CN104708009A - Method for preparing nanometer aluminum oxide inlaid in metal nanoparticles based on homogeneous phase coprecipitation method - Google Patents
Method for preparing nanometer aluminum oxide inlaid in metal nanoparticles based on homogeneous phase coprecipitation method Download PDFInfo
- Publication number
- CN104708009A CN104708009A CN201410468671.0A CN201410468671A CN104708009A CN 104708009 A CN104708009 A CN 104708009A CN 201410468671 A CN201410468671 A CN 201410468671A CN 104708009 A CN104708009 A CN 104708009A
- Authority
- CN
- China
- Prior art keywords
- distilled water
- temperature
- resistance furnace
- constant temperature
- reducing atmosphere
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
A method for preparing nanometer aluminum oxide inlaid in metal nanoparticles based on a homogeneous phase coprecipitation method comprises the following steps: 1, dissolving metal salt and aluminum sulfate or aluminum nitrate in distilled water in proportion, adding surfactant and carbamide into the distilled water, conducting ultrasonic stirring till complete dissolution is achieved, transferring a solution into a polytetrafluoroethylene lining reaction still, placing the reaction still in a drying oven, keeping the constant temperature of 125 DEG C for 12-16 hours, raising the temperature to 170 DEG C, keeping the constant temperature of 170 DEG C for from eight to ten hours, conducting suction filtration after cooling down, and after washing sediment with absolute ethyl alcohol and the distilled water, conducting air drying in the drying oven at a temperature ranging from 60 DEG C to 80 DEG C; 2, after pouring products obtained in step 1 into a crucible, placing the crucible into a resistance furnace, conducting air atmosphere annealing at the temperature of 600 DEG C for three hours, after cooling down, transferring the products into a porcelain ark, placing the porcelain ark into a tube type resistance furnace, annealing in reducing atmosphere at a temperature ranging from 600 DEG C to 800 DEG C for three hours, and conducting furnace cooling in the reducing atmosphere to reach a room temperature. By means of the method, the preparation process is quite simple, the equipment requirement is not high, the method is applicable to multiple varieties of metal, the products are mixed uniformly, the shapes and appearances are good, and the dimensions, shapes, appearances and phase structures of the products can be controlled by changing the dosing quantity of ingredients and the temperature of subsequent hot treatment.
Description
Technical field
The invention belongs to field of material technology, particularly the preparation method of nano composite structural material.
Technical background
Aluminium oxide has many significant physical characteristics, as high-melting-point, good hydrophobicity, high elastic modulus, high optical transparency, high index of refraction, good heat endurance and chemical stability, low surface acidity, excellent optical property and insulating properties etc.Aluminium oxide has the different crystal forms of more than 15 kinds, and multiple crystal transfer can occur for it, is widely used in space technology, catalysis load, laser and energy technology field.But along with countries in the world deepening continuously to nano materials research, the nano material that composition is single can not be satisfied with the requirement of present development in science and technology.
Summary of the invention
The object of this invention is to provide a kind of functional, preparation method that pattern is excellent metal nanoparticle inlays amorphous or γ nano aluminium oxide.
The present invention is achieved by the following technical solutions.
The concrete preparation process of the present invention is as follows.
(1) raw material and aluminum sulfate or aluminum nitrate are dissolved in a certain amount of distilled water by certain mol ratio, add surfactant and the urea such as appropriate softex kw (CTAB) or neopelex (SDBS) again, after liquid ultrasonic agitation to be mixed is extremely dissolved completely, solution is proceeded in band teflon-lined reactor, be placed in baking oven, 125 DEG C, constant temperature 12-16 h, cooling after suction filtration, gained sediment absolute ethyl alcohol and distilled water washing after in 60-80 DEG C of baking oven air oxygen detrition 10 more than h.
