阅读说明：本技术 一种氧化铝-二氧化锆复相陶瓷的凝胶注模方法 (Gel injection molding method of aluminum oxide-zirconium dioxide complex phase ceramic ) 是由 刘名剑 王征 于 2020-12-15 设计创作，主要内容包括：本发明属于陶瓷领域,具体涉及一种氧化铝-二氧化锆复相陶瓷的凝胶注模方法,包括：将氯化铝加入至无水乙醇中搅拌均匀,然后加入氧氯化锆低温超声分散形成混合液；将乙基纤维素加入至混合液中超声分散2-4h,得到分散醇液；将氨气与水蒸气共混形成混合气,并缓慢通入分散醇液中直至沉淀不再产生,得到悬浊分散液,然后减压蒸馏3-6h,得到粘稠浆料；将粘稠浆料注入至模具中恒温恒压反应形成干料,然后光照体系下恒温恒压反应2-4h,马弗炉烧结6-10h,得到氧化铝-二氧化锆复相陶瓷。本发明解决了现有凝胶注模工艺制备的陶瓷易剥落的问题,利用乙基纤维素作为粘合剂,实现粘稠的同时在压制过程中光降解,防止烧结过程中有机物致孔。(The invention belongs to the field of ceramics, and particularly relates to a gel injection molding method of an aluminum oxide-zirconium dioxide complex phase ceramic, which comprises the following steps: adding aluminum chloride into absolute ethyl alcohol, stirring uniformly, adding zirconium oxychloride, and performing low-temperature ultrasonic dispersion to form a mixed solution; adding ethyl cellulose into the mixed solution, and performing ultrasonic dispersion for 2-4h to obtain a dispersed alcohol solution; mixing ammonia gas and water vapor to form mixed gas, slowly introducing the mixed gas into the dispersed alcohol solution until no precipitate is generated, obtaining suspended dispersion liquid, and then distilling under reduced pressure for 3-6h to obtain viscous slurry; and injecting the viscous slurry into a mold to perform constant-temperature and constant-pressure reaction to form a dry material, performing constant-temperature and constant-pressure reaction for 2-4h under an illumination system, and sintering for 6-10h in a muffle furnace to obtain the aluminum oxide-zirconium dioxide composite ceramic. The invention solves the problem that the ceramic prepared by the existing gel casting process is easy to peel off, utilizes ethyl cellulose as an adhesive, realizes the light degradation in the pressing process while realizing the viscosity, and prevents the hole formation of organic matters in the sintering process.)

1. A gel injection molding method of alumina-zirconium dioxide complex phase ceramics is characterized in that: the method comprises the following steps:

step 1, adding aluminum chloride into absolute ethyl alcohol, uniformly stirring, adding zirconium oxychloride, and performing low-temperature ultrasonic dispersion to form a mixed solution;

step 2, adding ethyl cellulose into the mixed solution, and performing ultrasonic dispersion for 2-4 hours to obtain a dispersed alcohol solution;

step 3, mixing ammonia gas and water vapor to form mixed gas, slowly introducing the mixed gas into the dispersed alcohol solution until no precipitate is generated, obtaining suspended dispersion liquid, and then distilling under reduced pressure for 3-6 hours to obtain viscous slurry;

and 4, injecting the viscous slurry into a mold to perform constant-temperature and constant-pressure reaction to form a dry material, performing constant-temperature and constant-pressure reaction for 2-4h under an illumination system, and sintering for 6-10h in a muffle furnace to obtain the aluminum oxide-zirconium dioxide composite ceramic.

2. The method of gel-casting an alumina-zirconia composite ceramic according to claim 1, wherein: the concentration of the aluminum chloride in the step 1 in the absolute ethanol is 100-200g/L, and the stirring speed is 1000-2000 r/min.

3. The method of gel-casting an alumina-zirconia composite ceramic according to claim 1, wherein: the adding amount of the zirconium oxychloride in the step 1 is 20-40% of the mass of the aluminum chloride, the low-temperature ultrasonic temperature is 5-10 ℃, and the ultrasonic frequency is 60-80 kHz.

4. The method of gel-casting an alumina-zirconia composite ceramic according to claim 1, wherein: the adding amount of the ethyl cellulose in the step 2 is 50-80% of the mass of the aluminum chloride, the ultrasonic dispersion temperature is 20-30 ℃, and the ultrasonic frequency is 90-120 kHz.

5. The method of gel-casting an alumina-zirconia composite ceramic according to claim 1, wherein: the introduction amount of the ammonia gas and the steam in the step 3 is 1:1-1.5, the temperature is 100-.

