Preparation method of CaCu3Ti4O12 ceramic

[0019] Embodiment 1: with high-purity 3.0414g CaCO 3 (>99%), 7.2514g CuO (>99%), 9.7074gTiO 2 (>99%) powder as the raw material, according to the CCTO stoichiometric ratio, mix 20g of material, ball mill in distilled water medium for 12h; dry and sieve the powder and pre-calcine at 960°C for 2h. Add 15.4ml ethanol, 0.25ml n-butanol and 0.36ml trioleic acid glyceride to the powder after pre-burning, then put into the nylon ball mill jar, and use ZrO 2 The ball is used as the grinding medium, and it is put into a planetary ball mill with a speed of 400rad/min for wet grinding for 23 hours; 0.9592g of polyethylene glycol, 1.0ml of dioctyl phthalate, and 1.3174g of polyethylene are added to the wet material that has been ground for 23 hours. Alcohol butyral and 0.24ml cyclohexane, and then ball milled for 20h at a speed of 350rad/min; pour the slurry into a small beaker and take out all the ZrO 2 Then pour the slurry into a casting machine with a clean and smooth glass plate, so that it moves at a constant speed on the glass ribbon to form a thin casting belt. The thickness of the cast is controlled by the cast blade, and the speed of movement also has a direct impact on the thickness of the thin strip; open the blowing equipment to dry for 12 hours, and then remove the film to obtain the cast green body, and the formed green The billet is cut into rectangular slices; then degumming is performed, and the degumming heating rate is controlled as follows: from room temperature to 100°C, 2°C/min, at 100°C for 1 hour; from 100°C to 550°C, 1°C/min, at 550°C Keep it warm for 2 hours to ensure that the organic matter can be completely removed, create conditions for firing and make the green body obtain a certain mechanical strength; sinter the green body after debinding treatment at 1025°C, and control the sintering heating rate: from room temperature to the required sintering Temperature 1050°C, 3°C/min; 1025°C to 960°C, 4°C/min, then cool with the furnace.

[0020] Embodiment 2: with high-purity 3.344g CaCO 3 (>99%), 7.9765g CuO (>99%), 10.6788gTiO 2 (>99%) powder as the raw material, according to the CCTO stoichiometric ratio of 22g material, ball milled in distilled water medium for 12h; the dried and sieved powder was pre-fired at 960°C for 2h. Add 15.48ml ethanol, 0.3ml n-butanol and 0.4ml triolein to the powder after pre-burning, then put it into a nylon ball mill jar, and use ZrO 2 The ball is used as the grinding medium, and it is put into a planetary ball mill with a speed of 400rad/min for wet grinding for 20 hours; 0.960g of polyethylene glycol, 0.997ml of dioctyl phthalate, and 1.321g of polyethylene are added to the wet material that has been ground for 20 hours. Alcohol butyral and 0.28ml cyclohexane, and then ball milled for 20h at a speed of 400rad/min; pour the slurry into a small beaker and take out all the ZrO 2Then pour the slurry into a casting machine with a clean and smooth glass plate, so that it moves at a constant speed on the glass ribbon to form a thin casting belt. The thickness of the cast is controlled by the cast blade, and the speed of movement also has a direct impact on the thickness of the thin strip; open the blowing equipment to dry for 12 hours, and then remove the film to obtain the cast green body, and the formed green The billet is cut into rectangular slices; then degumming is performed, and the degumming heating rate is controlled as follows: from room temperature to 100°C, 2°C/min, at 100°C for 1 hour; from 100°C to 550°C, 1°C/min, at 550°C Keep it warm for 2 hours to ensure that the organic matter can be completely removed, create conditions for firing and make the green body obtain a certain mechanical strength; the green body after debinding treatment is sintered at 1050°C, and the sintering temperature rise rate is controlled: from room temperature to the required sintering Temperature 1050°C, 3°C/min; 1050°C to 960°C, 4°C/min, then cool with the furnace. from figure 1 It can be seen from the figure that it is relatively dense, the particles are evenly arranged and have clear prismatic boundaries, forming better polygonal particles, and the crystal shape is better, but the crystal grains are relatively small and there are small grain inclusions.

[0021] Embodiment 3: with high-purity 3.7561g CaCO 3 (>99%), 8.9555g CuO (>99%), 11.9886gTiO 2 (>99%) powder as the raw material, according to the CCTO stoichiometric ratio of 24.7g material, ball milled in distilled water medium for 10h; the dried and sieved powder was pre-fired at 960°C for 2h. ; Add 15.5ml ethanol, 0.4ml n-butanol and 0.4ml trioleic acid glyceride to the powder after pre-burning, then put into the nylon ball mill jar, and use ZrO 2 The ball is used as the grinding medium, put it into a planetary ball mill with a rotation speed of 400rad/min for 24 hours; add 0.9663g of polyethylene glycol, 0.99ml of dioctyl phthalate, and 1.34g of polyethylene to the wet material that has been ground for 24 hours Alcohol butyral and 0.3ml cyclohexane, and then ball milled for 20h at a speed of 400rad/min; pour the slurry into a small beaker and take out all the ZrO 2 Then pour the slurry into a casting machine with a clean and smooth glass plate, so that it moves at a constant speed on the glass ribbon to form a thin casting belt. The thickness of the cast is controlled by the cast blade, and the speed of movement also has a direct impact on the thickness of the thin strip; open the blowing equipment to dry for 12 hours, and then remove the film to obtain the cast green body, and the formed green The billet is cut into rectangular slices; then degumming is performed, and the degumming heating rate is controlled as follows: from room temperature to 100°C, 2°C/min, at 100°C for 1 hour; from 100°C to 550°C, 1°C/min, at 550°C Keep warm for 2 hours to ensure that the organic matter can be completely removed, create conditions for firing and make the green body obtain a certain mechanical strength; the green body after debinding treatment is sintered at 1075°C, and the sintering temperature rise rate is controlled: from room temperature to the required sintering Temperature 1750°C, 3°C/min; 1750°C to 960°C, 4°C/min, then cool with the furnace. from figure 2 It can be seen that the particles are obviously enlarged and the contact between particles is close.