CN1725388A - A kind of magnetic flow liquid magnetic-particle and preparation method thereof with high antioxidant - Google Patents
A kind of magnetic flow liquid magnetic-particle and preparation method thereof with high antioxidant Download PDFInfo
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- CN1725388A CN1725388A CN 200510026850 CN200510026850A CN1725388A CN 1725388 A CN1725388 A CN 1725388A CN 200510026850 CN200510026850 CN 200510026850 CN 200510026850 A CN200510026850 A CN 200510026850A CN 1725388 A CN1725388 A CN 1725388A
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Abstract
The invention belongs to magnetic material and technical field of function materials, be specifically related to a kind of magnetic flow liquid iron-base soft magnetic particle and preparation method thereof with high antioxidant.The present invention utilizes the method for tetraethoxysilane (TEOS) hydrolysis-polycondensation reaction to coat one deck SiO on the magnetic-particle surface
2Film is prepared into magnetic composite particle.This magnetic-particle has better antioxygenic property, and has good resistance acid corrosion performance and higher saturation induction density, can be used as the soft magnetic particles of magnetic flow liquid.
Description
Technical field
The invention belongs to magnetic material and technical field of function materials, be specifically related to a kind of magnetic flow liquid iron-base soft magnetic particle and preparation method thereof with high antioxidant.
Background technology
Magnetic flow liquid (MRF) is a kind of new-type functional material, and under externally-applied magnetic field, rapid variation can take place its shear stress.(ERF) compares with electrorheological fluid, magnetic flow liquid has characteristics such as volume is little, power consumption is few, damping force is big, dynamic range is wide, frequency response is high, applicable surface is big, particularly it can produce optimal damping power according to the vibration characteristics of system, thereby has broad application prospects in fields such as intelligence structure, automobile, machinery, building, medical treatment.At present, iron-based grains is one of soft magnetic particles the most frequently used in the magnetic flow liquid, but one of its shortcoming is its easily oxidation of surface, and the magnetic property of magnetic-particle will descend after the oxidation, and influences the service efficiency and the useful life of magnetorheological devices.Saturation induction density as the oxide of iron has only 1/4th of iron powder, so the oxidation meeting of iron powder reduces the yield stress of MRF, thereby can shorten the useful life of magnetorheological device greatly.In order to address this problem, the researcher has used various methods to improve the antioxygenic property of magnetic-particle both at home and abroad.These methods comprise: the coat of metal (Ulicny J.C., Mance A.M., Mater.Sci.﹠amp; Eng., 2004, A369:309-313); Use ferroalloy (Carlson J.D., Weiss K.D., US Patent5382373); Polymer overmold (Kormann C.S., Ekkehard L.M., US Patent 5505880) etc.But, the coat of metal and use the ferroalloy complex process, cost an arm and a leg, and the coating layer thicker (greater than tens microns) of the method for general polymer overmold preparation, the increase of null field viscosity, the shear yield stress of magnetic flow liquid are reduced, and this application to magnetic flow liquid is very disadvantageous.The present invention utilizes the method for tetraethoxysilane (TEOS) hydrolysis-condensation reaction to coat one deck SiO on the magnetic-particle surface
2Film has prepared magnetic composite particle, obtains a kind of nanometer SiO that uses with this
2Film magnetic-particle that coat, that have better antioxygenic property, its method do not see that domestic and foreign literature openly reports.
Summary of the invention
The objective of the invention is to propose a kind of magnetic flow liquid magnetic-particle and preparation method thereof with high antioxidant.
The magnetic flow liquid magnetic-particle that the present invention proposes is by magnetic-particle surface coated Si O
2Nano thin-film is formed, and is a kind of iron-base soft magnetic particle, and its raw material is composed as follows:
100 parts of soft magnetic particles (weight)
Tetraethoxysilane 5-100 part (weight)
Hydrolytic accelerating agent 0-30 part (weight)
Aqueous components 0-1000 part (weight)
Dispersant 100-1000 part (weight)
Wherein, the particle diameter of described soft magnetic particles is 0.1-50 μ m, and material is one or more in the oxide, carbonyl iron dust, nitrided iron, cementite, stainless iron, cobalt, nickel, ferrocobalt, iron-nickel alloy of iron powder, iron.
Described tetraethoxysilane (TEOS), its user mode thing can be various teos solutions, or contains the mixture of tetraethoxysilane, guarantees the tetraethoxysilane consumption in these user mode things.
Described hydrolytic accelerating agent is meant chemical reagent that can promote the teos hydrolysis reaction and composition thereof, as NH
3H
2O, NH
3Deng, but not only for therewith.
