CN116103760A - Processing method of cerium-doped yttrium iron garnet wafer - Google Patents
Processing method of cerium-doped yttrium iron garnet wafer Download PDFInfo
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- 239000002223 garnet Substances 0.000 title claims abstract description 28
- MTRJKZUDDJZTLA-UHFFFAOYSA-N iron yttrium Chemical compound [Fe].[Y] MTRJKZUDDJZTLA-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000003672 processing method Methods 0.000 title claims abstract description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000000843 powder Substances 0.000 claims abstract description 63
- 239000002243 precursor Substances 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 229910052742 iron Inorganic materials 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 150000002500 ions Chemical class 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 4
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000012266 salt solution Substances 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 25
- 238000000227 grinding Methods 0.000 claims description 23
- 230000001105 regulatory effect Effects 0.000 claims description 19
- 238000000975 co-precipitation Methods 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 16
- 238000004448 titration Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 13
- 229910052727 yttrium Inorganic materials 0.000 claims description 13
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 13
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 11
- 238000000967 suction filtration Methods 0.000 claims description 11
- 229910052684 Cerium Inorganic materials 0.000 claims description 10
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010532 solid phase synthesis reaction Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims 1
- 238000005498 polishing Methods 0.000 description 26
- 239000012071 phase Substances 0.000 description 10
- 239000000126 substance Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- ZPDRQAVGXHVGTB-UHFFFAOYSA-N gallium;gadolinium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Gd+3] ZPDRQAVGXHVGTB-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
- C30B1/023—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing from solids with amorphous structure
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compounds Of Iron (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a processing method of a cerium-doped yttrium iron garnet wafer, which comprises the following steps: step one: iron and yttrium oxide are used as raw materials, and YIG powder is obtained through synthesis; step two: mixing YIG powder obtained in the first step with cerium oxide raw materials to obtain a coprecipitate; step three: washing and filtering the coprecipitate to remove soluble impurity ions; then drying to obtain a precursor; step four: calcining the precursor at high temperature to obtain Ce: YIG wafer, the invention prepares Ce by comparison: the optimal temperature range and the optimal pH range of YIG powder can effectively ensure that the temperature of the YIG powder is equal to the optimal pH range of Ce: the appearance of miscellaneous phase is reduced when YIG powder is prepared, ce is improved: purity of YIG preparation.
Description
Technical Field
The invention relates to the technical field of yttrium iron garnet wafer processing, in particular to a processing method of a cerium-doped yttrium iron garnet wafer.
Background
Chinese patent CN202111359070.2 discloses a method for processing an ion doped gadolinium gallium garnet wafer, comprising the steps of: step one, mechanical grinding: placing the GGG coarse crystal plate in a cast iron plate at room temperature, then adding grinding fluid, carrying out mechanical grinding to obtain a coarse-grinding GGG crystal plate, controlling the grinding speed to be 60-65r/min, the grinding pressure to be 105-108g/cm < 2 >, the grinding time to be 30-40min, and carrying out ultrasonic vibration on the grinding fluid which is alumina (particle size of 4-6 mu m) and deionized water for 20-30min to obtain the coarse-grinding GGG crystal plate, wherein the concentration of the alumina is 0.05-0.07g/mL; step two, mechanical polishing: an IC1000 polishing pad is adopted as a polishing pad for mechanical polishing, the polishing pad is trimmed, a coarse-grinding GGG wafer is loaded, mechanical polishing solution flows into the polishing pad, and then mechanical polishing is carried out at room temperature to obtain the mechanically polished GGG wafer, wherein the polishing pressure is 125g/cm < 2 >, the polishing disc rotating speed is 60r/min, the polishing time is 20-30min, the flow rate of the mechanical polishing solution is 4mL/min, the mechanical polishing solution is obtained by ultrasonic oscillation of alumina (particle size is 1 mu m) and deionized water for 20-30min, and the concentration of the alumina is 0.08g/mL; step three, chemical mechanical polishing: the flannelette polishing pad is adopted as a polishing pad for chemical mechanical polishing, the flannelette polishing pad is trimmed, the silica sol polishing solution is adopted as the chemical mechanical polishing solution, the GGG wafer after mechanical polishing is loaded, then the chemical mechanical polishing is carried out at room temperature, and the ion doped gadolinium gallium garnet wafer is obtained, the polishing pressure is controlled to be 130g/cm < 2 >, the polishing disc rotating speed is 70r/min, the polishing time is 40-70min, and the flow rate of the chemical mechanical polishing solution is 6mL/min.
