CN114133235B - Axial hot-pressing sintering preparation method of rare earth iron garnet magneto-optical ceramic with good infrared permeability - Google Patents
Axial hot-pressing sintering preparation method of rare earth iron garnet magneto-optical ceramic with good infrared permeability Download PDFInfo
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Abstract
The invention relates to an axial hot-pressing sintering preparation method of rare earth iron garnet magneto-optical ceramic with good infrared permeability, which comprises the following steps: (1) The component general formula of the rare earth iron garnet magneto-optical ceramic material is M x R 3‑x Fe 5 O 12 Weighing and mixing the M source, the R source and the Fe source according to the stoichiometric ratio to obtain mixed powder; (2) Pressing and molding the obtained mixed powder by a dry pressing method to obtain a biscuit; (3) And placing the obtained biscuit in a hot pressing furnace for hot pressing and sintering to obtain the rare earth iron garnet magneto-optical ceramic material.
Description
Technical Field
The invention relates to a preparation method of a rare earth iron garnet magneto-optical ceramic material, in particular to an axial hot-pressing sintering preparation method of a rare earth iron garnet magneto-optical ceramic with good infrared permeability.
Background
The magneto-optical material plays an important role in the fields of laser, optical communication, optical fiber sensing and the like based on the Faraday effect of the non-reciprocity, is a key core material for forming magneto-optical devices such as an optical isolator, an optical circulator, a high-speed magneto-optical switch and the like, and is widely applied to the fields of high and new technology, medical treatment, military, industry and the like. The current common magneto-optical materials mainly comprise magneto-optical glass, magneto-optical crystal, magneto-optical ceramic and the like. The magneto-optical glass has the advantages of good isotropy, low cost, capability of preparing large-size optical fibers, easy drawing, and the like, but has poor heat-conducting property and small laser damage resistance threshold value, and is not suitable for being applied to a high-power laser system. The magneto-optical crystal has the advantages of good magneto-optical property, small optical absorption coefficient, high thermal conductivity and the like, but the magneto-optical crystal is difficult to prepare a large-volume block material, and has long preparation period and high cost. Compared with magneto-optical glass, the magneto-optical ceramic has better mechanical properties, and the properties of thermal, optical and magneto-optical are all comparable to those of magneto-optical crystal, and meanwhile, the magneto-optical ceramic also has the advantages of short preparation period, low cost and good isotropy. Among the magneto-optical ceramics, the rare-earth iron garnet magneto-optical ceramic has good infrared transmittance, can obtain a Faraday rotation angle far higher than that of the commercially-used Terbium Gallium Garnet (TGG), terbium Aluminum Garnet (TAG) and rare-earth sesquioxide ceramic under a lower magnetic field, and is an appropriate material urgently required for miniaturization of magneto-optical devices such as optical isolators and the like.
At present, the commercially available rare earth iron garnet materials in the field of optical communication are gadolinium iron garnet (GdIG) doping materials and Yttrium Iron Garnet (YIG) magneto-optical materials, and only single crystal materials are used, and the materials are prepared by a liquid phase epitaxy method, so that the period is long, the size of the prepared single crystal is small, and the cost is high. The preparation of rare earth iron garnet magneto-optical ceramic began to appear in almost two years, and the pressure-free sintering-oxygen atmosphere (V) was adopted in 2018 by Akio Ikesue of Japan at the earliest O2 Not more than 20%) and a hot isostatic pressing two-step sintering method successfully prepare the high-transparency YIG magneto-optical ceramic, and then the same method is adopted between 2019 and 2020 for successfully preparing TIG and Ce: YIG and Bi: YIG magneto-optical ceramics (J.Am.Ceram.Soc.101 (2018): 5120-5126.), J.alloys.Compd.773 (2019) 739-742, J.Allos.Compd.811 (2019) 152059, J.Eur.Ceram.Soc.2020,40 (15). In addition, other reports related to the preparation of rare earth iron garnet magneto-optical ceramics are not seen in the previous research, and reports related to the successful preparation of high-transmittance rare earth iron garnet magneto-optical ceramics are not found at home, so that the preparation of the rare earth iron garnet magneto-optical ceramics is a technical difficulty at home and abroad. Two-step sintering reported abroadThe key process in the process, namely oxygen atmosphere hot isostatic pressing, has extremely high requirements on the adopted oxygen atmosphere hot isostatic pressing sintering equipment, the equipment is expensive, the equipment cannot realize high-concentration oxygen atmosphere, and no relevant report is seen in China.
