CN112851348A - 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
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- 239000002223 garnet Substances 0.000 title claims abstract description 63
- MTRJKZUDDJZTLA-UHFFFAOYSA-N iron yttrium Chemical compound [Fe].[Y] MTRJKZUDDJZTLA-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000000919 ceramic Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 35
- 239000002243 precursor Substances 0.000 claims abstract description 31
- 239000000843 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 24
- 239000011812 mixed powder Substances 0.000 claims abstract description 24
- 238000000227 grinding Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000009768 microwave sintering Methods 0.000 claims abstract description 14
- 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
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 24
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 20
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 11
- 238000009837 dry grinding Methods 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims 1
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 abstract 2
- 229910052779 Neodymium Inorganic materials 0.000 abstract 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 abstract 1
- 230000000087 stabilizing effect Effects 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 229910052768 actinide Inorganic materials 0.000 description 1
- 150000001255 actinides Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000005365 phosphate glass Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本发明提出了一种掺钕钇铁石榴石基陶瓷固化体的制备方法，其包括以下流程：根据掺钕钇铁石榴石(Y3‑xNdxFe5O12，x＝0.5‑2.0)化学计量比即Fe2O3∶Y2O3∶Nd2O3＝5∶3‑x∶x/2的比例取干燥后的赤铁矿、Y2O3及Nd2O3粉体混合，制得混合粉体；将所述混合粉体先干磨到无色差，再加入适量乙醇进行研磨得到前驱体，将所述前驱体放入干燥箱内进行干燥；将干燥后的前驱体使用粉末压片机在12MPa压力下，稳压压制成直径12mm的圆形薄片；将压制好的圆形薄片放入微波烧结炉中升温至1100‑1300℃，并保温2小时，冷却至室温后即可得到纯净的掺钕钇铁石榴石基陶瓷固化体。所述掺钕钇铁石榴石基陶瓷固化体的制备方法制得陶瓷固化体致密性好且操作简单。
The present invention provides a method for preparing a neodymium - doped yttrium - iron garnet-based ceramic solidified body, which comprises the following procedures: The stoichiometric ratio is Fe 2 O 3 : Y 2 O 3 : Nd 2 O 3 =5:3-x:x/2, and the dried hematite, Y 2 O 3 and Nd 2 O 3 powders are mixed , to obtain a mixed powder; first dry-grind the mixed powder until there is no color difference, then add an appropriate amount of ethanol for grinding to obtain a precursor, and put the precursor into a drying box for drying; use the dried precursor to use Under the pressure of 12MPa, the powder tableting machine presses it into circular slices with a diameter of 12mm; put the pressed circular slices into a microwave sintering furnace to heat up to 1100-1300°C, keep the temperature for 2 hours, and then cool down to room temperature. Pure neodymium-doped yttrium iron garnet-based ceramic solidified body can be obtained. The preparation method of the neodymium-doped yttrium iron garnet-based ceramic solidified body produces the ceramic solidified body with good compactness and simple operation.
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
Nuclear waste disposal is one of the most formidable challenges for sustainable nuclear energy growth. High level nuclear waste (HLW) accounts for only 3% of the total radioactive volume disposed of, however, it accounts for 95% of radioactivity because it contains a wide variety of radionuclides in waste streams with long half-lives. Borosilicate and phosphate glass matrices are now widely used in the form of nuclear waste, but the tolerance of the glass matrix is of concern and there is still a need for more durable forms of waste. Garnet is a strong silicate mineral that can remain stable over a wide range of pressures and temperatures and on geological time scales; and the garnet structure has 8, 6 and 4 coordination positions to better accommodate different nuclides; meanwhile, the garnet is limited in topological structure, the radiation tolerance of the garnet is weakly connected with chemical components, and the garnet can be well used as a new storage form of actinide nuclide. As a result, garnet ceramic solidification matrices are receiving more and more extensive research and attention.
