CN102320565A - Single preparation technology who disperses the complex component nano material with universality - Google Patents
Single preparation technology who disperses the complex component nano material with universality Download PDFInfo
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- CN102320565A CN102320565A CN201110265370A CN201110265370A CN102320565A CN 102320565 A CN102320565 A CN 102320565A CN 201110265370 A CN201110265370 A CN 201110265370A CN 201110265370 A CN201110265370 A CN 201110265370A CN 102320565 A CN102320565 A CN 102320565A
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Abstract
The invention discloses a kind of single preparation technology who disperses the complex component nano material with universality, adopting weight is oleic acid and the oleyl amine surfactant of initial powder weight 5%-10%, the n-hexane solvent of 200% volume ratio; Ball milling is 4 hours on the high energy ball mill; Open ball grinder and shift milled product to centrifuge tube, add n-hexane solvent dilution and ultrasonic dispersion 5-10 minute, with the acceleration centrifugation of 1000g; Obtain nano-particle product; The present invention is with low cost, can prepare the nano particle of various different complicated ingredients, has good universality.
Description
Technical field
The present invention relates to a kind of preparation technology of nano material, particularly a kind of single preparation technology who disperses the complex component nano material with universality.
Background technology
Nano material is meant the material of particle size less than 100nm; Particle size is dwindled and skin effect, defective effect etc. cause material production novel physical character and new application; Be the research focus of present field of new, the extensive use of various nano materials then possibly bring revolutionary impact to many fields.
In general, the preparation of nano material can be divided into two kinds of approach: (1) bottom-up (from small to large), and this approach is normally to concrete material; Adopt the method for various chemical syntheses, from solution, generate the nano material of required size, this approach nano particle is to grow out of nothing or from small to large; Chemical synthesis has its many advantages, but process transplanting property is poor, for material different; Even but same material heterogeneity and doping content all need be groped synthesis technique again; Cause material synthetic work amount very huge, further, for the material of complicated component such as the various doping functional oxides of extensive use etc.; Composition and structural integrity are poor between the nano particle that causes easily being synthesized, even are difficult to synthesize.(2) top-down (from big to small); This approach is from bulk material, through methods such as ball millings bulk material is crushed to nano-scale, and this method has universality preferably; Can adapt to material different; Therefore also obtained using more widely, but the fatal shortcoming of this method is that multiple sized particles mixes, because this method can not be all levigate to nano-scale with all particles; What therefore obtain usually is from the mixture of nano-scale up to micron-scale or submicron-scale, can not obtain the mono-dispersed nano particle.
Summary of the invention
In order to overcome above-mentioned defective, the invention provides a kind of single preparation technology who disperses the complex component nano material with universality.
The present invention for the technical scheme that solves its technical problem and adopt is: a kind of single preparation technology who disperses the complex component nano material with universality mainly may further comprise the steps:
A. adopt solid phase reaction to synthesize or buy the initial powder (micron-scale or bigger) of nano material to be prepared;
B. in initial powder, add oleic acid and the oleyl amine surfactant account for initial powder weight 5%-10%, quality such as oleic acid surfactant and oleyl amine surfactant add the n-hexane solvent of initial powder 200% volume ratio again, pack into then and gather the tetrafluoro ball grinder.
C. in ball grinder, add ball-milling medium, seal ball grinder then, ball milling is 4 hours on the high energy ball mill;
D. open ball grinder and shift milled product to centrifuge tube, add n-hexane solvent dilution and ultrasonic dispersion 5-10 minute, with the acceleration centrifugation of 1000g, obtain nano-particle product then.
As further improvement of the present invention, oleic acid surfactant purity >=90%, said oleyl amine surfactant purity >=90%.
As further improvement of the present invention, ball-milling medium is a zirconia ball.
The invention has the beneficial effects as follows:
1. compare with chemical synthesis; This method technology is simple, and is with low cost, changes parent material and can prepare corresponding nano material; Process transplanting property is good; Because solid phase reaction synthesis oxide parent material is simple more than direct chemical solution nano materials, thereby for the very preparation of the oxide-based nanomaterial of complicated ingredient, this method especially possesses outstanding advantage.
2. compare with traditional Prepared by Ball Milling nano material technology; This method can obtain the mono-dispersed nano material; Ball-milling method can only obtain the mix powder that distributes from the non-constant width of tens nanometers to 1 micron usually; This method adopts surfactant and nano particle effect, and surfactant can be suspended in nano particle in the solvent, thereby separates with bigger micron particles.
3. owing to further adopted centrifugal classification technology, can obtain the nano material that Size Distribution is concentrated very much, the Size Distribution concentration degree is less than 50%, and size reaches below the 10nm, and this is that traditional ball grinding method is inaccessiable fully.
The specific embodiment
In order to deepen to understanding of the present invention, will combine embodiment that the present invention is made further detailed description below, this embodiment only is used to explain the present invention, does not constitute the qualification to protection domain of the present invention.
