CN115676870B - Preparation method of LaOF nano powder suitable for industrial production - Google Patents
Preparation method of LaOF nano powder suitable for industrial production Download PDFInfo
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- CN115676870B CN115676870B CN202211095399.7A CN202211095399A CN115676870B CN 115676870 B CN115676870 B CN 115676870B CN 202211095399 A CN202211095399 A CN 202211095399A CN 115676870 B CN115676870 B CN 115676870B
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000009776 industrial production Methods 0.000 title claims abstract description 7
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 30
- 239000002243 precursor Substances 0.000 claims abstract description 24
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000011780 sodium chloride Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 150000002603 lanthanum Chemical class 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 229910017569 La2(CO3)3 Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 claims description 3
- 229960001633 lanthanum carbonate Drugs 0.000 claims description 3
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical group [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 2
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 12
- 230000007613 environmental effect Effects 0.000 abstract 1
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000843 powder Substances 0.000 description 12
- 235000013024 sodium fluoride Nutrition 0.000 description 11
- 239000011775 sodium fluoride Substances 0.000 description 11
- 239000007789 gas Substances 0.000 description 7
- 239000007791 liquid phase Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- VRPQIIJGEJVXBK-UHFFFAOYSA-N fluoro hypofluorite lanthanum Chemical compound [La].FOF VRPQIIJGEJVXBK-UHFFFAOYSA-N 0.000 description 4
- KGDJAQAMSDMZCD-UHFFFAOYSA-M hydrogen carbonate lanthanum(3+) oxygen(2-) Chemical compound C([O-])(O)=O.[O-2].[La+3] KGDJAQAMSDMZCD-UHFFFAOYSA-M 0.000 description 4
- 238000010532 solid phase synthesis reaction Methods 0.000 description 4
- 229910002420 LaOCl Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- -1 rare earth fluoride Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910017768 LaF 3 Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- QJMKVFKYZXYKIG-UHFFFAOYSA-M [F].[F-].[Na+] Chemical compound [F].[F-].[Na+] QJMKVFKYZXYKIG-UHFFFAOYSA-M 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- JRWCQCMTTGPTAU-UHFFFAOYSA-N lanthanum(3+);oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[La+3].[La+3] JRWCQCMTTGPTAU-UHFFFAOYSA-N 0.000 description 1
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Provides a preparation method of LaOF nano powder suitable for industrial production, which comprises the following steps: (1) obtaining a lanthanum containing precursor; (2) Mixing and ball milling the lanthanum-containing precursor, naCl and NaF for 3-24 hours to obtain a ball milling mixture, wherein the mass ratio of the lanthanum-containing precursor to the NaCl is 1:3-20, and the mass ratio of the lanthanum-containing precursor to the NaF is 5:1-25; (3) Calcining the ball-milling mixture at 600-1000 ℃ to obtain the LaOF nano powder. The method can obtain the LaOF nano powder with uniform particle size distribution and particle size below 150nm, and has lower cost and more environmental protection.
Description
Technical Field
The invention belongs to the technical field of inorganic powder material preparation, and in particular relates to a preparation method of LaOF nano powder suitable for industrial production.
Background
Lanthanum oxyfluoride (LaOF) is used as an important functional material in various fields such as: polishing powder, high-quality luminescent materials, catalysts and the like. The lanthanum oxyfluoride nano-powder is prepared by a solid phase method and a liquid phase precipitation-calcination method:
(1) The solid phase method is to calcine lanthanum oxide as raw material, rare earth fluoride or organic fluoride as fluorine source under the condition of no oxygen and high temperature to synthesize lanthanum oxyfluoride. The path is a path used relatively early, and has the defects of harsh synthesis conditions, large particle size, uneven distribution and the like, and is not suitable for industrialized amplified production.
(2) The liquid phase precipitation-calcination method uses inorganic salt of lanthanum as raw material, urea as precipitant, naF, KF, naBF 4 HF is a fluorine source, under the heating condition<And (3) obtaining a precursor after the reaction at 100 ℃, and finally obtaining lanthanum oxyfluoride through high-temperature calcination. The path is a method used in most documents, has the advantages of controllable particle size and morphology, but most of the particles with smaller particle size (nanometer level) are required to be added with surfactant, and in addition, the liquid phase reaction is required to be carried out under the heating condition, so that the cost is not reduced, and the method is not suitable for industrialized scale-up production.