6. The method of gel-casting an alumina-zirconia composite ceramic according to claim 1, wherein: the pressure of the reduced pressure distillation in the step 3 is 70-80% of the standard atmospheric pressure, and the temperature is 100-120 ℃.

7. The method of gel-casting an alumina-zirconia composite ceramic according to claim 1, wherein: the temperature of the constant temperature and the constant pressure in the step 4 is 100-120 ℃, and the pressure is 0.2-0.4 MPa.

8. The method of gel-casting an alumina-zirconia composite ceramic according to claim 1, wherein: the illumination intensity in the step 4 is 10-20W/cm2, the pressure is 0.2-0.5MPa, and the temperature is 180-250 ℃.

9. The method of gel-casting an alumina-zirconia composite ceramic according to claim 1, wherein: the temperature rise speed of the sintering in the step 4 is 20-50 ℃/min, and the sintering temperature is 1300-1500 ℃.

Technical Field

The invention belongs to the field of ceramics, and particularly relates to a gel injection molding method of an aluminum oxide-zirconium dioxide complex phase ceramic.

Background

Gel casting is a new forming technology for ceramic products with complex shapes, which has been developed in recent years, and has received much attention. Briefly, this technique consists of three basic steps. Firstly, preparing ceramic slurry with high solid content and low viscosity by taking a water-soluble organic monomer as a crosslinking medium; then injecting the slurry into a mould and fully curing; finally, the green body is demolded, dried and sintered. Compared with the traditional forming process, the gel casting technology has many advantages, such as near net size forming, forming of products with complex shapes, simple operation, good mechanical properties of green bodies and the like.

Many organic materials that can produce cross-linking can be used for gel casting, such as acrylic acid, polyvinyl alcohol, proteins, etc. Among the numerous organic monomers, Acrylamide (AM) and methylenebisacrylamide (MBAM) systems are widely used for water-based gel injection molding. In the system, the lamella peeling phenomenon is easy to generate on the surface of the formed green body.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a gel injection molding method of an aluminum oxide-zirconium dioxide complex phase ceramic, which solves the problem that the ceramic prepared by the existing gel injection molding process is easy to peel off, and takes ethyl cellulose as a binder to realize the purposes of thickening, photodegradation in the pressing process and pore-forming of organic matters in the sintering process.

In order to achieve the technical purpose, the technical scheme of the invention is as follows:

a gel-casting method of alumina-zirconium dioxide complex phase ceramics comprises the following steps:

step 1, adding aluminum chloride into absolute ethyl alcohol, uniformly stirring, adding zirconium oxychloride, and performing low-temperature ultrasonic dispersion to form a mixed solution; the concentration of aluminum chloride in the absolute ethyl alcohol is 100-200g/L, the stirring speed is 1000-2000r/min, the adding amount of the zirconium oxychloride is 20-40% of the mass of the aluminum chloride, the low-temperature ultrasonic temperature is 5-10 ℃, and the ultrasonic frequency is 60-80 kHz;

step 2, adding ethyl cellulose into the mixed solution, and performing ultrasonic dispersion for 2-4 hours to obtain a dispersed alcohol solution; the adding amount of the ethyl cellulose is 50-80% of the mass of the aluminum chloride, the ultrasonic dispersion temperature is 20-30 ℃, and the ultrasonic frequency is 90-120 kHz;

step 3, mixing ammonia gas and water vapor to form mixed gas, slowly introducing the mixed gas into the dispersed alcohol solution until no precipitate is generated, obtaining suspended dispersion liquid, and then distilling under reduced pressure for 3-6 hours to obtain viscous slurry; the introduction amount of the ammonia and the water vapor is 1:1-1.5, the temperature is 100-110 ℃, the slow introduction speed is 5-10mL/min, the pressure of the reduced pressure distillation is 70-80% of the standard atmospheric pressure, and the temperature is 100-120 ℃;

step 4, injecting the viscous slurry into a mold to perform constant-temperature and constant-pressure reaction to form a dry material, performing constant-temperature and constant-pressure reaction for 2-4h under a lighting system, and sintering for 6-10h in a muffle furnace to obtain the alumina-zirconium dioxide composite ceramic; the temperature of the constant temperature and the constant pressure is 100-120 ℃, and the pressure is 0.2-0.4 MPa; the illumination intensity is 10-20W/cm2, the pressure is 0.2-0.5MPa, and the temperature is 180-250 ℃; the temperature rise speed of the sintering is 20-50 ℃/min, and the sintering temperature is 1300-1500 ℃.