(2) pouring dried product in step (1) into crucible is placed in chamber type electric resistance furnace, 600 DEG C of air atmospheres are annealed 3 h, after stove is cold, product is moved into porcelain Noah's ark and be placed in tube type resistance furnace, at reducing atmosphere in 600 DEG C-800 DEG C annealing 3 h, keep reducing atmosphere stove to be chilled to room temperature subsequently, obtain the material that metal nanoparticle inlays amorphous or γ nano aluminium oxide.
Raw material described in step of the present invention (1) is ferrous sulfate (FeSO
4), silver nitrate (AgNO
3), gold chloride (HAuCl
4), chloroplatinic acid (H
14cl
6o
6pt), palladium bichloride (PdCl
2) or nickel nitrate (Ni (NO
3)
2).
In raw material described in step of the present invention (1), metal ion and aluminum ions mol ratio are 1:200-5:1, and wherein aluminum ions molar concentration is 0.2mol/L-5mol/L.
Softex kw (CTAB) described in step of the present invention (1) or neopelex (SDBS) addition are 0.05mol/L-0.3mol/L.
Urea addition described in step of the present invention (1) is 1mol/L-3mol/L.
The preferred hydrogen of reducing atmosphere described in step of the present invention (2), nitrogen and hydrogen mixture (5%H
2-95%N
2), argon hydrogen gaseous mixture (5%H
2-95%Ar).
What the present invention adopted is homogeneous co-precipitation process, and being annealed under air atmosphere and reducing atmosphere successively by gained sediment after reaction prepares the material that final metal nanoparticle inlays amorphous or γ nano aluminium oxide.Preparation process is very simple, and is applicable to the metal of multiple types, and products therefrom mixes, pattern is excellent.And the size of product, pattern and phase structure can be controlled by the dosage of feed change and subsequent heat treatment temperature.The method is less demanding to experimental facilities, is extremely conducive to the operation in reality.
Accompanying drawing explanation
Fig. 1 is that iron granule of the present invention inlays amorphous nano alumina material at ferrous sulfate: the environmental scanning electronic microscope figure of products therefrom when the mol ratio of aluminum sulfate is 0.25:1.
Fig. 2 is that iron granule of the present invention inlays amorphous nano alumina material at ferrous sulfate: the environmental scanning electronic microscope figure of products therefrom when the mol ratio of aluminum sulfate is 0.5:1.
Fig. 3 is that iron granule of the present invention inlays amorphous nano alumina material at ferrous sulfate: the transmission electron microscope picture of products therefrom when the mol ratio of aluminum sulfate is 0.5:1.Vignette is wherein the full resolution pricture inlaying region.
Fig. 4 is that iron granule of the present invention inlays amorphous nano alumina material at ferrous sulfate: when the mol ratio of aluminum sulfate is 0.5:1, products therefrom can spectrogram.
Fig. 5 is that metallic silver particles of the present invention inlays the XRD test analysis figure of amorphous nano alumina material in the reducing annealing stage after 600 DEG C of annealing.
Fig. 6 is that metallic silver particles of the present invention inlays the XRD test analysis figure of γ nano alumina material in the reducing annealing stage after 800 DEG C of annealing.
Detailed description of the invention
The present invention will be described further by following examples.
It is pure that the chemical reagent purity that this experiment adopts is analysis.This method adopts CTAB or SDBS as surfactant, urea is as precipitating reagent, raw material and aluminum sulfate (or aluminum nitrate) are obtained initial product by homogeneous co-precipitation process, then acquisition metallic particles of being annealed under air atmosphere and reducing atmosphere successively by initial product inlays the material of amorphous or γ nano aluminium oxide.The surface topography of material can be controlled by the dosage of feed change and subsequent heat treatment temperature.
Embodiment 1.
Preparation process is as follows.
(1) ferrous sulfate of 0.00125 mol and 0.005 mol aluminum sulfate are dissolved in 30ml distilled water, add 1g CTAB and 3.5g urea again, after liquid ultrasonic agitation to be mixed is extremely dissolved completely, mixed liquor is proceeded in band teflon-lined reactor, be placed in 125 DEG C of baking oven constant temperature 15 h, be warming up to 170 DEG C of constant temperature 9 h again, cooling after suction filtration, gained sediment absolute ethyl alcohol and distilled water washing after in 60 DEG C of baking ovens air oxygen detrition 10 h.
(2) pouring dried product in step (1) into crucible is placed in chamber type electric resistance furnace, 600 DEG C of air anneal 3 h, after stove is cold, product being moved into porcelain Noah's ark is placed in tube type resistance furnace, 600 DEG C of hydrogen atmospheres are annealed 3 h, finally obtainedly inlay the material of amorphous nano aluminium oxide as metallic iron nano particle in figure (1).
Embodiment 2.
Preparation process is as follows.
(1) ferrous sulfate of 0.0025 mol and 0.005 mol aluminum sulfate are dissolved in 30ml distilled water, add 1g CTAB and 3.5g urea again, after liquid ultrasonic agitation to be mixed is extremely dissolved completely, mixed liquor is proceeded in band teflon-lined reactor, be placed in 125 DEG C of baking oven constant temperature 15 h, be warming up to 170 DEG C of constant temperature 9 h again, cooling after suction filtration, gained sediment absolute ethyl alcohol and distilled water washing after in 60 DEG C of baking ovens air oxygen detrition 10 h.
(2) pouring dried product in step (1) into crucible is placed in chamber type electric resistance furnace, 600 DEG C of air anneal 3 h, the cold product obtained of stove moves into porcelain Noah's ark and is placed in tube type resistance furnace, 600 DEG C of hydrogen atmospheres are annealed 3 h, finally obtainedly inlay the material of amorphous nano aluminium oxide as metallic iron nano particle in figure (2) (3) (4).
Embodiment 3.
Preparation process is as follows.
(1) silver nitrate of 0.005 mol and 0.01 mol aluminum nitrate are dissolved in 30ml distilled water, add 1g SDBS and 3.5g urea again, after liquid ultrasonic agitation to be mixed is extremely dissolved completely, mixed liquor is proceeded in band teflon-lined reactor, be placed in 125 DEG C of baking oven constant temperature 15 h, be warming up to 170 DEG C of constant temperature 9 h again, cooling after suction filtration, gained sediment absolute ethyl alcohol and distilled water washing after in 60 DEG C of baking ovens air oxygen detrition 10 h.
(2) pouring dried product in step (1) into crucible is placed in chamber type electric resistance furnace, 600 DEG C of air anneal 3 h, the cold product obtained of stove moves into porcelain Noah's ark and is placed in tube type resistance furnace, 600 DEG C of hydrogen atmospheres are annealed 3 h, finally obtainedly inlay the material of amorphous nano aluminium oxide as argent nano particle in figure (5).
Embodiment 4.
Preparation process is as follows.
(1) silver nitrate of 0.005 mol and 0.01 mol aluminum nitrate are dissolved in 30ml distilled water, add 1g SDBS and 3.5g urea again, after liquid ultrasonic agitation to be mixed is extremely dissolved completely, mixed liquor is proceeded in band teflon-lined reactor, be placed in 125 DEG C of baking oven constant temperature 15 h, be warming up to 170 DEG C of constant temperature 9 h again, cooling after suction filtration, gained sediment absolute ethyl alcohol and distilled water washing after in 60 DEG C of baking ovens air oxygen detrition 10 h.
(2) pouring dried product in step (1) into crucible is placed in chamber type electric resistance furnace, 600 DEG C of air anneal 3 h, the cold product obtained of stove moves into porcelain Noah's ark and is placed in tube type resistance furnace, 800 DEG C of hydrogen atmospheres are annealed 3 h, finally obtainedly inlay the material of γ nano aluminium oxide as argent nano particle in figure (6).
Embodiment 5.
Preparation process is as follows.
(1) gold chloride of 0.0005 mol and 0.005 mol aluminum sulfate are dissolved in 30ml distilled water, add 1g CTAB and 3.5g urea again, after liquid ultrasonic agitation to be mixed is extremely dissolved completely, mixed liquor is proceeded in band teflon-lined reactor, be placed in 125 DEG C of baking oven constant temperature 15 h, be warming up to 170 DEG C of constant temperature 9 h again, cooling after suction filtration, gained sediment absolute ethyl alcohol and distilled water washing after in 60 DEG C of baking ovens air oxygen detrition 10 h.
