rapeseed oil, one or more mixed in sunflower oil
It closes.
In step（1）Described in beta-silicon nitride powder grain size in 0.1 ~ 0.2 μ m.
In step（1）Described in sintering aid be that scandium oxide, lanthana, one or both of zirconium dioxide are mixed
It closes.
In step（2）Described in carbomer and ethylenediamine mass ratio be 1：1.1.
In step（4）Described in biscuit silicon nitride 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 ammonium oxalate, makes Carbopol 941 low-viscosity gel, hands over
It is unified into as gel, is homogeneous reaction, can be very good the uniformity of control gel, Carbopol 941 viscosity when pH value is low is small
In the case of can improve solid content, this method solid content volume ratio is up to 55%.
（2）It need not be heated when batch mixing, heating curing molding, prepared pottery under ammonium oxalate decomposition after casting
The compactness of porcelain is 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.
Specific implementation mode
Embodiment 1
（1）Beta-silicon nitride powder pre-processes：In the ball mill, it is separately added into, silicon nitride：960g, scandium oxide：10g, soya-bean oil：
30g opens ball mill grinding 2h, dry, obtains pretreatment beta-silicon nitride powder, grain size is between 0.15 ~ 0.25 μm；
（2）Gel solution is prepared：In the reactor, it is separately added into, deionized water：950 mL, Carbopol 941：10g, citric acid
Amine：30g, ethylenediamine：10g, stirring and dissolving obtain gel solution；
（3）Silicon nitride ceramics slurry preparation：In the ball mill, it is separately added into, pre-processes beta-silicon nitride powder：500 mL, gel are molten
Liquid：450 mL, ammonium oxalate：50g, grinds 11h, and froth in vacuum processing obtains silicon nitride ceramics slurry；
（4）The preparation of silicon nitride biscuit：By step（3）Silicon nitride ceramics slurry injects in mold, slow heating, and temperature to 85 ±
3 DEG C of 17 h of constant temperature, after natural cooling, through drying, demoulding obtains silicon nitride biscuit.
Embodiment 2
（1）Beta-silicon nitride powder pre-processes：In the ball mill, it is separately added into, silicon nitride：950g, lanthana：20g, peanut oil：
30g opens ball mill grinding 2h, dry, obtains pretreatment beta-silicon nitride powder, grain size is between 0.15 ~ 0.25 μm；
（2）Gel solution is prepared：In the reactor, it is separately added into, deionized water：980 mL, Carbopol 941：5g, citric acid
Amine：10g, ethylenediamine：5g, stirring and dissolving obtain gel solution；
（3）Silicon nitride ceramics slurry preparation：In the ball mill, it is separately added into, pre-processes beta-silicon nitride powder：480 mL, gel are molten
Liquid：460 mL, ammonium oxalate：60g, grinds 10h, and froth in vacuum processing obtains silicon nitride ceramics slurry；
（4）The preparation of silicon nitride biscuit：By step（3）Silicon nitride ceramics slurry injects in mold, slow heating, and temperature to 85 ±
3 DEG C of constant temperature 16h, after natural cooling, through drying, demoulding obtains silicon nitride biscuit.
Embodiment 3
（1）Beta-silicon nitride powder pre-processes：In the ball mill, it is separately added into, silicon nitride：970g, zirconium dioxide：2g, rapeseed oil：
28g opens ball mill grinding 2h, dry, obtains pretreatment beta-silicon nitride powder, grain size is between 0.15 ~ 0.25 μm；
（2）Gel solution is prepared：In the reactor, it is separately added into, deionized water：940 mL, Carbopol 941：20g, citric acid
Amine：20g, ethylenediamine：20g, stirring and dissolving obtain gel solution；
（3）Silicon nitride ceramics slurry preparation：In the ball mill, it is separately added into, pre-processes beta-silicon nitride powder：530 mL, gel are molten
Liquid：440 mL, ammonium oxalate：30g, grinds 12h, and froth in vacuum processing obtains silicon nitride ceramics slurry；
（4）The preparation of silicon nitride biscuit：By step（3）Silicon nitride ceramics slurry injects in mold, slow heating, and temperature to 85 ±
3 DEG C of 18 h of constant temperature, after natural cooling, through drying, demoulding obtains silicon nitride biscuit.
Embodiment 4
（1）Beta-silicon nitride powder pre-processes：In the ball mill, it is separately added into, silicon nitride：950g, scandium oxide：5g, titanium dioxide
Zirconium：5 g, sunflower oil：40g opens ball mill grinding 2h, dry, obtains pretreatment beta-silicon nitride powder, grain size 0.15 ~
Between 0.25 μm；
（2）Gel solution is prepared：In the reactor, it is separately added into, deionized water：940 mL, Carbopol 941：10g, citric acid
Amine：40g, ethylenediamine：10g, stirring and dissolving obtain gel solution；
（3）Silicon nitride ceramics slurry preparation：In the ball mill, it is separately added into, pre-processes beta-silicon nitride powder：480 mL, gel are molten
Liquid：480 mL, ammonium oxalate：40g, grinds 10.5h, and froth in vacuum processing obtains silicon nitride ceramics slurry；
（4）The preparation of silicon nitride biscuit：By step（3）Silicon nitride ceramics slurry injects in mold, slow heating, and temperature to 85 ±
3 DEG C of 16.5 h of constant temperature, after natural cooling, through drying, demoulding obtains silicon nitride biscuit.