Therefore, a new preparation method of LaOF nano powder suitable for industrial production is needed to solve the technical problems.
Disclosure of Invention
The invention provides a preparation method of LaOF nano powder suitable for industrial production, which comprises the following steps:
(1) Obtaining a lanthanum-containing precursor;
(2) Mixing and ball milling the lanthanum-containing precursor, naCl and NaF for 3-24 hours to obtain a ball milling mixture, wherein the mass ratio of the lanthanum-containing precursor to the NaCl is 1:3-20, and the mass ratio of the lanthanum-containing precursor to the NaF is 5:1-25;
(3) Calcining the ball-milling mixture at 600-1000 ℃ to obtain the LaOF nano powder.
Wherein the LaOF nano powder is spheroidic, has particle size below 150nm and uniform particle size distribution.
Wherein the lanthanum-containing precursor is hydrated lanthanum oxide carbonate, basic lanthanum carbonate, lanthanum hydroxide.
Wherein, in the step (1), the obtaining a lanthanum-containing precursor comprises:
(1.1) preparation of a liquid precipitant: mixing amine with water to obtain CO 2 A gas trapping agent, and then CO is introduced into the gas trapping agent 2 After the gas is saturated, the liquid precipitant is obtained;
(1.2) preparing a lanthanum containing precursor: adding a lanthanum source into the liquid precipitant, mixing and stirring for reaction, centrifuging to obtain white precipitate, washing and drying to obtain the lanthanum-containing precursor.
Wherein in the step (1.1), the amine is at least one selected from ethylenediamine, diethylamine, ethanolamine and diethanolamine.
Wherein in the step (1.1), the volume ratio of the amine to the water is 1:9-30.
Wherein in the step (1.2), the lanthanum source is lanthanum salt or lanthanum salt water solution, and the lanthanum salt is selected from lanthanum nitrate and/or lanthanum chloride; in the added lanthanum source, lanthanum salt and CO 2 The mass ratio of the gas trapping agent is 1:1-40; the concentration of the lanthanum salt aqueous solution is 0.03-0.10mol/L.
Wherein in the step (1.2), the stirring temperature is 20-150 ℃ and the stirring time is 1-2h.
Wherein in the step (1.2), the washing is performed by using water and ethanol respectively.
Wherein in the step (2), the ball milling rotating speed is 200-400r/min.
The beneficial effects of the invention are as follows:
(1) The preparation method adopts a mode of combining a solid phase method and a liquid phase precipitation-calcination method, firstly synthesizes a precursor through the liquid phase method, then ball-mills through the solid phase method while doping fluorine, and finally calcines to obtain the LaOF nano powder with uniform particle size distribution and low cost, wherein the particle size of the LaOF can be controlled below 150 nm.
(2) Compared with organic fluoride (such as PVDF and PTFE) used in the prior art, the F source adopts sodium fluoride, and the use of the sodium fluoride as a fluorine source is more environment-friendly and has low use cost; laF is also used in the prior art 3 As F source, but LaF 3 The preparation itself also involves problems of pollution of the F source, and of being expensive.
(3) According to the invention, the particle size and morphology of LaOF are controlled by utilizing NaCl ball milling, and a sodium fluoride fluorine source is added to prepare the LaOF nano powder with particle size below 150nm and uniform particle size distribution, so that the problems of larger particle size and nonuniform particle size distribution of LaOF in the prior art are effectively solved.
Brief description of the drawings
FIG. 1 is a scanning electron microscope image of LaOF nano powder prepared in example 1;
FIG. 2 is a particle size distribution diagram of LaOF nano-powder prepared in example 1;
FIG. 3 is an XRD pattern of LaOF nano-powder prepared in example 1;
FIG. 4 is a scanning electron microscope image of the LaOF powder prepared in comparative example 1;
FIG. 5 is a particle size distribution diagram of LaOF powder prepared in comparative example 1;
FIG. 6 is an XRD pattern of LaOF powder prepared in comparative example 1;
FIG. 7 is a scanning electron microscope image of the LaOF powder prepared in comparative example 2;
FIG. 8 is a particle size distribution diagram of LaOF powder prepared in comparative example 2;
FIG. 9 is an XRD pattern of LaOF powder prepared in comparative example 2;
fig. 10 is an XRD pattern of the product prepared in comparative example 3.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that these examples are for illustration only and are not intended to limit the scope of the invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims of the present application.
