CN109095916B - Method for preparing YAG transparent ceramic by SPS sintering - Google Patents
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Abstract
The invention discloses a method for preparing YAG transparent ceramic by SPS sintering, which comprises the steps of calcining, burdening, ball-milling, drying, sieving and the like to obtain powder, then filling the powder into a mould, then placing the mould into an SPS sintering furnace for SPS sintering, and controlling parameters such as temperature rise rate, pressure rise temperature, pressure rise rate and the like in the sintering stage to obtain the YAG transparent ceramic with good optical quality and high strength. According to the invention, the pressure-increasing temperature and the pressure-increasing rate are accurately controlled during SPS sintering, and abnormal growth of YAG ceramic grains in the sintering stage can be effectively inhibited, so that residual pores in the ceramic are effectively eliminated, no sintering aid is required to be added, the sintering time is short, the sintering temperature is low, and the energy-saving and environment-friendly effects are achieved.
Description
Technical Field
The invention belongs to the technical field of transparent ceramic preparation, and particularly relates to a method for preparing YAG transparent ceramic by SPS sintering.
Background
YAG transparent ceramics have the characteristics of high strength, strong corrosion resistance and small high-temperature creep deformation, and have good permeability to visible light and infrared light, and the properties enable the YAG transparent ceramics to be widely applied to laser matrix materials and also can be used for manufacturing high-temperature visible light and infrared windows. Therefore, the YAG transparent ceramic with high optical quality has wide application prospect and is one of the hot spots of material science research.
In the sintering process of YAG transparent ceramics, the application of vacuum sintering is common, but the vacuum sintering temperature is very high, generally more than 1700 ℃, and the required heat preservation time is very long, often more than 8 hours, sometimes even about 40-50 hours. In addition, the ceramic prepared by vacuum sintering is often large in grain size, about 10-50 μm, poor in mechanical property and poor in thermal shock resistance, and is difficult to meet the current commercial requirements.
SPS sintering (also called spark plasma sintering) is used as a novel ceramic sintering mode, and has the characteristics of high temperature rise speed, high efficiency, short time, energy conservation, environmental protection and the like, and the prepared ceramic has small crystal grain size of only 20-200 nm and excellent mechanical properties. However, there are many problems in the SPS sintering process, such as that it is difficult to precisely control the grain growth rate and the pore removal rate of the ceramic due to the high SPS sintering speed and the high densification rate. When the temperature for boosting is not reasonably set, high-strength pressure can be generated at the joint of the particles, so that the particles are tightly connected, the abnormal growth of the grain size is caused, the increase of closed pores is caused, and the optical quality of the ceramic is poor. However, in the current common solution, a sintering aid (MgO, TEOS, etc.) is added in the previous burdening process to regulate the densification process of the ceramic, but the use of the sintering aid often causes abnormal growth of ceramic grains, resulting in uneven size of the sintered ceramic grains, and simultaneously, the problems of mechanical property and heat conductivity reduction are accompanied, and thus the commercial application is difficult to meet.
Disclosure of Invention
The invention aims to provide a method for preparing YAG transparent ceramic by SPS sintering, which does not need to add sintering aid, and the YAG transparent ceramic after sintering has uniform size and high transmittance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for preparing YAG transparent ceramics by SPS sintering,
firstly, respectively calcining yttrium oxide and alumina powder, then carrying out processes of material preparation, ball milling, drying, sieving and the like to obtain uniformly mixed yttrium oxide and alumina powder, then filling the powder into a mold of an SPS sintering furnace, setting parameters such as pressure, temperature, pressure rise rate, temperature rise rate and the like, and then carrying out SPS sintering on a biscuit in the mold. Then, removing oxygen vacancies generated in the SPS sintering of the YAG ceramic by an annealing process, and finally grinding and polishing to obtain the YAG transparent ceramic with excellent optical quality. The method specifically comprises the following steps:
1) and (3) calcining: respectively calcining yttrium oxide and aluminum oxide powder to remove moisture and impurities in the powder;
2) ball milling: pouring the calcined yttrium oxide and aluminum oxide powder into a ball milling tank, wherein the molar ratio of yttrium ions to aluminum ions is 3:5, adding alcohol and grinding balls into the ball milling tank, and carrying out ball milling;
3) drying and sieving: putting the ball-milled slurry into an oven for drying, and sieving the dried powder;
4) and (3) sintering: and pouring the sieved powder into a mold, and then placing the mold into an SPS sintering furnace for SPS sintering, wherein the sintering pressure is kept unchanged after rising to P1, and the sintering pressure P1 is 15-25 MPa. When the sintering temperature reaches T1, the sintering pressure is increased from P1 to P2, the sintering temperature T1 is 1250-1280 ℃, and the sintering pressure P2 is 85-90 MPa. Stopping heating when the sintering temperature reaches T2, keeping the sintering pressure at P2 constant, keeping the sintering temperature at T2 to 1330 ℃, keeping the temperature at T2 for 2 to 4 hours, wherein the whole heating rate is 100 to 125 ℃/min, and the pressure increasing rate is 60 to 80 MPa/min;
5) annealing: placing the sintered ceramic in a muffle furnace, and annealing in air atmosphere;
6) grinding and polishing: and grinding and polishing the double surfaces of the annealed ceramic wafer to 1-3 mm to obtain the YAG transparent ceramic.