Disclosure of Invention
Aiming at the problems, the invention provides an axial hot-pressing sintering preparation method of rare earth iron garnet magneto-optical ceramic with good infrared permeability, wherein the general formula of the component of the rare earth iron garnet magneto-optical ceramic material is M x R 3-x Fe 5 O 12 (ii) a Wherein R is at least one of Y, sm, eu, gd, tb, dy, ho, er, tm, yb and Lu in rare earth elements; the doping ion M is at least one of Ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb, lu and Bi, and x is more than or equal to 0 and less than or equal to 2; the preparation method of the rare earth iron garnet magneto-optical ceramic material comprises the following steps: (1) The component general formula of the rare earth iron garnet magneto-optical ceramic material is M x R 3-x Fe 5 O 12 Weighing and mixing the M source, the R source and the Fe source according to the stoichiometric ratio to obtain mixed powder; (2) Pressing and molding the obtained mixed powder by a dry pressing method to obtain a biscuit; (3) And placing the obtained biscuit in a hot pressing furnace for hot pressing and sintering to obtain the rare earth iron garnet magneto-optical ceramic material.
The magneto-optical ceramic has the action mechanism of Faraday effect, namely, after linearly polarized light passes through the magneto-optical ceramic placed in a magnetic field, the polarization direction of the linearly polarized light is deflected, and the rotation amount of the polarization direction is in linear direct proportion to the component of the magnetic field in the light wave propagation direction. In the faraday effect, the rotation direction of the polarization plane of linearly polarized light is related to the magnetic field direction only, and is not related to the propagation direction of light, and is irreversible (see fig. 1).
The Faraday rotation angle and the magnetic field of common paramagnetic magneto-optical ceramics (such as TGG, TAG and the like) are linearly changed, and the slope of the linear change of the Faraday rotation angle and the magnetic field of the paramagnetic magneto-optical ceramics with unit length is a Verdet constant, and is an important parameter for measuring the magneto-optical performance of the paramagnetic magneto-optical ceramics. The ferrimagnetic rare earth iron garnet magneto-optical ceramic is characterized in that the Faraday rotation angle and the magnetic field size are in a nonlinear relationship,before the external magnetic field does not enable the ceramic to reach the saturation magnetization, the Faraday rotation angle of the ceramic increases rapidly along with the increase of the external magnetic field, and the Faraday rotation angle does not increase obviously along with the increase of the magnetic field after the ceramic reaches the saturation magnetization. Therefore, the specific Faraday rotation angle theta under a saturation magnetic field should be used for measuring the magneto-optical performance of the ferrimagnetic rare earth iron garnet magneto-optical ceramic F (i.e., the amount of Faraday rotation angle generated by linearly polarized light passing through a unit length of ceramic in a saturated magnetization state of the ceramic).
In the invention, the internal mechanism of the sintering by adopting the axial hot pressing sintering method is that the heating and the pressurizing are simultaneously carried out in the sintering process, which is beneficial to the mass transfer processes of contact, diffusion, flow and the like of powder particles in a biscuit, thereby promoting the sintering compactness and preparing the high-transparency magneto-optical ceramic. Different from the traditional axial hot-pressing sintering method, the axial hot-pressing sintering method disclosed by the disclosure controls the sintering atmosphere by using methods of vacuumizing, adjusting the oxidizing atmosphere, adjusting the gas flow and the like, realizes the random adjustment from the inert atmosphere to the oxidizing atmosphere by regulating and controlling the mixing ratio of nitrogen and oxygen, and promotes the densification process of the rare earth iron garnet magneto-optical ceramic under the synergistic effect of different sintering atmospheres, temperatures and pressures. Particularly, the reduction of ferric iron into ferrous iron at high temperature is inhibited by regulating and controlling the oxygen content in the atmosphere, and the preparation of the rare earth iron garnet magneto-optical ceramic with good infrared permeability is realized.
Preferably, x is more than or equal to 0 and less than or equal to 0.6; preferably, the following components: x is more than or equal to 0 and less than or equal to 0.24.
Preferably, the M source is selected from M 2 O 3 、MO 2 、M 4 O 7 、M 2 (CO 3 ) 3 、M(HCO 3 ) 3 、M 2 (C 2 O 4 ) 3 、M(Ac) 3 、M(NO 3 ) 3 At least one of (1).
Preferably, the R source is selected from R 2 O 3 (or R) 4 O 7 )、R 2 (CO 3 ) 3 、RPO 4 、R(HCO 3 ) 3 、R 2 (C 2 O 4 ) 3 、R(Ac) 3 、R(NO 3 ) 3 At least one of (a).
