CN105174317A - Novel technology for synthesizing nanometer Fe3O4 particles for magnetic liquid - Google Patents
Novel technology for synthesizing nanometer Fe3O4 particles for magnetic liquid Download PDFInfo
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- CN105174317A CN105174317A CN201510564933.8A CN201510564933A CN105174317A CN 105174317 A CN105174317 A CN 105174317A CN 201510564933 A CN201510564933 A CN 201510564933A CN 105174317 A CN105174317 A CN 105174317A
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- particle
- magnetic liquid
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- active agent
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Abstract
The invention relates to a novel technology for synthesizing nanometer Fe3O4 particles for magnetic liquid, and belongs to the technical field of material preparation. Nanometer Fe3O4 particles obtained are suitable for serving as raw materials for preparing magnetic liquid. The novel technology performs Fe3O4 preparation and surfactant coating at the same time; firstly, a uniform mixed liquor of Fe3 plus, Fe2 plus and surfactant is prepared; then ammonium hydroxide is added, to serve as a precipitator; intermediate isolation is not required, steps of temperature and PH regulation are not required during reaction, and surfactant coated nanometer Fe3O4 is directly obtained. The technology has the advantages that raw materials and equipment are simple and easy to get, multi-people operation is not required for the preparation method, the method is simple, the repeatability is high, the prepared particles are spherical and are beneficial to the improvement of the lubricating property of magnetic liquid, abrasion is reduced, meanwhile the technology can be applied to high molecular surfactant of high-viscosity and low-saturation vapor pressure magnetic liquid, stable chemical adsorption quantity, of surfactant on the surface of Fe3O4, measured through a thermogravimetric analyzer can reach 40 to 60 percent, the oxidation resistance is high, and the high-temperature stability is high.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of synthesizing magnetic liquid nanometer Fe
3o
4the novel process of particle.The Fe that gained tensio-active agent is coated
3o
4work done in the manner of a certain author is prepare the raw material of magnetic liquid.
Background technology
Magnetic liquid is otherwise known as magnetic fluid, and a kind of new function material is (as Fe the nano magnetic particle after tensio-active agent is coated
3o
4) be highly dispersed in base load liquid, and the stable colloidal solutions formed.After last century, the sixties was successfully synthesized, because it had both had the magnetic of solid material, there is again the mobility of fluent material, the effect that solid magnetic material can not play can be played, be widely used in sealing, lubrication, vibration damping, medicine and other fields.
The preparation table surface-active agent clad nano Fe commonly used at present
3o
4the method of particle is first by preparation nanometer Fe
3o
4particle, regulates the reaction conditions such as temperature of reaction, PH afterwards, then carries out Coated with Oleic Acid, and as Chinese patent CN104091678A, first the method is owing to preparing Fe
3o
4after particle, artificial adjustment is needed to react PH and make synthesized Fe
3o
4particle is subject to interference from human factor, poor repeatability, secondly first synthesizes Fe because of it
3o
4particle, synthesized Fe
3o
4particle is octahedra spinel structure, if magnetic-particle is used for lubricating area, to be unfavorable for reducing wearing and tearing, again because the molecules surfactant of coated high viscosity, low saturation vapour pressure magnetic liquid, often need under high temperature, condition of high voltage, this method can not be used for the molecules surfactant of coated high viscosity, low saturation vapour pressure magnetic liquid.
Pertinent literature is had to point out, size, shape that tensio-active agent contributes to controlling nano particle was added in advance before synthesis of nano particle, as one section of summary about tensio-active agent that the people such as Tsing-Hua University Niu Zhiqiang deliver in CHEMISTRYOFMATERIALS, before synthesis of nano particle, add tensio-active agent and can suppress particle growth and reunion, the shape of the synthesized crystal grain of impact simultaneously.
But the nanometer Fe of magnetic liquid is used in synthesis
3o
4tensio-active agent (for oleic acid) is added, due to synthesis of nano Fe before particle
3o
4particle often needs to use excesses of basic precipitation agent (as ammoniacal liquor), at synthesis of nano Fe
3o
4after particle, often make solution be strong basicity, form ammonium oleate simultaneously, be unfavorable in nanometer Fe
3o
4particle surface forms stable chemisorbed layer, and the magnetic liquid stability of final synthesis does not reach service requirements.
Summary of the invention
Technical problem to be solved by this invention is:
Existing nanometer Fe
3o
4in particle technology of preparing, synthesized particle before coated, needs artificially to regulate the reaction conditions such as temperature, PH, this process easily makes particle agglomeration, increases particle size, reduces the stability of made magnetic liquid, simultaneously because manual operation is too much, make this technology of preparing repeatability poor.
Existing nanometer Fe
3o
4in particle technology of preparing, synthesized particle mostly is " side " shape, is unfavorable for the tribological property promoting magnetic liquid.
