CN111533445B - Tb 3 Al 5 O 12 Magneto-optical material and preparation method thereof - Google Patents
Tb 3 Al 5 O 12 Magneto-optical material and preparation method thereof Download PDFInfo
- Publication number
- CN111533445B CN111533445B CN202010393268.1A CN202010393268A CN111533445B CN 111533445 B CN111533445 B CN 111533445B CN 202010393268 A CN202010393268 A CN 202010393268A CN 111533445 B CN111533445 B CN 111533445B
- Authority
- CN
- China
- Prior art keywords
- magneto
- optical glass
- optical
- preparation
- melt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/125—Silica-free oxide glass compositions containing aluminium as glass former
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Glass Compositions (AREA)
Abstract
The invention belongs to the field of new materials, and particularly relates to Tb 3 Al 5 O 12 Magneto-optical material and preparation method thereof, including Tb 3 Al 5 O 12 Magneto-optical glass and Tb 3 Al 5 O 12 Magneto-optical ceramics. Tb of the invention 3 Al 5 O 12 The magneto-optical glass is prepared by the steps of material preparation, material mixing, drying and screening, dry pressing, sintering, melting and the like. In the prepared Tb 3 Al 5 O 12 Tb can be made up by further heat treatment on the basis of magneto-optical glass 3 Al 5 O 12 Magneto-optical ceramics. The invention can prepare Tb by a set of process flow 3 Al 5 O 12 Magnetic-optical glass capable of preparing Tb 3 Al 5 O 12 The magneto-optical ceramic has high preparation efficiency. Tb prepared by the invention 3 Al 5 O 12 The melt of magneto-optical glass does not contact with the container in the high-temperature melting stage, no impurity is introduced, and the prepared Tb 3 Al 5 O 12 The magneto-optical glass has high purity and good quality. The invention can add B 2 O 3 And SiO 2 Avoidance of Tb under conditions of equal glass network formers 3 Al 5 O 12 Crystallizing to obtain high-purity Tb with high Tb content and fixed stoichiometric ratio 3 Al 5 O 12 Magneto-optical glass. Tb prepared by the invention 3 Al 5 O 12 Tb not easy to be prepared by conventional method can be further prepared by fine heat treatment process on the basis of magneto-optical glass 3 Al 5 O 12 Magneto-optical ceramics.
Description
Technical Field
The invention belongs to the field of new materials, and particularly relates to Tb 3 Al 5 O 12 Magneto-optical material and its preparation method are provided.
Background
The rare earth magneto-optical material is a novel optical information functional material which changes the electromagnetic property of the material and enables the transmission of the Techibeige to change in the transmission process of light waves. The unique magneto-optical property of the material enables the material to be widely applied to the fields of laser, computers, information, optical fiber communication and the like. The magneto-optical materials are various, and mainly include crystal films, magnetic photonic crystals, magneto-optical ceramics and magneto-optical glass. The Verdet constant of the magneto-optical crystal is generally larger than that of magneto-optical glass, but the preparation process of the crystal is complex, the growth cost is high, a large-size sample is difficult to prepare, the preparation period is long, and a concentration gradient exists. The glass preparation process is simple, the technology is mature, the glass sample is easy to prepare large-size products, the processing is convenient, and the batch preparation is easy to realize. Therefore, the magneto-optical glass has a better application prospect in optical fiber current sensors and optical fiber communication. Tb 3+ Ion unlike Dy 3+ 、Ho 3+ 、Er 3+ The rare earth ions have a plurality of absorption peaks from visible light to infrared light, have good spectral performance and are beneficial to the application of magneto-optical glass, so that the common magneto-optical glass at present is terbium-doped heavy lead glass, terbium-doped cerium phosphate glass and terbium-doped silicate glassThe glass. Among such magneto-optical glasses, tb is decisive for magneto-optical properties 3+ The more ions, generally, the greater the Verdet constant of the material. However, tb 3+ Ions have a very high tendency to devitrify, and a large amount of B needs to be added to the glass seed 2 O 3 And SiO 2 As a network former of the glass, further devitrification of the glass is prevented to cause devitrification. In view of the above problems, the present invention prepares Tb with a fixed stoichiometric ratio by not adding a glass network former 3 Al 5 O 12 And (3) glass. The difficulty in glass preparation is Tb 4 O 7 And Al 2 O 3 The melting points are 2340 ℃ and 2015 ℃, containers resistant to high temperature are few, the glass needs to be cooled quickly, and the traditional method cannot achieve the purpose of quickly cooling to prevent crystallization. The container-free method suspends objects by external forces such as gas, electricity, magnetism and the like, avoids heterogeneous nucleation points, does not need a high-temperature container, realizes ultrahigh temperature and rapid cooling by laser heating, and can prepare Tb which can not be prepared by the conventional method 3 Al 5 O 12 And (3) glass.