Preferably, the Fe source is selected from Fe 2 O 3 、FeO、Fe 3 O 4 、Fe(NO 3 ) 3 、Fe 2 (C 2 O 4 ) 3 、Fe(Ac) 3 At least one of (a).
Preferably, a binder is also added into the mixed powder; the binder is selected from at least one of polyvinyl alcohol, ammonium polyacrylate and carboxymethyl cellulose; the addition amount of the binder is 0.3 to 1 weight percent of the total mass of the mixed powder; preferably, the binder is 0.5 to 0.7wt% of the total mass of the mixed powder.
Preferably, an oxygen atmosphere with different oxygen partial pressures is used as the atmosphere for hot-pressing sintering through vacuum and introduction of a nitrogen-oxygen mixed gas; preferably, the atmosphere of the hot-pressing sintering is a vacuum atmosphere or a nitrogen-oxygen mixed gas. In fact, the invention does not allow sintering of high transparency magneto-optical ceramics by simple hot pressing, unlike 10% O in the H isostatic pressing sintering of document J.Eur.Ceram.Soc.2020,40 (15) 2 An Ar atmosphere, and in the case of the Ce: YIG magneto-optical ceramic, the ceramic can be prepared by vacuum atmosphere sintering. 20% O by hot isostatic pressing sintering, different from the document J.Am.Ceram.Soc.101 (2018): 5120-5126 2 An Ar atmosphere, which can be prepared by 100% pure oxygen atmosphere sintering for YIG magneto-optical ceramics.
Preferably, N in the nitrogen-oxygen mixed gas 2 And O 2 The volume ratio of (1) 2 And O 2 The range of volume ratios of (a) to (b) is different. For pure phase YIG, N is selected 2 :O 2 The volume ratio is 0.7; more preferably, N is selected 2 :O 2 The volume ratio is 0.5-0. For Bi: YIG ceramics, N is preferably selected 2 :O 2 The volume ratio is 1; more preferably, N is selected 2 :O 2 The volume ratio is 1.
Preferably, the flow rate of the nitrogen-oxygen mixed gas is 1-25L/min; preferably, the flow rate of the nitrogen-oxygen mixed gas is 3 to 15L/min.
Preferably, the temperature of the hot-pressing sintering is 1150-1400 ℃, and preferably 1200-1350 ℃; the time for hot-pressing sintering is 6 to 24 hours, preferably 8 to 12 hours.
Preferably, the heating rate of the hot-pressing sintering is 1-10 ℃/min, and preferably 3-8 ℃/min
Preferably, the axial pressure of the hot-pressing sintering is 10 to 80MPa, and the preferred axial pressure is 20 to 60MPa.
Advantageous effects
The present disclosure provides a composition range of rare earth iron garnet and doped magneto-optical ceramic thereof, and introduces in detail a preparation method for obtaining infrared high transmittance rare earth iron garnet magneto-optical ceramic by using an axial hot pressing method, which has the following advantages:
(1) Compared with the oxygen atmosphere hot isostatic pressing two-step sintering method, the axial hot pressing method provided by the invention has the advantages that the sintering process is simplified, the requirement on equipment is low, the process is simple and convenient, the sintering is successful in one step, the preparation period is shortened, and the preparation cost is reduced. In addition, the high-quality rare earth iron garnet ceramic is finally sintered by precisely regulating and controlling the atmosphere, the pressurizing time, the heating rate and the sintering temperature, particularly the atmosphere (prepared by vacuum and nitrogen-oxygen mixed gas).
(2) The density of the ceramic material can reach more than 99% of theoretical value, the transmittance can reach more than 76% (wavelength is 2.0 μ M, thickness is 0.5 mm) by adopting the process for preparing the yttrium iron garnet magneto-optical ceramic, and the M: RIG block ceramic with high density and good infrared transparency can be obtained by adopting the sintering method disclosed by the invention. The rare earth iron garnet magneto-optical ceramic is applied to the field of magneto-optical, has extremely high requirements on compactness, permeability and impurity phase tolerance, is not achieved by simply firing a ceramic solidified body, needs extremely high density (more than 99 percent), has good permeability (reaching 40 to 100 percent of theoretical permeability), and has no obvious impurity phase in the obtained ceramic body.