Embodiment 5
（1）Beta-silicon nitride powder pre-processes：In the ball mill, it is separately added into, silicon nitride：955g, scandium oxide：5g, soya-bean oil：
40g opens ball mill grinding 2h, dry, obtains pretreatment beta-silicon nitride powder, grain size is between 0.15 ~ 0.25 μm；
（2）Gel solution is prepared：In the reactor, it is separately added into, deionized water：960 mL, Carbopol 941：18g, citric acid
Amine：5g, ethylenediamine：18g, stirring and dissolving obtain gel solution；
（3）Silicon nitride ceramics slurry preparation：In the ball mill, it is separately added into, pre-processes beta-silicon nitride powder：490 mL, gel are molten
Liquid：470 mL, ammonium oxalate：40g, grinds 11.5h, and froth in vacuum processing obtains silicon nitride ceramics slurry；
（4）The preparation of silicon nitride biscuit：By step（3）Silicon nitride ceramics slurry injects in mold, slow heating, and temperature to 85 ±
3 DEG C of constant temperature 17.5h, after natural cooling, through drying, demoulding obtains silicon nitride biscuit.
Silicon nitride biscuit prepared by the application carries out high temperature sintering and can be obtained silicon nitride ceramics by simple processing.
The compactness of prepared ceramics is up to 99%.
Claims (5)
1. a kind of method that environment-friendly type gel casting forming prepares silicon nitride ceramics biscuit, which is characterized in that this method have with
Lower processing step：
（1）Beta-silicon nitride powder pre-processes：In the ball mill, it is added by mass percentage, silicon nitride：95% ~ 97%, sintering aid：
0.1% ~ 2.0%, edible oil：2% ~ 4%, the sum of each component is absolutely, to open ball mill grinding 2h, dry, is pre-processed
Beta-silicon nitride powder, grain size is between 0.15 ~ 0.25 μm；
（2）Gel solution is prepared：In the reactor, it is added by mass percentage concentration, deionized water：94% ~ 98%, Carbopol 941：
0.5% ~ 2.0%, lemon acid amide：0.5 ~ 4.0%, ethylenediamine：0.5 ~ 2.0%, the sum of each component is that absolutely, stirring and dissolving obtains
To gel solution；
（3）Silicon nitride ceramics slurry preparation：In the ball mill, it is added by percent by volume, pre-processes beta-silicon nitride powder：48%~
53%, gel solution：43% ~ 48%, ammonium oxalate：3% ~ 6%, the sum of each component is absolutely, 10 ~ 12h to be ground, at froth in vacuum
Reason, obtains silicon nitride ceramics slurry；
（4）The preparation of silicon nitride biscuit：By step（3）Silicon nitride ceramics slurry injects in mold, slow heating, and temperature to 85 ±
3 DEG C of 16 ~ 18 h of constant temperature, after natural cooling, through drying, demoulding obtains silicon nitride biscuit.
2. the method that a kind of environment-friendly type gel casting forming according to claim 1 prepares silicon nitride ceramics biscuit, special
Sign is, step（1）Described in edible oil be soya-bean oil, peanut oil, rapeseed oil, one or more mixing in sunflower oil.
3. the method that a kind of environment-friendly type gel casting forming according to claim 1 prepares silicon nitride ceramics biscuit, special
Sign is, step（1）Described in beta-silicon nitride powder grain size in 0.1 ~ 0.2 μ m.
4. the method that a kind of environment-friendly type gel casting forming according to claim 1 prepares silicon nitride ceramics biscuit, special
Sign is, step（1）Described in sintering aid be scandium oxide, lanthana, the mixing of one or both of zirconium dioxide.
5. the method that a kind of environment-friendly type gel casting forming according to claim 1 prepares silicon nitride ceramics biscuit, special
Sign is, step（2）Described in carbomer and ethylenediamine mass ratio be 1：1.1.
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Cited By (3)
| 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 |
| CN112851367A (en) * | 2021-01-26 | 2021-05-28 | 泰晟新材料科技有限公司 | Extrusion molding thin-wall silicon nitride pipe fitting and preparation method thereof |
| CN114195552A (en) * | 2021-12-27 | 2022-03-18 | 杭州电子科技大学 | Film forming method for grafting nitrogen-doped carbon quantum dots on surface of silicon nitride ceramic ball |
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| 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 |
| CN114195552A (en) * | 2021-12-27 | 2022-03-18 | 杭州电子科技大学 | Film forming method for grafting nitrogen-doped carbon quantum dots on surface of silicon nitride ceramic ball |
| CN114195552B (en) * | 2021-12-27 | 2022-09-23 | 杭州电子科技大学 | Film forming method for grafting nitrogen-doped carbon quantum dots on surface of silicon nitride ceramic ball |
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