CN111302784B - Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body - Google Patents
Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body Download PDFInfo
- Publication number
- CN111302784B CN111302784B CN202010004079.0A CN202010004079A CN111302784B CN 111302784 B CN111302784 B CN 111302784B CN 202010004079 A CN202010004079 A CN 202010004079A CN 111302784 B CN111302784 B CN 111302784B
- Authority
- CN
- China
- Prior art keywords
- neodymium
- iron garnet
- doped yttrium
- solidified body
- based ceramic
- 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.)
- Expired - Fee Related
Links
- 239000002223 garnet Substances 0.000 title claims abstract description 64
- MTRJKZUDDJZTLA-UHFFFAOYSA-N iron yttrium Chemical compound [Fe].[Y] MTRJKZUDDJZTLA-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000000919 ceramic Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 58
- 238000001035 drying Methods 0.000 claims abstract description 48
- 239000002243 precursor Substances 0.000 claims abstract description 37
- 239000000203 mixture Substances 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 230000005496 eutectics Effects 0.000 claims abstract description 27
- 150000003839 salts Chemical class 0.000 claims abstract description 27
- 239000011812 mixed powder Substances 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 229910052595 hematite Inorganic materials 0.000 claims abstract description 12
- 239000011019 hematite Substances 0.000 claims abstract description 12
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 claims abstract description 12
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 33
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000000967 suction filtration Methods 0.000 claims description 12
- 239000011780 sodium chloride Substances 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 5
- 239000002901 radioactive waste Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910052768 actinide Inorganic materials 0.000 description 1
- 150000001255 actinides Chemical class 0.000 description 1
- 230000003592 biomimetic effect Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- -1 diabase Chemical compound 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000002927 high level radioactive waste Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000005486 microgravity Effects 0.000 description 1
- 238000009768 microwave sintering Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052590 monazite Inorganic materials 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2675—Other ferrites containing rare earth metals, e.g. rare earth ferrite garnets
-
- 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
-
- 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
-
- 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Soft Magnetic Materials (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The inventionA preparation method of a neodymium-doped yttrium iron garnet-based ceramic solidified body is provided, which comprises the following steps: based on neodymium-doped yttrium-iron garnet (Y)3‑xNdxFe5O12X is 0.1 to 2.0), in accordance with Fe2O3∶Y2O3∶Nd2O3Taking dried hematite and Y according to the proportion of 5: 3-x: x/22O3And Nd2O3Mixing the powder to prepare mixed powder; mixing the mixed powder with eutectic salt according to a certain mass ratio, adding a proper amount of ethanol, grinding to obtain a precursor, and drying the precursor in a drying oven; and (3) putting the dried precursor into an atmosphere furnace, heating to 900-1100 ℃, preserving heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture. The preparation method of the neodymium-doped yttrium iron garnet-based ceramic solidified body is low in synthesis temperature and high in synthesis rate.
Description
Technical Field
The invention relates to a preparation method of a garnet-based ceramic solidified body, in particular to a preparation method of a neodymium-doped yttrium iron garnet-based ceramic solidified body.
Background
With the rapid development of nuclear energy, nuclear reactor fuels generate large amounts of High Level Waste (HLW) with radioactivity, toxicity and long half-life, posing a great threat to human survival. At present, the radioactive waste is disposed of by first solidifying the radioactive waste and then geologically treating the solidified radioactive waste. Since the early 70's of the 20 th century, various customized ceramic waste matrices containing mineral phases have been proposed, such as monazite, diabase, zircon and fluorite. Garnets have attracted considerable attention in recent years as a new matrix for the solidification of radioactive wastes due to their large solid solution content and good chemical stability towards actinides.
Meanwhile, the preparation method of the ceramic solidification matrix comprises the conventional solid-phase sintering, as well as the chemical vapor deposition method, the physical vapor deposition method, the microgravity and hypergravity synthesis method, the biomimetic synthesis method, the sol-gel method, the hydrothermal method, the microwave sintering method, the solid-phase method and other methods. However, in the above methods, each of them has its merits and demerits, such as the precipitation method is simple to operate, but is liable to introduce new impurities; the hydrothermal method has high cost and is difficult to produce in a large scale; the solid phase method is the most traditional method, has simple operation and low cost, can be used for large-scale production, but has high synthesis temperature and low synthesis rate.