The patent adopts a physical processing method to obtain the gadolinium gallium doped garnet wafer, however, the preparation flow of the garnet wafer is not researched, and the purity of the wafer is influenced by the difference of the temperature value and the PH value of the garnet wafer in the preparation process of the garnet wafer.
Disclosure of Invention
The invention aims to solve the problems of the background technology and provides a processing method of a cerium-doped yttrium-iron garnet wafer.
The aim of the invention can be achieved by the following technical scheme:
a processing method of a cerium-doped yttrium iron garnet wafer comprises the following steps:
step one: iron and yttrium oxide are used as raw materials, and YIG powder is obtained through synthesis;
step two: mixing YIG powder obtained in the first step with cerium oxide raw materials to obtain a coprecipitate;
step three: washing and filtering the coprecipitate to remove soluble impurity ions; then drying to obtain a precursor;
step four: calcining the precursor at high temperature to obtain Ce: YIG wafer.
Preparing Ce: the chemical reaction equation of YIG powder is as follows:
2xCeO 2 +(3-x)Y 2 O 3 +5Fe 2 O 3 →2Ce x Y 3-x Fe 5 O 12 +x/2O 2 ↑
the invention further technically improves that: the preparation of YIG powder adopts a high-temperature solid phase method, and the preparation of YIG powder by the high-temperature solid phase method adopts Y 2 O 3 、Fe 2 O 3 Is a raw material.
The invention further technically improves that: the preparation method of YIG powder by the high-temperature solid phase method comprises the following specific steps:
step A1: accurately weighing oxides of iron and yttrium according to stoichiometric ratio as raw materials;
step A2: the oxides of iron and yttrium are uniformly mixed in a grinding and mixing mode;
step A3: and sintering for multiple times at the high temperature of 1300-1400 ℃ to obtain YIG powder.
The chemical reaction equation for preparing YIG powder by using the high temperature solid phase method is as follows:
3Y 2 O 3 +5Fe 2 O 3 →2Y 3 Fe 5 O 12 +5O 2
the invention further technically improves that: and (C) filling nitrogen during sintering the YIG powder in the step A3, wherein the heating rate is 10 ℃/min, and the temperature is raised to 1300-1400 ℃ from the room temperature.
The invention further technically improves that: the preparation of YIG powder adopts a coprecipitation method, and the preparation of YIG powder by the coprecipitation method adopts Y 2 O 3 And Fe (Fe) 2 O 3 Is a raw material.
The invention further technically improves that: the preparation method of YIG powder by coprecipitation comprises the following specific steps:
step B1: accurately weighing a certain amount of Y on an electronic balance 2 O 3 And Fe (Fe) 2 O 3 Dissolved in the prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (Fe)(NO 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step B2: adjusting the pH value of the mother salt solution to 3-4 by using ammonia water, and uniformly stirring;
step B3: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step B4: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and performing suction filtration, drying and grinding to obtain YIG precursor;
step B5: and finally sintering the precursor powder in a muffle furnace at high temperature to obtain YIG powder.
The chemical reaction mechanism for preparing YIG powder by the coprecipitation method is as follows:
Y 2 O 3 +6HNO 3 →2Y(NO 3 ) 3 +3H 2 O
Fe 2 O 3 +6HNO 3 →2Fe(NO 3 ) 3 +3H 2 O
2Y(NO 3 ) 3 +6NH 4 HCO 3 →Y 2 (CO 3 ) 3 ↓+6NH 4 NO 3 +3CO 2 ↑
2Fe(NO 3 ) 3 +6NH 4 HCO 3 →Fe 2 (CO 3 ) 3 ↓+6NH 4 NO 3 +3CO 2 ↑
3Y 2 (CO 3 ) 3 +5Fe 2 (CO 3 ) 3 →2Y 3 Fe 5 O 12 +24CO 2 ↑
the invention further technically improves that: in step B1 at HNO 3 The solution was added HCl for Y 2 O 3 And Fe (Fe) 2 O 3 Is dissolved in the solvent.
