CN104276825A - Preparation method of rare-earth neodymium electrolysis ceramic crucible - Google Patents

Preparation method of rare-earth neodymium electrolysis ceramic crucible Download PDF

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Publication number
CN104276825A
CN104276825A CN201410516477.5A CN201410516477A CN104276825A CN 104276825 A CN104276825 A CN 104276825A CN 201410516477 A CN201410516477 A CN 201410516477A CN 104276825 A CN104276825 A CN 104276825A
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China
Prior art keywords
preparation
neodymium
rare earth
ceramic crucible
crucible
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Pending
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CN201410516477.5A
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Chinese (zh)
Inventor
陈学兵
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Suzhou Putin's Vacuum Technique Co Ltd
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Suzhou Putin's Vacuum Technique Co Ltd
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Priority to CN201410516477.5A priority Critical patent/CN104276825A/en
Publication of CN104276825A publication Critical patent/CN104276825A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632Organic additives
    • C04B35/636Polysaccharides or derivatives thereof
    • C04B35/6365Cellulose or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567Treatment time

Abstract

The invention discloses a preparation method of a rare-earth neodymium electrolysis ceramic crucible, which comprises the following steps: mixing a raw material composition, putting the mixture into a glass container, and precipitating to prepare a green blank; presintering the green blank to obtain a dry blank; putting the dry blank into a grinder, and grinding into powder; putting the powder into a forming machine, and carrying out compaction forming to obtain a crucible semifinished product; and sintering the crucible semifinished product to obtain a finished product crucible. The raw material composition comprises neodymium oxide, cerium oxide, copper oxide and a deionized water solution, wherein chitosan cellulose is added into the solution. The crucible prepared by the method has favorable corrosion resistance at high temperature, and has high thermal shock resistance; the quality of the product can not be influenced in the material consumption process; and the method can easily implement industrialization.

Description

A kind of preparation method of rare earth neodymium electrolytic ceramic crucible
Technical field
The present invention relates to crucible preparation, particularly relate to a kind of preparation method of rare earth neodymium electrolytic ceramic crucible.
Background technology
Along with the progress of science and technology, the application of rare earth metal in novel material, electronics, new ceramics is more and more wider, meanwhile, also more and more higher to the requirement of rare-earth metal material.
Fused salt electrolysis is topmost method during China's rare earth material is smelted, most neodymium is fluoride salt electrolytic preparation, but it is easily oxidation and corrosion under high-temperature electrolysis, detrimentally affect is brought to Rare Earth Production, such as add the cost producing rare earth, reduce the quality of rare earth metal, affect normally carrying out of electrolysis production, above various production defect has disclosed China and has produced rare earth element Problems existing.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of rare earth neodymium electrolytic ceramic crucible, product slate quality is not endangered in good, the materials consumption process of corrosion resistance under the crucible high temperature that the method is obtained, there is stronger heat resistanceheat resistant to shake performance, be easy to realize industrialization.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the preparation method providing a kind of rare earth neodymium electrolytic ceramic crucible, comprise and feedstock composition is mixed, obtaining liquid material will, then compound is put into Glass Containers to precipitate, make green compact, green compact are carried out pre-burning, the dry blank of system, dry blank is put into and carries out grinding inside shredder and make powder-material, powder-material after grinding is put into the crucible work in-process of the system of being pressed inside forming machine, compression moulding crucible work in-process are sintered, obtain finished product crucible, wherein, described feedstock composition comprises Neodymium trioxide, cerium oxide, cupric oxide and deionized water solution, and, chitin fiber element is also added with inside described solution.
In the present invention's preferred embodiments, in described solution, the mass fraction of Neodymium trioxide is 40 ~ 60wt%.
In the present invention's preferred embodiments, in described solution, the particle diameter of Neodymium trioxide is 30 ~ 80nm, and the specific surface area of Neodymium trioxide is 200 ~ 350m 2/ g.
In the present invention's preferred embodiments, the purity of described chitin fiber element is more than 99.0%.
In the present invention's preferred embodiments, in described feedstock composition, with the content of Neodymium trioxide for benchmark, in described solution, the content of cerium oxide is 5-10wt%, and the content of described cupric oxide is 3-6wt%, and the content of described deionized water is 15-20wt%.
In the present invention's preferred embodiments, described compound adds oxalate coprecipitation when precipitating.
In the present invention's preferred embodiments, described forming machine adopts the method for static(al) compacting, and pressure is 90Mpa.
In the present invention's preferred embodiments, described ceramic crucible sintering temperature is 950 ~ 1050 DEG C, and sintering time is 10 ~ 12 hours.
The invention has the beneficial effects as follows: the preparation method of a kind of rare earth neodymium electrolytic ceramic of the present invention crucible, product slate quality is not endangered in good, the materials consumption process of corrosion resistance under the crucible high temperature that the method is obtained, there is stronger heat resistanceheat resistant to shake performance, be easy to realize industrialization.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
The embodiment of the present invention comprises:
A kind of preparation method of rare earth neodymium electrolytic ceramic crucible, comprise and feedstock composition is mixed, obtaining liquid material will, then compound is put into Glass Containers to precipitate, make green compact, green compact are carried out pre-burning, the dry blank of system, dry blank is put into and carries out grinding inside shredder and make powder-material, powder-material after grinding is put into the crucible work in-process of the system of being pressed inside forming machine, compression moulding crucible work in-process are sintered, obtain finished product crucible, wherein, described feedstock composition comprises Neodymium trioxide, cerium oxide, cupric oxide and deionized water solution, and, chitin fiber element is also added with inside described solution.
Further, in described solution, the mass fraction of Neodymium trioxide is 40 ~ 60wt%.
Further, in described solution, the particle diameter of Neodymium trioxide is 30 ~ 80nm, and the specific surface area of Neodymium trioxide is 200 ~ 350m 2/ g.
Further, the purity of described chitin fiber element is more than 99.0%.
Further, in described feedstock composition, with the content of Neodymium trioxide for benchmark, in described solution, the content of cerium oxide is 5-10wt%, and the content of described cupric oxide is 3-6wt%, and the content of described deionized water is 15-20wt%.
Further, described compound adds oxalate coprecipitation when precipitating.
Further, described forming machine adopts the method for static(al) compacting, and pressure is 90Mpa.
Further, described ceramic crucible sintering temperature is 950 ~ 1050 DEG C, and sintering time is 10 ~ 12 hours.
The invention has the beneficial effects as follows: the preparation method of a kind of rare earth neodymium electrolytic ceramic of the present invention crucible, product slate quality is not endangered in good, the materials consumption process of corrosion resistance under the crucible high temperature that the method is obtained, there is stronger heat resistanceheat resistant to shake performance, be easy to realize industrialization.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical field, be all in like manner included in scope of patent protection of the present invention.