Preparation of Tb by conventional method 3 Al 5 O 12 The ceramic needs high-purity powder with uniform grain size, is sintered in a vacuum furnace at high temperature for a long time, internal grain boundaries slowly move to remove air holes, and even secondary hot isostatic pressing post-treatment is needed to further improve the density of a green body. We have found in the practice of the present invention that Tb 3 Al 5 O 12 Further melting the glass to remove air holes, keeping the interior in a highly compact state, and performing later heat treatment for crystallization to obtain Tb 3 Al 5 O 12 The microcrystal magneto-optical ceramic has simple process, high preparation efficiency and low cost.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a Tb 3 Al 5 O 12 Magneto-optical material and process for preparing the same, comprising Tb 3 Al 5 O 12 Magneto-optical glass and Tb 3 Al 5 O 12 Magneto-optical ceramics.
In order to achieve the purpose, the invention is realized by the following technical scheme: tb 3 Al 5 O 12 The preparation method of the magneto-optical glass comprises the following steps:
(S1) batching: according to Tb 3 Al 5 O 12 Weighing dry Tb according to the content of Tb and Al 4 O 7 And Al 2 O 3 ；
(S2) mixing materials: tb is to be 4 O 7 And Al 2 O 3 Mixing uniformly;
(S3) drying and sieving: drying the mixture obtained in the step (S2) and sieving the dried mixture by a sieve of 80-300 meshes;
(S4) dry pressing: dry pressing the mixture obtained in the step (S3) into a cake-shaped blank;
(S5) sintering: sintering the cake-shaped blank obtained in the step (S4) in a muffle furnace to obtain a sintered blank;
(S6) melting: cutting the sintered blank obtained in the step (S5) into small blocks, placing the small blocks in a cavity of a suspension furnace, heating the small blocks by using a laser to melt the small blocks to form a bubble-free clear transparent melt, and then closing the laser to obtain the Tb 3 Al 5 O 12 Magneto-optical glass.
Further, tb as described above 3 Al 5 O 12 Method for producing magneto-optical glass, step (S1), wherein before weighing, commercially pure Tb is used 4 O 7 And Al 2 O 3 Placing in a baking oven, heating to 30-200 deg.C at 1-6 deg.C/min, and drying for 2-10h.
Further, tb as described above 3 Al 5 O 12 The preparation method of the magneto-optical glass comprises the following steps (S2): tb is to be 4 O 7 And Al 2 O 3 Putting the mixture into a 200-800ml mixing tank, taking alcohol as a ball milling medium, and mixing the mixture for 4-12h at 10-30Hz by using a planetary ball mill.
Further, tb as described above 3 Al 5 O 12 The preparation method of the magneto-optical glass comprises the following steps (S4): weighing 10g-100g of the mixture obtained in the step (S3), putting the mixture into a steel mould with the diameter of 2cm-8cm, pressurizing for 2-30MPa, maintaining the pressure for 1-20min, and pressing into a cake shapeA green body.
