CN1319864C - Method for preparing superfine/nano iron oxide/iron powder - Google Patents

Method for preparing superfine/nano iron oxide/iron powder Download PDF

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CN1319864C
CN1319864C CNB2004100233027A CN200410023302A CN1319864C CN 1319864 C CN1319864 C CN 1319864C CN B2004100233027 A CNB2004100233027 A CN B2004100233027A CN 200410023302 A CN200410023302 A CN 200410023302A CN 1319864 C CN1319864 C CN 1319864C
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powder
present
superfine
ultra
iron
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CN1709799A (en
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范景莲
成会朝
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Central South University
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Central South University
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Abstract

The present invention relates to the field of powder metallurgy, particularly to a method for preparing superfine / nanometer ferric oxide by nanotechnology. The present invention is characterized in that ferric nitrate crystals (Fe(NO3)3.9H2O), ferrous sulphate crystals (FeSO4.7H2O) and ferric chloride crystals (FeCl. 6H2O) are used as raw materials; ferric salt solution the concentration of which is 30 wt% is prepared; ammonia water is added, and the pH value is adjusted from 1.5 to 3; then, 0.1% to 1.0% of a surface active agent and 0.01% to 0.1% of a crystal particle inhibitor are added. Transparent colloid is obtained by ultrasonic oscillation for 10 min to 60 min; subsequently, a precursor of superfine mixed powder is manufactured by drying; the precursor of the superfine mixed powder is calcined under the temperature from 350 DEG C to 700 DEG C so nanometer / superfine ferric oxide powder is obtained. The particle size of powder prepared by the present invention is thin and is smaller than 100 nm; the purity of the powder prepared by the present invention reaches as high as 99% to 99.5%. The powder can be used as high performance magnetic powder and microwave absorbing materials. The present invention has the advantages of simple manufacturing process, easy control of procedures and large yield of powder; the present invention is especially suitable for industrialized production.

