CA2018346A1 - Niobium oxide powder (nb o ) and a process for its preparation - Google Patents

Niobium oxide powder (nb o ) and a process for its preparation

Info

Publication number
CA2018346A1
CA2018346A1 CA002018346A CA2018346A CA2018346A1 CA 2018346 A1 CA2018346 A1 CA 2018346A1 CA 002018346 A CA002018346 A CA 002018346A CA 2018346 A CA2018346 A CA 2018346A CA 2018346 A1 CA2018346 A1 CA 2018346A1
Authority
CA
Canada
Prior art keywords
weight
niobium oxide
nb2o5
ppm
process according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
CA002018346A
Other languages
French (fr)
Inventor
Walter Bludssus
Erk-Rudiger Feuerhahn
Horst Zimmermann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HC Starck GmbH
Original Assignee
HC Starck GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HC Starck GmbH filed Critical HC Starck GmbH
Publication of CA2018346A1 publication Critical patent/CA2018346A1/en
Abandoned legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G33/00Compounds of niobium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/51Particles with a specific particle size distribution
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

Title: Niobium oxide powder (Nb2O5) and a process for its preparation ABSTRACT OF THE DISCLOSURE

Niobium oxide powders in non-agglomerated form with a narrow particle size distribution range, high specific surface area, high purity and 2-20 ppm Fe and 2-30 ppm Ni usable in carbide preparation, ferro alloy melting and as a raw material for optical glasses and electro-ceramic and electro-optical products. The powders are made by precipitation from fluoride solution, filtering, washing, annealing and milling. The washing is carried out to an extent that annealing losses are 10-50 % by weight, the calcining is at 600°C-1000°C and the calci-ned product is finley ground.

Description

201~33~6 Title; Niobium oxide powder (Nb2O5) and a process for its preparation _ _ _ . . . . .. .. . . _ _ .

BACK~ROUND OF THE INVENTION

This invention relates to an improved niobium oxide powder (Nb2O5) which consist~ to an extent of more than 90 % of the T-phase, has a fluorine value of under 1000 ppm, passes through a 45 micron sieve to an extent of over 99,9 % by weight, has a specific surface area according to Brunauer Emmett Tellertest/BET (ASTM
D 3037/~1) of more than 3,5 m~/g and has an Nb2O5 con-tent of over 99,8 % by weight, not taking into account the losses on annealing, and to a process for the pre-paration of this niobium oxide powder.
Ta2O and Nb2O5 are normally decomposed by means of an acid mixture of HF and H2SO4. The fluoro complexes of the two elements, dissolved in aqueous mineral acids, are extracted with organic solvents, preferably methyl isobutyl ketone (MIBK~. The niobium fluoro acid i~ then reextracted from the organic phase and the hydrated niobium oxide is precipitated from the aqueous strip solution with ammoniacal water, This procedure is followed by filtrat~on of the solid and drying and calcining at temperatures above about 1000C (Ullmanns "Enzyklopadie der techni~che Chemie, 4th Edition, 1979, Volume 17).

~5 20183~6 The oxides prepared by this process are used for the preparation of carbides for hard metals, the melting of ferro alloys, and as raw material for optical glasses and for electroceramic and electro-optical products.
Nb205 has for some time now been used to an increasing extent in ceramic condensers, especially in so-called relaxor-perovskites (See, t.: Swartz and Shrout, "Fabrication of Perovskite Lead Magnesium Niobate", Mat. Res. Bull., Volume 17, pages 1245-1250, 1982).
The presently available Nb205 powders are, in various respects, suitable only to a limited extent for the last mentioned purpose. It is an obgect of the present invention to provide suitable powders.

SUMMARY OF THE INVENTION

It has now been found that the requirements are fulfilled by niobium oxide powders which are present as fine powders in an non-agglomerated form with a narrow particle size distribution and uniformity of the partic-les. An additional characteristic of these powders is that they have as large a specific surface area (BET
surface) as possible and a very h;gh degree of purity.

X~83~i The invention compri 5 es a nobium oxide (Nb205) powder which a) consists to an extent of over 90 % by weight of T-phase, b) has a fluorine value of under 1000 ppm, c) passes through a 45 micron siev0 to an extent of over 99,9 % by weight, and d) has a specific surface area according to BET
(ASTM D 3037/81~ of more than 3,5 n~/g and e) an Nb205 content of over 99,8 % by weight, not taking into account the 10s5 on annealing and f) contains from 2 to 20 ppm of Fe an from 2 to 30 ppm of Ni.

An Nb205 powder of this type which has the following particle size distribution according to a Sedigraph 5000 D (ASTM B 761-86~ is particularly preferred:
90 % by weight, under 2,5 micro~s 50 % by weight, under 1,0 microns, preferably from 0,5 to 0,7 microns, 30 % by weight, 0,6 microns.