The invention further technically improves that: and B2, adding a mother salt solution by adopting a back titration method, wherein the titration speed is 1-2mL/min.
The invention has the beneficial effects that:
the invention adopts a coprecipitation method to prepare Ce: YIG powder, the prepared precursor has good chemical uniformity and reactivity, and the diffusion path of particles is shortened during calcination synthesis, so that the calcination temperature can be reduced, the calcination performance can be improved, and the particle size is easy to control. Accurate dosing can be performed by controlling the concentration of each component in the raw material solution, thereby achieving accurate control of the material composition. The method is easy to uniformly disperse a proper amount of additives, and can also avoid the introduction of impurities in the process of mechanical crushing such as ball milling and the like, so that the prepared crystal powder has high chemical purity and good quality.
Preparation of Ce by comparison: the optimal temperature range and the optimal pH range of YIG powder can effectively ensure that the temperature of the YIG powder is equal to the optimal pH range of Ce: the appearance of miscellaneous phase is reduced when YIG powder is prepared, ce is improved: purity of YIG preparation.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A processing method of a cerium-doped yttrium iron garnet wafer adopts a coprecipitation method to prepare Ce: the YIG powder comprises the following steps:
step one: weighing oxides of cerium, iron and yttrium with quantitative proportion as raw materials, dissolving in prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (NO) 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step two: ammonia water is used for regulating the pH value of the mother salt solution to 8-11, and the mother salt solution is stirred uniformly;
step three: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step four: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and carrying out suction filtration, drying and grinding to obtain Ce: YIG precursor;
step five: finally sintering the precursor powder in a muffle furnace at 800-1100 ℃ to obtain Ce: YIG powder.
Example 2
A processing method of a cerium-doped yttrium iron garnet wafer adopts a coprecipitation method to prepare Ce: the YIG powder comprises the following steps:
step one: weighing oxides of cerium, iron and yttrium with quantitative proportion as raw materials, dissolving in prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (NO) 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step two: ammonia water is used for adjusting the pH value of the mother salt solution to 8, and the mother salt solution is stirred uniformly;
step three: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step four: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and carrying out suction filtration, drying and grinding to obtain Ce: YIG precursor;
step five: finally sintering the precursor powder in a muffle furnace at 800-1100 ℃ to obtain Ce: YIG powder.
Example 3
A processing method of a cerium-doped yttrium iron garnet wafer adopts a coprecipitation method to prepare Ce: the YIG powder comprises the following steps:
step one: weighing oxides of cerium, iron and yttrium with quantitative proportion as raw materials, dissolving in prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (NO) 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step two: ammonia water is used for regulating the pH value of the mother salt solution to 9.5, and the mother salt solution is stirred uniformly;
step three: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step four: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and carrying out suction filtration, drying and grinding to obtain Ce: YIG precursor;
step five: finally sintering the precursor powder in a muffle furnace at 800-1100 ℃ to obtain Ce: YIG powder.
Example 4
A processing method of a cerium-doped yttrium iron garnet wafer adopts a coprecipitation method to prepare Ce: the YIG powder comprises the following steps:
step one: weighing oxides of cerium, iron and yttrium with quantitative proportion as raw materials, dissolving in prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (NO) 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step two: ammonia water is used for regulating the pH value of the mother salt solution to 10.5, and the mother salt solution is stirred uniformly;
step three: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step four: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and carrying out suction filtration, drying and grinding to obtain Ce: YIG precursor;
step five: finally sintering the precursor powder in a muffle furnace at 800-1100 ℃ to obtain Ce: YIG powder.
