CN107855539A - A kind of method for preparing superfine metal and metal oxide - Google Patents
A kind of method for preparing superfine metal and metal oxide Download PDFInfo
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- CN107855539A CN107855539A CN201711134449.7A CN201711134449A CN107855539A CN 107855539 A CN107855539 A CN 107855539A CN 201711134449 A CN201711134449 A CN 201711134449A CN 107855539 A CN107855539 A CN 107855539A
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- metal
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- metal oxide
- urea
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/02—Oxides
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Abstract
The invention discloses a kind of method for preparing superfine metal and metal oxide, step A. mixes urea, metal salt and water, stirs 5 20min so that hybrid solid melts completely, forms uniform precursor solution；Wherein the mass ratio of urea and metal salt is 100:1~1:1000；The ratio of urea and water is 1:10~10000；Step A is made precursor solution and forms aerosol droplets through atomization by step B.；Step C. is by heat drying after aerosol droplets microwave irradiation made from step B, you can obtains spherical powder particle.The present invention can be used for preparing numerous superfine nano metal materials, monodispersity is high, by adjusting synthesis condition, composition, crystalline phase of nano metal etc. can be controlled and synthetic route is simple and cost is cheap, therefore possess huge application prospect in all many-sides such as Industrial Catalysis, water process and electrochemistry.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, more particularly to a kind of superfine metal and metal oxide of preparing
Method.
Background technology
Nano material refers to be made up of superfine crystal grain, characteristic dimension size nanometer scale (~100nm) solid material
Material.Nano material possesses the performance not available for many conventional materials, including optical property, electromagnetic property, thermodynamic property,
Quantum mechanics performance etc., due to these performances, nano material is widely used in the fields such as lubrication, photoelectricity, magnetic recording, catalysis.So
And because its high surface energy, the easily spontaneous reunion of nano particle greatly limit the nano effect of nano material, reduce it
Application field and effect.Therefore nano material generally requires carrier, and porous carbon material has flourishing pore structure, very big ratio
Surface area, more surface compound and very strong adsorption capacity, also possess the system of high temperature resistant, acid and alkali-resistance, conduction and heat transfer etc. one
The advantages of row, therefore be the good carrier of load nano particle.But porous carbon materials are often low with mechanical strength, hydro-thermal is steady
The shortcomings of qualitative poor, and silica, aluminum oxide are ideal high intensity catalyst carriers, therefore prepare superfine metal and gold
Category oxide can hinder the reunion of loaded particle, there is provided the transfer passage of reaction solution, promote the expansion of generation material again
Dissipating, big specific surface area contributes to contact of the catalyst with reactant, and high mechanical strength extends the operation strategies of catalyst,
Therefore load-type nanometer metal or oxide material are all many-sided all with wide in Industrial Catalysis, water process and electrochemistry etc.
Application prospect.
Microwave heating method is to utilize high frequency microwave energy, substantial amounts of heat is produced within a very short time, so as to promote all kinds of chemistry
The progress of reaction, it is more effective energy utilization and mode of heating.Microwave heating synthesis can significantly accelerate the fortune of reaction molecular
Dynamic and impact velocity, is advantageous to a large amount of formation of nucleus, can limit the increase of crystal particle diameter, can synthesize than conventional method institute
The particle diameter for preparing crystal is smaller, nano material evenly.At present, microwave-assisted synthesis is widely used to the system of nano material
It is standby.Peiro etc. prepares TiO in two steps2Film：The first step, immerse the substrate in the TiO through microwave radiation2In colloidal solution, find
There is TiO on substrate2Crystal deposition；Second step, the substrate of above-mentioned processing is immersed and contains Ti4+The aqueous solution in, and use microwave radiation.
Experiment discovery, TiO made of second step2Film growth speed is faster than the first step, and crystal structure is complete, and particle size distribution is 50
[Peiro Ana M, ElenaVigil, et a1.Titanium (IV) oxide thin films between~100nm
Obtained by a two-step-solution method.Thin Solid Films, 2002,411:185].Wang etc.