Further, tb as described above 3 Al 5 O 12 The preparation method of the magneto-optical glass comprises the following steps (S5): placing the cake-shaped blank obtained in the step (S4) on a high-purity aluminum oxide plate; heating to 300 ℃ at a speed of 1-20 ℃/min in a muffle furnace, preserving heat for 10-60min, and removing the adsorbed water in the blank; heating to 600 ℃ at a speed of 1-10 ℃/min, preserving the heat for 10-30min, and removing the hydroxyl water in the blank; heating to 1000 deg.C at 10 deg.C/min, and maintaining for 60-120min; naturally cooling to room temperature to obtain a sintered green body with certain strength.
Further, tb as described above 3 Al 5 O 12 In the step (S6), the sintered blank obtained in the step (S5) is cut into small blocks by a glass cutter, the small blocks are placed in a stainless steel or high-purity aluminum cavity, a carbon dioxide laser control switch is turned on, the step number is gradually adjusted from 0 to 100 until the blank is in a melting state, a gas flow switch is turned on to enable the melt to be stably suspended, the laser power is increased until the melt is completely melted, the laser power is reduced to remove bubbles on the surface of the melt, and when the melt is clear and transparent and has no bubbles, the laser control step number is immediately adjusted to 0 to obtain Tb 3 Al 5 O 12 Magneto-optical glass. In the operation process, the melt is not contacted with the container in the high-temperature melting stage, and impurities are not introduced; meanwhile, the operation can realize ultrahigh-speed cooling of the melt, and glass which cannot be prepared by the conventional method can be prepared.
Preferably, tb as defined above 3 Al 5 O 12 The magneto-optical glass is prepared by using oxygen, air, argon or nitrogen as gas.
Further, tb is described above 3 Al 5 O 12 Tb can be conveniently made on the basis of magneto-optical glass 3 Al 5 O 12 Magneto-optical ceramic, specifically Tb 3 Al 5 O 12 Polishing magneto-optical glass into a wafer shape, placing on an alumina plate, heating to 880-1100 deg.C at 2-20 deg.C/min, maintaining the temperature for 60-180min, and naturally cooling to room temperature to obtain Tb 3 Al 5 O 12 Magneto-optical ceramics.
Has the advantages that: compared with the prior art, the invention has the following advantages that:
(1) The invention can prepare Tb by a set of process flow 3 Al 5 O 12 Magnetic-optical glass capable of preparing Tb 3 Al 5 O 12 The magneto-optical ceramic has high preparation efficiency and relatively simple preparation process, and can be prepared in batches.
(2) Tb prepared by the invention 3 Al 5 O 12 The melt of magneto-optical glass does not contact with the container in the high-temperature melting stage, no impurity is introduced, and the prepared Tb 3 Al 5 O 12 The magneto-optical glass has high purity and good quality.
(3) The invention can add B 2 O 3 And SiO 2 Tb avoidance under conditions of equal glass network formation 3 Al 5 O 12 Crystallizing to obtain high-purity Tb with high Tb content in a fixed stoichiometric ratio 3 Al 5 O 12 Magneto-optical glass.
(4) Tb prepared by the invention 3 Al 5 O 12 Tb not easy to be prepared by conventional method can be further prepared by fine heat treatment process on the basis of magneto-optical glass 3 Al 5 O 12 Magneto-optical ceramics.
Drawings
FIG. 1 shows Tb prepared in example 1 3 Al 5 O 12 Transmittance curve of magneto-optical glass;
FIG. 2 shows Tb prepared under different conditions in example 1 3 Al 5 O 12 An XRD pattern of the material;
FIG. 3 shows Tb obtained in example 2 3 Al 5 O 12 EDS element distribution spectrum of magneto-optical glass;
FIG. 4 shows Tb prepared under different conditions in example 2 3 Al 5 O 12 XRD pattern of the material.
Detailed Description
The invention will be further illustrated by the following specific examples, which are given for the purpose of illustration only and are not intended to be limiting.