Example 5
A processing method of a cerium-doped yttrium iron garnet wafer adopts a coprecipitation method to prepare Ce: the YIG powder comprises the following steps:
step one: weighing oxides of cerium, iron and yttrium with quantitative proportion as raw materials, dissolving in prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (NO) 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step two: ammonia water is used for regulating the pH value of the mother salt solution to 11, and the mother salt solution is stirred uniformly;
step three: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step four: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and carrying out suction filtration, drying and grinding to obtain Ce: YIG precursor;
step five: finally sintering the precursor powder in a muffle furnace at 800-1100 ℃ to obtain Ce: YIG powder.
In examples 2 to 5, the components in the solution were detected by adjusting the pH values to obtain Ce: optimal pH range in YIG preparation process, ce: YIG in the course of the reaction with Ce 3+ Ion pair Y 3+ Substitution of ions, however due to Ce 3+ The ionic radius is large and is easily oxidized into Ce at high temperature 4+ Ions such that a high content of Ce 3+ Doping of ions is difficult.
YIG and CeO were detected in the solutions by different pH values in examples 2-5 2 The obtained data are shown in the following table:
as is clear from the above table, when the pH value was 9.5, white precipitate was found in the filtrate, and Ce was detected by a qualitative detection means 3+ Due to Ce at pH values below 9.5 3+ Cannot be completely precipitated and therefore the pH should be chosen to be higher than 9.5. However, the pH cannot be too high because of the increased alkalinity and the increased Ce 3+ To Ce 4+ Trend of conversion. It can be similarly concluded that the appropriate pH range is selected to be 9.5-10.5.
Example 6
A processing method of a cerium-doped yttrium iron garnet wafer adopts a coprecipitation method to prepare Ce: the YIG powder comprises the following steps:
step one: weighing oxides of cerium, iron and yttrium with quantitative proportion as raw materials, dissolving in prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (NO) 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step two: ammonia water is used for regulating the pH value of the mother salt solution to 10, and the mother salt solution is stirred uniformly;
step three: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step four: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and carrying out suction filtration, drying and grinding to obtain Ce: YIG precursor;
step five: finally sintering the precursor powder in a muffle furnace at the temperature range of 800 ℃ to obtain Ce: YIG powder.
Example 7
A processing method of a cerium-doped yttrium iron garnet wafer adopts a coprecipitation method to prepare Ce: the YIG powder comprises the following steps:
step one: weighing oxides of cerium, iron and yttrium with quantitative proportion as raw materials, dissolving in prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (NO) 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step two: ammonia water is used for regulating the pH value of the mother salt solution to 10, and the mother salt solution is stirred uniformly;
step three: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step four: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and carrying out suction filtration, drying and grinding to obtain Ce: YIG precursor;
step five: finally sintering the precursor powder in a muffle furnace at 900 ℃ to obtain Ce: YIG powder.
Example 8
A processing method of a cerium-doped yttrium iron garnet wafer adopts a coprecipitation method to prepare Ce: the YIG powder comprises the following steps:
step one: weighing oxides of cerium, iron and yttrium with quantitative proportion as raw materials, dissolving in prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (NO) 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step two: ammonia water is used for regulating the pH value of the mother salt solution to 10, and the mother salt solution is stirred uniformly;
step three: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step four: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and carrying out suction filtration, drying and grinding to obtain Ce: YIG precursor;
step five: finally sintering the precursor powder in a muffle furnace at the temperature range of 1000 ℃ to obtain Ce: YIG powder.
Example 9
A processing method of a cerium-doped yttrium iron garnet wafer adopts a coprecipitation method to prepare Ce: the YIG powder comprises the following steps:
step one: weighing oxides of cerium, iron and yttrium with quantitative proportion as raw materials, dissolving in prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (NO) 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step two: ammonia water is used for regulating the pH value of the mother salt solution to 10, and the mother salt solution is stirred uniformly;
step three: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step four: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and carrying out suction filtration, drying and grinding to obtain Ce: YIG precursor;
step five: finally sintering the precursor powder in a muffle furnace at 1100 ℃ to obtain Ce: YIG powder.