(3) The Faraday rotation angle generated by the yttrium iron garnet magneto-optical transparent ceramic under the same magnetic field is far higher than that of paramagnetic magneto-optical ceramic (shown in figure 2) with the same size, and the yttrium iron garnet magneto-optical transparent ceramic is expected to provide a core material for preparing magneto-optical devices such as an optical isolator, an optical circulator, a high-speed magneto-optical switch and the like in the fields of high and new technologies, military, medical treatment, industry and the like.
Drawings
Figure 1 is a schematic representation of the faraday effect of a magneto-optical ceramic.
FIG. 2 shows the relationship between the optical rotation rates at 1064nm wavelength of YIG ceramic and TGG ceramic with the variation of magnetic field.
Fig. 3a is an XRD pattern of the magneto-optical ceramic prepared in example 1, and it can be seen from fig. 10 that the resulting magneto-optical ceramic is a single garnet phase.
Fig. 3b is a graph of the light transmission of the magneto-optical ceramic prepared in example 1.
Fig. 3c is a hot-etched SEM image of the polished face of the magneto-optical ceramic prepared in example 1.
Fig. 4a is an XRD pattern of the magneto-optical ceramic prepared in example 2, and referring to fig. 10, the resulting magneto-optical ceramic is a single garnet phase. The resulting magneto-optical ceramic is a single phase as can be seen from the figure.
Fig. 4b is a graph of the light transmittance of the magneto-optical ceramic prepared in example 2.
Figure 4c is an SEM image of a cross-section of the magneto-optical ceramic prepared in example 2.
Fig. 5a is an XRD pattern of the magneto-optical ceramic prepared in example 3, and referring to fig. 10, the resulting magneto-optical ceramic is a single garnet phase. The resulting magneto-optical ceramic is a single phase as can be seen from the figure.
Fig. 5b is a graph of the light transmittance of the magneto-optical ceramic prepared in example 3.
Fig. 5c is a hot-etched SEM image of the polished face of the magneto-optical ceramic prepared in example 3.
Fig. 6a is an XRD pattern of the magneto-optical ceramic prepared in example 4, and referring to fig. 10, it can be seen that the resulting magneto-optical ceramic is a single garnet phase. It can be seen that the resulting magneto-optical ceramic is a single phase.
Fig. 6b is a graph of the light transmittance of the magneto-optical ceramic prepared in example 4.
Fig. 6c is a hot-etched SEM image of the polished face of the magneto-optical ceramic prepared in example 4.
Fig. 7a is an XRD pattern of the magneto-optical ceramic prepared in example 5, and referring to fig. 10, the resulting magneto-optical ceramic is a single garnet phase. It can be seen that the resulting magneto-optical ceramic is a single phase.
Fig. 7b is a graph of the light transmittance of the magneto-optical ceramic prepared in example 5.
Fig. 7c is a hot-etched SEM image of the polished face of the magneto-optical ceramic prepared in example 5.
Fig. 8a is an XRD pattern of the magneto-optical ceramic prepared in example 6. Referring to fig. 10, it can be seen that the resulting magneto-optical ceramic is a single garnet phase. The resulting magneto-optical ceramic is a single phase as can be seen from the figure.
Fig. 8b is a hot-etched SEM image of the polished face of the magneto-optical ceramic prepared in example 6.
Fig. 8c is a graph of light transmission for the magneto-optical ceramic prepared in example 6.
Fig. 9a is an XRD pattern of the magneto-optical ceramic prepared in example 7, and referring to fig. 10, the resulting magneto-optical ceramic is a single garnet phase. The resulting magneto-optical ceramic is a single phase as can be seen from the figure.
Fig. 9b is a hot-etched SEM image of the polished face of the magneto-optical ceramic prepared in example 7.
Fig. 9c is a graph of the light transmittance of the magneto-optical ceramic prepared in example 7.
FIG. 10 is XRD pattern of YIG standard card (JCPDS document No. 43-0507) in standard database.
Detailed Description
The present invention is further illustrated by the following examples, which are to be construed as merely illustrative, and not a limitation of the present invention. Unless otherwise specified, each percentage refers to a mass percentage.
In the present disclosure, an axial hot-pressing preparation method of rare earth iron garnet magneto-optical ceramic is introduced. Particularly, the axial hot-pressing preparation method provided by the invention does not need special oxygen atmosphere hot isostatic pressing sintering equipment, and the rare earth iron garnet magneto-optical ceramic with high transparency can be obtained by one-step sintering, so that the operation is simple and convenient.
The following is an exemplary description of the preparation method of the rare earth iron garnet magneto-optical ceramic.