Example 1
Tb 3 Al 5 O 12 Magneto-optical glass, prepared by the following steps:
(S1) batching: the commercial high-purity terbium oxide and aluminum oxide are put in a baking oven and heated to 60 ℃ at the speed of 1 ℃/min for drying for 2h. According to Tb 3 Al 5 O 12 The mass fractions of Tb element and Al element are 59.3% and 16.8%, tb 4 O 7 Wherein Tb accounts for 85 percent in the mass fraction, and Al 2 O 3 The mass fraction of the medium aluminum element is 53 percent, if 2.09g Tb is weighed 4 O 7 0.951g of Al are weighed accordingly 2 O 3 。
(S2) mixing materials: tb 4 O 7 And Al 2 O 3 Put into a 200mL mixing tank, added with 20mL of alcohol and mixed for 4 hours at 20Hz in a planetary ball mill.
(S3) drying and sieving: the mixture was placed in a pan, dried at 70 ℃ and screened through a 100 mesh screen in a fume hood.
(S4) dry pressing: weighing 10g of the mixture, putting the mixture in a steel mould with the diameter of 2cm, pressurizing at 2MPa, and maintaining the pressure for 1min to obtain a cake-shaped blank.
(S5) sintering: placing the cake-shaped blank on a high-purity alumina plate with the thickness of about 5mm, heating to 300 ℃ at a speed of 2 ℃/min in a muffle furnace, preserving heat for 10min, removing adsorbed water in the blank, heating to 600 ℃ at a speed of 3 ℃/min, preserving heat for 10min, removing hydroxyl water, finally heating to 1000 ℃ at a speed of 10 ℃/min, preserving heat for 60min, and naturally cooling to room temperature to obtain a sintered blank with certain strength.
(S6) melting: dividing the sintered blank into small blocks by a glass cutter, placing the small blocks in a stainless steel cavity, turning on a carbon dioxide laser control switch, gradually adjusting the steps from 0 to 100 until the blank is molten, and turning on a gas flow switch, wherein the gas is oxygen. Making the melted material stably suspend under the combined action of surface tension and air flow, continuously increasing laser power until it is completely melted, then properly reducing temperature to remove air bubbles on the surface of melt, when the melt is clear and transparent and has no air bubbles, immediately regulating laser control step number to 0 to obtain Tb 3 Al 5 O 12 Magneto-optical glass.
Tb 3 Al 5 O 12 Preparing the ceramic: tb prepared in the above-mentioned 3 Al 5 O 12 Polishing glass into disk, placing on an alumina plate, heating to 880 deg.C at 2 deg.C/min, holding for 60min 3 Al 5 O 12 Glass is crystallized to prepare Tb 3 Al 5 O 12 A ceramic.
FIG. 1 shows Tb prepared in this example 3 Al 5 O 12 Transmittance curve of magneto-optical glass. Further, various Tb prepared by adjusting various gases and preparation methods in the step (S6) 3 Al 5 O 12 The XRD pattern of the material is shown in figure 2. It can be seen that Tb can only be produced from the melt without contact with the vessel wall 3 Al 5 O 12 And (3) glass.
Example 2
Tb 3 Al 5 O 12 Magneto-optical glass, prepared by the following steps:
(S1) batching: the commercial high-purity terbium oxide and aluminum oxide are dried for 10 hours in an oven at the temperature of 300 ℃ at the speed of 6 ℃/min. According to Tb 3 Al 5 O 12 The mass fractions of Tb element and Al element in the mixture were 20.9gTb 4 O 7 And 9.51gAl 2 O 3 。
(S2) mixing materials: tb 4 O 7 And Al 2 O 3 The mixture was placed in a 500mL mixing bowl, 40mL of alcohol was added and mixed in a planetary ball mill at 30Hz for 4h.
(S3) drying and sieving: the mixture was placed in a pan, dried at 200 ℃ and sieved through a 300 mesh screen in a fume hood.
(S4) dry pressing: weighing 20g of the mixture, placing the mixture in a steel mould with the diameter of 3cm, pressurizing at 30MPa, and maintaining the pressure for 20min to obtain a cake-shaped blank.
