CN1557715A - Method for preparing nanometer powder by spray pyrolysis - Google Patents
Method for preparing nanometer powder by spray pyrolysis Download PDFInfo
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- CN1557715A CN1557715A CNA2004100139398A CN200410013939A CN1557715A CN 1557715 A CN1557715 A CN 1557715A CN A2004100139398 A CNA2004100139398 A CN A2004100139398A CN 200410013939 A CN200410013939 A CN 200410013939A CN 1557715 A CN1557715 A CN 1557715A
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Abstract
The present invention is spraying and thermal cracking process of preparing high performance nano powder, and belongs to the field of inorganic material preparing technology. The preparation process includes covering the substrate of glass, ceramic and other heat resisting material with adsorptive medium carbon black; heating to 200-500 deg.c; introducing soluble easy-to-decompose metal solution via spraying to decompose the solution thermally with the product being adsorbed on the medium; collecting the adsorbing medium with adsorbed matter; and calcining the adsorbing medium with adsorbed matter to eliminate the adsorbing medium and to obtain loose nano powder with purity higher than 99 %. The present invention has high product purity, integral crystal lattice, homogeneously distributed granularity, simple production process, and low cost.
Description
Technical field
The present invention relates to a kind of method that adopts spray pyrolysis to prepare the high-performance nano powder, belong to field of inorganic material preparing technology.
Background technology
Nano material is owing to exist fundamental characteristics such as small-size effect, surface interface effect, quantum size effect and quantum tunneling effect, make nano material that incomparable special performance of traditional material and great potential using value be arranged, caused the very big concern of scientific circles and business circles.Wherein the preparation of nano-powder is the basis of nano materials research, and the performance of powder such as purity, composition profiles, size, particle scale distribution, aggregating state etc. have great influence to the performance of nano material.The preparation method of at present relevant nano-powder has multiple, mainly is divided into vapor phase process, liquid phase method, solid phase method three classes.Vapor phase process gained powder purity is higher, it is less to reunite, but apparatus expensive, output are lower, are difficult for popularizing.The solid phase method equipment used is simple, easy to operate, but the gained powder is often pure inadequately, and size-grade distribution is bigger, is only applicable to require lower occasion.Liquid phase method have equipment simple, need not harsh physical condition such as high vacuum, easy advantage such as amplification, be considered to the most rising, but liquid phase method general technology flow process is longer, easily produce hard aggregation in the powder last handling process, be not easy to obtain the powder of small particle size, and the change of processing condition is bigger to the powder characteristic influence.Though the spray pyrolysis in the liquid phase method has shortened technical process greatly, and powder does not need aftertreatment, operating process is simple, but owing to metal salt solution residence time in high-temperature atmosphere in the spray pyrolysis is extremely short, often decomposition reaction is incomplete, and crystallization degree is not high, therefore, produce by existing spray pyrolysis law technology, be difficult to obtain the nano particle of good dispersity.Publication number is in the Chinese patent " ammonia complex liquid spray pyrolysis prepares the method and apparatus of basic carbonate nano " of CN 1380255A, disclose a kind of spray pyrolysis and produced the method for nanoparticle, its processing step and react and separates and taking-up for the charging of getting the raw materials ready, atomizing, in this technology, nanoparticle just can be finished with needing to adopt special-purpose cyclonic separator separating of gas, higher to equipment requirements, and the capture of product is relatively more difficult.Therefore, what press for solution in the nano powder preparation at present is to improve the cost performance problem, promptly how to adopt cheapness, the simple preparation method of technology to obtain high performance nano-powder, and this also is the key of nano material industrialization, practicability, universalness.
Summary of the invention
The present invention is the improvement that spray pyrolysis is prepared nano material, the advantage that has kept spray pyrolysis, overcome its weak point, purpose is to provide a kind of product purity height, lattice perfection, even particle size distribution, and production technique spray pyrolysis simple, with low cost prepares the method for nano-powder.
Its technical scheme is: be substrate with the heat-stable material, be covered with adsorption medium nano carbon black post-heating to 200～500 ℃ on its surface; The easy decomposing metal salts solution of solubility is imported with spray method, resultant is attached on the adsorption medium during solution generation pyrolysis, collection contains the adsorption medium of dirt settling, be fired to adsorption medium and remove fully, loose shape, purity greater than 99% nano-powder.
In the technique scheme, the easy decomposing metal salt of described solubility adopts nitrate, nitrite, vitriol, sulphite usually at the soluble metallic salt that can be decomposed into metal oxide or metal below 500 ℃, and wherein the nitrate effect is best; Described heat-stable material is glass, stainless steel, ceramic-like materials.
Compared with prior art, outstanding advantage of the present invention is:
1. adopt adsorption medium heat of adsorption degradation production, avoided the reunion and the bonding of product, prevented growing up of crystal grain in the postorder calcination process simultaneously, therefore, the gained diameter of particle is little, is evenly distributed, and do not have and reunite, and product is suitable for collection.
2. do not have the intervention of other chemical substance in the reaction except that adsorption medium, adsorption medium can eliminate in calcining, and product need not mill, thereby has guaranteed the purity of product; Simultaneously, be reflected in several seconds to tens seconds and finish, and the calcination process in road, back helps pyrolysated and fully carry out, thereby further improved the crystallization degree and the purity of powder.
3. the technology simple and fast need not particular requirement to equipment, therefore, greatly reduces production cost, makes nano material industrialization, practicability, universalness become possibility, has broad application prospects.