Preferably, in the step (1), the calcination temperature of the yttrium oxide powder is 900-950 ℃, the heat preservation time is 2-5 hours, the calcination temperature of the aluminum oxide powder is 520-560 ℃, and the heat preservation time is 2-5 hours.
Preferably, in the step (2), the grinding balls are alumina balls, and the ball-to-material ratio is 2-4: 1, the volume ratio of the alcohol addition to the ball milling tank is 0.3-0.5, and the ball milling rotating speed is 160-200 rpm.
Preferably, in the step (3), the drying temperature is 40-60 ℃, and the drying time is 12-36 h.
Preferably, the sieve in step (3) has a sieve mesh size of 100-200 meshes, and the sieving frequency is 3-5 times.
Preferably, the diameter of the die in the step (4) is 15-25 mm.
Preferably, in the step (5), the annealing temperature is 1100-1250 ℃, and the heat preservation time is 10-20 h.
Compared with the prior art, the invention has the following beneficial effects:
(1) the YAG transparent ceramic is prepared by adopting a solid phase method, and the temperature rise rate, the pressure rise rate and the pressure rise temperature are accurately controlled in the SPS sintering stage, so that the pore residue caused by abnormal growth of crystal grains of the YAG transparent ceramic in the sintering stage is avoided, and the optical quality of the transparent ceramic is greatly improved.
(2) Compared with the traditional ceramic preparation method, the method does not need to add any sintering aid, effectively solves the problems of abnormal growth of crystal grains, reduction of heat conductivity and mechanical properties and the like, and can greatly promote the preparation and research and development of the YAG transparent ceramic.
(3) Compared with the traditional vacuum sintering, the method has the advantages of short SPS sintering time, low sintering temperature, more energy conservation and environmental protection, and great promotion effect on the batch production of YAG ceramics.
Drawings
FIG. 1 is an XRD pattern of a ceramic sample prepared according to example 1 of the present invention;
FIG. 2 is a pictorial representation of a ceramic sample made in accordance with example 1 of the present invention;
FIG. 3 is a graph showing the transmittance of the ceramic sample obtained in example 1 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
In the following examples, the purity of the yttrium oxide powder used was greater than 99.9%, and the purity of the aluminum oxide powder was greater than 99.9%.
Example 1
Respectively calcining yttrium oxide and aluminum oxide powder to remove moisture and impurities in the powder, wherein the calcining temperature of the yttrium oxide powder is 900 ℃, the heat preservation time is 5 hours, the calcining temperature of the aluminum oxide powder is 520 ℃, and the heat preservation time is 5 hours. And then pouring the calcined yttrium oxide and the alumina powder into a ball milling tank, wherein the molar ratio of yttrium ions to aluminum ions is ensured to be 3: 5. Then adding alcohol and high-purity alumina grinding balls into the ball milling tank, and carrying out ball milling. Wherein, the ball material ratio is 2: 1, the volume ratio of the alcohol addition to the ball milling tank is 0.3, and the ball milling rotating speed is 160 rpm.
And (3) putting the ball-milled slurry into an oven for drying at 40 ℃ for 36 h. And (3) sieving the dried powder, wherein the sieve is a 100-mesh sieve, and the sieving frequency is 3 times.