Disclosure of Invention
In view of the above technical problems, the present invention needs to provide a method for preparing a neodymium-doped yttrium iron garnet-based ceramic solidified body with simple operation, high synthesis rate and low synthesis temperature.
A preparation method of a neodymium-doped yttrium iron garnet-based ceramic solidified body comprises the following steps:
based on neodymium-doped yttrium-iron garnet (Y)3-xNdxFe5O12X is 0.1 to 2.0), in accordance with Fe2O3：Y2O3：Nd2O35: 3-x: taking dried hematite and Y according to the ratio of x/22O3And Nd2O3Mixing the powder to prepare mixed powder;
mixing the mixed powder with eutectic salt according to a set mass ratio, adding a proper amount of ethanol, grinding to obtain a precursor, and drying the precursor in a drying oven;
and (3) putting the dried precursor into an atmosphere furnace, heating to 900-1100 ℃, preserving the heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture.
Further, the preparation method of the neodymium-doped yttrium iron garnet-based ceramic solidified body further comprises the steps of dispersing the powder mixture in pure water, and obtaining pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder through washing, suction filtration, filtration and drying processes.
Further, the temperature increase rate was 5 ℃/min.
Further, the eutectic salt is a mixture of NaCl and KCl in equimolar proportion.
Further, the grinding time t11 hour.
Further, the drying time t214 hours.
Further, the mass ratio of the mixed powder to the eutectic salt is 1: 1-10.
The preparation method of the neodymium-doped garnet-based ceramic solidified body is implemented by mixing Fe2O3、Y2O3、Nd2O3And grinding and mixing the precursor with eutectic salt, and sintering in an atmosphere furnace, so that the neodymium-doped yttrium iron garnet-based ceramic solidified body can be prepared at a lower temperature, the process operation is simple, and the cost is reduced.
Drawings
FIG. 1 is a flow chart of the inventive method for preparing a neodymium-doped yttrium iron garnet-based ceramic solidified body.
FIG. 2 is an XRD pattern of a neodymium-doped yttrium iron garnet-based ceramic solidified body powder prepared in examples 1 to 3 of the present invention and a standard XRD pattern of neodymium-doped yttrium iron garnet.
FIG. 3 is an XRD pattern of a neodymium-doped yttrium iron garnet-based ceramic solidified body powder prepared in examples 4 to 8 of the present invention and a standard XRD pattern of neodymium-doped yttrium iron garnet.
The following detailed description will further illustrate the invention in conjunction with the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The following will explain the preparation method of the neodymium-doped yttrium iron garnet-based ceramic solidified body in detail by combining the attached drawings and the embodiment.
As shown in fig. 1, a method for preparing a neodymium-doped yttrium iron garnet-based ceramic solidified body comprises the following steps:
s101: based on neodymium-doped yttrium-iron garnet (Y)3-xNdxFe5O12X ═ 0.1-2.0) stoichiometric ratio, i.e. Fe2O3：Y2O3：Nd2O35: 3-x: taking dried hematite (Fe) according to the ratio of x/22O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder;
s102: mixing the mixed powder with eutectic salt according to a set mass ratio, adding a proper amount of ethanol, grinding for a grinding time t1Drying the precursor in a drying oven for 1 hour, wherein the drying time t is2The eutectic salt comprises but is not limited to an equimolar mixture of NaCl and KCl, and the mass ratio is 1: 1-10;
s103: putting the dried precursor into an atmosphere furnace, heating to 900-1100 ℃ at the heating rate of 5 ℃/min (centigrade per minute), preserving the heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture;
s104: and dispersing the powder mixture in pure water, and performing washing, suction filtration, drying and other processes to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder.