Existing nanometer Fe
3o
4in particle technology of preparing, at the molecules surfactant of coated high viscosity, low saturation vapour pressure magnetic liquid, often need under high temperature, condition of high voltage, but improve temperature and pressure, particle growth, reunion can be made, reduce the stability of magnetic liquid, therefore the molecules surfactant of current coated high viscosity, low saturation vapour pressure magnetic liquid adopts ball milled usually.
The present invention is intended to overcome existing Fe
3o
4poor repeatability in surface coating technology, and be unfavorable for lubrication, cannot the shortcoming such as coated molecules surfactant.The present invention is at protection Fe
3o
4while tissue, structure are constant, without the separation of intermediate, without the need to regulating the step such as temperature, PH in reaction process, directly obtain the coated nanometer Fe of tensio-active agent
3o
4, simultaneously can by nanometer Fe
3o
4average grain size controls within the scope of 8 ~ 20nm, makes particle shape trend towards " ball " shape, and saturation magnetization is greater than 50emu/g simultaneously, and chemical absorption of surface amount can reach 40 ~ 60%.
Technical scheme of the present invention:
The present invention adopts at Fe
3o
4surface coating compact surfaces promoting agent, is passing through traditional chemical Co deposited synthesis Fe
3o
4tensio-active agent is added before particle, particle growth, reunion is suppressed by adding tensio-active agent in advance, there is not the prerequisite of reuniting at particle under, utilize and improve temperature of reaction and time removal resultant, excessive ammonia the like waste, controlled in the reasonable scope by system pH value, technical scheme is as follows simultaneously:
1) Fe is prepared
3+, Fe
2+, tensio-active agent mixed solution, by iron concentration 1.5 ~ 3mol/L condition preparation Fe
3+and Fe
2+mixed solution, wherein Fe
3+and Fe
2+mol ratio be 2:1 ~ 5:3, tensio-active agent and Fe
2+mol ratio be 1:5 ~ 3:5;
2) the coated nanometer Fe of tensio-active agent is generated
3o
4particle, under the condition of rotating speed 300-500r/min, the mixing solutions that continuous whipping step 1 obtains, thermostat(t)ed water (oil) bath slaking, curing temperature 80 ~ 180 DEG C, slaking pressure 0.1-1.1MPa, curing time 10 ~ 30min, afterwards with concentration be the ammonia soln of 25% as precipitation agent, join fast in mixed solution, reaction times 30-120min;
3) the coated nanometer Fe of gained tensio-active agent is cleaned
3o
4particle, Magneto separate Fe
3o
4particle and solution, by washes of absolute alcohol 2 times, washed with de-ionized water 2-3 time, dry, pulverize.
Tensio-active agent, except conventional surfactants, as oleic acid, can be the molecules surfactant for high viscosity, low saturation vapour pressure magnetic liquid simultaneously, as Lignoceric acid, and perfluorocarboxylic acid.
Gained nanometer Fe
3o
4particle still can keep particle size in the reasonable scope while temperature rising, pressurization, does not reduce the stability of made magnetic liquid.
Gained nanometer Fe
3o
4particle is " ball " shape, improves the lubricity of prepared magnetic liquid, and its average particle size range is at 8 ~ 20nm simultaneously, and makes saturation magnetization be greater than 50emu/g.
Utilize thermogravimetric analyzer chart surface-active agent at Fe
3o
4the stable chemical adsorptive capacity formed on the surface can reach 40 ~ 60%, and its antioxidant property, high-temperature stability are stronger.
Without the need to too much manual operation, method is simple, and repeatability is high, without the separation of intermediate, without the need to regulating the step such as temperature, PH in process, directly obtains the coated nanometer Fe of tensio-active agent
3o
4particle.
Accompanying drawing explanation
Fig. 1. be coated front and back Fe
3o
4and Fe
3o
4the XRD figure of/oleic material;
Fig. 2 is coated front and back Fe
3o
4and Fe
3o
4the TEM figure of/oleic material;
Fig. 3 is coated front and back Fe
3o
4and Fe
3o
4the TGA figure of/oleic material;
Embodiment
Embodiment one
1) by the FeCl of 0.08mol
36H
2o, 0.04molFeCl
23H
2o and 0.016mol oleic acid is dissolved in the deionized water of 50mL, forms solution A;
2) under the condition of rotating speed 300r/min, solution A water bath with thermostatic control slaking is constantly uniformly mixed, curing temperature 95 DEG C, curing time 15min, afterwards with concentration be the ammonia soln 50ml of 25% as precipitation agent, join fast in mixed solution, reaction times 45min;
3) nanometer Fe of gained Coated with Oleic Acid is cleaned
3o
4particle, Magneto separate Fe
3o
4particle and solution, by washes of absolute alcohol 2 times, washed with de-ionized water 2-3 time, dry, pulverize.