Example 1
A method for preparing LaOF nano-powder, comprising:
(1) Preparing a liquid precipitant:
mixing ethylenediamine and water in a volume ratio of 1:10 to obtain CO 2 A gas trapping agent; CO is introduced into 2 The liquid precipitant is prepared after gas saturation;
(2) Preparation of hydrated lanthanum oxycarbonate:
adding lanthanum nitrate aqueous solution into the liquid precipitant, mixing, stirring at 25 ℃ for 12 hours for reaction, centrifuging to obtain white precipitate, washing with water and ethanol respectively, and drying to obtain hydrated lanthanum oxide carbonate; wherein the mass of lanthanum salt and CO 2 The mass ratio of the gas trapping agent is 1:10, and the concentration of the lanthanum salt aqueous solution is 0.10mol/L;
(3) Preparing spheroid LaOF nano powder:
mixing lanthanum oxide hydrate prepared in the step (2), naCl and NaF, ball-milling for 3 hours at a ball-milling rotating speed of 400r/min, and calcining the mixed solid in a muffle furnace at 700 ℃ after ball-milling to obtain spheroid LaOF nano powder; wherein, the mass ratio of the hydrated lanthanum oxide carbonate to NaCl is 1:5, and the mass ratio of the hydrated lanthanum oxide carbonate to NaF is 5:1.
As shown in FIGS. 1 to 3, the powder obtained in example 1 had a spheroidic morphology, and 90% or more of the particles had a particle size distribution of 150nm or less, and XRD showed that it was a crystalline LaOF powder.
Comparative example 1
Example 1 was repeated except that the amount of NaCl was reduced and the ratio of lanthanum oxycarbonate to NaCl was changed to 1:1.
As shown in FIGS. 4 to 6, although the LaOF powder of comparative example 1 was excellent in crystallization, the morphology of the particles was irregular, the particle size was not uniform, and 90% or more of the particles had a particle size distribution of 0.25 to 2. Mu.m, which was far larger than that of example 1. It can be seen that when the amount of NaCl added is insufficient, only micron-sized LaOF particles can be obtained, and it is difficult to obtain the spheroid-like LaOF nanoparticles of the present invention.
Comparative example 2
Example 1 was repeated except that the mixing and ball milling time of lanthanum oxycarbonate, naCl and NaF was changed to 1 h.
As shown in FIGS. 7 to 9, although the LaOF powder of comparative example 2 was excellent in crystallization, the morphology of particles was irregular, and 90% or more of the particles had a particle size distribution of 0.5 to 2. Mu.m, which was far larger than that of example 1. Therefore, when the mixing ball milling time of the hydrated lanthanum oxycarbonate, naCl and NaF is insufficient, only micron-sized LaOF particles can be obtained, and the spheroid LaOF nano particles are difficult to obtain.
Comparative example 3
Example 1 was repeated except that sodium fluoride was not added.
As shown in FIG. 10, the products obtained in comparative example 3 were LaOCl and La (OH) 3 It can be seen that not only LaOF is not obtained without the addition of sodium fluoride, but that Cl is also incorporated into the decomposition product of the La precursor to form LaOCl, i.e., sodium fluoride not only provides a source of F but also avoids the formation of LaOCl and La (OH) upon calcination of the La precursor 3 。
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (8)
1. The preparation method of the LaOF nano powder suitable for industrial production comprises the following steps:
(1) Obtaining a lanthanum-containing precursor;
(2) Mixing and ball milling the lanthanum-containing precursor, naCl and NaF for 3-24 hours to obtain a ball milling mixture, wherein the mass ratio of the lanthanum-containing precursor to the NaCl is 1:3-20, and the mass ratio of the lanthanum-containing precursor to the NaF is 5:1-25;
(3) Calcining the ball-milling mixture at 600-1000 ℃ to obtain the LaOF nano powder;
wherein, in the step (1), the step of obtaining the lanthanum-containing precursor comprises the following steps:
(1.1) preparation of a liquid precipitant: mixing an amine source with water to produce CO 2 A gas trapping agent, and then CO is introduced into the gas trapping agent 2 After the gas is saturated, the liquid precipitant is obtained;
(1.2) preparing a lanthanum containing precursor: adding a lanthanum source into the liquid precipitant, mixing and stirring for reaction, centrifuging to obtain white precipitate, washing and drying to obtain the lanthanum-containing precursor;
wherein in the step (1.1), the amine source is at least one selected from ethylenediamine, diethylamine, ethanolamine and diethanolamine;
wherein the particle size of the LaOF nano powder is below 150 nm.
