CN105801092A - Raw materials of transparent ceramic as well as preparation method and application - Google Patents
Raw materials of transparent ceramic as well as preparation method and application Download PDFInfo
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Abstract
The invention belongs to the field of ceramic products, and particularly relates to raw materials of transparent ceramic as well as a preparation method and an application. The invention provides the transparent ceramic. The transparent ceramic comprises the following raw materials: ceramic powder, a lubricating agent, a binder, a dispersing agent and citric acid. The invention further provides a preparation method of any transparent ceramic. The invention further provides an application of any transparent ceramic or any preparation method in a transparent ceramic component. The product prepared by the technical scheme is good in transparency and high in light transmittance, and can meet the operation requirements of nowadays society on the transparent ceramic; and meanwhile, the product prepared by the technical scheme also has the advantages of uniform particle distribution and no atmospheric hole.
Description
Technical field
The invention belongs to ceramic product field, particularly relate to the raw material of a kind of crystalline ceramics, preparation method and application.
Background technology
Transparent ceramic material has the attribute that the structural ceramicss such as high temperature resistant, corrosion-resistant, high intensity, high rigidity, chemical stability and biocompatibility are intrinsic, it is provided simultaneously with the functional characteristics such as printing opacity, wave transparent and laser, obtains more and more many application in high-tech sectors such as the energy, machinery, military project, electronics, quasiconductor and medical science.Since the sixties in last century, the aspects such as the synthesis of transparent ceramic material, sintering, crystal structure, performance, printing opacity mechanism and application have been done many explorations and research work by ceramic material scientist.As have studied oxidic transparent pottery and the Non-oxide Transparent Ceramics such as aluminium nitride, Sialon such as aluminium oxide, yttrium-aluminium-garnet, yittrium oxide, magnesium oxide, magnesium aluminate spinel.But in the past few years, along with development in science and technology, the preparation of crystalline ceramics performance is had higher requirement, such as, transparent alumina ceramics discharge tube in ceramic gold-halogen lamp, transparent alumina ceramics holding groove, transparent Indium zircon ceramic camera lens, yag laser crystalline ceramics, crystalline ceramics plate armour and magnesium-aluminum spinel ceramic trousers.But, in prior art, due to the restriction of technology, the transparency of crystalline ceramics is poor, and light transmittance is low, it is impossible to meet the user demand for crystalline ceramics.
Therefore, develop the raw material of a kind of crystalline ceramics, preparation method and application, be used for solving in prior art, the transparency of crystalline ceramics is poor, light transmittance is low, it is impossible to meets the user demand for crystalline ceramics, becomes those skilled in the art's problem demanding prompt solution.
Summary of the invention
In view of this, the invention provides the raw material of a kind of crystalline ceramics, preparation method and application, be used for solving in prior art, the transparency of crystalline ceramics is poor, and light transmittance is low, it is impossible to the problem meeting the user demand for crystalline ceramics.
The invention provides a kind of crystalline ceramics, the raw material of described crystalline ceramics includes: ceramic powder, lubricant, binding agent, dispersant and citric acid.
Preferably, in mass parts, the raw material of described crystalline ceramics includes: ceramic powder 84～94 parts, lubricant 1.5～4 parts, binding agent 1.5～4 parts, dispersant 1.5～4 parts and citric acid 1.5～4 parts.
Preferably, the purity of described ceramic powder is more than 99.9%, and the particle diameter of described ceramic powder is 10-7M, described ceramic powder is selected from: the one in aluminium oxide, yittrium oxide, magnesium aluminate spinel, aluminium nitride, A Long or calcium fluoride.
Preferably, described lubricant is Polyethylene Glycol, and described binding agent is polyvinyl alcohol.
Present invention also offers the preparation method including one described crystalline ceramics of any of the above, described preparation method includes: step one, supending, after ceramic powder, lubricant aqueous solution, adhesive solution, dispersant and citric acid mixing, regulate pH to 6, settle after ball milling, obtain the first product；Step 2, spray chilling: after described first product agitated, mist projection granulating successively and lyophilization, obtain the second product；Step 3, defat: described second product, after defat, obtains third product；Step 4, sintering, after described third product sintering, obtain product.
Preferably, the concentration of described lubricant aqueous solution is 0.2～0.4g/ml, and the concentration of described adhesive solution is 0.2～0.3g/ml, and the medium of described ball milling is high pure and ultra-fine translucent alumina abrading-ball, the time of described ball milling is 24h, and the radius of the granule that described sedimentation obtains is more than 2 μm.