This invention further relates to a process for the preparation of the acid niobium oxide powders. The process consists of a combination of known process steps in which hydrated niobium oxide is procipitated with ammoniacal water from a fluoride-containing solution and then filtered, wa~hed, annealed and milled, in which process Z018~46 a) washing to the filter cake obtained after fil-trat;on is followed by dry;ng to such an extent that the dry product has a loss on annealing of from 10 to 50 % we;ght, preferably from 20 to 30 X by we;ght, b) the dry product is calcined at temperatures from 600C to 1000C and c~ the calcined product thus obtained is finley ground, :
In the process according to the in~ention, calci-nation is preferably carr;ed out at temperatures from 800 to 900C, Th;s calcination may be carried out in known apparatus Calcination in an rotary tube furnace has proved to be particularly economical and should be carried out o~er a res;dence time of at least one hour, preferably not less than 2 hours, Particularly good results are obtained from the process according to the ;nv-ntion if the filter cake ;s washed unt;l ;t contains less than 0,5 X by weight of fluorine DETAILED DESCUPTION OF PREFERRED EMBODIMENTS

The ;n~ent;on ict d-scr;bed in dotail bolow with th- aid of a non-l;miting illu-trating a preferr-d embodiment of pratice, .

- ' , X0~83~6 EXAMPLE
2,5 cubic meters of niobium fluoride solution obtained from re-extraction and containing about 120 g of Nb205 per litre are added to 7 cubic meters of a 3 X aqueous ammonia solution, and ammoniacal water at a concen-tration of 25 X is added to this mixtrue until a pH of 9 is obtained. The precipitated hydrated oxide is sepa-rated off through a plate filter and neutralized by washing with 7 cubic meters of 3 X ammoniacal water and 6 cubic meters of demin-ralized water. Tho fluorine con-tent of the filter cake ist then less than 0,5 % by weight. The filter cake i6 dried. The loss on annealing of a sample crude product is then worked up in a rotary tube furnace at 900C and a residence time of 2 hours.
The annealed oxide is subsequently size reduced in a jet mill.
Ph~sical and chemical analysis Specific sufrace (BET): 4,26 n~/g Particle spectrum (Sedigraph 5000 D): 90 X under 1 micron 50 X under 0,56 micron 30 % under 0,48 micron Sie~e analysis: 99,9 % under 45 micron Proportion of T-phase: over 90 X by weight ~5 20~334~

Charac~eristic impuri~ies:

Fluorine : 360 ppm Calcium : 8 ppm Chromium : under 2 ppm Iron : ~ ppm Nickel : 4 ppm Tantalum : under 12 ppm

Claims (10)

1. Niobum oxide (Nb2O5) powder which a) comprises mor than 90 % by of T-phase, b) has a fluorine value of comprise less than 1000 pppm, c) passes through a 45 micron sieve to an extent of more than 99,9 X by weight and d) has a specific surface area according to BET
(ASTM D 3037/81) of more than 3,5 m2/g and e) an Nb2O5 content of more than 99,8 % by weigh, not taking into account the loss on annea-ling, and further characterised in that it contains from
2 to 20 ppm of Fe and from 2 to 30 ppm of Ni.

2. Niobium oxide powder in accordance with claim 1 characterised in that it has a particle size distribution according to a Sedigraph 5000 D (ASTM
B 761-86) of 90 % by weight less than 2,5 microns 50 % by weight less than 1,0 microns 30 % weight less than 0,6 microns.
3. Niobium oxide powder in accordance with claim 2 wherein at least 50 X by weight thereof is from 0,5 to 0,7 micron size sarge.
4. A process for the preparation of Nb2O5 powder as set forth in either of claims 1 or 2 by the pre-cipitation of hydrated niobium oxide with ammonical water from a solution containing fluoride followed by filtration, washing, annealing and grinding, in which a) washing of the filter cake obtained from filtration is followed by drying to such an extent that the dry product has a loss on annealing of from 10 to 50 % by weight, preferably from 20 to 30 % by weight, b) the dry product is calcined at temperatures from 600°C to 1000°C and c) the calcined product thus obtained is finley ground.
5. A process according to claim 4, wherein calcination is carried out at temperatures from 800°C to 900° C.
6. A process according to either of claims 4 or 5, wherein calcination is carried out in a rotary tube furnace.
7. A process according to Claim 6, wherein in calci-nation is carried out with a residence time of at least one hour.
8. A process according to claim 7 wherein the resi-dence time is at least two hours.
9. A process for the preparatio of Nb2O5 powder accor-ding to any of claims 4 to 8, wherein the filter cake is washed until it contains less than 0,5 X
by weight of fluorine.
10. A process according to eithers of Claims 4 or 5, wherein fine grinding of the calcined material is carried out in a je mill.
CA002018346A 1989-06-08 1990-06-06 Niobium oxide powder (nb o ) and a process for its preparation Abandoned CA2018346A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3918691A DE3918691A1 (en) 1989-06-08 1989-06-08 NIOBOXIDE POWDER (NB (DOWN ARROW) 2 (DOWN ARROW) O (DOWN ARROW) 5 (DOWN ARROW)) AND METHOD FOR THE PRODUCTION THEREOF
DEP3918691.1 1989-06-08