(S5) sintering: and (3) placing the cake-shaped blank on a high-purity alumina plate with the thickness of about 5mm, heating to 300 ℃ at a speed of 20 ℃/min in a muffle furnace, preserving heat for 60min, removing adsorbed water in the blank, heating to 600 ℃ at a speed of 10 ℃/min, preserving heat for 30min, removing hydroxyl water, finally heating to 1000 ℃ at a speed of 10 ℃/min, preserving heat for 120min, and naturally cooling to room temperature to obtain a sintered blank with certain strength.
(S6) melting: dividing the sintered blank into small blocks by a glass cutter, placing the small blocks in a stainless steel cavity, turning on a carbon dioxide laser control switch, gradually adjusting the steps from 0 to 100 until the blank is molten, and turning on a gas flow switch, wherein the gas is argon. Making the melted material stably suspend under the combined action of surface tension and air flow, continuously increasing laser power until it is completely melted, then properly reducing temperature to remove air bubbles on the surface of melt, when the melt is clear and transparent and has no air bubbles, immediately regulating laser control step number to 0 to obtain Tb 3 Al 5 O 12 Magneto-optical glass.
Tb 3 Al 5 O 12 Preparing the ceramic: tb prepared in the above-mentioned 3 Al 5 O 12 Polishing glass into disc shape, placing on an alumina plate, heating to 950 deg.C at 2 deg.C/min, maintaining for 120min 3 Al 5 O 12 Glass is crystallized to prepare Tb 3 Al 5 O 12 A ceramic.
FIG. 3 shows Tb prepared in this example 3 Al 5 O 12 The EDS element map of the magneto-optical glass polished into a wafer shape shows that Tb and Al are uniformly distributed on the whole glass surface.
Also at Tb 3 Al 5 O 12 In the preparation process of the ceramic, different heat treatment temperatures are adjusted to prepare a plurality of Tb 3 Al 5 O 12 The XRD pattern of the material is shown in figure 4. As can be seen from FIG. 4, the crystals were not crystallized at 750 ℃, weakly crystallized by heat treatment at 850 ℃, completely crystallized at 950 ℃ and Tb 3 Al 5 O 12 All diffraction peaks in the standard XRD pattern completely correspond to each other, which proves that Tb is successfully prepared 3 Al 5 O 12 A ceramic.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.
Claims (9)
1. Tb 3 Al 5 O 12 The preparation method of the magneto-optical glass is characterized by comprising the following steps: the method comprises the following steps:
(S1) batching: according to Tb 3 Al 5 O 12 The dry Tb is weighed according to the proportion of the Tb element and Al element 4 O 7 And Al 2 O 3 ；
(S2) mixing materials: tb is to be 4 O 7 And Al 2 O 3 Mixing uniformly;
(S3) drying and sieving: drying the mixture obtained in the step (S2) and sieving the dried mixture by a sieve of 80-300 meshes;
(S4) dry pressing: dry pressing the mixture obtained in the step (S3) into a cake-shaped blank;
(S5) sintering: sintering the cake-shaped blank obtained in the step (S4) in a muffle furnace to obtain a sintered blank;
(S6) melting: cutting the sintered green body obtained in the step (S5) into small blocks, placing the small blocks into a cavity of a suspension furnace, heating the small blocks by using a laser to melt the small blocks to form a bubble-free clear transparent melt, and then closing the laser to obtain the Tb 3 Al 5 O 12 Magneto-optical glass;
the step (S5) is: placing the cake-shaped blank obtained in the step (S4) on a high-purity aluminum oxide plate; heating to 300 deg.C in muffle furnace at 1-20 deg.C/min, and maintaining for 10-60min; heating to 600 deg.C at 1-10 deg.C/min, and maintaining for 10-30min; heating to 1000 deg.C at 10 deg.C/min, and maintaining for 60-120min; naturally cooling to room temperature to obtain a sintered green body;
in the step (S6), after the melt is completely melted, the laser power is reduced to cool the melt so as to remove bubbles on the surface of the melt, and thus a bubble-free clear transparent melt is obtained.
