CN108329028A - A kind of preparation method of environment-friendly type gel casting forming YAG crystalline ceramics biscuits - Google Patents
A kind of preparation method of environment-friendly type gel casting forming YAG crystalline ceramics biscuits Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of environment-friendly type gel casting forming YAG crystalline ceramics biscuits, which is characterized in that is pre-processed to YAG transparent ceramic powders using aluminate coupling agent LS 822 and methene succinic acid, obtains pretreatment YAG transparent ceramic powders；Gel solution is prepared using white sugar and xanthans；Then, in the ball mill, it is added by percent by volume, pre-processes YAG transparent ceramic powders：50% ~ 55%, gel solution：41% ~ 45%, Cericammoniumsulfate：1% ~ 3%, 5 ~ 7h is ground, dimethyl-ethylenediamine is added：1% ~ 3%, the sum of each component is absolutely, to grind 60min, and ultrasonic de-bubble processing obtains YAG crystalline ceramics slurries；YAG crystalline ceramics slurries are injected in mold again, slow heating, temperature to 55 ± 2 DEG C of 8 ~ 10 h of constant temperature, after natural cooling, through drying, demoulding obtains YAG crystalline ceramics biscuits.YAG crystalline ceramics biscuits prepared by this method have solid content high, and content of organics is low, environmental protection, and the YAG crystalline 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 YAG is saturating
The preparation method of bright biscuit of ceramics is a kind of easy to operate, environmentally friendly, high solids content, plastic complicated form part and large scale
Component.
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.It is disclosed in Chinese invention patent CN101698607 B
A kind of method that environment-friendly type gel injection-moulding prepares alumina-based ceramic material.It is disclosed in Chinese invention patent CN106079032 A
A kind of gel-casting method based on agarose, ceramic slurry mixed solution.
YAG is the abbreviation of yttrium-aluminium-garnet, chemical formula Y3Al5O12, it is by Y2O3And Al2O3One kind that reaction generates is multiple
Oxide is closed, cubic system is belonged to, there is garnet structure.Garnet structure cell is considered as dodecahedron, octahedron and four sides
The link net of body.Nd is prepared using solid phase reaction sintering process from Ikesue in 1995：YAG crystalline ceramics, and realize continuous
Since laser exports laser ceramics realize the advantages that uniform high-concentration dopant and design flexibility with its short preparation period, easily and
Fast development is obtained, monocrystalline will gradually be replaced to become next-generation laser gain material.Various ion (such as Nd3+、Yb3+、Er3+、
Ho3+、Tm3+、Ce4+And Cr4+Deng) YAG of activation is most wide as research with its excellent physical and chemical performance, laser output effect
The highest material system of rate.The preparation of high optical quality YAG base transparent ceramics has become the research hotspot in advanced ceramics field.
Residual Pores, grain boundary impurities and doping segregation are to influence the principal element of its optical quality in crystalline ceramics.It is burnt in solid phase reaction
During connection prepares YAG crystalline ceramics, convection drying ball milling slurry will lead to receive the serious agglomeration of micro-powder and irregular
Shape, dry powder fluidity is poor, and intergranular friction power is big, is unfavorable for subsequent forming process, this phenomenon prepare large scale,
Seem even more serious when complicated shape and composite construction, and as the main of the second phase in ceramic sintered bodies and remaining stomata
Source, it is also possible to lead to the inconsistent contraction of ceramic body, or even cracking.Disadvantages mentioned above can be overcome using gel casting forming,
And the advantages that making the precision of product improve.
Xanthans is also known as yellow glue, xanthan gum, is a kind of Extra-cellular acidic heteroglycan generated by Xanthomonas campestris fermentation.It is
2 are pressed by D-Glucose, D-MANNOSE and D-Glucose aldehydic acid:2:The polysaccharide high-molecular compound of 1 composition, relative molecular mass
1,000,000 or more.Xanthans is light yellow to white flowable powder, slightly band stink.It is soluble in hot water or cold water, solution neutral,
Resistance and freeze and defrosting do not dissolve in ethyl alcohol.It meets water-dispersed, emulsification and becomes stable hydrophily thick gel.Xanthans is current state
Integrate thickening on border, suspension, emulsifies, is stable at the biogum that best performances are got over.Contain the molecular side chain end of xanthans
The number of pyruvic acid group, has a significant impact to its performance.Xanthans has the general performance of long chain macromolecule, but it is than general
Macromolecule contains more functional group, can show special performance under given conditions.It is used as the stabilization of a variety of purposes in the industry
Agent, thickening agent and processing paving auxiliary agent.