Example 1:
based on neodymium-doped yttrium-iron garnet (Y)2.6Nd0.4Fe5O12) According to the chemical formula of Fe2O3：Y2O3：Nd2O3Taking dried hematite (Fe) according to the proportion of 5:2.6:0.22O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; mixing the mixed powder with eutectic salt according to the mass ratio of 1:1, adding a proper amount of ethanol, grinding for a time t to obtain a precursor1Drying the precursor in a drying oven for 1 hour, wherein the drying time t is2For 14 hours, in this example, the eutectic salt is an equimolar mixture of NaCl and KCl; putting the dried precursor into an atmosphere furnace, heating to 900 ℃ at the heating rate of 5 ℃/min (centigrade per minute), preserving the heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture; and dispersing the powder mixture in pure water, and performing washing, suction filtration, drying and other processes to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder.
Example 2:
based on neodymium-doped yttrium-iron garnet (Y)2.6Nd0.4Fe5O12) According to the chemical formula of Fe2O3：Y2O3：Nd2O3Taking dried hematite (Fe) according to the proportion of 5:2.6:0.22O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; mixing the mixed powder with eutectic salt according to the mass ratio of 1:5, mixing, adding a proper amount of ethanol, grinding for a time t to obtain a precursor1Drying the precursor in a drying oven for 1 hour, wherein the drying time t is2For 14 hours, in this example, the eutectic salt is an equimolar mixture of NaCl and KCl; will be provided withPutting the dried precursor into an atmosphere furnace, heating to 1000 ℃ at the heating rate of 5 ℃/min (centigrade per minute), preserving the heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture; and dispersing the powder mixture in pure water, and performing washing, suction filtration, drying and other processes to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder.
Example 3:
based on neodymium-doped yttrium-iron garnet (Y)2.6Nd0.4Fe5O12) According to the chemical formula of Fe2O3：Y2O3：Nd2O3Taking dried hematite (Fe) according to the proportion of 5:2.6:0.22O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; mixing the mixed powder with eutectic salt according to the mass ratio of 1:10, adding a proper amount of ethanol, grinding for a period of time t to obtain a precursor1Drying the precursor in a drying oven for 1 hour, wherein the drying time t is2For 14 hours, in this example, the eutectic salt is an equimolar mixture of NaCl and KCl; putting the dried precursor into an atmosphere furnace, heating to 1100 ℃ at the heating rate of 5 ℃/min (centigrade per minute), preserving the heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture; and dispersing the powder mixture in pure water, and performing washing, suction filtration, drying and other processes to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder.
FIG. 2 is an XRD pattern of the neodymium-doped yttrium iron garnet-based ceramic solidified body powder prepared in examples 1 to 3 and a standard XRD pattern of the neodymium-doped yttrium iron garnet. As can be seen from FIG. 2, the main phases of the neodymium-doped yttrium iron garnet-based ceramic solidified body powders prepared in examples 1 to 3 were Nd: y is3Fe5O12And the solidified body powder has a higher crystallinity. Meanwhile, as can be seen from fig. 2, the preparation method can prepare the neodymium-doped yttrium iron garnet-based ceramic solidified body at a relatively low temperature (about 1000 ℃).
Example 4:
based on neodymium-doped yttrium-iron garnet (Y)3-xNdxFe5O12And x is 0.1) taking dried hematite (Fe) according to the stoichiometric ratio2O3)、Y2O3And Nd2O3Mixing the powder to prepare mixed powder; mixing the mixed powder with eutectic salt according to the mass ratio of 1:1, adding a proper amount of ethanol, grinding for a time t to obtain a precursor1Drying the precursor in a drying oven for 1 hour, wherein the drying time t is2For 14 hours, in this example, the eutectic salt is an equimolar mixture of NaCl and KCl; putting the dried precursor into an atmosphere furnace, heating to 900 ℃ at the heating rate of 5 ℃/min (centigrade per minute), preserving the heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture; and dispersing the powder mixture in pure water, and performing washing, suction filtration, drying and other processes to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder.
Example 5:
based on neodymium-doped yttrium-iron garnet (Y)3-xNdxFe5O12X is 0.5) stoichiometric ratio and dried hematite (Fe)2O3)、Y2O3And Nd2O3Mixing the powder to prepare mixed powder; mixing the mixed powder with eutectic salt according to the mass ratio of 1:3, adding a proper amount of ethanol, grinding for a time t to obtain a precursor1Drying the precursor in a drying oven for 1 hour, wherein the drying time t is2For 14 hours, in this example, the eutectic salt is an equimolar mixture of NaCl and KCl; putting the dried precursor into an atmosphere furnace, heating to 1000 ℃ at the heating rate of 5 ℃/min (centigrade per minute), preserving the temperature for 3 hours, and cooling to room temperature to obtain a sintered powder mixture; and dispersing the powder mixture in pure water, and performing washing, suction filtration, drying and other processes to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder.