2. The Tb of claim 1 3 Al 5 O 12 The preparation method of the magneto-optical glass is characterized by comprising the following steps: in step (S1), it is necessary to separately supply commercially high-purity Tb before weighing 4 O 7 And Al 2 O 3 Placing in a baking oven, heating to 30-200 deg.C at 1-6 deg.C/min, and bakingDrying for 2-10h.
3. The Tb of claim 1 3 Al 5 O 12 The preparation method of the magneto-optical glass is characterized by comprising the following steps: the step (S2) is: tb is to be 4 O 7 And Al 2 O 3 Putting the mixture into a mixing tank of 200-800ml, using alcohol as a ball milling medium, and mixing the mixture for 4-12h at 10-30Hz by using a planetary ball mill.
4. The Tb of claim 1 3 Al 5 O 12 The preparation method of the magneto-optical glass is characterized by comprising the following steps: the step (S4) is: and (5) weighing 10g-100g of the mixture obtained in the step (S3), putting the mixture into a steel mould with the diameter of 2cm-8cm, pressurizing for 2-30MPa, maintaining the pressure for 1-20min, and pressing into a cake-shaped blank.
5. The Tb of claim 1 3 Al 5 O 12 The preparation method of the magneto-optical glass is characterized by comprising the following steps: in the step (S6), the sintered blank obtained in the step (S5) is cut into small blocks by a glass cutter, the small blocks are placed in a stainless steel or high-purity aluminum cavity, a carbon dioxide laser control switch is turned on, the step number is gradually adjusted from 0 to 100 until the blank is in a melting state, a gas flow switch is turned on to enable the melt to be stably suspended, the laser power is increased until the melt is completely melted, the laser power is reduced to remove bubbles on the surface of the melt, and when the melt is clear and transparent and has no bubbles, the laser control step number is immediately adjusted to 0 to obtain Tb 3 Al 5 O 12 Magneto-optical glass.
6. The Tb of claim 5 3 Al 5 O 12 The preparation method of the magneto-optical glass is characterized by comprising the following steps: the gas is oxygen, air, argon or nitrogen.
7. Tb 3 Al 5 O 12 The preparation method of the magneto-optical ceramic is characterized by comprising the following steps: tb prepared according to any one of claims 1 to 6 3 Al 5 O 12 The magneto-optical glass is polished into a disk shape and then placed inHeating to 880-1100 deg.C at 2-20 deg.C/min on alumina plate, maintaining for 60-180min, and naturally cooling to room temperature to obtain Tb 3 Al 5 O 12 Magneto-optical ceramics.
8. Tb 3 Al 5 O 12 Magneto-optical glass, characterized by: tb according to any one of claims 1 to 6 3 Al 5 O 12 The magneto-optical glass is prepared by the preparation method.
