CN115676870A - 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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- CN115676870A CN115676870A CN202211095399.7A CN202211095399A CN115676870A CN 115676870 A CN115676870 A CN 115676870A CN 202211095399 A CN202211095399 A CN 202211095399A CN 115676870 A CN115676870 A CN 115676870A
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000009776 industrial production Methods 0.000 title claims abstract description 7
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 34
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002245 particle Substances 0.000 claims abstract description 29
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000011780 sodium chloride Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 150000002603 lanthanum Chemical class 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000012716 precipitator 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
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing 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
- 238000006243 chemical reaction Methods 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 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
- 239000002244 precipitate Substances 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 229910017569 La2(CO3)3 Inorganic materials 0.000 claims description 2
- NKCVNYJQLIWBHK-UHFFFAOYSA-N carbonodiperoxoic acid Chemical compound OOC(=O)OO NKCVNYJQLIWBHK-UHFFFAOYSA-N 0.000 claims description 2
- 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
- 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 2
- 229960001633 lanthanum carbonate Drugs 0.000 claims description 2
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 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
- 238000000926 separation method Methods 0.000 claims description 2
- 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 13
- 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
- 238000010532 solid phase synthesis reaction Methods 0.000 description 4
- 229910002420 LaOCl Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000463 material Substances 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
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 230000009286 beneficial effect 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
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910017768 LaF 3 Inorganic materials 0.000 description 1
- 229910020808 NaBF 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
- 230000003321 amplification Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 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
- -1 rare earth fluoride Chemical class 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
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- 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 the lanthanum-containing precursor with NaCl and NaF, and performing ball milling for 3-24 hours to obtain a ball-milled mixture, wherein the mass ratio of the lanthanum-containing precursor to NaCl is 1; (3) And calcining the ball-milled mixture at 600-1000 ℃ to obtain the LaOF nano powder. The method can obtain LaOF nano powder with uniform particle size distribution and particle size below 150nm, and has the advantages of low cost and environmental protection.
Description
Technical Field
The invention belongs to the technical field of preparation of inorganic powder materials, and particularly relates to a preparation method of LaOF nano powder suitable for industrial production.
Background
Lanthanum oxyfluoride (LaOF) is an important functional material used in various fields such as: polishing powder, high-quality luminescent materials, catalysts and the like. The preparation of lanthanum oxyfluoride nano powder generally comprises a solid phase method, a liquid phase precipitation-calcination method:
(1) The solid phase method is to calcine lanthanum oxyfluoride under the conditions of no oxygen and high temperature by taking lanthanum oxide as a raw material and rare earth fluoride or organic fluoride as a fluorine source. The method is a relatively early-stage used method, has the defects of relatively harsh synthesis conditions, large particle size, uneven distribution and the like, and is not suitable for industrial amplification production.
(2) The liquid phase precipitation-calcination method uses inorganic lanthanum salt as raw material, urea as precipitant and NaF, KF and NaBF 4 HF as a fluorine source, under heating conditions: (<Obtaining a precursor after reaction at 100 ℃, and finally obtaining the lanthanum oxyfluoride by high-temperature calcination. This route is the method used in most literature and has the advantage of controllable particle size and morphology, but mostly requires the addition of surfactants for the synthesis of particles of smaller size (nanoscale), and furthermore liquid phase reactions requireThe method is carried out under the heating condition, which is not beneficial to reducing the cost and is not suitable for industrial scale-up production.
Therefore, a new method for preparing LaOF nano powder suitable for industrial production is needed to solve the above 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 the lanthanum-containing precursor with NaCl and NaF, and carrying out ball milling for 3-24h to obtain a ball-milled mixture, wherein the mass ratio of the lanthanum-containing precursor to NaCl is 1;
(3) And calcining the ball-milled mixture at 600-1000 ℃ to obtain the LaOF nano powder.
Wherein, the LaOF nano powder is spherical-like, the particle size is below 150nm, and the particle size distribution is uniform.
The lanthanum-containing precursor is hydrated lanthanum oxycarbonate, lanthanum hydroxycarbonate, lanthanum carbonate and lanthanum hydroxide.
Wherein, in the step (1), the obtaining of the lanthanum-containing precursor comprises:
(1.1) preparation of liquid precipitant: mixing amine and water to obtain CO 2 A gas trapping agent, then introducing CO into the gas trapping agent 2 Obtaining the liquid precipitator after the gas is saturated;
(1.2) preparing a lanthanum-containing precursor: and adding a lanthanum source into the liquid precipitator, mixing and stirring for reaction, performing centrifugal separation to obtain a 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 mixed amine and water is 1.
In the step (1.2), the lanthanum source is a lanthanum salt or a lanthanum salt aqueous solution, and the lanthanum salt is selected from lanthanum nitrate and/or lanthanum chloride; added ofIn the lanthanum source, lanthanum salt and CO 2 The mass ratio of the gas trapping agent is 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 washing with water and ethanol respectively.
Wherein in the step (2), the ball milling rotating speed is 200-400r/min.
The invention has the beneficial effects that:
(1) The 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-milling through the solid phase method while doping fluorine, and finally calcining to obtain the LaOF nano powder with uniform particle size distribution and lower cost, wherein the LaOF particle size can be controlled below 150 nm.
(2) The F source of the invention adopts sodium fluoride, and compared with organic fluorides (such as PVDF and PTFE) used in the prior art, the F source of the invention uses sodium fluoride as a fluorine source, is more environment-friendly and has low use cost; laF is also adopted in the prior art 3 As an F source, but LaF 3 The preparation itself also involves the problem of contamination of the source of F, which is expensive.