Using copper acetate and sodium hydroxide as raw material, in alcohol solvent, by microwave radiation, the CuO that average grain diameter is 4nm is successfully synthesized
Particle.Granule-morphology is spherical in shape, purity height [Wang Hui, Xu Jinzhong, the et a1.Preparation of of product
CuO nanopar-ticles by microwave irradiation.Cryst Growth,2002,244:88]。
Sum it up, traditional superfine metal and the synthetic method of metal oxide often there is nano-particles size not
It is easy to control, bad dispersibility, the problems such as template agent cost is high, and post-processing is seriously polluted.In addition, prior synthesizing method is due to preparing
The limitation of method can not be widely used in the preparation of various nano metals or oxide.Therefore, develop a kind of simple pervasive
The preparation method of nano metal or metal oxide composite, by the multiple blasting technique of nano particle, and it can synthesize
During control parameter, the extensive use for such material such as size, component, crystalline phase and loading of nano-particle to produce
Raw great impetus.
The content of the invention
Based on above the deficiencies in the prior art, technical problem solved by the invention is to provide a kind of simple pervasive surpass
The preparation method of thin nano-metal-oxide or nano metal material, this method can be widely suitable for nano metal or nanogold
Belong to the synthesis of oxide.
The present invention forms homogeneous phase solution using the ammonium salts such as urea and metal salt in water so that metal salt is evenly distributed on mixed
Close in liquid.Afterwards, after using high-temperature heating or microwave radiation heating explosion, heated stove is heated at high temperature secondary blasting, obtains
The controllable ultra-fine metal oxide nano particles of size.
In order to solve the above-mentioned technical problem, the present invention provides a kind of method for preparing superfine metal and metal oxide,
Step A. mixes urea, metal salt and water, stirs 5-20min so that hybrid solid melts completely, is formed uniform
Precursor solution；Wherein the mass ratio of urea and metal salt is 100:1~1:1000；The ratio of urea and water is 1:10~
10000；
Step A is made precursor solution and forms aerosol droplets through atomization by step B.；
Step C. is by heat drying after aerosol droplets microwave irradiation made from step B, you can obtains spherical powder particle.
It is provided by the invention to prepare superfine metal and the method for metal oxide enters one as the preferred of above-mentioned technical proposal
Step includes the part or all of of following technical characteristic：
As the improvement of above-mentioned technical proposal, urea could alternatively be ammonium carbonate, ammonium hydrogen carbonate, nitric acid in the step A
Ammonium or ammonium chloride.
As the improvement of above-mentioned technical proposal, metal salt described in the step A is metal nitrate, halide, secondary
One or more kinds of metal salt mixtures in chlorate, acetate, oxalates, phosphate or sulfate；The metal
The metal of salt be selected from Mg, Al, Pb, In, Sn, Sb, Zr, Nb, La, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu,
Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La or Os.
As the improvement of above-mentioned technical proposal, aerosol droplets are 0.001-200 μm in the step B.
As the improvement of above-mentioned technical proposal, the step C is that aerosol droplets made from step B are imported into microwave
By being dried in tube furnace after device progress microwave irradiation, you can obtain spherical powder particle.
As the improvement of above-mentioned technical proposal, microwave generator microwave irradiation power is 0.1W- in the step C
5000KW.The microwave action time is 0.1-600s；The tubular type furnace temperature is 100-1600 DEG C, residence time 0.2-600s,
Carrier gas is air, nitrogen, carbon dioxide, oxygen, hydrogen, argon gas or its mixed gas.
As the improvement of above-mentioned technical proposal, what the step C was obtained is single element oxide or combined oxidation
Thing, wherein single element oxide for following elements oxide in one kind, and composite oxides then include two kinds or two kinds with
The oxide of upper different elements：Mg、Al、Pb、In、Sn、Sb、Zr、Nb、La、Ce、Ta、Mo、W、Re、Ti、V、Cr、Mn、Fe、Co、
Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La or Os.
As the improvement of above-mentioned technical proposal, the nano metal that the step C is obtained can be a kind of list of metallic element
The alloy or intermetallic compound of matter either two kinds and above different metal element, wherein metallic element include Mg, Al, Pb,
In、Sn、Sb、Zr、Nb、La、Ce、Ta、Mo、W、Re、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ag、Pt、Pd、Ir、Ru、Rh、
Y, Ba, Sr, La or Os.
As the improvement of above-mentioned technical proposal, the particle diameter of the superfine metal and metal oxide is 2-2000nm.