Description

A kind of preparation method of superfine iron oxide powder
Technical field:
The present invention relates to field of powder metallurgy, particularly adopt nanotechnology to prepare the method for superfine iron oxide.
Background technology:
The preparation method of superfine iron oxide can be divided into wet method (Wet Method) and dry method (DryMethod) generally.Wet method is many to be raw material with industrial green vitriol, industrial iron protochloride and iron nitrate, adopt preparations such as oxidation-precipitation method, hydrothermal method, force water solution, colloid chemistry method, its characteristics are exactly that raw material is easy to get and can directly uses (only need suitable purifying treatment), particle is controlled, but technological process is oversize, yields poorly down, and is strict to operating environment, the production cost height is difficult to be applied on the industrial production.Dry method is often with iron carbonyl (Fe (CO) 5) or ferrocene (FeCP 2) be raw material, adopt flame thermolysis, low-temperature plasma chemical Vapor deposition process (PCVP) or the preparation of LASER HEAT decomposition method, have advantages such as technical process weak point, good operational environment, quality product height, particle are ultra-fine evenly, good dispersity, but its technical difficulty is big simultaneously, structure and material to equipment require high, one-time investment is big, and is domestic very few to its research.
Summary of the invention:
The present invention fully utilizes the strong point of prior art, overcome its deficiency, adopt colloidal sol and drying process with atomizing to prepare crystallite or amorphous mixed powder presoma, powder is calcined, preparation purity height, grain-size or powder single particle granularity are the nanometer superfine iron oxide powder of 15～30nm, the body of powder granularity is 1～1.5 μ m, by ball milling the granularity of body of powder is reduced to below the 100nm again, to satisfy the needs of electronics, Chemical Manufacture.
The present invention is for achieving the above object, and the scheme of employing is:
Adopt iron nitrate crystal (Fe (NO 3) 39H 2O), ferrous sulfate crystal (FeSO 47H 2O), iron(ic) chloride crystal (FeCl 36H 2O) be raw material, be mixed with the iron salt solutions that concentration is 30wt%;
In above-mentioned solution, add ammoniacal liquor and regulate pH1.5～3; Add 0.1～1.0% tensio-active agent and 0.01～0.1% grain inhibitor again,, obtain transparent colloid through ultra-sonic oscillation 10～60min;
Then that transparent colloid is dry on spray-drier, make ultra-fine mixed powder presoma;
The ultra-fine mixed powder that spraying drying is obtained obtains the superfine iron oxide powder at 350～700 ℃ of temperature lower calcinations;
To carry out ball-milling technology through the powder that calcining obtains and handle, powder size is reduced to below the 100nm;
The ultrafine powder presoma that makes or brown iron oxide reduced under reducing atmosphere obtain superfine iron powder.
Tensio-active agent is polyoxyethylene glycol-400, polyoxyethylene glycol-1000, polyoxyethylene glycol-10000, N, dinethylformamide, ethylene glycol, urea, tartrate, the third three acid, sodium laurylsulfonate, dimethyl phthalate, Citrate trianion, phosphoric acid salt.
Grain inhibitor is SnCl 2, Cr 2O 3
Advantage of the present invention and positively effect are embodied in:
(1) powder size of the present invention's preparation is thin, and less than 100nm, the purity height reaches 99%～99.5%, can be used as high performance magnetic powder and absorbing material.
(2) the present invention can prepare spherical powder or lamellar powder, and can control powder morphology.
(3) technology of the present invention is simple, and process is easy to control, and powder output is big, is fit to very much suitability for industrialized production.The present invention can make the superfine iron oxide powder as Fe 2O 3, Fe 3O 4Powder.
(4) the prepared superfine iron oxide powder of the present invention can carry out in a big way adjusting at aspect of performance, can prepare nonmagnetic to the very strong croci of magnetic.
Embodiment:
Example 1:
Take by weighing 100g Fe (NO 3) 39H 2O is dissolved in 500g H 2O;
Adding concentration is the ammoniacal liquor 120ml of 2.4wt%, is heated to 70 ℃ and makes it form Fe (OH) 3Colloid;
At Fe (OH) 3Add 0.5%N in the colloid, dinethylformamide, ultra-sonic oscillation 20min;
With above-mentioned colloid spraying drying, obtain amorphous/crystallite nanometer mixed powder presoma;
With amorphous/crystallite nanometer mixed powder presoma, calcining temperature is 350 ℃ of calcinings, obtains ultra-fine Fe 2O 3Powder;
To ultra-fine Fe 2O 3Powder carries out ball milling, makes its granularity further refine to below the 100nm;
With powder presoma or Fe 2O 3Powder is at H 2Reduce under the atmosphere, reduction temperature is 500 ℃, further obtains ultra-fine Fe powder.
Example 2:
(1) takes by weighing 100g Fe (NO 3) 39H 2O and 50g FeSO 47H 2O is dissolved in 600g H with it 2Op
(2) adding concentration is 2.4% ammoniacal liquor 300ml, and temperature is controlled at 40 ℃;
(3) add 0.5% polyoxyethylene glycol, 0.1% urea and 0.05%Cr 2O 3, through ultra-sonic oscillation 30min;
(4) the transparent colloid spraying drying be will obtain, amorphous or crystallite nanometer mixed powder presoma obtained;
(5) be to calcine in 600 ℃ of oxygen or the air atmosphere the powder presoma in calcining temperature, obtain ultra-fine/nanometer Fe 3O 4Powder;
(6) with powder presoma or nano level Fe 2O 3Powder is 400 ℃ in temperature, reduces in the hydrocarbon mixed gas, can further obtain ultra-fine Fe powder.