The present invention is using aluminate coupling agent LS-822, methene succinate modified YAG transparent ceramic powders surface, Ji Nengti
It is highly filled, and the viscosity of slurry can be reduced, improve surface cleanliness.Using xanthans as gel adhesive, sulfuric acid is added
Cerium ammonium is to cause gel polymerisation reaction to prepare YAG crystalline ceramics biscuits, then passes through high temperature sintering and prepares YAG crystalline ceramics, this
Application system can be that the volume ratio of solid content reaches 55%, and formed precision is high, and biscuit intensity is high, prepared YAG crystalline ceramics
Consistency reach 98%, structure is uniform, flawless.Preparation process is simple, environmental protection, at low cost.
Invention content
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of environment-friendly type gel casting forming YAG crystalline ceramics biscuits, which is characterized in that this method has
Following processing step：
（1）YAG transparent ceramic powders pre-process：In the ball mill, it is added by mass percentage, YAG transparent ceramic powders：96%~
98%, aluminate coupling agent LS-822：0.5% ~ 2.5%, methene succinic acid：0.5% ~ 2.5%, the sum of each component is absolutely, to open
Ball mill is opened, temperature rises to 50 ± 2 DEG C of constant temperature, grinds 2-4h, dry, obtains pretreatment YAG transparent ceramic powders；
（2）Gel solution is prepared：It is 10 in mass ratio by white sugar and xanthans：1 ratio ground and mixed is uniform, is dissolved in
In deionized water, the solution that the concentration expressed in percentage by volume of quality containing xanthans is 0.2% ~ 1% is obtained, which is gel solution；
（3）YAG crystalline ceramics slurry preparations：In the ball mill, it is added by percent by volume, pre-processes YAG transparent ceramic powders：
50% ~ 55%, gel solution：41% ~ 45%, Cericammoniumsulfate：1% ~ 3%, 5 ~ 7h is ground, dimethyl-ethylenediamine is added：1% ~ 3%, respectively
The sum of component is absolutely, to grind 60min, and ultrasonic de-bubble processing obtains YAG crystalline ceramics slurries；
（4）The preparation of YAG crystalline ceramics biscuits：By step（3）YAG crystalline ceramics slurries inject in mold, slow heating, temperature
To 55 ± 2 DEG C of 8 ~ 10 h of constant temperature, after natural cooling, through drying, demoulding obtains YAG crystalline ceramics biscuits.
In step（1）Described in YAG transparent ceramic powders grain size in 0.1 ~ 0.5 μ m.
In step（2）Described in white sugar be soft white sugar or white granulated sugar.
In step（4）Described in biscuit YAG crystalline 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 be by aluminate coupling agent LS-822, methene succinate modified YAG transparent ceramic powders surface, can
Solid content is improved, and the viscosity of slurry can be reduced, improves surface cleanliness, this method solid content volume ratio is up to 55%.
（2）The application uses biogum i.e. xanthans for adhesive, and white sugar is dispersant, reduces the use of chemical reagent,
Reduce environmental pollution.
（3）It is the acidity adjustment that Cericammoniumsulfate plays the role of system when starting that the application, which uses the advantages of Cericammoniumsulfate,
Play the role of initiator again, polymerisation terminates the cerium ion in high temperature sintering and plays sintering aid again, can improve
The physical and chemical performance of YAG crystalline ceramics.
（4）Content of organics is few in prepared YAG crystalline ceramics biscuits, drying and moulding process will not crack, it is made
Standby biscuit has certain intensity, can be processed before sintering, the compactness of prepared ceramics is up to 98%.
（5）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）YAG transparent ceramic powders pre-process：In the ball mill, it is separately added into, YAG transparent ceramic powders：970g, Aluminate
Coupling agent LS-822：15g, methene succinic acid：15g opens ball mill, and temperature rises to 50 ± 2 DEG C of constant temperature, grinds 3h, dry, obtains
To pretreatment YAG transparent ceramic powders；
（2）Gel solution is prepared：50g white sugar and 5g xanthans after ground and mixed is uniform in mortar, is dissolved in 1000mL and gone
In ionized water, the solution that the concentration expressed in percentage by volume of quality containing xanthans is 0.5% is obtained, which is gel solution；
（3）YAG crystalline ceramics slurry preparations：In the ball mill, it is separately added into, pre-processes YAG transparent ceramic powders：520mL coagulates
Sol solution：440mL, Cericammoniumsulfate：20g grinds 6h, adds dimethyl-ethylenediamine：25 mL grind 60min, ultrasonic de-bubble
Processing, obtains YAG crystalline ceramics slurries；
（4）The preparation of YAG crystalline ceramics biscuits：YAG crystalline ceramics slurries are injected in mold, slow heating, temperature to 55 ± 2
DEG C 9 h of constant temperature, after natural cooling, through drying, demoulding obtains YAG crystalline ceramics biscuits.