2. The method for preparing LaOF nano powder as defined in claim 1, wherein the LaOF nano powder is sphere-like.
3. The method for preparing LaOF nano powder as claimed in claim 1, wherein the lanthanum-containing precursor is hydrated lanthanum oxycarbonate, basic lanthanum carbonate, lanthanum carbonate.
4. The method for preparing LaOF nano powder as claimed in claim 1, wherein in the step (1.1), the volume ratio of the amine source to the water is 1:9-30.
5. The method for preparing LaOF nano powder as claimed in claim 1, wherein in step (1.2), the lanthanum source is lanthanum salt or lanthanum salt aqueous solution, and the lanthanum salt is selected from lanthanum nitrate and/or lanthanum chloride.
6. A process for preparing LaOF nano-powder as defined in claim 5, wherein, in the lanthanum source, lanthanum salt and CO 2 The mass ratio of the gas trapping agent is 1:1-40.
7. The method for preparing LaOF nano powder as claimed in claim 5, wherein the concentration of the aqueous lanthanum salt solution is 0.03-0.10mol/L.
8. The method for preparing LaOF nano powder as claimed in claim 1, wherein in the step (2), the ball milling rotation speed is 200-400r/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004339336A (en) * | 2003-05-15 | 2004-12-02 | Mitsui Mining & Smelting Co Ltd | Cerium abrasive and method for producing cerium abrasive |
| KR20130134314A (en) * | 2012-05-30 | 2013-12-10 | (주)에코맥스 | METHOD FOR SYNTHESIS OF LaFCO3 POWDER USING LANTHANUM SALT AND FIUORIDE SALT AND METHOD FOR SYNTHESIS OF LaOF POWDER USING THE SAME |
| KR20150093906A (en) * | 2014-02-07 | 2015-08-19 | 영남대학교 산학협력단 | Method of preparing the lanthanum aluminate powder |
| WO2018116688A1 (en) * | 2016-12-20 | 2018-06-28 | 三井金属鉱業株式会社 | Rare earth oxyfluoride sintered body and method for producing same |
| CN111268715A (en) * | 2020-03-02 | 2020-06-12 | 内蒙古科技大学 | Fused salt synthesis method of rare earth oxyfluoride with cubic crystal form |
-
2022
- 2022-09-05 CN CN202211095399.7A patent/CN115676870B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004339336A (en) * | 2003-05-15 | 2004-12-02 | Mitsui Mining & Smelting Co Ltd | Cerium abrasive and method for producing cerium abrasive |
| KR20130134314A (en) * | 2012-05-30 | 2013-12-10 | (주)에코맥스 | METHOD FOR SYNTHESIS OF LaFCO3 POWDER USING LANTHANUM SALT AND FIUORIDE SALT AND METHOD FOR SYNTHESIS OF LaOF POWDER USING THE SAME |
| KR20150093906A (en) * | 2014-02-07 | 2015-08-19 | 영남대학교 산학협력단 | Method of preparing the lanthanum aluminate powder |
| WO2018116688A1 (en) * | 2016-12-20 | 2018-06-28 | 三井金属鉱業株式会社 | Rare earth oxyfluoride sintered body and method for producing same |
| CN109923092A (en) * | 2016-12-20 | 2019-06-21 | 三井金属矿业株式会社 | Rare earth oxyfluoride sintered body and its manufacturing method |
| CN111268715A (en) * | 2020-03-02 | 2020-06-12 | 内蒙古科技大学 | Fused salt synthesis method of rare earth oxyfluoride with cubic crystal form |
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