Preferably, described stir speed (S.S.) is 200～400rpm, and the pump speed of described mist projection granulating is 1～3ml/min, the air pressure of described mist projection granulating is 0.4～0.6bar, the flow rate of described mist projection granulating is 40～60rpm, and described cryodesiccated temperature is-20 DEG C, and the described cryodesiccated time is 24h.
Preferably, the method for described molding is carry out high temperature insostatic pressing (HIP) after dry-pressing, and the temperature of described defat is 500 DEG C, and the time of described defat is 5h.
Preferably, the method for described sintering is: the one of hot pressing, air pressure, high temperature insostatic pressing (HIP) or discharge plasma sintering, and described sintering pressure is 10～100Pa.
Present invention also offers and include one described crystalline ceramics of any of the above or the application in crystalline ceramics parts of one the described preparation method of any of the above.
In sum, the invention provides a kind of crystalline ceramics, the raw material of described crystalline ceramics includes: ceramic powder, lubricant, binding agent, dispersant and citric acid.Present invention also offers the preparation method including one described crystalline ceramics of any of the above, described preparation method includes: step one, supending, after ceramic powder, lubricant aqueous solution, adhesive solution, dispersant and citric acid mixing, regulate pH to 6, settle after ball milling, obtain the first product；Step 2, spray chilling: after described first product agitated, mist projection granulating successively and lyophilization, obtain the second product；Step 3, defat: described second product, after defat, obtains third product；Step 4, sintering, after described third product sintering, obtain product.Present invention also offers and include one described crystalline ceramics of any of the above or the application in crystalline ceramics parts of one the described preparation method of any of the above.By the product that technical scheme provided by the present invention prepares, transparency is good, and light transmittance is high, can meet the society user demand for crystalline ceramics.Meanwhile, by the product that technical scheme provided by the present invention prepares, the advantage that also there is even particle distribution, do not have gross blow hole.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, the accompanying drawing used required in embodiment or description of the prior art will be briefly described below, apparently, accompanying drawing in the following describes is only embodiments of the invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to the accompanying drawing provided.
Fig. 1 is the schematic flow sheet of a kind of crystalline ceramics preparation method of the embodiment of the present invention；
Fig. 2 is product structural representation under the microscope in the embodiment of the present invention 1.
Detailed description of the invention
The invention provides the raw material of a kind of crystalline ceramics, preparation method and application, be used for solving in prior art, the transparency of crystalline ceramics is poor, and light transmittance is low, it is impossible to the problem meeting the user demand for crystalline ceramics.
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
In order to be described in more detail the present invention, below in conjunction with embodiment to the raw material of a kind of crystalline ceramics provided by the invention, preparation method and application, it is specifically described.
Embodiment 1
Supending: weigh ceramic powder 84g, dispersant 4g and citric acid 4g, it is dissolved in 100g water, add lubricant solution 10ml, adhesive solution 10ml, after mixing, pH to 6 is regulated with ammonia, adopt high pure and ultra-fine translucent alumina abrading-ball as ball-milling medium ball milling 24h, the particle diameter granule more than 2 μm is removed by settling, obtains the first product 1.In the present embodiment, ceramic powder be purity more than 99%, particle diameter be 10-7The aluminium oxide of m, dispersant is the mixture of DolapixCE64 and Darvan821a, and lubricant solution is the Aqueous Solutions of Polyethylene Glycol of 0.4g/ml, and dispersant is the polyvinyl alcohol water solution of 0.4g/ml.
Spray chilling: the first product 1 is placed in beaker, adopts magnetic stirrer stirring, and stir speed (S.S.) is 400rpm.Then carrying out mist projection granulating, the pump speed of mist projection granulating is 3ml/min, and the air pressure of mist projection granulating is 0.6bar, the flow rate of mist projection granulating is 60rpm, and the product obtained by mist projection granulating carries out lyophilization, and cryodesiccated temperature is-20 DEG C, the cryodesiccated time is 24h, obtains the second product 1.
Defat: the second product 1, after defat, obtains third product 1.In the present embodiment, the temperature of defat is 500 DEG C, and the time of defat is 5h.
Sintering, after third product 1 sintering, obtains product 1.In the embodiment of the present invention, the method for sintering is hot pressed sintering, and sintering pressure is 30MPa.