The solid-phase sintering method is a conventional ceramic solidified body synthesis method, but higher sintering temperature and longer heat preservation time are needed for obtaining a single pure phase; the self-propagating combustion method is simple and convenient to operate, but the compactness of the prepared ceramic solidified body is insufficient; discharge plasma sintering (SPS) can be rapidly sintered, but typically only one sample can be made at a time.
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 good sample compactness.
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 ═ 0.5-2.0) stoichiometric ratio, i.e. Fe2O3∶Y2O3∶Nd2O3Taking dried hematite (Fe) at the ratio of 5: 3-x: x/22O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder;
dry grinding the mixed powder until no color difference exists, adding a proper amount of ethanol, and grinding for a grinding time t1Putting the precursor into a drying oven for drying for 0.5 hour, wherein the drying time t is214 hours; the dried precursor is pressed into a round slice with the diameter of 12mm under the pressure of 12MPa by a powder tablet press, and the pressure stabilizing time t is32.5 minutes;
and (3) putting the pressed round slice into a microwave sintering furnace, heating to 1100 ℃ and 1300 ℃ at the heating rate of 10 ℃/min (centigrade per minute), preserving the heat for 0.5-6 hours, and cooling to room temperature to obtain the pure 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，Nd2O3After the mixed precursor is ground, the mixed precursor is sintered in a microwave sintering furnace, so that the neodymium-doped yttrium iron garnet-based ceramic solidified body with good compactness and high crystallinity can be prepared in a short time, and the process operation is simple.
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 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 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 method for preparing an yttrium iron garnet-based ceramic solidified body according to the present invention will be described in further detail with reference to the accompanying drawings and embodiments.
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 is 0-2.0) stoichiometric ratio, i.e. Fe2O3∶Y2O3∶Nd2O3Taking dried hematite (Fe) at the ratio of 5: 3-x: x/22O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder;
s102: dry grinding the mixed powder until no color difference exists, adding a proper amount of ethanol, and grinding for a grinding time t1Putting the precursor into a drying oven for drying for 0.5 hour, wherein the drying time t is214 hours;
s103: the dried precursor is pressed into a round slice with the diameter of 12mm under the pressure of 12MPa by a powder tablet press, and the pressure stabilizing time t is32.5 minutes;
s104: and (3) putting the pressed round slice into a microwave sintering furnace, heating to 1100 ℃ and 1300 ℃ at the heating rate of 10 ℃/min (centigrade per minute), preserving the heat for 0.5-6 hours, and cooling to room temperature to obtain the pure neodymium-doped yttrium iron garnet-based ceramic solidified body.
Example 1:
based on neodymium-doped yttrium-iron garnet (Y)2.5Nd0.5Fe5O12) Stoichiometric ratio of Fe2O3、Y2O3And Nd2O3Taking dried hematite (Fe) at a ratio of 5: 2.5: 0.252O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; dry grinding the mixed powder until no color difference exists, adding a proper amount of ethanol, and grinding for a grinding time t1Putting the precursor into a drying oven for drying for 0.5 hour, wherein the drying time t is214 hours; the dried precursor is pressed into a round slice with the diameter of 12mm under the pressure of 12MPa by a powder tablet press, and the pressure stabilizing time t is32.5 minutes; and (3) putting the pressed round slice into a microwave sintering furnace, heating to 1100 ℃ at the heating rate of 10 ℃/min (centigrade per minute), preserving the heat for 0.5 hour, and cooling to room temperature to obtain the pure neodymium-doped yttrium iron garnet-based ceramic solidified body.
Example 2:
based on neodymium-doped yttrium-iron garnet (Y)2.5Nd0.5Fe5O12) Stoichiometric ratio of Fe2O3、Y2O3And Nd2O3Taking dried hematite (Fe) at a ratio of 5: 2.5: 0.252O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; dry grinding the mixed powder until no color difference exists, and then addingGrinding with proper amount of ethanol for a period of time t to obtain a precursor1Putting the precursor into a drying oven for drying for 0.5 hour, wherein the drying time t is214 hours; the dried precursor is pressed into a round slice with the diameter of 12mm under the pressure of 12MPa by a powder tablet press, and the pressure stabilizing time t is32.5 minutes; and (3) putting the pressed round slice into a microwave sintering furnace, heating to 1200 ℃ at the heating rate of 10 ℃/min (centigrade per minute), preserving the heat for 0.5 hour, and cooling to room temperature to obtain the pure neodymium-doped yttrium iron garnet-based ceramic solidified body.