Example 6:
based on neodymium-doped yttrium-iron garnet (Y)3-xNdxFe5O12X is 1.0) stoichiometric ratio and dried hematite (Fe)2O3)、Y2O3And Nd2O3Mixing the powder to prepare mixed powder; mixing the mixed powder with eutectic salt according to the mass ratio of 1:5, adding a proper amount of ethanol, grinding for a time t to obtain a precursor1Drying the precursor in a drying oven for 1 hour, wherein the drying time t is2For 14 hours, in this example, the eutectic salt is an equimolar mixture of NaCl and KCl; putting the dried precursor into an atmosphere furnace, heating to 1100 ℃ at the heating rate of 5 ℃/min (centigrade per minute), preserving the heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture; and dispersing the powder mixture in pure water, and performing washing, suction filtration, drying and other processes to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder.
Example 7:
based on neodymium-doped yttrium-iron garnet (Y)3-xNdxFe5O12X is 1.5) taking dried hematite (Fe) in stoichiometric ratio2O3)、Y2O3And Nd2O3Mixing the powder to prepare mixed powder; mixing the mixed powder with eutectic salt according to the mass ratio of 1:5, adding a proper amount of ethanol, grinding for a time t to obtain a precursor1Drying the precursor in a drying oven for 1 hour, wherein the drying time t is2For 14 hours, in this example, the eutectic salt is an equimolar mixture of NaCl and KCl; putting the dried precursor into an atmosphere furnace, heating to 1100 ℃ at the heating rate of 5 ℃/min (centigrade per minute), preserving the heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture; and dispersing the powder mixture in pure water, and performing washing, suction filtration, drying and other processes to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder.
Example 8:
based on neodymium-doped yttrium-iron garnet (Y)3-xNdxFe5O12X is 2.0) stoichiometric ratio and dried hematite (Fe)2O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; mixing the mixed powder with eutectic salt according to the mass ratio of 1:10, adding a proper amount of ethanol, grinding for a time t to obtain a precursor1Drying the precursor in a drying oven for 1 hour, wherein the drying time t is2For 14 hours, in this example, the eutectic salt is an equimolar mixture of NaCl and KCl; putting the dried precursor into an atmosphere furnace, heating to 1100 ℃ at the heating rate of 5 ℃/min (centigrade per minute), preserving the heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture; and dispersing the powder mixture in pure water, and performing washing, suction filtration, drying and other processes to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder.
As shown in the figure, XRD patterns of the yttrium iron garnet-based ceramic solidified body powders prepared in examples 4 to 8 and a standard XRD pattern of the yttrium iron garnet-based ceramic solidified body were obtained. As can be seen from the figure, the yttrium iron garnet-based ceramic solidified body powders prepared in examples 5 and 6 have a main phase of yttrium iron garnet (Y)3Fe5O12) The Nd was successfully incorporated and the solidified powder had a higher crystallinity, and it was shown that pure phase yttrium iron garnet could be obtained at a lower temperature. Examples 7, 8 show new phases but still show successful Nd incorporation.
It is understood that in this embodiment, a method for preparing a neodymium-doped yttrium iron garnet-based ceramic solidified body includes dispersing the powder mixture in pure water, and performing the procedures of washing, filtering, drying, etc. to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder, but is not limited thereto, and in other embodiments, the procedures: dispersing the powder mixture in pure water, and performing washing, suction filtration, drying and other processes to obtain pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder which can be deleted without affecting the preparation method of the neodymium-doped yttrium iron garnet-based ceramic solidified body.
The preparation method of the neodymium-doped garnet-based ceramic solidified body is implemented by mixing Fe2O3、Y2O3、Nd2O3And grinding and mixing the precursor with eutectic salt, and sintering in an atmosphere furnace, so that the neodymium-doped yttrium iron garnet-based ceramic solidified body can be prepared at a lower temperature, the process operation is simple, and the cost is reduced.
In addition, other modifications within the spirit of the invention may occur to those skilled in the art, and such modifications are, of course, included within the scope of the invention as claimed.
Claims (6)
1. A preparation method of a neodymium-doped yttrium iron garnet-based ceramic solidified body is characterized by comprising the following steps: the preparation method of the neodymium-doped yttrium iron garnet-based ceramic solidified body comprises the following steps:
based on neodymium-doped yttrium-iron garnet (Y)3-xNdxFe5O12X is 0.1 to 2.0), in accordance with Fe2O3：Y2O3：Nd2O35: 3-x: taking dried hematite and Y according to the ratio of x/22O3And Nd2O3Mixing the powder to prepare mixed powder;
mixing the mixed powder with eutectic salt according to a set mass ratio, adding a proper amount of ethanol, grinding to obtain a precursor, and drying the precursor in a drying oven, wherein the eutectic salt is a mixture of NaCl and KCl in an equimolar amount;
and (3) putting the dried precursor into an atmosphere furnace, heating to 900-1100 ℃, preserving the heat for 3 hours, and cooling to room temperature to obtain a sintered powder mixture.
2. The method of preparing the neodymium-doped yttrium iron garnet-based ceramic solidified body of claim 1, wherein the method comprises the following steps: the preparation method of the neodymium-doped yttrium iron garnet-based ceramic solidified body further comprises the steps of dispersing the powder mixture in pure water, and obtaining pure neodymium-doped yttrium iron garnet-based ceramic solidified body powder through washing, suction filtration, filtration and drying processes.
3. The method of preparing the neodymium-doped yttrium iron garnet-based ceramic solidified body of claim 1, wherein the method comprises the following steps: the heating rate is 5 ℃/min.
4. The method of preparing the neodymium-doped yttrium iron garnet-based ceramic solidified body of claim 1, wherein the method comprises the following steps: the grinding time t11 hour.
5. The method of preparing the neodymium-doped yttrium iron garnet-based ceramic solidified body of claim 1, wherein the method comprises the following steps: the drying time t214 hours.
6. The method of preparing the neodymium-doped yttrium iron garnet-based ceramic solidified body of claim 1, wherein the method comprises the following steps: the mass ratio of the mixed powder to the eutectic salt is 1: 1-10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010004079.0A CN111302784B (en) | 2020-01-03 | 2020-01-03 | Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010004079.0A CN111302784B (en) | 2020-01-03 | 2020-01-03 | Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111302784A CN111302784A (en) | 2020-06-19 |
| CN111302784B true CN111302784B (en) | 2022-04-12 |
Family
ID=71158217
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010004079.0A Expired - Fee Related CN111302784B (en) | 2020-01-03 | 2020-01-03 | Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111302784B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851348A (en) * | 2021-01-11 | 2021-05-28 | 西南科技大学 | Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body |
| CN115180945A (en) * | 2021-04-02 | 2022-10-14 | 中国科学院上海硅酸盐研究所 | Iron-based garnet magneto-optical transparent ceramic and preparation method thereof |
| CN113603475B (en) * | 2021-07-27 | 2022-10-18 | 西南科技大学 | Preparation method of trivalent chromium ion doped magnesium aluminate spinel transparent ceramic |
| CN114702313B (en) * | 2022-04-02 | 2022-12-30 | 西南科技大学 | Neodymium-doped zircon-based ceramic solidified body and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1418597A1 (en) * | 2002-11-08 | 2004-05-12 | Van den Brandhof, Evert Alexander | Method for producing ferromagnetic garnet material, garnet material and its use |
| US7022303B2 (en) * | 2002-05-13 | 2006-04-04 | Rutgers, The State University | Single-crystal-like materials |
| CN101269956A (en) * | 2008-04-29 | 2008-09-24 | 烁光特晶科技有限公司 | Method of preparing yttrium aluminum garnet transparent ceramic doping neodymium |
| CN102942226A (en) * | 2012-11-10 | 2013-02-27 | 南昌航空大学 | Preparation method for yttrium iron garnet powder |
| CN103626487A (en) * | 2013-11-26 | 2014-03-12 | 中国科学院福建物质结构研究所 | Method for preparing yttrium aluminium garnet transparent ceramic with composite structure |