Embodiment 2
Supending: weigh ceramic powder 94g, dispersant 1.5g and citric acid 1.5g, it is dissolved in 100g water, add lubricant solution 1ml, adhesive solution 1ml, after mixing, pH to 6 is regulated with ammonia, adopt high pure and ultra-fine translucent alumina abrading-ball as ball-milling medium ball milling 24h, the particle diameter granule more than 2 μm is removed by settling, obtains the first product 2.In the present embodiment, ceramic powder be purity more than 99%, particle diameter be 10-7The yittrium oxide of m, dispersant is the mixture of DolapixCE64 and Darvan821a, and lubricant solution is the Aqueous Solutions of Polyethylene Glycol of 1.5g/ml, and dispersant is the polyvinyl alcohol water solution of 1.5g/ml.
Spray chilling: the first product 2 is placed in beaker, adopts magnetic stirrer stirring, and stir speed (S.S.) is 200rpm.Then carrying out mist projection granulating, the pump speed of mist projection granulating is 1ml/min, and the air pressure of mist projection granulating is 0.4bar, the flow rate of mist projection granulating is 40rpm, and the product obtained by mist projection granulating carries out lyophilization, and cryodesiccated temperature is-20 DEG C, the cryodesiccated time is 24h, obtains the second product 2.
Defat: the second product 2, after defat, obtains third product 2.In the present embodiment, the temperature of defat is 500 DEG C, and the time of defat is 5h.
Sintering, after third product 2 sintering, obtains product 2.In the embodiment of the present invention, the method for sintering is HIP sintering, and sintering pressure is 80MPa.
Embodiment 3
Supending: weigh ceramic powder 88g, dispersant 3g and citric acid 3g, it is dissolved in 100g water, add lubricant solution 10ml, adhesive solution 10ml, after mixing, pH to 6 is regulated with ammonia, adopt high pure and ultra-fine translucent alumina abrading-ball as ball-milling medium ball milling 24h, the particle diameter granule more than 2 μm is removed by settling, obtains the first product 3.In the present embodiment, ceramic powder be purity more than 99%, particle diameter be 10-7The magnesium oxide of m, dispersant is the mixture of DolapixCE64 and Darvan821a, and lubricant solution is the Aqueous Solutions of Polyethylene Glycol of 0.3g/ml, and dispersant is the polyvinyl alcohol water solution of 0.3g/ml.
Spray chilling: the first product 3 is placed in beaker, adopts magnetic stirrer stirring, and stir speed (S.S.) is 300rpm.Then carrying out mist projection granulating, the pump speed of mist projection granulating is 2ml/min, and the air pressure of mist projection granulating is 0.4bar, the flow rate of mist projection granulating is 50rpm, and the product obtained by mist projection granulating carries out lyophilization, and cryodesiccated temperature is-20 DEG C, the cryodesiccated time is 24h, obtains the second product 3.
Defat: the second product 3, after defat, obtains third product 3.In the present embodiment, the temperature of defat is 500 DEG C, and the time of defat is 5h.
Sintering, after third product 3 sintering, obtains product 3.In the embodiment of the present invention, the method for sintering is discharge plasma sintering, and sintering pressure is 100MPa.
Embodiment 4
The product 1～3 embodiment 1～3 prepared does determination of light transmittance experiment with commercial clear pottery.
The light transmittance recording product 1 is 80%, and the light transmittance of product 2 is 85%, and the light transmittance of product 3 is 90%, and the light transmittance of commercial clear pottery is 60%.
Can being obtained from above, the product light transmittance that technical scheme provided by the invention prepares is higher than commercial like product, and transparency is good, can meet the society user demand for crystalline ceramics.
Embodiment 5
Product 1 is placed in basis of microscopic observation, see Fig. 2 at microscope in the microstructure of obtained product 1.As can be seen from Figure 2, product 1 even particle distribution, there is no gross blow hole.
Product 2 and product 3 are placed in basis of microscopic observation, the microstructure of Fig. 2 can be similar to, do not repeat them here.