Publications (1)

Publication Number Publication Date
CA2018346A1 true CA2018346A1 (en) 1990-12-08

Family

ID=6382335

Family Applications (1)

Application Number Title Priority Date Filing Date
CA002018346A Abandoned CA2018346A1 (en) 1989-06-08 1990-06-06 Niobium oxide powder (nb o ) and a process for its preparation

Country Status (11)

Country Link
EP (1) EP0402687B1 (en)
JP (1) JPH0323222A (en)
KR (1) KR0140871B1 (en)
CN (1) CN1025669C (en)
AT (1) ATE101104T1 (en)
AU (1) AU630967B2 (en)
BR (1) BR9002693A (en)
CA (1) CA2018346A1 (en)
DD (1) DD297949A5 (en)
DE (2) DE3918691A1 (en)
ZA (1) ZA904388B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7066979B2 (en) 2002-03-12 2006-06-27 H. C. Starck Gmbh Valve metal powders and process for producing them
US7099143B1 (en) 2005-05-24 2006-08-29 Avx Corporation Wet electrolytic capacitors
WO2022036427A1 (en) * 2020-08-17 2022-02-24 Fras-Le S.A. Preparation of niobium nanoparticles, use and method for obtaining same
EP4105180A4 (en) * 2020-02-14 2023-08-30 Mitsui Mining & Smelting Co., Ltd Niobic acid aqueous solution

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4030707A1 (en) * 1990-09-28 1992-04-02 Starck Hermann C Fa METHOD FOR THE PRODUCTION OF LOW FLUORIDE TANTALY / NIOB OXIDE HYDRODATES OR OXIDES
US6338832B1 (en) * 1995-10-12 2002-01-15 Cabot Corporation Process for producing niobium and tantalum compounds
US6416730B1 (en) 1998-09-16 2002-07-09 Cabot Corporation Methods to partially reduce a niobium metal oxide oxygen reduced niobium oxides
IL151549A0 (en) 2000-03-01 2003-04-10 Cabot Corp Nitrided valve metals and processes for making the same
JP4996016B2 (en) * 2001-06-01 2012-08-08 三井金属鉱業株式会社 Niobium oxide slurry, niobium oxide powder and production method thereof
US20040062709A1 (en) * 2001-12-27 2004-04-01 Kenji Higashi Powder of tantalum oxide or niobium oxide, and method for production thereof
JP4202195B2 (en) * 2003-06-10 2008-12-24 三井金属鉱業株式会社 Tantalum hydroxide, niobium hydroxide, tantalum oxide, niobium oxide, and production methods thereof
CN103253708B (en) * 2013-05-08 2014-11-05 北京工业大学 Solvothermal preparation method of niobium pentoxide nanowire by use of acetic acid
CN107055613B (en) * 2017-02-27 2018-10-30 湖南工业大学 A kind of no substrate niobium pentoxide nano chip arrays negative material and its preparation method and application
JP7290921B2 (en) * 2018-07-06 2023-06-14 太陽誘電株式会社 Piezoelectric ceramic composition, manufacturing method thereof, piezoelectric ceramic, piezoelectric element, and piezoelectric vibration device
US11058883B2 (en) * 2019-02-15 2021-07-13 Medtronic, Inc. Feedthrough assembly
CN110386623B (en) * 2019-07-04 2022-04-19 江西海协稀有金属材料有限公司 Method for preparing high-purity niobium oxide by filtering niobium ceramic membrane
GB2616009B (en) 2022-02-23 2024-05-01 Echion Tech Limited Electrode and method of manufacture