The specific embodiment: a kind of single preparation technology who disperses the complex component nano material with universality mainly may further comprise the steps:
A. adopt solid phase reaction to synthesize or buy the initial powder (micron-scale or bigger) of nano material to be prepared;
B. in initial powder, add oleic acid and the oleyl amine surfactant that accounts for initial powder weight 8%; Quality such as oleic acid surfactant and oleyl amine surfactant; Oleic acid surfactant purity is 92%; Oleyl amine surfactant purity is 92%, adds the n-hexane solvent of initial powder 200% volume ratio again, packs into then and gathers the tetrafluoro ball grinder.
C. in ball grinder, add ball-milling medium, ball-milling medium is a zirconia ball, seals ball grinder then, and ball milling is 4 hours on the high energy ball mill;
D. open ball grinder and shift milled product to centrifuge tube, add n-hexane solvent dilution and ultrasonic dispersion 8 minutes, with the acceleration centrifugation of 1000g (g is an acceleration of gravity), obtain nano-particle product then.
The present invention is directed to that the Size Distribution that nano material top-down (from big to small) approach exists is big, nano particle can not with key issues such as micron particles separates; Adopt the method pulverized particles of high energy ball mill ball milling, in the process of ball milling, add surfactant, Action of Surfactant is in nano grain surface; Make nano particle be suspended in the solution and separate with micron particles; Adopt centrifugation method that the size of nano material is carried out classification simultaneously, distribute, obtain the multiple size nano material that Size Distribution is concentrated thereby greatly dwindle nanoparticle size; The preparation technology of nano material is simple; With low cost, can prepare the nano particle of various different complicated ingredients, have good universality.
Claims (3)
1. the list with universality disperses the preparation technology of complex component nano material, it is characterized in that: mainly may further comprise the steps:
A. adopt solid phase reaction to synthesize or buy the initial powder (micron-scale or bigger) of nano material to be prepared;
B. in initial powder, add oleic acid and the oleyl amine surfactant account for initial powder weight 5%-10%, quality such as oleic acid surfactant and oleyl amine surfactant add the n-hexane solvent of initial powder 200% volume ratio again, pack into then and gather the tetrafluoro ball grinder;
C. in ball grinder, add ball-milling medium, seal ball grinder then, ball milling is 4 hours on the high energy ball mill;
D. open ball grinder and shift milled product to centrifuge tube, add n-hexane solvent dilution and ultrasonic dispersion 5-10 minute, with the acceleration centrifugation of 1000g, obtain nano-particle product then.
2. the single preparation technology who disperses the complex component nano material with universality according to claim 1 is characterized in that: described oleic acid surfactant purity >=90%, said oleyl amine surfactant purity >=90%.
3. the single preparation technology who disperses the complex component nano material with universality according to claim 1, it is characterized in that: described ball-milling medium is a zirconia ball.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109093124A (en) * | 2017-06-21 | 2018-12-28 | 北京大学 | A kind of method that high-energy ball milling reduction method prepares metal nano material |
CN110407166A (en) * | 2019-07-09 | 2019-11-05 | 江苏科技大学 | Can low temperature inhale hydrogen Mg nano particle, preparation method and application |
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US20030121364A1 (en) * | 2002-01-02 | 2003-07-03 | International Business Machines Corporation | Metal salt reduction to form alloy nanoparticles |
CN1439451A (en) * | 2002-11-18 | 2003-09-03 | 长沙矿冶研究院 | Nano-diamond deagglomeration and grading method |
CN1956922A (en) * | 2004-05-19 | 2007-05-02 | 夏普株式会社 | Method for producing halosilane and method for purifying solid component |
CN101618891A (en) * | 2009-07-02 | 2010-01-06 | 浙江大学 | Preparation method of self-assembled superlattice materials of titanium dioxide nano rod |
CN101804968A (en) * | 2010-03-19 | 2010-08-18 | 清华大学 | Direct synthesis method of nanometer oxide powder |
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2011
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US20030121364A1 (en) * | 2002-01-02 | 2003-07-03 | International Business Machines Corporation | Metal salt reduction to form alloy nanoparticles |
CN1439451A (en) * | 2002-11-18 | 2003-09-03 | 长沙矿冶研究院 | Nano-diamond deagglomeration and grading method |
CN1956922A (en) * | 2004-05-19 | 2007-05-02 | 夏普株式会社 | Method for producing halosilane and method for purifying solid component |
CN101618891A (en) * | 2009-07-02 | 2010-01-06 | 浙江大学 | Preparation method of self-assembled superlattice materials of titanium dioxide nano rod |
CN101804968A (en) * | 2010-03-19 | 2010-08-18 | 清华大学 | Direct synthesis method of nanometer oxide powder |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109093124A (en) * | 2017-06-21 | 2018-12-28 | 北京大学 | A kind of method that high-energy ball milling reduction method prepares metal nano material |
CN109093124B (en) * | 2017-06-21 | 2020-11-27 | 北京大学 | Method for preparing metal nano material by high-energy ball milling reduction method |
CN110407166A (en) * | 2019-07-09 | 2019-11-05 | 江苏科技大学 | Can low temperature inhale hydrogen Mg nano particle, preparation method and application |
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