(2) pouring dried product in step (1) into crucible is placed in chamber type electric resistance furnace, 600 DEG C of air anneal 3 h, the cold product obtained of stove moves into porcelain Noah's ark and is placed in tube type resistance furnace, 600 DEG C of hydrogen atmospheres are annealed 3 h, and final obtained metallic gold nano particle inlays the material of amorphous nano aluminium oxide.
Embodiment 6.
Preparation process is as follows.
(1) chloroplatinic acid of 0.001 mol and 0.005 mol aluminum sulfate are dissolved in 30ml distilled water, add 1g CTAB and 3.5g urea again, after liquid ultrasonic agitation to be mixed is extremely dissolved completely, mixed liquor is proceeded in band teflon-lined reactor, be placed in 125 DEG C of baking oven constant temperature 15 h, be warming up to 170 DEG C of constant temperature 9 h again, cooling after suction filtration, gained sediment absolute ethyl alcohol and distilled water washing after in 60 DEG C of baking ovens air oxygen detrition 10 h.
(2) pouring dried product in step (1) into crucible is placed in chamber type electric resistance furnace, 600 DEG C of air anneal 3 h, the cold product obtained of stove moves into porcelain Noah's ark and is placed in tube type resistance furnace, 600 DEG C of hydrogen atmospheres are annealed 3 h, and final obtained metal platinum nano particle inlays the material of amorphous nano aluminium oxide.
Embodiment 7.
Preparation process is as follows.
(1) nickel nitrate of 0.0002 mol and 0.005 mol aluminum sulfate are dissolved in 30ml distilled water, add 1g CTAB and 3.5g urea again, after liquid ultrasonic agitation to be mixed is extremely dissolved completely, mixed liquor is proceeded in band teflon-lined reactor, be placed in 125 DEG C of baking oven constant temperature 15 h, be warming up to 170 DEG C of constant temperature 9 h again, cooling after suction filtration, gained sediment absolute ethyl alcohol and distilled water washing after in 60 DEG C of baking ovens air oxygen detrition 10 h.
(2) pouring dried product in step (1) into crucible is placed in chamber type electric resistance furnace, 600 DEG C of air anneal 3 h, the cold product obtained of stove moves into porcelain Noah's ark and is placed in tube type resistance furnace, 600 DEG C of hydrogen atmospheres are annealed 3 h, and final obtained metallic nickel nano granule inlays the material of amorphous nano aluminium oxide.
Claims (1)
1. prepare a method for metal nanoparticle embedding nano aluminium oxide based on homogeneous co-precipitation process, it is characterized in that preparation process is as follows:
(1) raw material and aluminum sulfate or aluminum nitrate are dissolved in a certain amount of distilled water by certain mol ratio, add appropriate softex kw or neopelex and urea again, after liquid ultrasonic agitation to be mixed is extremely dissolved completely, solution is proceeded in band teflon-lined reactor, be placed in baking oven, 125 DEG C, constant temperature 12-16 h, be warming up to 170 DEG C of constant temperature 8-10 h again, cooling after suction filtration, gained sediment absolute ethyl alcohol and distilled water washing after in 60-80 DEG C of baking oven air oxygen detrition 10 more than h;
(2) pouring dried product in step (1) into crucible is placed in chamber type electric resistance furnace, 600 DEG C of air atmospheres are annealed 3 h, after stove is cold, product is moved into porcelain Noah's ark and be placed in tube type resistance furnace, at reducing atmosphere in 600 DEG C-800 DEG C annealing 3 h, keep reducing atmosphere stove to be chilled to room temperature subsequently, obtain the material that metal nanoparticle inlays amorphous or γ nano aluminium oxide;
Raw material described in step (1) is ferrous sulfate, silver nitrate, gold chloride, chloroplatinic acid, palladium bichloride or nickel nitrate;
In raw material described in step (1), metal ion and aluminum ions mol ratio are 1:200-5:1, and wherein aluminum ions molar concentration is 0.2mol/L-5mol/L;
Softex kw described in step (1) or neopelex addition are 0.05mol/L-0.3mol/L;
Urea addition described in step (1) is 1mol/L-3mol/L;
The preferred hydrogen of weakly reducing atmosphere described in step (2), nitrogen and hydrogen mixture, argon hydrogen gaseous mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410468671.0A CN104708009A (en) | 2014-09-15 | 2014-09-15 | Method for preparing nanometer aluminum oxide inlaid in metal nanoparticles based on homogeneous phase coprecipitation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410468671.0A CN104708009A (en) | 2014-09-15 | 2014-09-15 | Method for preparing nanometer aluminum oxide inlaid in metal nanoparticles based on homogeneous phase coprecipitation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104708009A true CN104708009A (en) | 2015-06-17 |
Family
ID=53408018
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410468671.0A Pending CN104708009A (en) | 2014-09-15 | 2014-09-15 | Method for preparing nanometer aluminum oxide inlaid in metal nanoparticles based on homogeneous phase coprecipitation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104708009A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108479767A (en) * | 2018-03-30 | 2018-09-04 | 河北伟量环保科技有限公司 | A kind of Large ratio surface purifying formaldehyde catalyst and preparation method thereof prepared by one kettle way |
| CN109465464A (en) * | 2018-12-17 | 2019-03-15 | 湘潭大学 | A method of preparing alumina-based ceramic metal nano composite powder |
| CN115010492A (en) * | 2022-04-20 | 2022-09-06 | 清华大学 | Low-infrared-transmittance precious metal nanoparticle composite ceramic and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004290881A (en) * | 2003-03-27 | 2004-10-21 | Japan Science & Technology Agency | Ultrafine particle of compound catalyst comprising quasicrystal aluminum alloy particle as carrier, and production thereof |
| CN101240387A (en) * | 2007-11-23 | 2008-08-13 | 中南大学 | Cu-Al2O3 nano strengthened dispersion alloy and preparation method thereof |
| CN101314182A (en) * | 2008-06-16 | 2008-12-03 | 南昌大学 | Method for preparing hollow metal nano-particle with gamma-aluminum oxide nano-particle as mould plate |
| CN103922384A (en) * | 2014-04-14 | 2014-07-16 | 陕西科技大学 | Method for preparing cubic phase Sm2O3 nano crystal with combination of uniform precipitation-thermal treatment |
| CN103978229A (en) * | 2013-12-06 | 2014-08-13 | 南昌大学 | Preparation method of aluminum oxide loaded nanoscale zero-valent iron nanorod |
-
2014
- 2014-09-15 CN CN201410468671.0A patent/CN104708009A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004290881A (en) * | 2003-03-27 | 2004-10-21 | Japan Science & Technology Agency | Ultrafine particle of compound catalyst comprising quasicrystal aluminum alloy particle as carrier, and production thereof |
| CN101240387A (en) * | 2007-11-23 | 2008-08-13 | 中南大学 | Cu-Al2O3 nano strengthened dispersion alloy and preparation method thereof |
| CN101314182A (en) * | 2008-06-16 | 2008-12-03 | 南昌大学 | Method for preparing hollow metal nano-particle with gamma-aluminum oxide nano-particle as mould plate |
| CN103978229A (en) * | 2013-12-06 | 2014-08-13 | 南昌大学 | Preparation method of aluminum oxide loaded nanoscale zero-valent iron nanorod |
| CN103922384A (en) * | 2014-04-14 | 2014-07-16 | 陕西科技大学 | Method for preparing cubic phase Sm2O3 nano crystal with combination of uniform precipitation-thermal treatment |
Non-Patent Citations (1)
| Title |
|---|
| 陈春雨等: "低温等离子体与 MnOx/γ-Al2O3 协同催化降解正己醛", 《催化学报》, vol. 33, no. 6, 30 June 2012 (2012-06-30) * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108479767A (en) * | 2018-03-30 | 2018-09-04 | 河北伟量环保科技有限公司 | A kind of Large ratio surface purifying formaldehyde catalyst and preparation method thereof prepared by one kettle way |