Described aqueous components comprises water, ammoniacal liquor, Na
2CO
3The aqueous solution etc., and the mixture that contains these components, but be not limited only to this.
Described dispersant comprises the mixture of various alcohol, polyalcohol and they and water, as absolute ethyl alcohol, glycerol, ethanol water etc., but is not limited only to this.
Preparation method of the present invention is as follows:
(1) takes by weighing magnetic-particle according to weight proportion, place dispersant, abundant dispersed with stirring behind the adding tetraethoxysilane;
(2) drip by required hydrolytic accelerating agent and the aqueous components of proportioning, isothermal reaction 15-24h under the reaction mixing speed of 100-500rpm forms SiO outside soft magnetic particles
2Film;
(3) wash with water, the composite soft magnetic particle separation is come out with magnet.
By the present invention at magnetic-particle surface coated Si O
2The magnetic flow liquid that nano thin-film makes has good antioxygenic property, antiacid corrosive nature and higher saturation induction density with the magnetic composite particles.
Performance characterization method of the present invention is as follows:
(1) microstructure and the SiO of the H-800 type transmission electron microscope observation composite particles of the Japanese Hitachi of employing company
2The thickness of film.
(2) adopt NETZSCH STA 449C type thermogravimetric analyzer that the ferrous powder granules before and after coating is carried out thermogravimetric analysis (TGA), characterize their thermal oxidation resistance performance with this.
(3) iron powder that adopts the solubility in acid analysis to be about to equal in quality coating front and back is put into certain density acid solution respectively, tests the pH value of the solution of different time correspondence with PHS-25 type digital pH meter, thereby comes their antiacid corrosive nature of comparison.
(4) magnetic hysteresis loop of employing HH type vibrating specimen magnetometer (Nanjing Univ. Instrument Factory) test compound particle, saturation induction density (Bs).
The result shows, the composite magnetic particle of the present invention's preparation, and thermal oxidation resistance performance and antiacid corrosive nature are good, and have very high saturated magnetic induction.
Description of drawings
Fig. 1 coated Si O
2The TEM photo of the iron powder composite particles of nano thin-film.
Fig. 2 ferrous powder granules and coated Si O
2The thermogravimetric curve of the iron powder composite particles of nano thin-film.
Fig. 3 iron powder and coated Si O
2The antiacid corrosive nature of the iron powder composite particles of nano thin-film.
Fig. 4 iron powder and coated Si O
2The magnetic hysteresis loop of the iron powder composite particles of nano thin-film.
Embodiment
Following examples are only for further specifying the present invention, are not violating under the purport of the present invention, and the present invention should be not limited to the content that following experimental example is specifically expressed.
Embodiment 1
Embodiment is raw materials used as follows:
Reduced iron powder (analyzing pure), China Medicine (Group) Shanghai Chemical Reagent Co., provides.
Absolute ethyl alcohol (analyzing pure), Shanghai San'aisi Reagent Co., Ltd. provides.
Ammoniacal liquor (analyzing pure), Shanghai chemical reagent Co., Ltd of Chinese Medicine group
Tetraethoxysilane (TEOS), Shanghai chemical reagent Co., Ltd of Chinese Medicine group.
Raw materials used proportioning is as follows:
100 parts of reduced iron powders (weight)
5 parts of tetraethoxysilanes (weight)
30 parts of ammoniacal liquor (weight)
100 parts of absolute ethyl alcohols (weight)
Nanometer SiO
2The preparation of film coated magnetic particle:
Take by weighing the iron powder of 100g, place the 100g absolute ethyl alcohol, add behind the 5g tetraethoxysilane fully dispersed with stirring, slowly drip 30g concentration and be 25% ammoniacal liquor, normal-temperature reaction is 24 hours under the mixing speed of 500rpm.After reaction finishes, use the absolute ethanol washing suction filtration earlier, use deionized water wash, magnetic separates, and uses deionized water wash again, and repeated multiple times is to remove remaining TEOS, SiO
2Colloidal sol and the SiO that is not coated on the iron powder surface
2Particle.
Nanometer SiO
2The performance characterization of film coated magnetic composite particles:
(1) microstructure and the SiO of the H-800 type transmission electron microscope observation composite particles of the Japanese Hitachi of employing company
2The thickness of film, the result as shown in Figure 1, the magnetic composite particles that the present invention is prepared, surface coating layer thickness has only about 50nm.
(2) adopt NETZSCH STA 449C type thermogravimetric analyzer that the ferrous powder granules before and after coating is carried out thermogravimetric analysis (TGA), characterize their thermal oxidation resistance performance with this, the result as shown in Figure 2, the prepared magnetic composite particles of the present invention is compared with the iron powder that does not coat, and antioxygenic property obviously improves.