Embodiment 2
（1）YAG transparent ceramic powders pre-process：In the ball mill, it is separately added into, YAG transparent ceramic powders：960g, Aluminate
Coupling agent LS-822：20g, methene succinic acid：20g opens ball mill, and temperature rises to 50 ± 2 DEG C of constant temperature, grinds 4h, dry, obtains
To pretreatment YAG transparent ceramic powders；
（2）Gel solution is prepared：100g white sugar and 10g xanthans after ground and mixed is uniform in mortar, are dissolved in 1000mL
In deionized water, the solution that the concentration expressed in percentage by volume of quality containing xanthans is 1% is obtained, which is gel solution；
（3）YAG crystalline ceramics slurry preparations：In the ball mill, it is separately added into, pre-processes YAG transparent ceramic powders：500mL coagulates
Sol solution：450mL, Cericammoniumsulfate：25g grinds 5h, adds dimethyl-ethylenediamine：30mL grinds 60min, at ultrasonic de-bubble
Reason, obtains YAG crystalline ceramics slurries；
（4）The preparation of YAG crystalline ceramics biscuits：YAG crystalline ceramics slurries are injected in mold, slow heating, temperature to 55 ± 2
DEG C 8 h of constant temperature, after natural cooling, through drying, demoulding obtains YAG crystalline ceramics biscuits.
Embodiment 3
（1）YAG transparent ceramic powders pre-process：In the ball mill, it is separately added into, YAG transparent ceramic powders：980g, Aluminate
Coupling agent LS-822：10g, methene succinic acid：10g opens ball mill, and temperature rises to 50 ± 2 DEG C of constant temperature, grinds 2h, dry, obtains
To pretreatment YAG transparent ceramic powders；
（2）Gel solution is prepared：20g white sugar and 2g xanthans after ground and mixed is uniform in mortar, is dissolved in 1000mL and gone
In ionized water, the solution that the concentration expressed in percentage by volume of quality containing xanthans is 0.2% is obtained, which is gel solution；
（3）YAG crystalline ceramics slurry preparations：In the ball mill, it is separately added into, pre-processes YAG transparent ceramic powders：550mL coagulates
Sol solution：410mL, Cericammoniumsulfate：30g grinds 7h, adds dimethyl-ethylenediamine：12 mL grind 60min, ultrasonic de-bubble
Processing, obtains YAG crystalline ceramics slurries；
（4）The preparation of YAG crystalline ceramics biscuits：YAG crystalline ceramics slurries are injected in mold, slow heating, temperature to 55 ± 2
DEG C 10 h of constant temperature, after natural cooling, through drying, demoulding obtains YAG crystalline ceramics biscuits.
Embodiment 4
（1）YAG transparent ceramic powders pre-process：In the ball mill, it is separately added into, YAG transparent ceramic powders：970g, Aluminate
Coupling agent LS-822：25g, methene succinic acid：0.5g opens ball mill, and temperature rises to 50 ± 2 DEG C of constant temperature, grinds 3.5h, does
It is dry, obtain pretreatment YAG transparent ceramic powders；
（2）Gel solution is prepared：80g white sugar and 8g xanthans after ground and mixed is uniform in mortar, is dissolved in 1000mL and gone
In ionized water, the solution that the concentration expressed in percentage by volume of quality containing xanthans is 0.8% is obtained, which is gel solution；
（3）YAG crystalline ceramics slurry preparations：In the ball mill, it is separately added into, pre-processes YAG transparent ceramic powders：540mL coagulates
Sol solution：420mL, Cericammoniumsulfate：00g grinds 6h, adds dimethyl-ethylenediamine：37 mL grind 60min, ultrasonic de-bubble
Processing, obtains YAG crystalline ceramics slurries；
（4）The preparation of YAG crystalline ceramics biscuits：YAG crystalline ceramics slurries are injected in mold, slow heating, temperature to 55 ± 2
DEG C 9.5 h of constant temperature, after natural cooling, through drying, demoulding obtains YAG crystalline ceramics biscuits.