Compared with prior art, technical scheme has the advantages that：The present invention utilizes urea and metal
Salt forms homogeneous liquid in water so that metal salt is evenly distributed in mixing liquid.Afterwards, using the method for fabricated in situ,
Superfine nano metallic particles is obtained finally by high-temperature heat treatment.The present invention can be used for preparing numerous superfine nano metal materials
Material, its size is 2~2000nm and monodispersity is high, by adjusting synthesis condition, can control composition, the crystalline phase of nano metal
Deng.In addition, the present invention also has the advantages such as synthetic route is simple and cost is cheap, therefore in Industrial Catalysis, water process and electrification
Etc. all many-sides possess huge application prospect.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, and in order to allow the above and other objects, features and advantages of the present invention can
Become apparent, below in conjunction with preferred embodiment, describe in detail as follows.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, the accompanying drawing of embodiment will be simply situated between below
Continue.
Fig. 1 is the XRD of nano metal Cu made from embodiment 1；
The SEM that Fig. 2 is nano metal Cu made from embodiment 1 schemes；
Fig. 3 is the XRD of nano metal Cu made from embodiment 2；
The SEM that Fig. 4 is nano metal Cu made from embodiment 2 schemes.
Embodiment
The following detailed description of the present invention embodiment, its as part of this specification, by embodiment come
Illustrate the principle of the present invention, other aspects of the present invention, feature and its advantage will become apparent by the detailed description.
Embodiment 1：Prepare nanometer Cu
Synthesis material：Urea, water, Cu (NO3)23H2O (copper nitrate)
(1) 1g urea, 98g water and 1g Cu (NO are weighed3)2·3H2O in a 250mL beaker, stirring 10min until
Medicine dissolves in beaker.
(2) solution described in (1) is passed through into N2Under the conditions of aerosol generator produce aerosol particle.
(3) aerosol particle dries explosion at 800 DEG C into high temperature process furnances.Collect and produce by individual layer panel filter
Product.
Fig. 1 is nano metal Cu XRD, is analyzed from XRD spectrum, the characteristic peak containing CuO and Cu, wherein cupric oxide
PDF cards correspond to 89-5899 characteristic peak, are 1-1241 characteristic peak corresponding to copper, cupric oxide occur in the characteristic peak of copper
The reason for be because Nanometer Copper be easily oxidized to cupric oxide in atmosphere.It can not avoid connecing with air in storage and test process
Touch, cause copper nanoparticle to be oxidized.Scheme in the SEM that Fig. 2 is nano metal Cu.It can be found that copper powder particle size is from figure
The particle of 20-50 nanometers, even particle size.
Embodiment 2：Prepare nanometer Cu
Synthesis material：Urea, water, Cu (NO3)2·3H2O (copper nitrate)
(1) 5g urea, 94g water and 1g Cu (NO are weighed3)2·3H2O in a 250mL beaker, stirring 10min until
Medicine dissolves in beaker.
(2) solution described in (1) is passed through into 5%H2/N2Under the conditions of aerosol generator produce aerosol particle.
(3) aerosol particle is after microwave heats, and at 800 DEG C, explosion is dried into high temperature process furnances.By individual layer
Panel filter collects product.
Fig. 3 is nano metal Cu XRD, is compared by the PDF cards with copper, the phase of characteristic peak and card 65-9026
Symbol, the SEM that Fig. 4 is nano metal Cu scheme, and as seen in Figure 4, under the double action of ammonium salt and microwave, size controlling exists
In the range of 20-50nm, and particle diameter surface is smooth.Compare from Fig. 2 and Fig. 4 as can be seen that passing through ammonium salt secondary blasting, uniform particle sizes
It is adjustable, it is more smooth by microwave action, nano grain surface.
Each raw material cited by the present invention, and bound, the section value of each raw material of the present invention, and technological parameter
Bound, the section value of (such as temperature, time) can realize the present invention, embodiment numerous to list herein.
Described above is the preferred embodiment of the present invention, can not limit the right model of the present invention with this certainly
Enclose, it is noted that for those skilled in the art, under the premise without departing from the principles of the invention, may be used also
To make some improvement and variation, these are improved and variation is also considered as protection scope of the present invention.
Claims (9)
- A kind of 1. method for preparing superfine metal and metal oxide, it is characterised in that comprise the following steps：Step A. mixes urea, metal salt and water, stirs 5-20min so that hybrid solid melts completely, before being formed uniformly Body solution；Wherein the mass ratio of urea and metal salt is 100:1~1:1000；The ratio of urea and water is 1:10~10000；Step A is made precursor solution and forms aerosol droplets through atomization by step B.；Step C. is by heat drying after aerosol droplets microwave irradiation made from step B, you can obtains spherical powder particle.
- 2. the method as claimed in claim 1 for preparing superfine metal and metal oxide, it is characterised in that：In the step A Urea could alternatively be ammonium carbonate, ammonium hydrogen carbonate, ammonium nitrate or ammonium chloride.