Claims (8)

1. the preparation method of a rare earth neodymium electrolytic ceramic crucible, it is characterized in that, comprise and feedstock composition is mixed, obtaining liquid material will, then compound is put into Glass Containers to precipitate, make green compact, green compact are carried out pre-burning, the dry blank of system, dry blank is put into and carries out grinding inside shredder and make powder-material, powder-material after grinding is put into the crucible work in-process of the system of being pressed inside forming machine, compression moulding crucible work in-process are sintered, obtain finished product crucible, wherein, described feedstock composition comprises Neodymium trioxide, cerium oxide, cupric oxide and deionized water solution, and, chitin fiber element is also added with inside described solution.
2. the preparation method of rare earth neodymium electrolytic ceramic crucible according to claim 1, is characterized in that, in described solution, the mass fraction of Neodymium trioxide is 40 ~ 60wt%.
3. the preparation method of rare earth neodymium electrolytic ceramic crucible according to claim 1, is characterized in that, in described solution, the particle diameter of Neodymium trioxide is 30 ~ 80nm, and the specific surface area of Neodymium trioxide is 200 ~ 350m2/g.
4. the preparation method of rare earth neodymium electrolytic ceramic crucible according to claim 1, is characterized in that, the purity of described chitin fiber element is more than 99.0%.
5. the preparation method of rare earth neodymium electrolytic ceramic crucible according to claim 1, it is characterized in that, in described feedstock composition, with the content of Neodymium trioxide for benchmark, in described solution, the content of cerium oxide is 5-10wt%, the content of described cupric oxide is 3-6wt%, and the content of described deionized water is 15-20wt%.
6. the preparation method of rare earth neodymium electrolytic ceramic crucible according to claim 1, is characterized in that, described compound adds oxalate coprecipitation when precipitating.
7. the preparation method of rare earth neodymium electrolytic ceramic crucible according to claim 1, is characterized in that, described forming machine adopts the method for static(al) compacting, and pressure is 90Mpa.
8. the preparation method of rare earth neodymium electrolytic ceramic crucible according to claim 1, is characterized in that, described ceramic crucible sintering temperature is 950 ~ 1050 DEG C, and sintering time is 10 ~ 12 hours.
CN201410516477.5A 2014-09-30 2014-09-30 Preparation method of rare-earth neodymium electrolysis ceramic crucible Pending CN104276825A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105218109A (en) * 2015-08-18 2016-01-06 安泰科技股份有限公司 A kind of fluorochemical ceramic crucible and manufacture method thereof
CN114044687A (en) * 2021-12-17 2022-02-15 江西离子型稀土工程技术研究有限公司 Rare earth oxide body crucible and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1188162A (en) * 1997-11-19 1998-07-22 西北有色金属研究院 Rare earth molten-salt electrolysis ceramic anode and preparing method thereof
KR20120043984A (en) * 2010-10-27 2012-05-07 한국세라믹기술원 Stabilized zirconia with black color and manufacturing method of the same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1188162A (en) * 1997-11-19 1998-07-22 西北有色金属研究院 Rare earth molten-salt electrolysis ceramic anode and preparing method thereof
KR20120043984A (en) * 2010-10-27 2012-05-07 한국세라믹기술원 Stabilized zirconia with black color and manufacturing method of the same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105218109A (en) * 2015-08-18 2016-01-06 安泰科技股份有限公司 A kind of fluorochemical ceramic crucible and manufacture method thereof
CN105218109B (en) * 2015-08-18 2017-11-07 安泰科技股份有限公司 A kind of fluoride ceramic crucible and its manufacture method
CN114044687A (en) * 2021-12-17 2022-02-15 江西离子型稀土工程技术研究有限公司 Rare earth oxide body crucible and preparation method thereof

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Application publication date: 20150114