9. Tb 3 Al 5 O 12 Magneto-optical ceramic characterized by: the Tb of claim 7 3 Al 5 O 12 The magneto-optical ceramic is prepared by the preparation method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010393268.1A CN111533445B (en) | 2020-05-11 | 2020-05-11 | Tb 3 Al 5 O 12 Magneto-optical material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010393268.1A CN111533445B (en) | 2020-05-11 | 2020-05-11 | Tb 3 Al 5 O 12 Magneto-optical material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111533445A CN111533445A (en) | 2020-08-14 |
| CN111533445B true CN111533445B (en) | 2023-02-17 |
Family
ID=71972331
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010393268.1A Active CN111533445B (en) | 2020-05-11 | 2020-05-11 | Tb 3 Al 5 O 12 Magneto-optical material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111533445B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753473A (en) * | 2016-02-25 | 2016-07-13 | 江苏师范大学 | Preparation method of magneto-optic terbium oxide transparent ceramic |
| CN106103364A (en) * | 2014-07-14 | 2016-11-09 | 日本电气硝子株式会社 | The manufacture device of the manufacture method of glass material and glass material |
| CN109336381A (en) * | 2018-10-16 | 2019-02-15 | 中国科学院上海硅酸盐研究所 | A kind of black bio glass and its preparation method and application |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107555800A (en) * | 2017-08-18 | 2018-01-09 | 中国科学院理化技术研究所 | A kind of transparent Sr3Al2O6‑SrAl2O4Glass ceramics and preparation method thereof |
-
2020
- 2020-05-11 CN CN202010393268.1A patent/CN111533445B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106103364A (en) * | 2014-07-14 | 2016-11-09 | 日本电气硝子株式会社 | The manufacture device of the manufacture method of glass material and glass material |
| CN105753473A (en) * | 2016-02-25 | 2016-07-13 | 江苏师范大学 | Preparation method of magneto-optic terbium oxide transparent ceramic |
| CN109336381A (en) * | 2018-10-16 | 2019-02-15 | 中国科学院上海硅酸盐研究所 | A kind of black bio glass and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 《Synthesis of Tb3Al5O12 (TAG) transparent ceramics for potential magneto-optical applications》;Hui Lin等;《Optical Materials》;20110720;第33卷;第1633页右栏最后一段 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111533445A (en) | 2020-08-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5236483A (en) | Method of preparing silica glass | |
| CN101935208B (en) | Rare earth aluminate single-phase or complex-phase nanocrystalline transparent ceramic material and preparation method thereof | |
| CN102311258B (en) | Active ion controlled doping yttrium aluminum garnet base laser transparent ceramic material and preparation method thereof | |
| CN103806100B (en) | A kind of terraced method growing method of vertical temperature of five oxidation Tritanium/Trititanium polycrystalline | |
| EP1314701B1 (en) | Modification process of synthetic quartz powder and its quartz glass product | |
| CN112552032B (en) | Synthetic beta-spodumene solid solution, microcrystalline glass manufactured by using same and manufacturing method thereof | |
| CN107130289A (en) | A kind of growing method for improving heat exchange large size sapphire crystal | |
| CN104451564B (en) | A kind of method preparing siliceous target | |
| CN107699950A (en) | One kind mixes scandium terbium aluminium garnet magneto-optical crystal and preparation method thereof | |
| CN108395102B (en) | LTCC substrate material with low thermal expansion coefficient and preparation method thereof | |
| CN111533445B (en) | Tb 3 Al 5 O 12 Magneto-optical material and preparation method thereof | |
| CN112341003A (en) | Photochromic glass and preparation method thereof | |
| CN117105655A (en) | Preparation and polishing method of high-quality magnesia-alumina spinel transparent ceramic | |
| CN116947467A (en) | Sintering method of high-purity fused quartz ceramic roller | |
| CN106518072A (en) | Method for preparing high-transmittance NaLaS2 infrared transparent ceramic | |
| CN109354497A (en) | The transparent Indium scandium ceramics and preparation method thereof of Ho doping | |
| CN114804850A (en) | Preparation method of fluorescent transparent ceramic with high optical performance | |
| CN113149429B (en) | High borosilicate glass containing metal nanoparticles and preparation method thereof | |
| CN114853347A (en) | High-thermal-conductivity low-temperature co-fired glass ceramic substrate and preparation method thereof | |
| CN104357904A (en) | Growth method for large-dimension titanium sapphire crystals | |
| CN115304259A (en) | Low-expansion magnesium-aluminum-silicon cordierite microcrystalline glass and preparation method thereof | |
| CN110093660B (en) | Growth device and process capable of growing bubble-free crystal material at high speed | |
| JPH10502324A (en) | Sintered quartz glass product and method for producing the same | |
| CN115490427A (en) | High-crystallinity lithium-aluminum-silicon transparent glass ceramic and preparation method thereof | |
| JPH0912322A (en) | High-purity transparent quartz glass and its production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |