CN100460092C - Method for improving quality of nanometer particle material - Google Patents

Method for improving quality of nanometer particle material Download PDF

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Publication number
CN100460092C
CN100460092C CNB2004100371582A CN200410037158A CN100460092C CN 100460092 C CN100460092 C CN 100460092C CN B2004100371582 A CNB2004100371582 A CN B2004100371582A CN 200410037158 A CN200410037158 A CN 200410037158A CN 100460092 C CN100460092 C CN 100460092C
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Prior art keywords
nanoparticle material
acid
nano
aluminium flake
secondary water
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Expired - Fee Related
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CNB2004100371582A
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Chinese (zh)
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CN1689713A (en
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程发良
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Dongguan University of Technology
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Dongguan University of Technology
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Abstract

The method of raising the quality of nanometer particle material is to screen nanometer particle material with nanometer template. The method can raise the homogeneity of nanometer particle material greatly, and has low cost. The nanometer particle material can meet the requirement of industrial application.

Description

A kind of method that improves the nanoparticle material quality
Technical field
The present invention relates to improve the method for nanoparticle material quality.
Technical background
Nanometer technology is a new and high technology of rising after the eighties in 20th century, it is based on the emerging subject crossing system of multidisciplinary formations such as physics, chemistry, material, manufacturing, information, biology, environment, the energy, nanometer technology will guide technological revolution next time, replace micron to become new industrial standard.No matter it is at present domestic with the precipitation method, hydro-thermal method, spray-on process, sol-gel process, explosion method, organic resin method etc., synthetic nanoparticle all has big or small uneven characteristics, this also is the gap of homemade nanoparticle material and import nanoparticle material, this shortcoming has limited homemade nanoparticle material greatly and has used in industry, has reduced homemade nanoparticle material quality.A lot of nanoparticle material just have using value in certain size range, begin conduction when for example Jue Yuan silica is in 20nm; A kind of to disperse to sneak into particle diameter in polymer such as polyester be the bonding cream of nanometer that the Nano silver grain of tens nanometer forms, and sneaking into particle diameter with original dispersion is that the common bonding cream of micron-sized silver particles is compared, and specific insulation has been reduced to about 1/2~1/3; Process for modern precision; as the nanoparticle in the grinding agent; have only the size of working as even; get rid of larger particles or the requirements at the higher level of particle greater than 15nm; just can reach processing request; and present homemade Nano diamond accounts for more than 10% greater than the particle of 18nm, and purity can only reach 97%.Though the import nanoparticle material can satisfy industrial application requirements substantially, price is very high.
Summary of the invention
The nanoparticle material that the object of the present invention is to provide a kind of low cost, obtains can satisfy the method for the raising nanoparticle material quality of commercial Application.
The present invention improves the method for nanoparticle material quality, for utilizing nano-form screening nanoparticle material.
Wherein nano-form is a nano-alumina template, and the size of the nanoparticle material that obtains as required prepares respectively that 200nm or 200nm are following, 60nm or 60nm is following and the nano material of 20nm or the following Three Estate of 20nm.
Nano-alumina template can prepare by the following method:
99.999% aluminium flake after 5%NaOH and acetone cleaning, was polished 5~10 minutes down at 0~5 ℃ with 70% perchloric acid and absolute ethyl alcohol mixed liquor (volume ratio 1:4), and voltage is 15~22V; Aluminium flake cleans the back with secondary water, and (sulfuric acid 18~22V, oxalic acid 30~50V, phosphatase 11 00~130V) oxidation first 1~2 hour are done electrode with corrosion resistant plate with each self-corresponding voltage at polyacid (0.5~1.5mol/L sulfuric acid, 0.1~0.5mol/L oxalic acid, 0.3~1.0mol/L phosphoric acid); Under 60 ℃, mix washing lotion again and clean aluminium flake half an hour, remove oxide-film with the chromic acid of 6% phosphoric acid and 1.8%; Aluminium flake carried out anodic oxidation 6 hours with same voltage after cleaning with secondary water; Peel off aluminum matrix with the chloride saturated aqueous solution, the phosphoric acid through hole with 5% 30 minutes, obtaining the aperture successively is 20nm, 60nm, 200nm nano-alumina template, cleans at last and is kept in the secondary water.
Earlier nanoparticle material is added in the dispersion before the screening, and with activating agent nanoparticle material is carried out modification and handle.With sonic oscillation nanoparticle material is scatter then, utilize negative pressure that nanoparticle material is sieved again, isolate each grade products that needs.Wherein dispersion is water or organic facies.
The present invention utilizes the method for nano-form screening nanoparticle material, can improve the uniformity of nanoparticle material greatly, improve many that the cost of nanoparticle material quality will be low with respect to the technology of improving the production nano material, the nanoparticle material of gained is compared with the import nanoparticle material, have the low advantage of price, and can satisfy industrial application requirements.
Description of drawings
Fig. 1 is for implementing technological process device schematic diagram of the present invention.
The specific embodiment
Embodiment 1
1, the preparation of nano-alumina template
99.999% aluminium flake after 5%NaOH and acetone cleaning, was polished 8 minutes down at 2 ℃ with 70% perchloric acid and absolute ethyl alcohol mixed liquor (volume ratio 1:4), and voltage is 20V; , do electrode with corrosion resistant plate with each self-corresponding voltage (sulfuric acid 20V, oxalic acid 40V, phosphatase 11 20V) oxidation first 1.5 hours at polyacid (1.0mol/L sulfuric acid, 0.8mol/L oxalic acid, 0.5mol/L phosphoric acid) aluminium flake usefulness secondary water cleaning back; Under 60 ℃, mix washing lotion again and clean aluminium flake half an hour, remove oxide-film with the chromic acid of 6% phosphoric acid and 1.8%; Aluminium flake carried out anodic oxidation 6 hours with same voltage after cleaning with secondary water; Peel off aluminum matrix with the stannous chloride saturated aqueous solution, the phosphoric acid through hole with 5% 30 minutes, obtaining the aperture successively is 20nm, 60nm, 200nm nano-alumina template, cleans at last and is kept in the secondary water.
2, the modification in Nano diamond and aluminium oxide duct and the dispersion in the aqueous solution
Add weight ratio at water and be 1% anion surfactant RDC-25S and non-ionic (polymeric surfactant) RGN-10, Nano diamond is carried out surface modification, add 0.5 weight % Nano diamond powder again, with (150 watts of water-bath type ultrasound sources, 35 kilo hertzs), handled gained aqueous medium dispersion 20 minutes.
3, add negative pressure 500Pa at Fig. 1 device, slow suction filtration, the product that obtains needs is handled in classification.Nano-form is a nano-alumina template.

Claims (2)

1. method that improves the nanoparticle material quality, it is characterized in that utilizing nano-alumina template screening nanoparticle material, earlier nanoparticle material is added in the dispersion before comprising the steps: to screen, and with activating agent nanoparticle material is carried out modification and handle, with sonic oscillation nanoparticle material is scatter then, utilize negative pressure that nanoparticle material is sieved again, isolate each grade products that needs;
The preparation method of described nano-alumina template comprises the steps:
(1) with aluminium flake after 5%NaOH and acetone clean, 0~5 ℃ of polishing 5~10 minutes down, voltage is 15~22V with 70% perchloric acid of volume ratio 1:4 and absolute ethyl alcohol mixed liquor;
(2), do electrode with corrosion resistant plate with each self-corresponding voltage oxidation first 1~2 hour at polyacid aluminium flake usefulness secondary water cleaning back;
Described polyacid is 0.5~1.5mol/L sulfuric acid, 0.1~0.5mol/L oxalic acid, 0.3~1.0mol/L phosphoric acid, and its corresponding voltage is sulfuric acid 18~22V, oxalic acid 30~50V, phosphatase 11 00~130V;
(3) under 60 ℃, mix washing lotion again and clean aluminium flake half an hour, remove oxide-film with the chromic acid of 6% phosphoric acid and 1.8%;
(4) after aluminium flake cleans with secondary water, carried out anodic oxidation 6 hours with same voltage;
(5) peel off aluminum matrix with the chloride saturated aqueous solution, the phosphoric acid through hole with 5% 30 minutes, obtaining the aperture successively is 20nm, 60nm, 200nm nano-alumina template, cleans at last and is kept in the secondary water.
2. improve the method for nanoparticle material quality according to claim 1, it is characterized in that dispersion is water or organic facies.
CNB2004100371582A 2004-04-28 2004-06-04 Method for improving quality of nanometer particle material Expired - Fee Related CN100460092C (en)

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CNB2004100371582A CN100460092C (en) 2004-04-28 2004-06-04 Method for improving quality of nanometer particle material

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CN200410027026.1 2004-04-28
CN200410027026 2004-04-28
CNB2004100371582A CN100460092C (en) 2004-04-28 2004-06-04 Method for improving quality of nanometer particle material

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CN100460092C true CN100460092C (en) 2009-02-11

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5729595A (en) * 1980-07-28 1982-02-17 Mitsubishi Alum Co Ltd Formation of colored film of aluminum
JPS5956594A (en) * 1982-09-24 1984-04-02 Nippon Light Metal Co Ltd Method for coloring aluminum
US5486283A (en) * 1993-08-02 1996-01-23 Rohr, Inc. Method for anodizing aluminum and product produced
CN1278024A (en) * 2000-07-04 2000-12-27 南京大学 Method for preparing template with macro nanometer sequential holes
CN1125891C (en) * 1996-08-26 2003-10-29 日本电信电话株式会社 Method of manufacturing porous anodized alumina film

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5729595A (en) * 1980-07-28 1982-02-17 Mitsubishi Alum Co Ltd Formation of colored film of aluminum
JPS5956594A (en) * 1982-09-24 1984-04-02 Nippon Light Metal Co Ltd Method for coloring aluminum
US5486283A (en) * 1993-08-02 1996-01-23 Rohr, Inc. Method for anodizing aluminum and product produced
CN1125891C (en) * 1996-08-26 2003-10-29 日本电信电话株式会社 Method of manufacturing porous anodized alumina film
CN1278024A (en) * 2000-07-04 2000-12-27 南京大学 Method for preparing template with macro nanometer sequential holes

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