According to magneto-optical M: stoichiometric ratios of RIG ceramics the M source, Y source, and Fe source are weighed and mixed (e.g., ball mill mixed, solvent may be added) to give a homogeneous mixed slurry.
And drying and sieving the mixed slurry to obtain mixed powder.
Pressing and molding the mixed powder by adopting a dry pressing method to obtain a biscuit;
and (3) placing the biscuit in a hot pressing furnace, and sintering in a specific atmosphere under hot pressure to obtain the rare earth iron garnet magneto-optical ceramic.
In the invention, the relative density of the rare earth iron garnet magneto-optical ceramic is tested by an Archimedes method. And testing the specific Faraday rotation angle of the rare earth iron garnet magneto-optical ceramic by adopting an extinction method through a Faraday rotation angle testing platform. The transmittance profile was divided into two parts, and the crystal structure was identified by XRD (X-ray diffraction, D/max 2550V, japan) using a UV-visible spectrophotometer (Cary-5000, america) for the near infrared band (1.0 μm-2.5 μm), and FTIR infrared spectrometer (Fourier-induced spectrometer, tensor 27, germany) for the mid infrared band (2.5 μm-10.0 μm).
The present invention will be described in further detail with reference to examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing description are intended to be included within the scope of the invention. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
According to Y 3 Fe 5 O 12 And (3) performing powder proportioning, weighing iron oxide and yttrium oxide powder according to a stoichiometric ratio, adding 0.7 part of absolute ethyl alcohol (namely, 70g of powder is added into 100g of anhydrous ethyl alcohol), performing ball milling for 36 hours, drying, and sieving by using a 200-mesh sieve. Adding PVA into the above mixed powder by 0.5%, mixing, sieving with 40 mesh sieve, granulating, pressing into biscuit with diameter of 15mm and thickness of 1-2 cm, placing biscuit sample in hot pressing mold, and introducing nitrogen-oxygen mixed gas 2 :O 2 At a temperature of 0.2:0.8 to 0: 1) is sintered, and a pressurizing device is used for applying axial pressure to the sample and pressingThe force is 20MPa, the temperature is raised to 1350 ℃ (the temperature raising rate is 3-5 ℃/min), the temperature is kept for 6 hours, the temperature of the sample is lowered after the temperature is kept at the constant temperature, the pressure is unloaded, and the temperature is lowered to the room temperature along with the furnace. After cutting, grinding, polishing and other processes, the ceramic blocks are respectively processed into phi 13mm multiplied by 0.5mm ceramic plates, optical transmittance and Faraday rotation angle tests are respectively carried out after double-side polishing, and SEM scanning is carried out after hot corrosion. Fig. 3a, 3b and 3c show the XRD pattern, light transmittance profile and ceramic polished surface hot corrosion SEM image of the sintered YIG magneto-optical ceramic in example 1, respectively. As can be seen from the figure, the sintered YIG magneto-optical ceramic has a uniform garnet structure, is dense, and has excellent light transmittance.
Example 2
According to Bi 0.3 Y 2.7 Fe 5 O 12 And (3) performing powder proportioning, weighing ferric oxalate, bismuth oxide and yttrium oxide powder according to a stoichiometric ratio, adding 0.7 part of absolute ethyl alcohol (namely, 70g of powder added in 100 g) g, performing ball milling for 36 hours, drying, and sieving by a 200-mesh sieve. Adding PVA into the above mixed powder by 0.6%, mixing, sieving with 40 mesh sieve, granulating, pressing into biscuit with diameter of 15mm and thickness of 1-2 cm, placing biscuit sample in hot pressing mold, and introducing nitrogen-oxygen mixed gas 2 :O 2 At a temperature of 1.0:0 to 0.9: 0.1), sintering, applying axial pressure to the sample by using a pressurizing device, keeping the pressure constant when the pressure is 20MPa, heating to 1250 ℃ (the heating rate is 5-8 ℃/min), keeping the temperature for 4 hours, cooling the sample after constant temperature preservation, unloading the pressure, and cooling to room temperature along with the furnace. After cutting, grinding, polishing and other processes, the ceramic blocks are respectively processed into phi 13mm multiplied by 0.5mm ceramic plates, and optical transmittance and Faraday rotation angle tests and SEM section scanning are respectively carried out after double-side polishing. Fig. 4a, 4b and 4c show the XRD pattern, light transmittance profile and SEM image of the ceramic cross-section of the sintered Bi: YIG magneto-optical ceramic of example 2, respectively. It can be seen from the figure that the sintered YIG magneto-optical ceramic has a uniform garnet structure, is dense, and has good light transmittance.