| CN108530058A (en) * | 2018-05-17 | 2018-09-14 | 合肥工业大学 | A kind of preparation method with negative permittivity barium titanate/yttrium iron garnet composite ceramics |
-
2020
- 2020-01-03 CN CN202010004079.0A patent/CN111302784B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7022303B2 (en) * | 2002-05-13 | 2006-04-04 | Rutgers, The State University | Single-crystal-like materials |
| EP1418597A1 (en) * | 2002-11-08 | 2004-05-12 | Van den Brandhof, Evert Alexander | Method for producing ferromagnetic garnet material, garnet material and its use |
| CN101269956A (en) * | 2008-04-29 | 2008-09-24 | 烁光特晶科技有限公司 | Method of preparing yttrium aluminum garnet transparent ceramic doping neodymium |
| CN102942226A (en) * | 2012-11-10 | 2013-02-27 | 南昌航空大学 | Preparation method for yttrium iron garnet powder |
| CN103626487A (en) * | 2013-11-26 | 2014-03-12 | 中国科学院福建物质结构研究所 | Method for preparing yttrium aluminium garnet transparent ceramic with composite structure |
| CN108530058A (en) * | 2018-05-17 | 2018-09-14 | 合肥工业大学 | A kind of preparation method with negative permittivity barium titanate/yttrium iron garnet composite ceramics |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111302784A (en) | 2020-06-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111302784B (en) | Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body | |
| CN102584018B (en) | A kind of method of preparing high-radioactivity effluent glass-ceramic solidified body in microwave process | |
| CN105777101B (en) | A kind of sodium zirconium phosphate-monazite glass ceramics firming body and preparation method thereof | |
| CN101826376B (en) | Preparation method of vitrification substrate for radioactive nuclear waste | |
| CN111039674B (en) | Gadolinium zirconate ceramic for solidifying TRPO simulation waste and preparation method thereof | |
| CN104844190B (en) | A kind of preparation method of fluor-apatite ceramic solidification body | |
| CN110734283A (en) | Preparation method of novel phosphate composite ceramic solidified material | |
| CN110817875A (en) | Ti3AlC2Powder and preparation method thereof | |
| CN112466503A (en) | Preparation method of glass ceramic body for solidifying Cs-containing soil | |
| CN110335693A (en) | A kind of preparation method for radioactive waste glass solidification basic material and glass solidified body | |
| CN103408304B (en) | Preparation method of kularite ceramic solidifying body | |
| CN108585803B (en) | Preparation method of ring-formation-free pellet rotary kiln lining | |
| CN112851348A (en) | Preparation method of neodymium-doped yttrium iron garnet-based ceramic solidified body | |
| CN110723977B (en) | With Cu2+Formation of CuAl in alumina porcelain2O4Method for preparing black alumina ceramic by using main colorant | |
| AU2021101600A4 (en) | Preparation method of neodymium-doped yttrium iron garnet-based ceramic immobilized matrices | |
| CN112125281B (en) | Method for preparing lanthanide oxide material by using coprecipitation combined with molten salt deposition method and application thereof | |
| CN114075075A (en) | Preparation method and application of high-entropy ceramic material with gamma radiation shielding effect | |
| CN102583491A (en) | Method for preparing high-purity yttrium oxide from gemstone waste and/or ceramic waste | |
| CN102557687B (en) | FeAl2O4-Al2O3 composite powder and method for preparing FeAl2O4-Al2O3 composite powder under reducing atmosphere | |
| Li et al. | Preparation and densification study of sodium zirconium phosphate-doped microwave-sintered uranium tailing ceramics | |
| KR970008749B1 (en) | Process for the preparation of nickel-zinc ferrite powder | |
| CN110028248B (en) | Method for preparing pollucite microcrystalline glass by low-temperature liquid phase sintering | |
| CN112159240A (en) | Preparation method for synthesizing lanthanum hafnate powder by molten salt growth method | |
| KR960701804A (en) | Doped zinc oxide powder, its preparation method and ceramics prepared from the powder | |
| CN114702313B (en) | Neodymium-doped zircon-based ceramic solidified body and preparation method thereof |
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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20220412 |