| CN108479767B (en) * | 2018-03-30 | 2021-06-29 | 河北伟量环保科技有限公司 | Large-specific-surface formaldehyde purification catalyst prepared by one-pot method and preparation method thereof |
| CN109465464A (en) * | 2018-12-17 | 2019-03-15 | 湘潭大学 | A method of preparing alumina-based ceramic metal nano composite powder |
| CN109465464B (en) * | 2018-12-17 | 2022-02-01 | 湘潭大学 | Method for preparing alumina-based metal ceramic nano composite powder |
| CN115010492A (en) * | 2022-04-20 | 2022-09-06 | 清华大学 | Low-infrared-transmittance precious metal nanoparticle composite ceramic and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101716685B (en) | Method for preparing spherical superfine silver powder by using chemical reduction method | |
| CN103193262B (en) | The preparation method of a kind of indium gallium zinc oxide powder and ceramic target thereof | |
| CN104289722B (en) | A kind of preparation method of nanometer silver | |
| Lin et al. | The effects of citric acid on the synthesis and performance of silver–tin oxide electrical contact materials | |
| CN102775141B (en) | Method for finely synthesizing ternary ZnO-Nb2O5-TiO2 microwave dielectric ceramics by wet chemical process | |
| CN103754953B (en) | Preparation method of multi-morphologynano-sized zinc ferrite | |
| CN102632246A (en) | Method for preparing series silver nano-sheets in batch | |
| CN106811832B (en) | A kind of pearl-decorated curtain shape BiFeO3The preparation method and products obtained therefrom of micro nanometer fiber | |
| CN108723379B (en) | Preparation method of multi-principal-element alloy nano powder | |
| CN109175394A (en) | A kind of even silver wire controllable method for preparing of minor diameter and superelevation draw ratio | |
| CN104498914B (en) | A kind of method that sol-gel technique prepares siller tin oxide electric contact material | |
| CN1443811A (en) | Synthesizing nano crystal cobalt aluminium spinelle pigment by using solution combustion method | |
| CN104708009A (en) | Method for preparing nanometer aluminum oxide inlaid in metal nanoparticles based on homogeneous phase coprecipitation method | |
| CN104505287A (en) | Preparation method of rod-shaped tin oxide-reinforced silver-based electric contact material | |
| CN103708834A (en) | New method for finely preparing ixiolite structure MgTiNb2O8 microwave dielectric ceramic by using chemical process | |
| CN109692971A (en) | A kind of nano-silver powder and its preparation and the application in low-temperature cured conductive silver paste | |
| CN1285511C (en) | Method for synthesizing Y2O3 nano material directly from combustion method of citric acid | |
| CN106521551B (en) | A kind of preparation method of the NiAu nanocatalyst for ammonia borane hydrogen manufacturing | |
| CN103708838A (en) | New method for preparing monoclinic structure ZnZrNb2O8 microwave dielectric ceramic through low temperature sintering | |
| Xue et al. | Hollow rods of nanocrystalline NiGa2O4: hydrothermal synthesis, formation mechanism, and application in photocatalysis | |
| CN104889416B (en) | A kind of preparation method of silver tin ash intermediate composite granule | |
| CN101837466B (en) | Method for preparing nano aluminum oxide dispersion iron powder | |
| CN103708537A (en) | Method for finely synthesizing ilmenite structure ZnTiO3 nanometer powder by using water-soluble sol-gel process | |
| CN102787250A (en) | Preparation method for diphasic nanometer particle dispersion strengthening copper matrix composite material | |
| CN105036181B (en) | Preparation method for mixed particle morphology ITO powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150617 |
|
| WD01 | Invention patent application deemed withdrawn after publication |