Example 3
According to Ce 0.24 Y 2.76 Fe 5 O 12 Mixing the powder, and oxidizing iron oxide and iron dioxideWeighing cerium and yttrium oxide powder according to a stoichiometric ratio, adding 0.7 part (namely, 70g of powder added to 100 g) g of absolute ethyl alcohol, carrying out ball milling for 36 hours, drying, and sieving by a 200-mesh sieve. Adding 0.5 percent of PVA into the mixed powder, uniformly mixing, sieving by a 40-mesh sieve for granulation, pressing the powder into a biscuit with the diameter phi of 15mm and the thickness of 1-2 cm, putting a biscuit sample into a hot-pressing mould, sintering in a vacuum atmosphere, applying axial pressure to the sample by using a pressurizing device, keeping the pressure constant when the pressure is 20MPa, heating to 1250 ℃ (the heating rate is 2-6 ℃/min), keeping the temperature for 8 hours, cooling and unloading the pressure after the sample is kept at the constant temperature, and cooling to the room temperature along with a furnace. After cutting, grinding, polishing and other processes, the ceramic blocks are respectively processed into phi 13mm multiplied by 0.5mm ceramic plates, optical transmittance and Faraday rotation angle tests are respectively carried out after double-side polishing, and SEM scanning is carried out after hot corrosion. Fig. 5a, 5b and 5c show XRD patterns, light transmittance graphs and ceramic cross-sectional SEM images, respectively, of the sintered Bi: YIG magneto-optical ceramic in example 3. As can be seen from the figure, the sintered YIG magneto-optical ceramic has a uniform garnet structure, is dense, and has excellent light transmittance.
Example 4
According to Y 3 Fe 5 O 12 And (3) performing powder proportioning, weighing iron oxide and yttrium oxalate powder according to a stoichiometric ratio, adding 0.7 part of absolute ethyl alcohol (namely, 70g of powder is added into 100g of anhydrous ethyl alcohol), performing ball milling for 36 hours, drying, and sieving by using a 200-mesh sieve. Adding 0.5 percent of PVA into the mixed powder, uniformly mixing, sieving by a 40-mesh sieve for granulation, pressing the powder into a biscuit with the diameter phi of 15mm and the thickness of 1-2 cm, putting a biscuit sample into a hot-pressing mould, sintering in a vacuum atmosphere, applying axial pressure to the sample by using a pressurizing device, keeping the pressure constant when the pressure is 30MPa, heating to 1250 ℃ (the heating rate is 3-5 ℃/min), keeping the temperature for 12 hours at constant temperature, cooling and unloading the pressure after the sample is kept at constant temperature, and cooling to the room temperature along with a furnace. After cutting, grinding, polishing and other procedures, the ceramic blocks are respectively processed into phi 13mm multiplied by 0.5mm ceramic plates, optical transmittance and Faraday rotation angle tests are respectively carried out after double-side polishing, and SEM scanning is carried out after hot corrosion. Fig. 6a, 6b and 6c show the XRD pattern, light transmittance profile and ceramic polished surface hot corrosion SEM image of the sintered YIG magneto-optical ceramic in example 4, respectively.It can be seen from the figure that the sintered YIG magneto-optical ceramic has a uniform garnet structure, is dense, and has good light transmittance.
Example 5
According to Ce 0.12 Y 2.88 Fe 5 O 12 And (3) performing powder proportioning, weighing iron oxide, cerium oxide and yttrium oxide powder according to a stoichiometric ratio, adding 0.7 part of absolute ethyl alcohol (namely 100g of powder is added with 70g of powder), ball-milling for 36 hours, drying, and sieving by a 200-mesh sieve. Adding 0.5 percent of PVA into the mixed powder, uniformly mixing, sieving by a 40-mesh sieve for granulation, pressing the powder into a biscuit with the diameter phi of 15mm and the thickness of 1-2 cm, putting a biscuit sample into a hot-pressing mould, sintering in a vacuum atmosphere, applying axial pressure to the sample by using a pressurizing device, keeping the pressure constant when the pressure is 20MPa, heating to 1250 ℃ (the heating rate is 2-6 ℃/min), keeping the temperature for 8 hours, cooling and unloading the pressure after the sample is kept at the constant temperature, and cooling to the room temperature along with a furnace. After cutting, grinding, polishing and other procedures, the ceramic blocks are respectively processed into phi 13mm multiplied by 0.5mm ceramic plates, optical transmittance and Faraday rotation angle tests are respectively carried out after double-side polishing, and SEM scanning is carried out after hot corrosion. Fig. 7a, 7b and 7c show the XRD pattern, light transmittance profile and ceramic polished surface hot corrosion SEM image of the sintered YIG magneto-optical ceramic in example 5, respectively. It can be seen from the figure that the sintered YIG magneto-optical ceramic has a uniform garnet structure, is dense, and has excellent light transmittance.
