CN115594502A - Magneto-optical transparent ceramic and preparation method and application thereof - Google Patents
Magneto-optical transparent ceramic and preparation method and application thereof Download PDFInfo
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Abstract
The application discloses magneto-optical transparent ceramic and a preparation method and application thereof, wherein the magneto-optical transparent ceramic has a chemical general formula of Ho 3 Sc 2 Al 3 O 12 The preparation method comprises the following steps: step S1, pressing and forming mixed powder containing holmium oxide, scandium oxide, aluminum oxide and sintering aid to obtain a biscuit; and S2, pre-sintering, vacuum sintering and annealing the biscuit obtained in the step S1 to obtain the magneto-optical transparent ceramic. The magneto-optical transparent ceramic prepared by the method has excellent linear transmittance, stable thermal performance and higher magneto-optical performance, and compared with a mainstream commercial terbium-based magneto-optical material, the magneto-optical transparent ceramic prepared by the method has the advantages of low raw material cost and low preparation cost. The application of magneto-optical transparent materials in optical isolators or optical modulators can be further facilitated.
Description
Technical Field
The application relates to a magneto-optical transparent ceramic and a preparation method and application thereof, belonging to the technical field of magneto-optical ceramic material preparation.
Background
Garnet is an excellent magneto-optical material and has the advantages of less absorption in near infrared band, good Faraday rotation effect and the like. At present, the mainstream commercial terbium-based magneto-optical material has important application in a high-power Faraday magneto-optical isolator due to the advantages of excellent magneto-optical performance, high thermal conductivity, high laser damage threshold and the like.
Disclosure of Invention
According to one aspect of the application, a holmium-scandium-aluminum garnet (HoSAG) magneto-optical transparent ceramic is provided, has excellent linear transmittance, stable thermal performance and higher magneto-optical performance, and also has the advantages of low raw material cost and low preparation cost compared with a mainstream commercial terbium-based magneto-optical material.
The technical scheme is as follows:
a magneto-optical transparent ceramic with chemical formula of Ho 3 Sc 2 Al 3 O 12 ；
Wherein Ho is a +3 valent metal ion.
Optionally, the magneto-optical transparent ceramic has an average grain size of 5 to 15 μm.
Optionally, the magneto-optical transparent ceramic has a linear transmittance of 68 to 78% at a wavelength of 1550 nm.
Optionally, the magneto-optical transparent ceramic has a Verdet constant of-32 rad/T.m at a wavelength of 1064 nm.
According to another aspect of the present application, there is provided a method for preparing the magneto-optical transparent ceramic, comprising:
s1, pressing and forming mixed powder containing holmium oxide, scandium oxide, aluminum oxide and sintering aids to obtain a biscuit;
and S2, pre-sintering, vacuum sintering and annealing the biscuit obtained in the step S1 to obtain the magneto-optical transparent ceramic.
Optionally, in the step S1, holmium oxide, scandium oxide and aluminum oxide are used according to the chemical formula Ho 3 Sc 2 Al 3 O 12 The atomic molar ratio of (a) and (b) are weighed and mixed.
Optionally, in the step S1, the mass ratio of the sintering aid in the mixed powder is 0.05 to 0.1wt%.
The sintering aid is magnesium oxide.
The sintering temperature can be effectively reduced by adding the sintering aid.
Optionally, in the step S1, ball milling and drying are performed after the mixed powder and the ball milling assistant are mixed.
Optionally, the ball milling aid is absolute ethanol.
Optionally, the mass ratio of the ball milling aid to the mixed powder is 3-20.
Optionally, the ball milling comprises the steps of:
according to the mass ratio of the agate balls to the mixed powder of 10-12: 1, ball milling is carried out for 40-50 h, and the rotating speed of the ball mill is 230-250 r/min.
Optionally, the ball milling is performed in a planetary ball mill.
Optionally, the drying temperature is 60 ℃ to 70 ℃.
Optionally, in the step S1, drying the mixed powder, and then placing the dried mixed powder into a 200-mesh screen for sieving.