The sieved powder was poured into a mold (diameter 15mm) and prepared for sintering. Wherein the sintering pressure is kept unchanged after the sintering pressure is increased to P1, and the sintering pressure P1 is 15 MPa. When the sintering temperature reaches the sintering temperature T1, the sintering pressure is increased from P1 to P2, the sintering temperature T1 is 1250 ℃, and the sintering pressure P2 is 85 MPa. And when the sintering temperature reaches the sintering temperature T2, stopping heating, keeping the sintering pressure at P2 constant, keeping the sintering temperature at T2 at 1300 ℃, keeping the temperature at T2 for 2h, wherein the whole heating rate is 100 ℃/min, and the pressure increasing rate is 60 MPa/min.
And (3) placing the sintered ceramic in a muffle furnace, and annealing in an air atmosphere at 1100 ℃ for 20 h.
And (3) carrying out double-sided grinding and polishing on the annealed ceramic wafer to 1mm to obtain YAG transparent ceramic, wherein a XRD (X-ray diffraction) diagram of a ceramic sample is shown in figure 1, and the sample is a YAG phase, has no other impurity phase and has high purity. Fig. 2 is a real image of the ceramic sample, the lower font content can be clearly seen through the ceramic, and the optical quality of the ceramic sample is high. FIG. 3 is a graph of the transmittance of the ceramic sample, showing that the transmittance of the ceramic at 800nm reached 83.5%, which is very close to the theoretical transmittance. As no sintering aid is added, the mechanical property of the ceramic sample is excellent, and the bending strength of the ceramic sample is 362MPa and the fracture toughness reaches 2.2 MPa.ml/2Can meet the requirements of the current market on optical and mechanical properties.
Example 2
Respectively calcining yttrium oxide and aluminum oxide powder to remove moisture and impurities in the powder, wherein the calcining temperature of the yttrium oxide powder is 930 ℃, the heat preservation time is 3 hours, the calcining temperature of the aluminum oxide powder is 540 ℃, and the heat preservation time is 3 hours. And then pouring the calcined yttrium oxide and the alumina powder into a ball milling tank, wherein the molar ratio of yttrium ions to aluminum ions is ensured to be 3: 5. Then adding alcohol and high-purity alumina grinding balls into the ball milling tank, and carrying out ball milling. Wherein, the ball material ratio is 3: 1, the volume ratio of the alcohol addition to the ball milling tank is 0.4, and the ball milling rotating speed is 180 rpm.
And (3) putting the ball-milled slurry into an oven for drying at the drying temperature of 50 ℃ for 24 h. And (3) sieving the dried powder, wherein the sieve is 200 meshes in the specification of a sieve, and the sieving frequency is 4 times.
The sieved powder was poured into a mold (diameter 20mm) and prepared for sintering. Wherein the sintering pressure is kept unchanged after the sintering pressure is increased to P1, and the sintering pressure P1 is 20 MPa. When the sintering temperature reaches the sintering temperature T1, the sintering pressure is increased from P1 to P2, the sintering temperature T1 is 1265 ℃, and the sintering pressure P2 is 88 MPa. And when the sintering temperature reaches the sintering temperature T2, stopping heating, keeping the sintering pressure at P2 constant, keeping the sintering temperature at T2 ℃ and keeping the temperature at T2 for 3h, wherein the whole heating rate is 110 ℃/min, and the pressure increasing rate is 70 MPa/min.
And (3) placing the sintered ceramic in a muffle furnace, and annealing in an air atmosphere at the annealing temperature of 1200 ℃ for 15 h.
And (4) carrying out double-sided grinding and polishing on the annealed ceramic wafer to 2mm to obtain the YAG transparent ceramic.
Through tests, the bending strength of the ceramic sample is 354MPa, and the fracture toughness reaches 2.2 MPa.ml/2。
Example 3
Respectively calcining yttrium oxide and aluminum oxide powder to remove moisture and impurities in the powder, wherein the calcining temperature of the yttrium oxide powder is 950 ℃, the heat preservation time is 2 hours, the calcining temperature of the aluminum oxide powder is 560 ℃, and the heat preservation time is 2 hours. And then pouring the calcined yttrium oxide and the alumina powder into a ball milling tank, wherein the molar ratio of yttrium ions to aluminum ions is ensured to be 3: 5. Then adding alcohol and high-purity alumina grinding balls into the ball milling tank, and carrying out ball milling. Wherein, the ball material ratio is 4: 1, the volume ratio of the alcohol addition to the ball milling tank is 0.5, and the ball milling rotating speed is 200 rpm.