Example 6
According to Dy 3 Fe 5 O 12 And (2) performing powder proportioning, weighing iron oxide and dysprosium oxide powder according to a stoichiometric ratio, adding 0.7 part of absolute ethyl alcohol (namely adding 70g of 100g of powder), performing ball milling for 36 hours, drying, and sieving by using a 200-mesh sieve. Adding PVA into the mixed powder in an amount of 0.5 percent, uniformly mixing, sieving with a 40-mesh sieve for granulation, pressing the powder into a biscuit with the diameter phi of 15mm and the thickness of 1-2 cm, putting a biscuit sample into a hot-pressing mould, and carrying out nitrogen-oxygen mixed gas atmosphere (N oxygen mixed gas atmosphere) 2 :O 2 At a temperature of 0.6:0.4 to 0: 1) and sintering, applying axial pressure to the sample by a pressurizing device, keeping the pressure constant when the pressure is 20MPa, heating to 1300 ℃ (the heating rate is 1-6 ℃/min), keeping the temperature for 6 hours, and allowing the sample to pass throughAnd (5) cooling and unloading the pressure after constant temperature heat preservation, and cooling to room temperature along with the furnace. After cutting, grinding, polishing and other processes, the ceramic blocks are respectively processed into phi 13mm multiplied by 0.5mm ceramic plates, optical transmittance and Faraday rotation angle tests are respectively carried out after double-side polishing, and SEM scanning is carried out after hot corrosion. Fig. 8a, 8b and 8c show XRD patterns, light transmittance graphs and ceramic polished-surface hot corrosion SEM images of the sintered DyIG magneto-optical ceramic of example 6, respectively. It can be seen from the figure that the sintered YIG magneto-optical ceramic has a uniform garnet structure, is dense, and has excellent light transmittance.
Example 7
According to Gd 3 Fe 5 O 12 And (3) performing powder blending, weighing ferric oxide and gadolinium oxide powder according to a stoichiometric ratio, adding 0.7 part (namely, 70g of powder added with 100 g) of absolute ethyl alcohol, performing ball milling for 36 hours, drying, and sieving by using a 200-mesh sieve. Adding PVA into the mixed powder in an amount of 0.6 percent, uniformly mixing, sieving with a 40-mesh sieve for granulation, pressing the powder into a biscuit with the diameter phi of 15mm and the thickness of 1-2 cm, putting a biscuit sample into a hot-pressing mould, and carrying out nitrogen-oxygen mixed gas atmosphere (N oxygen mixed gas atmosphere) 2 :O 2 At a temperature of 0.5:0.5 to 0: 1), sintering, applying axial pressure to the sample by using a pressurizing device, keeping the pressure constant when the pressure is 25MPa, heating to 1300 ℃ (the heating rate is 1-7 ℃/min), keeping the temperature for 6 hours, cooling the sample after constant temperature preservation, unloading the pressure, and cooling to room temperature along with the furnace. After cutting, grinding, polishing and other procedures, the ceramic blocks are respectively processed into phi 13mm multiplied by 0.5mm ceramic plates, optical transmittance and Faraday rotation angle tests are respectively carried out after double-side polishing, and SEM scanning is carried out after hot corrosion. Fig. 9a, 9b and 9c show XRD patterns, light transmittance graphs and ceramic polished-surface hot corrosion SEM images of the sintered GdIG magneto-optical ceramic in example 7, respectively. It can be seen from the figure that the sintered YIG magneto-optical ceramic has a uniform garnet structure, is dense, and has good light transmittance.