From the above description, it can be seen that the present invention has the following advantages:

1. the invention solves the problem that the ceramic prepared by the existing gel casting process is easy to peel off, utilizes ethyl cellulose as an adhesive, realizes the light degradation in the pressing process while realizing the viscosity, and prevents the hole formation of organic matters in the sintering process.

2. The invention uses absolute ethyl alcohol as solvent, realizes anhydrous preparation, solves the problem of agglomeration of the subsequent zirconium dioxide, and effectively promotes the nanoscale uniform dispersion of the zirconium dioxide and the aluminum oxide.

3. The invention adopts a double constant temperature and pressure treatment mode, reduces the solvent, effectively converts aluminum hydroxide and zirconium hydroxide into aluminum oxide and zirconium dioxide in situ, effectively prevents the materials from agglomerating, and greatly improves the combination uniformity of the aluminum oxide and the zirconium dioxide.

Detailed Description

A specific embodiment of the present invention will be described in detail with reference to examples, but the present invention is not limited to the claims.

Example 1

A gel-casting method of alumina-zirconium dioxide complex phase ceramics comprises the following steps:

step 1, adding aluminum chloride into absolute ethyl alcohol, uniformly stirring, adding zirconium oxychloride, and performing low-temperature ultrasonic dispersion to form a mixed solution; the concentration of aluminum chloride in the absolute ethyl alcohol is 100-200g/L, the stirring speed is 1000-2000r/min, the adding amount of the zirconium oxychloride is 20-40% of the mass of the aluminum chloride, the low-temperature ultrasonic temperature is 5-10 ℃, and the ultrasonic frequency is 60-80 kHz;

step 2, adding ethyl cellulose into the mixed solution, and performing ultrasonic dispersion for 2-4 hours to obtain a dispersed alcohol solution; the adding amount of the ethyl cellulose is 50-80% of the mass of the aluminum chloride, the ultrasonic dispersion temperature is 20-30 ℃, and the ultrasonic frequency is 90-120 kHz;

step 3, mixing ammonia gas and water vapor to form mixed gas, slowly introducing the mixed gas into the dispersed alcohol solution until no precipitate is generated, obtaining suspended dispersion liquid, and then distilling under reduced pressure for 3-6 hours to obtain viscous slurry; the introduction amount of the ammonia and the water vapor is 1:1-1.5, the temperature is 100-110 ℃, the slow introduction speed is 5-10mL/min, the pressure of the reduced pressure distillation is 70-80% of the standard atmospheric pressure, and the temperature is 100-120 ℃;

step 4, injecting the viscous slurry into a mold to perform constant-temperature and constant-pressure reaction to form a dry material, performing constant-temperature and constant-pressure reaction for 2-4h under a lighting system, and sintering for 6-10h in a muffle furnace to obtain the alumina-zirconium dioxide composite ceramic; the temperature of the constant temperature and the constant pressure is 100-120 ℃, and the pressure is 0.2-0.4 MPa; the illumination intensity is 10-20W/cm2, the pressure is 0.2-0.5MPa, and the temperature is 180-250 ℃; the temperature rise speed of the sintering is 20-50 ℃/min, and the sintering temperature is 1300-1500 ℃.

The bending strength of the complex phase ceramic prepared by the embodiment can reach 290MPa, the sintering density can reach 98.5%, and the mechanical property is good.

Example 2

A gel-casting method of alumina-zirconium dioxide complex phase ceramics comprises the following steps:

step 1, adding aluminum chloride into absolute ethyl alcohol, uniformly stirring, adding zirconium oxychloride, and performing low-temperature ultrasonic dispersion to form a mixed solution; the concentration of aluminum chloride in the absolute ethyl alcohol is 100-200g/L, the stirring speed is 1000-2000r/min, the adding amount of the zirconium oxychloride is 20-40% of the mass of the aluminum chloride, the low-temperature ultrasonic temperature is 5-10 ℃, and the ultrasonic frequency is 60-80 kHz;

step 2, adding ethyl cellulose into the mixed solution, and performing ultrasonic dispersion for 2-4 hours to obtain a dispersed alcohol solution; the adding amount of the ethyl cellulose is 50-80% of the mass of the aluminum chloride, the ultrasonic dispersion temperature is 20-30 ℃, and the ultrasonic frequency is 90-120 kHz;