In sum, the invention provides a kind of crystalline ceramics, the raw material of described crystalline ceramics includes: ceramic powder, lubricant, binding agent, dispersant and citric acid.Present invention also offers the preparation method including one described crystalline ceramics of any of the above, described preparation method includes: step one, supending, after ceramic powder, lubricant aqueous solution, adhesive solution, dispersant and citric acid mixing, regulate pH to 6, settle after ball milling, obtain the first product；Step 2, spray chilling: after described first product agitated, mist projection granulating successively and lyophilization, obtain the second product；Step 3, defat: described second product, after defat, obtains third product；Step 4, sintering, after described third product sintering, obtain product.Present invention also offers and include one described crystalline ceramics of any of the above or the application in crystalline ceramics parts of one the described preparation method of any of the above.By the product that technical scheme provided by the present invention prepares, transparency is good, and light transmittance is high, can meet the society user demand for crystalline ceramics.Meanwhile, by the product that technical scheme provided by the present invention prepares, the advantage that also there is even particle distribution, do not have gross blow hole.
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a crystalline ceramics, it is characterised in that the raw material of described crystalline ceramics includes: ceramic powder, lubricant, binding agent, dispersant and citric acid.
2. crystalline ceramics according to claim 1, it is characterised in that in mass parts, the raw material of described crystalline ceramics includes: ceramic powder 84～94 parts, lubricant 1.5～4 parts, binding agent 1.5～4 parts, dispersant 1.5～4 parts and citric acid 1.5～4 parts.
3. crystalline ceramics according to claim 1, it is characterised in that the purity of described ceramic powder is more than 99.9%, and the particle diameter of described ceramic powder is 10-7M, described ceramic powder is selected from: the one in aluminium oxide, yittrium oxide, magnesium aluminate spinel, aluminium nitride, A Long and calcium fluoride.
4. crystalline ceramics according to claim 1, it is characterised in that described lubricant is Polyethylene Glycol, described binding agent is polyvinyl alcohol.
5. the preparation method of the crystalline ceramics included described in Claims 1-4 any one, it is characterised in that described preparation method includes:
Step one, supending, after ceramic powder, lubricant aqueous solution, adhesive solution, dispersant and citric acid mixing, regulate pH to 6, settle, obtain the first product after ball milling；
Step 2, spray chilling: after described first product agitated, mist projection granulating successively and lyophilization, obtain the second product；
Step 3, defat: after described second product defat, obtain third product；
Step 4, sintering, after described third product sintering, obtain product.
6. preparation method according to claim 5, it is characterized in that, the concentration of described lubricant aqueous solution is 0.2～0.4g/ml, the concentration of described adhesive solution is 0.2～0.3g/ml, the medium of described ball milling is high pure and ultra-fine translucent alumina abrading-ball, the time of described ball milling is 24h, and the radius of the granule that described sedimentation obtains is more than 2 μm.
7. preparation method according to claim 5, it is characterized in that, the speed of described stirring is 200～400rpm, the pump speed of described mist projection granulating is 1～3ml/min, the air pressure of described mist projection granulating is 0.4～0.6bar, the flow rate of described mist projection granulating is 40～60rpm, and described cryodesiccated temperature is-20 DEG C, and the described cryodesiccated time is 24h.
8. preparation method according to claim 5, it is characterised in that the temperature of described defat is 500 DEG C, the time of described defat is 5h.
9. preparation method according to claim 5, it is characterised in that the method for described sintering is: the one of hot pressing, air pressure, high temperature insostatic pressing (HIP) or discharge plasma sintering, described sintering pressure is 10～100Pa.
10. the application in crystalline ceramics parts of the preparation method described in the crystalline ceramics included described in Claims 1-4 any one or claim 5 to 9 any one.
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| CN110981528A (en) * | 2019-12-06 | 2020-04-10 | 西安交通大学 | Directional porous aluminum nitride ceramic and rapid preparation method thereof |
| CN111960465A (en) * | 2020-08-13 | 2020-11-20 | 厦门厦瑞博科技有限公司 | Spherical ZrO2Method for preparing powder |
| CN116514537A (en) * | 2022-11-02 | 2023-08-01 | 中国科学院上海硅酸盐研究所 | Preparation method of high-light-transmittance magnesia-alumina spinel transparent ceramic |
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| CN110981528B (en) * | 2019-12-06 | 2021-02-26 | 西安交通大学 | Directional porous aluminum nitride ceramic and rapid preparation method thereof |
| CN111960465A (en) * | 2020-08-13 | 2020-11-20 | 厦门厦瑞博科技有限公司 | Spherical ZrO2Method for preparing powder |
| CN116514537A (en) * | 2022-11-02 | 2023-08-01 | 中国科学院上海硅酸盐研究所 | Preparation method of high-light-transmittance magnesia-alumina spinel transparent ceramic |
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