Table 1 shows the composition and performance parameters of rare earth iron garnet prepared according to the present invention
Claims (12)
1. The axial hot-pressing sintering preparation method of the rare earth iron garnet magneto-optical ceramic with good infrared permeability is characterized in that the general formula of the component of the rare earth iron garnet magneto-optical ceramic material is M x R 3-x Fe 5 O 12 (ii) a Wherein R is at least one of Y, sm, eu, gd, tb, dy, ho, er, tm, yb and Lu in rare earth elements; the doping ion M is at least one of Ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb, lu and Bi, and x is more than or equal to 0 and less than or equal to 2;
the axial hot-pressing sintering preparation method of the rare earth iron garnet magneto-optical ceramic material comprises the following steps:
(1) The component general formula of the rare earth iron garnet magneto-optical ceramic material is M x R 3-x Fe 5 O 12 Weighing and mixing the M source, the R source and the Fe source according to the stoichiometric ratio to obtain mixed powder;
(2) Pressing and molding the obtained mixed powder by a dry pressing method to obtain a biscuit;
(3) Placing the obtained biscuit in a hot pressing furnace for hot pressing sintering to obtain the rare earth iron garnet magneto-optical ceramic material; the hot-pressing sintering atmosphere is a vacuum atmosphere or a nitrogen-oxygen mixed gas; the method comprises the following steps of (1) realizing oxygen atmospheres with different oxygen partial pressures as hot-pressing sintering atmospheres by vacuum and introducing nitrogen-oxygen mixed gas, wherein the flow rate of the nitrogen-oxygen mixed gas is 1-25L/min;
the temperature of the hot-pressing sintering is 1150-1400 ℃; the time of the hot-pressing sintering is 6 to 24 hours; the axial pressure of the hot-pressing sintering is 10-80 MPa;
the rare earth iron garnet magneto-optical ceramic is a single garnet phase, the density is more than 99%, and the transmittance reaches 40% -100% of the theoretical transmittance.
2. The axial hot-pressing sintering production method as claimed in claim 1, wherein x is 0. Ltoreq. X.ltoreq.0.6.
3. The axial hot-pressing sintering production method as claimed in claim 2, wherein x is 0. Ltoreq. X.ltoreq.0.24.
4. The axial hot-pressing sintering production method according to claim 1, wherein the M source is selected from M 2 O 3 、MO 2 、M 4 O 7 、M 2 (CO 3 ) 3 、M(HCO 3 ) 3 、M 2 (C 2 O 4 ) 3 、M(Ac) 3 、M(NO 3 ) 3 At least one of (a);
the R source is selected from R 2 O 3 、R 4 O 7 、R 2 (CO 3 ) 3 、RPO 4 、R(HCO 3 ) 3 、R 2 (C 2 O 4 ) 3 、R(Ac) 3 、R(NO 3 ) 3 At least one of;
the Fe source is selected from Fe 2 O 3 、FeO、Fe 3 O 4 、Fe(NO 3 ) 3 、Fe 2 (C 2 O 4 ) 3 、Fe(Ac) 3 At least one of (1).
5. The axial hot-pressing sintering preparation method according to claim 1, wherein a binder is further added to the mixed powder; the binder is selected from at least one of polyvinyl alcohol PVA, ammonium polyacrylate and carboxymethyl cellulose; the addition amount of the binder is 0.3-1 wt% of the total mass of the mixed powder.
6. The axial hot-pressing sintering preparation method as claimed in claim 5, wherein the binder is 0.5-0.7 wt% of the total mass of the mixed powder.
7. The axial hot-pressing sintering preparation method according to claim 1, wherein N in the nitrogen-oxygen mixed gas is 2 And O 2 The volume ratio of (1) to (0) to (1), and the sum of the volumes of the two is 1;
n in the nitrogen-oxygen mixed gas for different systems and different doping ions 2 And O 2 The volume ratio of (a):
for pure phase YIG, N is selected 2 :O 2 The volume ratio is 0.7;
for Bi YIG ceramic, N is selected 2 :O 2 The volume ratio is 1.
8. The axial hot-pressing sintering preparation method as claimed in claim 7, wherein N is selected for pure phase YIG 2 :O 2 The volume ratio is 0.5; for Bi YIG ceramic, N is selected 2 :O 2 The volume ratio is 1.
9. The axial hot-pressing sintering preparation method according to claim 1 or 7, wherein the flow rate of the nitrogen-oxygen mixed gas is 3 to 15L/min.
10. The axial hot-pressing sintering preparation method as claimed in claim 1, wherein the temperature of the hot-pressing sintering is 1200-1350 ℃; the time of the hot-pressing sintering is 8-12 hours.
11. The production method of axial hot-pressing sintering according to claim 1 or 10, wherein the heating rate of the hot-pressing sintering is 1-10 ℃/min.
12. The axial hot-pressing sintering preparation method according to claim 1, wherein the axial pressure of the hot-pressing sintering is 20 to 60MPa.
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