And (3) putting the ball-milled slurry into an oven for drying at the drying temperature of 60 ℃ for 12 h. And (3) sieving the dried powder, wherein the sieve is 200 meshes in the specification of a sieve, and the sieving frequency is 5 times.
The sieved powder was poured into a mold (diameter 25mm) and prepared for sintering. Wherein the sintering pressure is kept unchanged after the sintering pressure is increased to P1, and the sintering pressure P1 is 25 MPa. When the sintering temperature reaches the sintering temperature T1, the sintering pressure is increased from P1 to P2, the sintering temperature T1 is 1280 ℃, and the sintering pressure P2 is 90 MPa. And when the sintering temperature reaches the sintering temperature T2, stopping heating, keeping the sintering pressure at P2, keeping the sintering temperature at T2 of 1330 ℃, keeping the temperature at T2 for 4h, wherein the whole heating rate is 125 ℃/min, and the pressure increasing rate is 80 MPa/min.
And (3) placing the sintered ceramic in a muffle furnace, and annealing in air atmosphere at 1250 ℃ for 10 h.
And grinding and polishing the double surfaces of the annealed ceramic wafer to 3mm to obtain the YAG transparent ceramic.
Through tests, the bending strength of the ceramic sample is 347MPa, and the fracture toughness reaches 2.1 MPa.ml/2。
Claims (7)
1. A method for preparing YAG transparent ceramic by SPS sintering is characterized in that: the method comprises the following steps:
1) and (3) calcining: respectively calcining yttrium oxide and aluminum oxide powder to remove moisture and impurities in the powder;
2) ball milling: pouring the calcined yttrium oxide and aluminum oxide powder into a ball milling tank, ensuring the molar ratio of yttrium ions to aluminum ions to be 3:5, adding alcohol and grinding balls into the ball milling tank, and carrying out ball milling;
3) drying and sieving: putting the ball-milled slurry into an oven for drying, and sieving the dried powder;
4) and (3) sintering: pouring the sieved powder into a mold, and then placing the mold into an SPS sintering furnace for SPS sintering, wherein the sintering pressure is kept unchanged after rising to P1, and the sintering pressure P1 is 15-25 Mpa; when the sintering temperature reaches the sintering temperature T1, the sintering pressure is increased from P1 to P2, the sintering temperature T1 is 1250-1280 ℃, and the sintering pressure P2 is 85-90 MPa; stopping heating when the sintering temperature reaches T2, keeping the sintering pressure at P2 constant, keeping the sintering temperature at T2 to 1330 ℃, keeping the temperature at T2 for 2 to 4 hours, wherein the whole heating rate is 100 to 125 ℃/min, and the pressure increasing rate is 60 to 80 MPa/min;
5) annealing: placing the sintered ceramic in a muffle furnace, and annealing in air atmosphere;
6) grinding and polishing: and grinding and polishing the double surfaces of the annealed ceramic wafer to 1-3 mm to obtain the YAG transparent ceramic.
2. The method for preparing YAG transparent ceramic by SPS sintering as claimed in claim 1, wherein: in the step (1), the calcination temperature of the yttrium oxide powder is 900-950 ℃, the heat preservation time is 2-5 h, the calcination temperature of the aluminum oxide powder is 520-560 ℃, and the heat preservation time is 2-5 h.
3. The method for preparing YAG transparent ceramic by SPS sintering as claimed in claim 1, wherein: in the step (2), the grinding balls are alumina balls, and the ball material ratio is 2-4: 1, the volume ratio of the alcohol addition to the ball milling tank is 0.3-0.5, and the ball milling rotating speed is 160-200 rpm.
4. The method for preparing YAG transparent ceramic by SPS sintering as claimed in claim 1, wherein: in the step (3), the drying temperature is 40-60 ℃, and the drying time is 12-36 h.
5. The method for preparing YAG transparent ceramic by SPS sintering as claimed in claim 1, wherein: the size of the screen used for sieving in the step (3) is 100-200 meshes, and the sieving frequency is 3-5 times.
6. The method for preparing YAG transparent ceramic by SPS sintering as claimed in claim 1, wherein: the diameter of the die in the step (4) is 15-25 mm.
7. The method for preparing YAG transparent ceramic by SPS sintering as claimed in claim 1, wherein: in the step (5), the annealing temperature is 1100-1250 ℃, and the heat preservation time is 10-20 h.
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