Optionally, in the step S1, the mixed powder is calcined, the calcining temperature is 1300 to 1400 ℃, and the calcining time is 4 to 6 hours.
Optionally, in the step S1, the mixed powder is pressed and molded under a pressure of 10 to 12MPa, and then is subjected to cold isostatic pressing under a pressure of 180 to 250MPa for 3 to 5min, so as to obtain a biscuit.
Optionally, in step S2, the process conditions of the pre-sintering are: the pre-sintering temperature is 700-900 ℃, the pre-sintering time is 2-3 h, and the pre-sintering atmosphere is air.
The pre-sintering process can degrease and remove the adhesive of the biscuit and improve the density.
Optionally, in step S2, the process conditions of vacuum sintering are: the ambient vacuum degree is 1 × 10 -4 ～1×10 -3 Pa, the sintering temperature is 1690-1710 ℃, and the sintering time is 10-20 h.
The ceramic wafer after vacuum sintering has oxygen vacancy, and in this case, annealing treatment needs to be carried out in oxygen.
Optionally, in step S2, the annealing process conditions are: the annealing temperature is 1200-1300 ℃, the annealing time is 4-6 h, and the annealing atmosphere is air.
Optionally, the magneto-optical transparent ceramic obtained in step S2 is further subjected to a machining process.
According to still another aspect of the present application, there is provided a use of the above-mentioned magneto-optical transparent ceramic or the magneto-optical transparent ceramic obtained according to the above-mentioned manufacturing method in an optical isolator or an optical modulator.
The beneficial effect that this application can produce includes:
1) The magneto-optical transparent ceramic provided by the application has the highest linear transmittance of 78 percent, and the Verdet constant at 1064nm can reach-32.3 rad/T.m.
2) Compared with terbium-based magneto-optical materials, the magneto-optical transparent ceramic material and the preparation method provided by the application have the advantages of lower raw material cost and low manufacturing cost.
Drawings
FIG. 1 is a drawing of a magneto-optical transparent ceramic according to example 1 of the present application;
FIG. 2 is an XRD spectrum comparison of the magneto-optical transparent ceramic in example 1 of the present application with a standard PDF card;
FIG. 3 is a linear transmittance curve map of the magneto-optical transparent ceramic in example 1 of the present application;
FIG. 4 is a verdet constant test curve at 1064nm for the magneto-optical transparent ceramic of example 1 of the present application.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
Example 1
According to Ho 3 Sc 2 Al 3 O 12 Weighing Ho with the total mass of 25-30 g according to the stoichiometric ratio 2 O 3 、Sc 2 O 3 、Al 2 O 3 Dissolving the raw materials in 100-120 ml of absolute ethyl alcohol, adding magnesium oxide which accounts for 0.05-0.1wt% of the total mass of the raw materials and is used as a sintering aid, transferring the mixture into an agate ball milling tank, adding 250-350 g of agate pellets, putting the mixture into a planetary ball mill at the rotating speed of 230-250 r/min, carrying out ball milling for 40-50 h, drying the solution at the temperature of 60-70 ℃, sieving the mixture after the absolute ethyl alcohol is volatilized, selecting a 200-mesh stainless steel sieve as the sieve, and calcining the sieved powder for 4-6 h at the temperature of 1300-1400 ℃. 2.2 to 2.3g of calcined powder is pressed into a biscuit under the uniaxial pressure of 10 to 12MPa, then the biscuit is subjected to cold isostatic pressing for 5min under 250MPa, and the biscuit is subjected to heat preservation for 2 to 3h at the temperature of 700 to 900 ℃ for glue removal. Finally, the vacuum degree is 1 multiplied by 10 -3 ～1×10 -4 Pa, the temperature of 1690-1710 ℃ to be made into a ceramic chip, and annealing is carried out for 4-6 h at the temperature of 1200-1300 ℃ to finally obtain the magneto-optical transparent ceramic, as shown in figure 1.
Example 2
The sintering temperature is 1500 ℃, the sintering time is 10h, other conditions are the same as the example 1, and the transmittance of the magneto-optical transparent ceramic prepared at the wavelength of 1550nm is 36%.