Embodiment two
1) by the FeCl of 0.08mol
36H
2o, 0.04molFeCl
23H
2o and 0.016mol Ammonium benzoate is dissolved in the deionized water of 50mL, forms solution A;
2) under the condition of rotating speed 300r/min, be constantly uniformly mixed solution A water bath with thermostatic control slaking, curing temperature 95 DEG C, curing time 15min, afterwards with concentration be the ammonia soln 50ml of 25% as precipitation agent, join fast in mixed solution, reaction times 1h;
3) nanometer Fe of gained Coated with Oleic Acid is cleaned
3o
4particle, Magneto separate Fe
3o
4particle and solution, by washes of absolute alcohol 2 times, washed with de-ionized water 2-3 time, dry, pulverize.
Claims (5)
1. a synthesizing magnetic liquid nanometer Fe
3o
4the novel process of particle, is characterized in that method steps is as follows:
1) Fe is prepared
3+, Fe
2+, tensio-active agent mixed solution, by iron concentration 1.5 ~ 3mol/L condition preparation Fe
3+and Fe
2+mixed solution, wherein Fe
3+and Fe
2+mol ratio be 2:1 ~ 5:3, tensio-active agent and Fe
2+mol ratio be 1:5 ~ 3:5;
2) the coated nanometer Fe of tensio-active agent is generated
3o
4particle, under the condition of rotating speed 300-500r/min, the mixing solutions that continuous whipping step 1 obtains, thermostat(t)ed water (oil) bath slaking, curing temperature 80 ~ 180 DEG C, slaking pressure 0.1-1.1MPa, curing time 10 ~ 30min, afterwards with concentration be the ammonia soln of 25% as precipitation agent, join fast in mixed solution, reaction times 30-120min;
3) the coated nanometer Fe of gained tensio-active agent is cleaned
3o
4particle, Magneto separate Fe
3o
4particle and solution, by washes of absolute alcohol 2 times, washed with de-ionized water 2-3 time, dry, pulverize.
2. a kind of synthesizing magnetic liquid nanometer Fe according to claim 1
3o
4the novel process of particle, is characterized in that: in described step (1), tensio-active agent is except conventional surfactants, as oleic acid, can be the molecules surfactant for high viscosity, low saturation vapour pressure magnetic liquid simultaneously, as Lignoceric acid, perfluorocarboxylic acid.
3. a kind of synthesizing magnetic liquid nanometer Fe according to claim 1
3o
4the novel process of particle, is characterized in that: gained nanometer Fe
3o
4particle still can keep particle mean size within the scope of 8 ~ 20nm while temperature rising, pressurization, does not reduce the stability of made magnetic liquid.
4. a kind of synthesizing magnetic liquid nanometer Fe according to claim 1
3o
4the novel process of particle, is characterized in that: gained nanometer Fe
3o
4particle is " ball " shape, improves the lubricity of prepared magnetic liquid, and its average particle size range is at 8 ~ 20nm simultaneously, and makes saturation magnetization be greater than 50emu/g.
5. a kind of synthesizing magnetic liquid nanometer Fe according to claim 1
3o
4the novel process of particle, is characterized in that: method is simple, and repeatability is high, without the separation of intermediate, without the need to regulating the step such as temperature, PH in process, directly obtains the coated nanometer Fe of tensio-active agent
3o
4particle, utilizes thermogravimetric analyzer to measure Fe
3o
4the stable chemisorption amount of particle surface can reach 40 ~ 60%, its antioxidant property and high-temperature stability stronger.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510564933.8A CN105174317A (en) | 2015-09-08 | 2015-09-08 | Novel technology for synthesizing nanometer Fe3O4 particles for magnetic liquid |
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|---|---|---|---|
| CN201510564933.8A CN105174317A (en) | 2015-09-08 | 2015-09-08 | Novel technology for synthesizing nanometer Fe3O4 particles for magnetic liquid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106409464A (en) * | 2016-05-23 | 2017-02-15 | 南昌航空大学 | Preparation method of magnetic liquid for damping shock absorbing effect |
| CN110317573A (en) * | 2018-03-29 | 2019-10-11 | 福吉米株式会社 | Composition for polishing and its manufacturing method and magnetic grinding method |
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2015
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| CN101029355A (en) * | 2007-04-13 | 2007-09-05 | 北京科技大学 | Method for producing nano-magnetic FeO particle by iron extracted and utilized in tin tails |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106409464A (en) * | 2016-05-23 | 2017-02-15 | 南昌航空大学 | Preparation method of magnetic liquid for damping shock absorbing effect |
| CN110317573A (en) * | 2018-03-29 | 2019-10-11 | 福吉米株式会社 | Composition for polishing and its manufacturing method and magnetic grinding method |
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Application publication date: 20151223 |