(3) iron powder that adopts the solubility in acid analysis to be about to equal in quality coating front and back is put into certain density acid solution respectively, test the pH value of the solution of different time correspondence with PHS-25 type digital pH meter, thereby come their antiacid corrosive nature of comparison, the result as shown in Figure 3, the prepared magnetic composite particles of the present invention is compared with the iron powder that does not coat, and antiacid corrosive nature obviously improves.
(4) magnetic hysteresis loop and the saturation induction density (Bs) of employing HH type vibrating specimen magnetometer (Nanjing Univ. Instrument Factory) test compound particle, its result as shown in Figure 4, the prepared magnetic composite particles of the present invention has higher saturation induction density (1.19 tesla).
Embodiment 2
Raw materials used proportioning is as follows:
100 parts of reduced iron powders (weight)
100 parts of tetraethoxysilanes (weight)
15 parts of ammoniacal liquor (weight)
500 parts of absolute ethyl alcohols (weight)
30 parts of deionized waters (weight)
Nanometer SiO
2The preparation of film coated magnetic particle:
Take by weighing the iron powder of 100g, place the 500g absolute ethyl alcohol, add behind the 30g tetraethoxysilane fully dispersed with stirring, slowly drip 15g concentration and be 25% ammoniacal liquor and 30g deionized water, normal-temperature reaction is 24 hours under the mixing speed of 500rpm.After reaction finishes, use the absolute ethanol washing suction filtration earlier, use deionized water wash, magnetic separates, and uses deionized water wash again, and repeated multiple times is to remove remaining TEOS, SiO
2Colloidal sol and the SiO that is not coated on the iron powder surface
2Particle.
The mensuration of magnetic composite particles performance is similar to Example 1, and its antioxygenic property, antiacid corrosive nature and saturation induction density are also similar with result shown in the embodiment 1.
Embodiment 3
Raw materials used proportioning is as follows:
100 parts of reduced iron powders (weight)
50 parts of tetraethoxysilanes (weight)
500 parts of absolute ethyl alcohols (weight)
1000 parts of deionized waters (weight)
Nanometer SiO
2The preparation of film coated magnetic particle:
Take by weighing the iron powder of 100g, place the 500g absolute ethyl alcohol, add behind the 50g tetraethoxysilane fully dispersed with stirring, slowly drip the deionized water of 1000g, normal-temperature reaction is 24 hours under the mixing speed of 200rpm.After reaction finishes, use the absolute ethanol washing suction filtration earlier, use deionized water wash, magnetic separates, and uses deionized water wash again, and repeated multiple times is to remove remaining TEOS, SiO
2Colloidal sol and the SiO that is not coated on the iron powder surface
2Particle.
The mensuration of magnetic composite particles performance is similar to Example 1, and its antioxygenic property, antiacid corrosive nature and saturation induction density are also similar with result shown in the embodiment 1.
Embodiment 4
Raw materials used proportioning is as follows:
100 parts of reduced iron powders (weight)
20 parts of tetraethoxysilanes (weight)
7 parts of ammoniacal liquor (weight)
600 parts of absolute ethyl alcohols (weight)
10 parts of deionized waters (weight)
Nanometer SiO
2The preparation of film coated magnetic particle:
Take by weighing the iron powder of 100g, place the 600g absolute ethyl alcohol, add behind the 20g tetraethoxysilane fully dispersed with stirring, slowly drip 7g concentration and be 25% ammoniacal liquor and 10g deionized water, normal-temperature reaction is 24 hours under the mixing speed of 100rpm.After reaction finishes, use the absolute ethanol washing suction filtration earlier, use deionized water wash, magnetic separates, and uses deionized water wash again, and repeated multiple times is to remove remaining TEOS, SiO
2Colloidal sol and the SiO that is not coated on the iron powder surface
2Particle.
The mensuration of magnetic composite particles performance is similar to Example 1, and its antioxygenic property, antiacid corrosive nature and saturation induction density are also similar with result shown in the embodiment 1.
Embodiment 5
Raw materials used proportioning is as follows:
100 parts of reduced iron powders (weight)
80 parts of tetraethoxysilanes (weight)
20 parts of ammoniacal liquor (weight)
400 parts of absolute ethyl alcohols (weight)
Nanometer SiO
2The preparation of film coated magnetic particle:
Take by weighing the iron powder of 100g, place the 400g absolute ethyl alcohol, add behind the 80g tetraethoxysilane fully dispersed with stirring, slowly drip 20g concentration and be 25% ammoniacal liquor, normal-temperature reaction is 24 hours under the mixing speed of 500rpm.After reaction finishes, use the absolute ethanol washing suction filtration earlier, use deionized water wash, magnetic separates, and uses deionized water wash again, and repeated multiple times is to remove remaining TEOS, SiO
2Colloidal sol and the SiO that is not coated on the iron powder surface
2Particle.