Example 3:
based on neodymium-doped yttrium-iron garnet (Y)2.5Nd0.5Fe5O12) Stoichiometric ratio of Fe2O3、Y2O3And Nd2O3Taking dried hematite (Fe) at a ratio of 5: 2.5: 0.252O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; dry grinding the mixed powder until no color difference exists, adding a proper amount of ethanol, and grinding for a grinding time t1Putting the precursor into a drying oven for drying for 0.5 hour, wherein the drying time t is214 hours; the dried precursor is pressed into a round slice with the diameter of 12mm under the pressure of 12MPa by a powder tablet press, and the pressure stabilizing time t is32.5 minutes; and (3) putting the pressed round slice into a microwave sintering furnace, heating to 1300 ℃ at the heating rate of 10 ℃/min (centigrade per minute), preserving the heat for 0.5 hour, and cooling to room temperature to obtain the pure 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 prepared in examples 1 to 3 and a standard XRD pattern of 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 bodies 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 be rapidly performed at high temperatureThen preparing the pure neodymium-doped yttrium iron garnet-based ceramic solidified body.
Example 4:
based on neodymium-doped yttrium-iron garnet (Y)2.5Nd0.5Fe5O12) Stoichiometric ratio of Fe2O3、Y2O3And Nd2O3Taking dried hematite (Fe) at a ratio of 5: 2.5: 0.252O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; dry grinding the mixed powder until no color difference exists, adding a proper amount of ethanol, and grinding for a grinding time t1Putting the precursor into a drying oven for drying for 0.5 hour, wherein the drying time t is214 hours; the dried precursor is pressed into a round slice with the diameter of 12mm under the pressure of 12MPa by a powder tablet press, and the pressure stabilizing time t is32.5 minutes; and (3) putting the pressed round slice into a microwave sintering furnace, heating to 1200 ℃ at the heating rate of 10 ℃/min (centigrade per minute), preserving the heat for 2 hours, and cooling to room temperature to obtain the pure neodymium-doped yttrium iron garnet-based ceramic solidified body.
Example 5:
based on neodymium-doped yttrium-iron garnet (Y)2.0Nd1.0Fe5O12) Stoichiometric ratio of Fe2O3、Y2O3And Nd2O3Taking dried hematite (Fe) at a ratio of 5: 2: 0.52O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; dry grinding the mixed powder until no color difference exists, adding a proper amount of ethanol, and grinding for a grinding time t1Putting the precursor into a drying oven for drying for 0.5 hour, wherein the drying time t is214 hours; the dried precursor is pressed into a round slice with the diameter of 12mm under the pressure of 12MPa by a powder tablet press, and the pressure stabilizing time t is32.5 minutes; placing the pressed round slices into a microwave sintering furnace at a temperature of 10 ℃/min (centigrade per minute) literThe temperature is raised to 1200 ℃ at a speed rate, the temperature is kept for 4 hours, and the pure neodymium-doped yttrium iron garnet-based ceramic solidified body can be obtained after cooling to the room temperature.
Example 6:
based on neodymium-doped yttrium-iron garnet (Y)1.5Nd1.5Fe5O12) Stoichiometric ratio of Fe2O3、Y2O3And Nd2O3Taking dried hematite (Fe) at a ratio of 5: 1.5: 0.752O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; dry grinding the mixed powder until no color difference exists, adding a proper amount of ethanol, and grinding for a grinding time t1Putting the precursor into a drying oven for drying for 0.5 hour, wherein the drying time t is214 hours; the dried precursor is pressed into a round slice with the diameter of 12mm under the pressure of 12MPa by a powder tablet press, and the pressure stabilizing time t is32.5 minutes; and (3) putting the pressed round slice into a microwave sintering furnace, heating to 1200 ℃ at the heating rate of 10 ℃/min (centigrade per minute), preserving the heat for 6 hours, and cooling to room temperature to obtain the pure neodymium-doped yttrium iron garnet-based ceramic solidified body.