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3640679A (en) * 1969-02-06 1972-02-08 Molybdenum Corp Process for recovery of columbium
JPS4930354A (en) * 1972-07-17 1974-03-18
JPS5110197A (en) * 1974-07-16 1976-01-27 Ishihara Sangyo Kaisha Suisankaniobu mataha suisankatantaruno seizohoho
DK449074A (en) * 1974-08-22 1976-02-23 Atomenergikommissionen PROCEDURE FOR EXTRACTING TANTALS AND / OR NIOB IN FREE OR BASED FORM FROM TANTAL AND NIOB CONTAINING SOLUTIONS
DE3428788C2 (en) * 1983-08-11 1986-07-10 Günter J. 8510 Fürth Bauer Process for the continuous production of low-fluoride tantalum or niobium pentoxides
DD250706A1 (en) * 1986-07-01 1987-10-21 Mansfeld Kombinat W Pieck Veb PROCESS FOR THE PREPARATION OF FLUORIDE TANTAL OR NITROPOXIDE OXIDE

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7066979B2 (en) 2002-03-12 2006-06-27 H. C. Starck Gmbh Valve metal powders and process for producing them
US7485257B2 (en) 2002-03-12 2009-02-03 H.C. Starck Gmbh Valve metal powders
US7099143B1 (en) 2005-05-24 2006-08-29 Avx Corporation Wet electrolytic capacitors
US7456073B2 (en) 2005-05-24 2008-11-25 Avx Corporation Wet electrolytic capacitors
EP4105180A4 (en) * 2020-02-14 2023-08-30 Mitsui Mining & Smelting Co., Ltd Niobic acid aqueous solution
WO2022036427A1 (en) * 2020-08-17 2022-02-24 Fras-Le S.A. Preparation of niobium nanoparticles, use and method for obtaining same

Also Published As

Publication number Publication date
DD297949A5 (en) 1992-01-30
CN1025669C (en) 1994-08-17
AU5704390A (en) 1990-12-13
JPH0323222A (en) 1991-01-31
DE59004470D1 (en) 1994-03-17
ATE101104T1 (en) 1994-02-15
DE3918691C2 (en) 1991-07-04
BR9002693A (en) 1991-08-20
AU630967B2 (en) 1992-11-12
KR0140871B1 (en) 1998-06-01
KR910000537A (en) 1991-01-29
EP0402687A1 (en) 1990-12-19
ZA904388B (en) 1991-03-27
DE3918691A1 (en) 1990-12-13
CN1047842A (en) 1990-12-19
EP0402687B1 (en) 1994-02-02

Similar Documents

Publication Publication Date Title
CA2018346A1 (en) Niobium oxide powder (nb o ) and a process for its preparation
EP0357959B1 (en) Sinterable raw material based on aluminium titanate, process for its preparation and sintered articles made therefrom, and its use
EP0265013B1 (en) Process for the preparation of barium titanate bati03
AU604710B2 (en) Preparation of high purity, homogeneous zirconia mixtures
DE3633030A1 (en) ALUMINUM OXIDE-TITANIUM DIOXIDE COMPOSITE POWDER AND METHOD FOR THE PRODUCTION THEREOF
EP0593695A1 (en) Method for the synthesis of mixed metal oxide crystalline powders
EP0601453A2 (en) Process for the preparation of aluminium oxide particles, aluminium oxide powder obtained according to this process and the use of this powder
AT389693B (en) METHOD FOR PRODUCING ALUMINUM TITANATE
DE3932780A1 (en) ZIRCONDIOXIDE POWDER, METHOD FOR THE PRODUCTION THEREOF, THE USE THEREOF AND THE SINTER BODIES MADE THEREOF
DE3604848A1 (en) ABRASIVE GRAIN AND METHOD FOR THE PRODUCTION THEREOF
EP1606355B1 (en) Iron oxide pigments
US3264124A (en) Production of ultra-fine alpha alumina and such alpha alumina
DE1814113A1 (en) Process for the production of lead oxides
EP0421076A1 (en) Zirconium dioxide powder, process for its preparation, its use and sintered bodies prepared therefrom
Duran et al. Study of the behaviour of Al2TiO5 materials in reducing atmosphere by spectroscopic techniques
JP2557344B2 (en) Method for treating inorganic hydroxide precipitate
EP1606356B1 (en) Iron oxide pigments
DE3415324A1 (en) METHOD FOR PRODUCING SINTERABLE POWDER FROM (GAMMA) -LIAL0 (DOWN ARROW) 2 (DOWN ARROW) AND THE USE THEREOF
DE1954138C3 (en) Process for the production of high purity alpha alumina
EP1663870A1 (en) Valve metal-oxide powder and method for producing said powder
DE2322255C3 (en) Process for the production of calcium zirconate
DE4039181A1 (en) Fine metal oxide powder prodn. - by pptn. from soln. under turbulence produced by oxygen stream
Ramachandran Raw materials for alumina ceramics
Roy et al. Isothermal Sintering of Size-Graded Sillimanite
DE4414570A1 (en) Mfr. of alpha-aluminium oxide sintered microcrystalline bodies

Legal Events

Date Code Title Description
EEER Examination request
FZDE Discontinued