The mensuration of magnetic composite particles performance is similar to Example 1, and its antioxygenic property, antiacid corrosive nature and saturation induction density are also similar with result shown in the embodiment 1.
In the foregoing description, the parameter of each component raw material and consumption and preparation process only is the representative of choosing in order to describe invention.In fact a large amount of experiments show, in summary of the invention part institute restricted portion, all can obtain the similar nanometer SiO of the foregoing description
2Film coated magnetic composite particles.
Claims (6)
1, a kind of magnetic flow liquid magnetic-particle with high antioxidant is characterized in that by magnetic-particle surface clad nano SiO
2Film constitutes, and its raw material components is as follows:
100 parts of soft magnetic particles (weight)
Tetraethoxysilane 5-100 part (weight)
Hydrolytic accelerating agent 0-30 part (weight)
Aqueous components 0-1000 part (weight)
Dispersant 100-1000 part (weight)
Wherein, the soft magnetic particles particle diameter is 0.1-50 μ m.
2, magnetic flow liquid magnetic-particle according to claim 1 is characterized in that described soft magnetic particles material is one or more in the oxide of iron powder, iron, carbonyl iron dust, nitrided iron, cementite, stainless iron, cobalt, nickel, ferrocobalt, the iron-nickel alloy.
3, magnetic flow liquid magnetic-particle according to claim 1 is characterized in that described hydrolytic accelerating agent is NH
3H
2O or NH
3
4, magnetic flow liquid magnetic-particle according to claim 1 is characterized in that described aqueous components is deionized water, ammoniacal liquor, Na
2CO
3The aqueous solution.
5, magnetic flow liquid magnetic-particle according to claim 1 is characterized in that the mixture of described dispersant for alcohol, polyalcohol and they and water.
6, a kind of magnetic flow liquid as claimed in claim 1 preparation method of magnetic-particle is characterized in that step is:
(1) takes by weighing soft magnetic particles according to weight proportion, place dispersant, abundant dispersed with stirring behind the adding tetraethoxysilane;
(2) drip required by weight ratio hydrolytic accelerating agent and aqueous components, isothermal reaction 15-24h under the reaction mixing speed of 100-500rpm forms SiO on the soft magnetic particles surface
2Film;
(3) wash with water, with magnet the composite soft magnetic particle separation is come out again.
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| CN102046310A (en) * | 2008-11-26 | 2011-05-04 | 住友电气工业株式会社 | Method for producing soft magnetic material and method for producing dust core |
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| US8568644B2 (en) | 2008-05-23 | 2013-10-29 | Sumitomo Electric Industries, Ltd. | Method for producing soft magnetic material and method for producing dust core |
| CN102046310B (en) * | 2008-11-26 | 2013-09-25 | 住友电气工业株式会社 | Method for producing soft magnetic material and method for producing dust core |
| CN102046310A (en) * | 2008-11-26 | 2011-05-04 | 住友电气工业株式会社 | Method for producing soft magnetic material and method for producing dust core |
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| CN103192297B (en) * | 2012-08-24 | 2016-09-21 | 广东工业大学 | A kind of chemical cluster magneto-rheological combined processing method of single crystal silicon carbide wafer |
| CN103192297A (en) * | 2012-08-24 | 2013-07-10 | 广东工业大学 | Combined machining method for chemistry cluster magneto-rheological of monocrystal silicon carbide wafer |
| CN103177838B (en) * | 2012-12-30 | 2016-08-03 | 中南大学 | A kind of soft magnetic composite powder and preparation method thereof |
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| CN104766687A (en) * | 2015-04-27 | 2015-07-08 | 山东大学 | Alloyed carried liquid magnetic liquid and preparation method thereof |
| CN104766687B (en) * | 2015-04-27 | 2017-08-15 | 山东大学 | A kind of alloy carrier liquid magnetic liquid and preparation method |
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| CN108148505B (en) * | 2016-12-06 | 2021-01-19 | 江苏天一超细金属粉末有限公司 | Method for manufacturing composite particles for magnetorheological polishing |
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| CN110283373A (en) * | 2019-07-19 | 2019-09-27 | 航天特种材料及工艺技术研究所 | A kind of thermoplastic magnetic composite and preparation method |
| CN110534329A (en) * | 2019-08-26 | 2019-12-03 | 深圳大学 | A kind of preparation method of iron-nickel alloy magnetic fluid |
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