Example 3
The sintering temperature is 2000 ℃, the sintering time is 20h, and other conditions are the same as the example 1, so that the transmittance of the magneto-optical transparent ceramic at the wavelength of 1550nm is 68 percent.
Test example 1
XRD pattern analysis was performed on the magneto-optical transparent ceramic obtained in example 1. As shown in fig. 2: under the reaction conditions in example 1, the obtained magneto-optical transparent ceramics are all garnet structures, and compared with a standard PDF card, the main peaks correspond to one another one to indicate that the sample is successfully synthesized.
The magneto-optical transparent ceramic obtained in example 1 was subjected to linear transmittance analysis, as shown in fig. 3: under the reaction conditions of example 1, the magneto-optical transparent ceramic obtained has a linear transmittance of up to 78%.
Verdet constant analysis was performed on the magneto-optical transparent ceramic obtained in example 1, as shown in fig. 4: the Verdet constant at a wavelength of 1064nm of the magneto-optical transparent ceramic obtained under the reaction conditions of example 1 was-32.3 rad/T.m.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. The magneto-optical transparent ceramic is characterized by having a chemical formula of Ho 3 Sc 2 Al 3 O 12 。
2. The magneto-optical transparent ceramic according to claim 1, wherein the magneto-optical transparent ceramic has a linear transmittance of 68 to 78% at a wavelength of 1550 nm.
3. A magneto-optical transparent ceramic according to claim 1, wherein said magneto-optical transparent ceramic has a Verdet constant of-32 rad/T-m at a wavelength of 1064 nm.
4. A method for the preparation of a magneto-optical transparent ceramic according to any one of claims 1 to 3, comprising the steps of:
s1, pressing and forming mixed powder containing holmium oxide, scandium oxide, aluminum oxide and sintering aids to obtain a biscuit;
and S2, pre-sintering, vacuum sintering and annealing the biscuit obtained in the step S1 to obtain the magneto-optical transparent ceramic.
5. The method of claim 4, wherein the step ofIn S1, holmium oxide, scandium oxide and aluminum oxide are used according to a chemical formula Ho 3 Sc 2 Al 3 O 12 The atomic molar ratio of (a) and (b) are weighed and mixed.
6. The preparation method according to claim 4, wherein in the step S1, the mass ratio of the sintering aid in the mixed powder is 0.05-0.1wt%;
the sintering aid is magnesium oxide;
preferably, the step S1 further comprises calcining the mixed powder, wherein the calcining temperature is 1300-1400 ℃, and the calcining time is 4-6 h;
preferably, in the step S1, the mixed powder is pressed and molded under a pressure of 10 to 12MPa, and then is subjected to cold isostatic pressing under a pressure of 180 to 250MPa for 3 to 5min to obtain a biscuit.
7. The preparation method according to claim 4, wherein in the step S2, the process conditions of the pre-sintering are as follows: the pre-sintering temperature is 700-900 ℃, the pre-sintering time is 2-3 h, and the pre-sintering atmosphere is air.
8. The preparation method according to claim 4, wherein in the step S2, the process conditions of the vacuum sintering are as follows: the ambient vacuum degree is 1 × 10 -4 ～1×10 -3 Pa, the sintering temperature is 1690-1710 ℃, and the sintering time is 10-20 h.
9. The manufacturing method according to claim 4, wherein in the step S2, the annealing process conditions are as follows: the annealing temperature is 1200-1300 ℃, the annealing time is 4-6 h, and the annealing atmosphere is air.
10. Use of the magneto-optical transparent ceramic according to any one of claims 1 to 3, the magneto-optical transparent ceramic produced by the production method according to any one of claims 4 to 9, in an optical isolator or an optical modulator.
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| P MUKHERJEE1: ""Sensitivity of magnetic properties to chemical pressure in lanthanide garnets Ln3A2X3O12,Ln = Gd, Tb, Dy, Ho, A = Ga, Sc, In, Te, X = Ga, Al, Li"，P Mukherjee1，《IPO science》，第1-23页", pages 1 - 23 * |
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| CN115594502B (en) | 2023-10-03 |
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