step 3, mixing ammonia gas and water vapor to form mixed gas, slowly introducing the mixed gas into the dispersed alcohol solution until no precipitate is generated, obtaining suspended dispersion liquid, and then distilling under reduced pressure for 3-6 hours to obtain viscous slurry; the introduction amount of the ammonia and the water vapor is 1:1-1.5, the temperature is 100-110 ℃, the slow introduction speed is 5-10mL/min, the pressure of the reduced pressure distillation is 70-80% of the standard atmospheric pressure, and the temperature is 100-120 ℃;

step 4, injecting the viscous slurry into a mold to perform constant-temperature and constant-pressure reaction to form a dry material, performing constant-temperature and constant-pressure reaction for 2-4h under a lighting system, and sintering for 6-10h in a muffle furnace to obtain the alumina-zirconium dioxide composite ceramic; the temperature of the constant temperature and the constant pressure is 100-120 ℃, and the pressure is 0.2-0.4 MPa; the illumination intensity is 10-20W/cm2, the pressure is 0.2-0.5MPa, and the temperature is 180-250 ℃; the temperature rise speed of the sintering is 20-50 ℃/min, and the sintering temperature is 1300-1500 ℃.

The bending strength of the complex phase ceramic prepared by the embodiment can reach 310MPa, the sintering density can reach 98.8 percent, and the complex phase ceramic has good mechanical property.

Example 3

A gel-casting method of alumina-zirconium dioxide complex phase ceramics comprises the following steps:

step 1, adding aluminum chloride into absolute ethyl alcohol, uniformly stirring, adding zirconium oxychloride, and performing low-temperature ultrasonic dispersion to form a mixed solution; the concentration of aluminum chloride in the absolute ethyl alcohol is 100-200g/L, the stirring speed is 1000-2000r/min, the adding amount of the zirconium oxychloride is 20-40% of the mass of the aluminum chloride, the low-temperature ultrasonic temperature is 5-10 ℃, and the ultrasonic frequency is 60-80 kHz;

step 2, adding ethyl cellulose into the mixed solution, and performing ultrasonic dispersion for 2-4 hours to obtain a dispersed alcohol solution; the adding amount of the ethyl cellulose is 50-80% of the mass of the aluminum chloride, the ultrasonic dispersion temperature is 20-30 ℃, and the ultrasonic frequency is 90-120 kHz;

step 3, mixing ammonia gas and water vapor to form mixed gas, slowly introducing the mixed gas into the dispersed alcohol solution until no precipitate is generated, obtaining suspended dispersion liquid, and then distilling under reduced pressure for 3-6 hours to obtain viscous slurry; the introduction amount of the ammonia and the water vapor is 1:1-1.5, the temperature is 100-110 ℃, the slow introduction speed is 5-10mL/min, the pressure of the reduced pressure distillation is 70-80% of the standard atmospheric pressure, and the temperature is 100-120 ℃;

step 4, injecting the viscous slurry into a mold to perform constant-temperature and constant-pressure reaction to form a dry material, performing constant-temperature and constant-pressure reaction for 2-4h under a lighting system, and sintering for 6-10h in a muffle furnace to obtain the alumina-zirconium dioxide composite ceramic; the temperature of the constant temperature and the constant pressure is 100-120 ℃, and the pressure is 0.2-0.4 MPa; the illumination intensity is 10-20W/cm2, the pressure is 0.2-0.5MPa, and the temperature is 180-250 ℃; the temperature rise speed of the sintering is 20-50 ℃/min, and the sintering temperature is 1300-1500 ℃.

The bending strength of the complex phase ceramic prepared by the embodiment can reach 300MPa, the sintering density can reach 98.6 percent, and the complex phase ceramic has good mechanical property.

In summary, the invention has the following advantages:

1. the invention solves the problem that the ceramic prepared by the existing gel casting process is easy to peel off, utilizes ethyl cellulose as an adhesive, realizes the light degradation in the pressing process while realizing the viscosity, and prevents the hole formation of organic matters in the sintering process.

2. The invention uses absolute ethyl alcohol as solvent, realizes anhydrous preparation, solves the problem of agglomeration of the subsequent zirconium dioxide, and effectively promotes the nanoscale uniform dispersion of the zirconium dioxide and the aluminum oxide.

3. The invention adopts a double constant temperature and pressure treatment mode, reduces the solvent, effectively converts aluminum hydroxide and zirconium hydroxide into aluminum oxide and zirconium dioxide in situ, effectively prevents the materials from agglomerating, and greatly improves the combination uniformity of the aluminum oxide and the zirconium dioxide.

It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.