Embodiment 5
（1）YAG transparent ceramic powders pre-process：In the ball mill, it is separately added into, YAG transparent ceramic powders：970g, Aluminate
Coupling agent LS-822：0.5g, methene succinic acid：25g opens ball mill, and temperature rises to 50 ± 2 DEG C of constant temperature, grinds 2.5h, does
It is dry, obtain pretreatment YAG transparent ceramic powders；
（2）Gel solution is prepared：40g white sugar and 4g xanthans after ground and mixed is uniform in mortar, is dissolved in 1000mL and gone
In ionized water, the solution that the concentration expressed in percentage by volume of quality containing xanthans is 0.4% is obtained, which is gel solution；
（3）YAG crystalline ceramics slurry preparations：In the ball mill, it is separately added into, pre-processes YAG transparent ceramic powders：510mL coagulates
Sol solution：430mL, Cericammoniumsulfate：30g grinds 6h, adds dimethyl-ethylenediamine：36 mL grind 60min, ultrasonic de-bubble
Processing, obtains YAG crystalline ceramics slurries；
（4）The preparation of YAG crystalline ceramics biscuits：YAG crystalline ceramics slurries are injected in mold, slow heating, temperature to 55 ± 2
DEG C 8.5 h of constant temperature, after natural cooling, through drying, demoulding obtains YAG crystalline ceramics biscuits.
YAG crystalline ceramics biscuits prepared by the application, can be with molding structure complex component and big ruler by simple processing
Very little component, molding precision is high, and the intensity of biscuit is high, carries out high temperature sintering and can be obtained YAG crystalline ceramics.Prepared YAG is saturating
The compactness of bright ceramics is up to 98%.
Claims (3)
1. a kind of preparation method of environment-friendly type gel casting forming YAG crystalline ceramics biscuits, which is characterized in that this method have with
Lower processing step：
（1）YAG transparent ceramic powders pre-process：In the ball mill, it is added by mass percentage, YAG transparent ceramic powders：96%~
98%, aluminate coupling agent LS-822：0.5% ~ 2.5%, methene succinic acid：0.5% ~ 2.5%, the sum of each component is absolutely, to open
Ball mill is opened, temperature rises to 50 ± 2 DEG C of constant temperature, grinds 2-4h, dry, obtains pretreatment YAG transparent ceramic powders；
（2）Gel solution is prepared：It is 10 in mass ratio by white sugar and xanthans：1 ratio ground and mixed is uniform, is dissolved in
In deionized water, the solution that the concentration expressed in percentage by volume of quality containing xanthans is 0.2% ~ 1% is obtained, which is gel solution；
（3）YAG crystalline ceramics slurry preparations：In the ball mill, it is added by percent by volume, pre-processes YAG transparent ceramic powders：
50% ~ 55%, gel solution：41% ~ 45%, Cericammoniumsulfate：1% ~ 3%, 5 ~ 7h is ground, dimethyl-ethylenediamine is added：1% ~ 3%, respectively
The sum of component is absolutely, to grind 60min, and ultrasonic de-bubble processing obtains YAG crystalline ceramics slurries；
（4）The preparation of YAG crystalline ceramics biscuits：By step（3）YAG crystalline ceramics slurries inject in mold, slow heating, temperature
To 55 ± 2 DEG C of 8 ~ 10 h of constant temperature, after natural cooling, through drying, demoulding obtains YAG crystalline ceramics biscuits.
2. a kind of preparation method of environment-friendly type gel casting forming YAG crystalline ceramics biscuits according to claim 1, special
Sign is, step（1）Described in YAG transparent ceramic powders grain size in 0.1 ~ 0.5 μ m.
3. a kind of preparation method of environment-friendly type gel casting forming YAG crystalline ceramics biscuits according to claim 1, special
Sign is, step（2）Described in white sugar be soft white sugar or white granulated sugar.
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| CN112299828A (en) * | 2020-11-09 | 2021-02-02 | 新沂市锡沂高新材料产业技术研究院有限公司 | Preparation method of transparent ceramic back plate applied to 5G solar mobile phone |
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| CN112299828A (en) * | 2020-11-09 | 2021-02-02 | 新沂市锡沂高新材料产业技术研究院有限公司 | Preparation method of transparent ceramic back plate applied to 5G solar mobile phone |
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