By rotating the pH to 10 as a result of examples 2 to 5, YIG and CeO of the final product were obtained by varying the sintering temperature 2 The obtained data are shown in the following table:
from the above table, it is clear that YIP impurity phase appears when the calcination temperature is 800 ℃, because the calcination temperature is lower than the temperature at which YIP is completely converted into YIG, and thus no pure YIG phase is formed, and no YIP impurity phase exists at the calcination temperature higher than 900 ℃. However, when the temperature reaches 1100 ℃, ceO appears 2 And (3) impurity phase. At 900 ℃ and 1000 ℃, two hetero-phases YIP and CeO 2 Are all absent and get pureYIG phase of (a), and thus concludes: within the calcination temperature range of 900-1000 ℃, pure YIG phases can be synthesized, below which YIP impurity phases can be formed, above which CeO can be formed 2 And (3) impurity phase.
The foregoing describes one embodiment of the present invention in detail, but the description is only a preferred embodiment of the present invention and should not be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the present invention are intended to be covered by the present invention.
Claims (8)
1. The processing method of the cerium-doped yttrium iron garnet wafer is characterized by comprising the following steps of:
step one: iron and yttrium oxide are used as raw materials, and YIG powder is obtained through synthesis;
step two: mixing YIG powder obtained in the first step with cerium oxide raw materials to obtain a coprecipitate;
step three: washing and filtering the coprecipitate to remove soluble impurity ions; then drying to obtain a precursor;
step four: calcining the precursor at high temperature to obtain Ce: YIG wafer.
2. The method for processing cerium-doped yttrium-iron garnet wafer according to claim 1, wherein the preparation of YIG powder is carried out by a high-temperature solid phase method, and the preparation of YIG powder by a high-temperature solid phase method is carried out by Y 2 O 3 、Fe 2 O 3 Is a raw material.
3. The processing method of the cerium-doped yttrium iron garnet wafer according to claim 2, wherein the specific steps of preparing YIG powder by a high-temperature solid phase method are as follows:
step A1: accurately weighing oxides of iron and yttrium according to stoichiometric ratio as raw materials;
step A2: the oxides of iron and yttrium are uniformly mixed in a grinding and mixing mode;
step A3: and sintering for multiple times at the high temperature of 1300-1400 ℃ to obtain YIG powder.
4. The method for processing cerium-doped yttrium-iron garnet wafer according to claim 3, wherein nitrogen is filled during sintering of YIG powder in step A3, and the temperature rising rate is 10 ℃/min, and the temperature rises from room temperature to 1300 ℃ to 1400 ℃.
5. The method for processing cerium-doped yttrium-iron garnet wafer according to claim 1, wherein YIG powder is prepared by coprecipitation method, and Y is used as the material 2 O 3 And Fe (Fe) 2 O 3 Is a raw material.
6. The method for processing cerium-doped yttrium-iron garnet wafer according to claim 5, wherein the specific steps of preparing Y I G powder by a coprecipitation method are as follows:
step B1: accurately weighing a certain amount of Y on an electronic balance 2 O 3 And Fe (Fe) 2 O 3 Dissolved in the prepared HNO 3 In the mixed solution, Y (NO) 3 ) 3 And Fe (NO) 3 ) 3 Uniformly mixing the two solutions to obtain a mother salt solution;
step B2: adjusting the pH value of the mother salt solution to 3-4 by using ammonia water, and uniformly stirring;
step B3: titrating the mother salt solution with the pH value regulated to NH 4 HCO 3 In solution;
step B4: continuously stirring for 0.5h after titration is finished, standing and aging for 15-20h, and performing suction filtration, drying and grinding to obtain YIG precursor;
step B5: and finally sintering the precursor powder in a muffle furnace at high temperature to obtain YIG powder.
7. The method of claim 6, wherein in step B1, HNO is used to process the cerium doped yttrium iron garnet wafer 3 The solution was added HCl for Y 2 O 3 And Fe (Fe) 2 O 3 Is a solution of (2)And (5) solving.
8. The method for processing a cerium-doped yttrium-iron garnet wafer according to claim 6, wherein the mother salt solution is added in the step B3 by a back titration method, and the titration speed is 1-2mL/min.
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