Description of drawings
Fig. 1 is the laser particle size analysis figure of the prepared γ phase nano aluminium oxide powder of the embodiment of the invention 1;
Fig. 2 is the transmission electron microscope picture of the prepared γ phase nano aluminium oxide powder of the embodiment of the invention 1;
Fig. 3 is the X diffraction analysis figure as a result of the prepared γ phase nano aluminium oxide powder of the embodiment of the invention 1;
Fig. 4 is the X diffraction analysis figure as a result of the prepared nano oxidized iron powder of the embodiment of the invention 2;
Fig. 5 is the X diffraction analysis figure as a result of the prepared nano aluminum nitride powder of the embodiment of the invention 3;
Embodiment
Below by embodiment also in conjunction with the accompanying drawings, technical scheme of the present invention is further elaborated.
Embodiment 1:
With glass is that base material is made container, is covered with nano carbon black on container inner wall, is heated to 400 ℃; Preparation concentration is the aluminum nitrate ethanolic soln of 2.5mol/L, imports in the container with spray method, treats finish carbon black on the collector wall of back of solvent evaporates, 700 ℃ of temperature lower calcinations 1 hour, promptly gets the white powder aluminum oxide.
Referring to accompanying drawing 1, by the laser particle size analyzer analytical results as can be known, by the alumina powder that embodiment 1 described preparation method makes, median size is 13.62nm, size distribution ± 0.6nm.
Referring to accompanying drawing 2, by the alumina powder that embodiment 1 described preparation method makes, shown in the transmission electron microscope image, dispersion of particles and homogeneity are very good.
Referring to accompanying drawing 3, by the alumina powder that embodiment 1 described preparation method makes, X diffraction analysis result and γ phase alumina facies analysis normal data (JCPDF) are in full accord.
Embodiment 2
With the pottery is that base material is made container, is covered with nano carbon black on container inner wall, is heated to 450 ℃; The ferric sulfate alcohol solution (volume ratio is 5: 1) that with concentration is 2.5mol/L imports in the container with spray method, and all the other steps are with embodiment 1, and making median size is the red powder shape ferric oxide of 27.5nm.The X diffraction analysis is referring to accompanying drawing 4.
Embodiment 3
With the stainless steel is that base material is made container, is covered with nano carbon black on container inner wall, is heated to 350 ℃; The aluminum nitrate alcohol solution (volume ratio is 5: 1) that with concentration is 2.5mol/L imports in the said vesse with spray method, treat the solvent evaporates adsorption medium of back on the collector wall that finish, in nitrogen atmosphere, under 1600 ℃ of high temperature, handled 3 hours, calcined 1 hour down at 600 ℃ in air then, promptly getting particle diameter is the pale powder shape aluminium nitride of 42.5nm.The X diffraction analysis is referring to accompanying drawing 5.
Embodiment 4
With glass is that base material is made container, is covered with nano carbon black on container inner wall, is heated to 450 ℃; The silver nitrite chloroformic solution that with concentration is 2.0mol/L imports in the container with spray method, and all the other steps are with embodiment 1, and obtaining particle diameter is the pale powder shape nanometer metallic silver of 18.2nm.
Claims (4)
1. a spray pyrolysis prepares the method for nano-powder, it is characterized in that: be substrate with the heat-stable material, be covered with adsorption medium nano carbon black post-heating to 200～500 ℃ on its surface; The easy decomposing metal salts solution of solubility is imported with spray method, resultant is attached on the adsorption medium during solution generation pyrolysis, collection contains the adsorption medium of dirt settling, be fired to adsorption medium and remove fully, loose shape, purity greater than 99% nano-powder.
2. a kind of spray pyrolysis according to claim 1 prepares the method for nano-powder, it is characterized in that: the easy decomposing metal salt of described solubility is nitrate, nitrite, vitriol, sulphite.
3. a kind of spray pyrolysis according to claim 1 prepares the method for nano-powder, it is characterized in that: described heat-stable material is glass, stainless steel, ceramic-like materials.
4. a kind of spray pyrolysis according to claim 1 and 2 prepares the method for nano-powder, it is characterized in that: the easy decomposing metal salt of described solubility is that the nitrate effect is best.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410013939 CN1235805C (en) | 2004-01-15 | 2004-01-15 | Method for preparing nanometer powder by spray pyrolysis |
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| CN 200410013939 CN1235805C (en) | 2004-01-15 | 2004-01-15 | Method for preparing nanometer powder by spray pyrolysis |
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| CN1557715A true CN1557715A (en) | 2004-12-29 |
| CN1235805C CN1235805C (en) | 2006-01-11 |
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| CN 200410013939 Expired - Fee Related CN1235805C (en) | 2004-01-15 | 2004-01-15 | Method for preparing nanometer powder by spray pyrolysis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105081352A (en) * | 2014-05-07 | 2015-11-25 | 中国科学院宁波材料技术与工程研究所 | Method for growing nanometer particles on substrate |
| CN105347376A (en) * | 2015-10-13 | 2016-02-24 | 刘冠华 | Preparation method for high-purity ultrafine alumina |
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2004
- 2004-01-15 CN CN 200410013939 patent/CN1235805C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105081352A (en) * | 2014-05-07 | 2015-11-25 | 中国科学院宁波材料技术与工程研究所 | Method for growing nanometer particles on substrate |
| CN105347376A (en) * | 2015-10-13 | 2016-02-24 | 刘冠华 | Preparation method for high-purity ultrafine alumina |
| CN105347376B (en) * | 2015-10-13 | 2018-04-13 | 刘冠华 | A kind of preparation method of high-purity superfine aluminium oxide |
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| CN1235805C (en) | 2006-01-11 |
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