(3) According to the invention, while the particle size and morphology of LaOF are controlled by NaCl ball milling, the LaOF nano powder with particle size below 150nm and uniform particle size distribution is prepared by adding the sodium fluoride source, so that the problems of large LaOF particle size and non-uniform particle size distribution in the prior art are effectively solved.
Brief description of the drawings
FIG. 1 is a scanning electron micrograph of a LaOF nanopowder prepared in example 1;
FIG. 2 is a particle size distribution diagram of LaOF nanopowder prepared in example 1;
FIG. 3 is an XRD pattern of LaOF nanopowder prepared in example 1;
FIG. 4 is a scanning electron micrograph of a 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 micrograph of a LaOF powder prepared in comparative example 2;
FIG. 8 is a particle size distribution diagram of the 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 present invention. Furthermore, it should be understood that various changes and modifications can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the claims of the present application.
Example 1
A preparation method of LaOF nano powder comprises the following steps:
(1) Preparing a liquid precipitator:
mixing ethylenediamine and water in a volume ratio of 1 2 A gas trapping agent; introducing CO 2 Preparing a liquid precipitator after the gas is saturated;
(2) Preparation of hydrated lanthanum oxycarbonate:
adding lanthanum nitrate water solution into the liquid precipitator, mixing, stirring at 25 ℃, reacting for 12h, centrifugally separating to obtain white precipitate, washing with water and ethanol respectively, and drying to obtain hydrated lanthanum oxycarbonate; wherein the mass of lanthanum salt and CO 2 The mass ratio of the gas trapping agent is 1;
(3) Preparing spherical-like LaOF nano powder:
mixing the hydrated lanthanum oxycarbonate prepared in the step (2) with NaCl and NaF, and carrying out ball milling for 3 hours at the ball milling rotation speed of 400r/min, and calcining the mixed solid in a muffle furnace at the temperature of 700 ℃ to obtain quasi-spherical LaOF nano powder; wherein the mass ratio of hydrated lanthanum oxycarbonate to NaCl is 1.
As shown in fig. 1 to 3, the powder obtained in example 1 had a spheroidal morphology, and the XRD result showed that the powder was LaOF powder having a good crystal quality, with 90% or more of the particles having a particle size distribution of 150nm or less.
Comparative example 1
The same procedure as in example 1 was repeated, except that the amount of NaCl used was decreased and the ratio of hydrated lanthanum oxycarbonate to NaCl was changed to 1.
As shown in fig. 4 to 6, although the LaOF powder having good crystallinity obtained in comparative example 1 had irregular particle morphology and non-uniform particle size, 90% or more of the particles had a particle size distribution of 0.25 to 2 μm, which was much 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
The same procedure as in example 1 was repeated, except that the mixing ball-milling time of hydrous lanthanum oxycarbonate with NaCl and NaF was changed to 1 hour.
As shown in fig. 7 to 9, laOF powder having good crystallinity obtained in comparative example 2 had irregular particle morphology, and 90% or more of the particles had a particle size distribution of 0.5 to 2 μm or more, which was much larger than that of example 1. Therefore, when the mixing and ball milling time of the hydrated lanthanum oxycarbonate, naCl and NaF is short, only micron-sized LaOF particles can be obtained, and the spherical-like LaOF nanoparticles are difficult to obtain.
Comparative example 3
The procedure of example 1 was followed 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 does not yield LaOF without the addition of sodium fluoride, but also Cl can be incorporated into the decomposition products of the La precursor to form LaOCl, i.e. sodium fluoride can not only provide the source of F but also avoid the formation of LaOCl and La (OH) after calcination of the La precursor 3 。
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A preparation method of LaOF nano powder suitable for industrial production comprises the following steps:
(1) Obtaining a lanthanum-containing precursor;
(2) Mixing the lanthanum-containing precursor with NaCl and NaF, and carrying out ball milling for 3-24h to obtain a ball-milled mixture, wherein the mass ratio of the lanthanum-containing precursor to NaCl is 1;
(3) And calcining the ball-milled mixture at 600-1000 ℃ to obtain the LaOF nano powder.
2. The method of claim 1, wherein the LaOF nanopowder is spheroidal and has a particle size of less than 150 nm.
3. The method of claim 1, wherein the lanthanum-containing precursor is lanthanum oxycarbonate hydrate, lanthanum hydroxycarbonate, lanthanum carbonate, lanthanum hydroxide.
4. The method of preparing LaOF nanopowder of claim 1, wherein in step (1), the step of obtaining a lanthanum containing precursor comprises:
(1.1) preparing a liquid precipitator: mixing amine and water to obtain CO 2 A gas trapping agent, then introducing CO into the gas trapping agent 2 Obtaining the liquid precipitator after the gas is saturated;
(1.2) preparing a lanthanum-containing precursor: and adding a lanthanum source into the liquid precipitator, mixing and stirring for reaction, performing centrifugal separation to obtain a white precipitate, washing, and drying to obtain the lanthanum-containing precursor.
5. The method for preparing LaOF nanopowder according to claim 4, wherein in the step (1.1), the amine is at least one selected from ethylenediamine, diethylamine, ethanolamine, and diethanolamine.
6. The LaOF nanopowder preparation method of claim 4, wherein in step (1.1), the volume ratio of the amine mixed with water is 1.
7. The LaOF nano powder preparation method according to claim 4, wherein in the step (1.2), the lanthanum source is a lanthanum salt or a lanthanum salt aqueous solution, and the lanthanum salt is selected from lanthanum nitrate and/or lanthanum chloride.
8. The method of claim 7, wherein the lanthanum source comprises a lanthanum salt and CO 2 The mass ratio of the gas trapping agent is 1.
9. The LaOF nano-powder preparation method of claim 7, wherein the concentration of the lanthanum salt aqueous solution is 0.03-0.10mol/L.
10. The LaOF nano powder preparation method of claim 4, 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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