Claims (1)

1. the preparation method of a superfine iron oxide powder is characterized in that: adopting iron nitrate crystal, ferrous sulfate crystal, iron(ic) chloride crystal is raw material, is mixed with the iron salt solutions that concentration is 30wt%;
Adding ammoniacal liquor adjusting pH in above-mentioned solution is 1.5～3; Add 0.1～1.0% polyoxyethylene glycol-400, polyoxyethylene glycol-1000, polyoxyethylene glycol-10000, N again, dinethylformamide, ethylene glycol, urea, tartrate, the third three acid, sodium laurylsulfonate, dimethyl phthalate, Citrate trianion or phosphoric acid salt is as tensio-active agent, 0.01～0.1% SnCl 2Or Cr 2O 3As grain inhibitor,, obtain transparent colloid through ultra-sonic oscillation 10～60min;
Then that transparent colloid is dry on spray-drier, make ultra-fine mixed powder presoma;
The ultra-fine mixed powder that spraying drying is obtained obtains the superfine iron oxide powder at 350～700 ℃ of temperature lower calcinations.
CNB2004100233027A 2004-06-16 2004-06-16 Method for preparing superfine/nano iron oxide/iron powder Expired - Fee Related CN1319864C (en)

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CN100348501C (en) * 2006-01-10 2007-11-14 江苏天一超细金属粉末有限公司 Production and producer for nanometer ferric oxide
CN100406171C (en) * 2006-04-07 2008-07-30 北京科技大学 Process for preparing nano iron powder
CN100429152C (en) * 2006-11-21 2008-10-29 浙江大学 Process for preparing oxide nano sphere
CN102470441B (en) * 2009-07-30 2013-10-30 国立大学法人京都大学 Metal nanoparticles, dispersion containing same, and process for production of same
CN101664710B (en) * 2009-09-30 2011-02-16 南通宝聚颜料有限公司 Manufacturing method of ultra-fine iron oxide black
CN101823767B (en) * 2010-05-17 2012-06-13 哈尔滨师范大学 Method for preparing nano ferric oxide powder material with controllable grain size with pickling waste liquor
CN103204547A (en) * 2012-01-16 2013-07-17 中国科学院化学研究所 Ferrum oxyhydroxide and ferrum oxide hierarchical nanostructured material, preparation methods and applications thereof
CN102775739B (en) * 2012-08-17 2013-11-13 张宇 Composite wave-absorbing material adopting mesoporous silica foam material as matrix and preparation method of composite wave-absorbing material
CN103898736B (en) * 2014-01-23 2015-11-18 上海嘉乐股份有限公司 A kind of radiation resistant finish processing method of fabric
CN103833086B (en) * 2014-03-18 2015-09-30 济南大学 A kind of preparation method of sheet ferric oxide
CN103922421B (en) * 2014-05-13 2017-05-03 西北大学 Method for preparing alpha-Fe2O3
CN104058464B (en) * 2014-06-09 2016-05-11 青岛东方循环能源有限公司 A kind of method of preparing nano-sized iron oxide
CN104839202A (en) * 2015-05-05 2015-08-19 贺州学院 Nanometer iron oxide composite triazophos type pesticide and preparation method thereof
CN108655411B (en) * 2017-03-31 2022-04-01 深圳光启高等理工研究院 Preparation method of wave-absorbing material and wave-absorbing coating
CN107244698B (en) * 2017-06-17 2019-03-08 浙江正奇世荣科技有限公司 A kind of preparation method of iron oxide red
CN111733430B (en) * 2020-07-31 2022-08-05 北京化工大学 Fe-Fe 3 O 4 Composite anode and method for preparing ferrate by electrolysis of composite anode
CN115332500A (en) * 2022-07-28 2022-11-11 广东邦普循环科技有限公司 Preparation method and application of high-capacity battery active material

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Patent Citations (6)

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CN1312224A (en) * 2000-10-16 2001-09-12 童忠良 Liquid phase synthesis process of producing nanometer iron oxide red
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KR20040029871A (en) * 2002-10-02 2004-04-08 한국과학기술연구원 Shape anisotropic metal oxide nano-particles and synthetic method thereof

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