Example 7:
based on neodymium-doped yttrium-iron garnet (Y)1.2Nd1.8Fe5O12) Stoichiometric ratio of Fe2O3、Y2O3And Nd2O3Taking dried hematite (Fe) at a ratio of 5: 1.2: 0.92O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; dry grinding the mixed powder until no color difference exists, adding a proper amount of ethanol, and grinding for a grinding time t1Putting the precursor into a drying oven for drying for 0.5 hour, wherein the drying time t is214 hours; the dried precursor is pressed into a round slice with the diameter of 12mm under the pressure of 12MPa by a powder tablet press, and the pressure stabilizing time t is32.5 minutes; the pressed round shapeAnd (3) putting the slices into a microwave sintering furnace, heating to 1300 ℃ at the heating rate of 10 ℃/min (centigrade per minute), preserving the heat for 2 hours, and cooling to room temperature to obtain the pure neodymium-doped yttrium iron garnet-based ceramic solidified body.
Example 8:
based on neodymium-doped yttrium-iron garnet (Y)1.0Nd2.0Fe5O12) Stoichiometric ratio of Fe2O3、Y2O3And Nd2O3Taking dried hematite (Fe) at a ratio of 5: 1.02O3)，Y2O3And Nd2O3Mixing the powder to prepare mixed powder; dry grinding the mixed powder until no color difference exists, adding a proper amount of ethanol, and grinding for a grinding time t1Putting the precursor into a drying oven for drying for 0.5 hour, wherein the drying time t is214 hours; the dried precursor is pressed into a round slice with the diameter of 12mm under the pressure of 12MPa by a powder tablet press, and the pressure stabilizing time t is32.5 minutes; and (3) putting the pressed round slice into a microwave sintering furnace, heating to 1300 ℃ at the heating rate of 10 ℃/min (centigrade per minute), preserving the heat for 2 hours, and cooling to room temperature to obtain the pure neodymium-doped yttrium iron garnet-based ceramic solidified body.
As shown in the figure, XRD patterns of the yttrium iron garnet-based ceramic solidified bodies 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 4 and 5 have a main phase of yttrium iron garnet (Y)3Fe5O12) The Nd was successfully doped and the solidified body had higher crystallinity, and it was shown that pure phase yttrium iron garnet could be obtained at lower temperature. Example 8 shows a new phase but still shows the successful incorporation of Nd.
The preparation method of the neodymium-doped garnet-based ceramic solidified body is implemented by mixing Fe2O3，Y2O3，Nd2O3After grinding the mixed precursor, sintering the mixed precursor in a microwave sintering furnace, thereby preparing the ceramic material in a short timeThe pure neodymium-doped yttrium iron garnet-based ceramic solidified body with good compactness is obtained, and the process operation is simple.
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 (5)
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 ═ 0.5-2.0) stoichiometric ratio, i.e. Fe2O3∶Y2O3∶Nd2O3Taking dried hematite and Y according to the proportion of 5: 3-x: x/22O3And Nd2O3Mixing the powder to prepare mixed powder;
dry-grinding the mixed powder until no color difference exists, adding a proper amount of ethanol for grinding to obtain a precursor, and drying the precursor in a drying oven;
pressing the dried precursor into a circular sheet with the diameter of 12mm under the pressure of 12MPa by using a powder tablet press;
and (3) putting the pressed round slice into a microwave sintering furnace, heating to 1100-1300 ℃, preserving the heat for 0.5-6 hours, and cooling to room temperature to obtain the pure neodymium-doped yttrium iron garnet-based ceramic solidified body.
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 heating rate is 10 ℃/min.
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 grinding time t10.5 hour.
4. The method of claim 1The preparation method of the neodymium-doped yttrium iron garnet-based ceramic solidified body is characterized by comprising the following steps of: the drying time t214 hours.
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 voltage stabilization time t32.5 min.
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