- 3. the method for preparing superfine metal and metal oxide as described in claim 1-2, it is characterised in that：The step A Described in metal salt be metal nitrate, halide, hypochlorite, acetate, oxalates, phosphate or sulfate in one Kind or more than one metal salt mixture；The metal of the metal salt be selected from Mg, Al, Pb, In, Sn, Sb, Zr, Nb, La, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La or Os.
- 4. the method for preparing superfine metal and metal oxide as described in claim 1-2, it is characterised in that：The step B Middle aerosol droplets are 0.001-200 μm.
- 5. the method for preparing superfine metal and metal oxide as described in claim 1-2, it is characterised in that：The step C For aerosol droplets made from step B are imported after microwave generator progress microwave irradiation by being dried in tube furnace, you can To spherical powder particle.
- 6. the method as claimed in claim 5 for preparing superfine metal and metal oxide, it is characterised in that：In the step C Microwave generator microwave irradiation power is 0.1W-5000KW；The microwave action time is 0.1-600s；The tubular type furnace temperature is 100-1600 DEG C, residence time 0.2-600s, carrier gas is air, nitrogen, carbon dioxide, oxygen, hydrogen, argon gas or it is mixed Close gas.
- 7. the method for preparing superfine metal and metal oxide as described in claim 1-2, it is characterised in that：The step C What is obtained is single element oxide or composite oxides, and wherein single element oxide is one in the oxide of following elements Kind, and composite oxides then include the oxide of two or more different element：Mg、Al、Pb、In、Sn、Sb、Zr、Nb、 La, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La or Os.
- 8. the method for preparing superfine metal and metal oxide as described in claim 1-2, it is characterised in that：The step C Obtained nano metal can be the alloy or gold of a kind of either two kinds of simple substance of metallic element and above different metal element Compound between category, wherein metallic element include Mg, Al, Pb, In, Sn, Sb, Zr, Nb, La, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La or Os.
- 9. the method for preparing superfine metal and metal oxide as described in claim 1-8, it is characterised in that：The ultra-fine gold The particle diameter of category and metal oxide is 2-2000nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108975360A (en) * | 2018-07-20 | 2018-12-11 | 大连理工大学 | A kind of preparation method, device and the application of spherical shape magnesia |
| CN110514700A (en) * | 2019-09-27 | 2019-11-29 | 西安电子科技大学 | A kind of copper oxide and cobaltosic oxide heterogeneous structural nano line composite sensitive material, ethylene glycol sensor and preparation method |
| CN111842924A (en) * | 2020-07-16 | 2020-10-30 | 西安交通大学 | Microwave-assisted metal nanoparticle preparation method and system |
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| CN1152487A (en) * | 1995-08-25 | 1997-06-25 | 纳幕尔杜邦公司 | Method for preparation of golden powder by decomposing aerosol |
| CN103949192A (en) * | 2014-01-16 | 2014-07-30 | 常州大学 | Method for preparing hollow spheres through microwave-assisted aerosol |
| CN104690295A (en) * | 2013-12-05 | 2015-06-10 | 南通建陵纳米科技有限公司 | Method for preparing monodispersed ultrafine particles |
| CN106334801A (en) * | 2016-09-09 | 2017-01-18 | 常州大学 | Method for preparing porous carbon loaded nano-metal through microwave assistance |
-
2017
- 2017-11-16 CN CN201711134449.7A patent/CN107855539A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1152487A (en) * | 1995-08-25 | 1997-06-25 | 纳幕尔杜邦公司 | Method for preparation of golden powder by decomposing aerosol |
| CN104690295A (en) * | 2013-12-05 | 2015-06-10 | 南通建陵纳米科技有限公司 | Method for preparing monodispersed ultrafine particles |
| CN103949192A (en) * | 2014-01-16 | 2014-07-30 | 常州大学 | Method for preparing hollow spheres through microwave-assisted aerosol |
| CN106334801A (en) * | 2016-09-09 | 2017-01-18 | 常州大学 | Method for preparing porous carbon loaded nano-metal through microwave assistance |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108975360A (en) * | 2018-07-20 | 2018-12-11 | 大连理工大学 | A kind of preparation method, device and the application of spherical shape magnesia |
| CN110514700A (en) * | 2019-09-27 | 2019-11-29 | 西安电子科技大学 | A kind of copper oxide and cobaltosic oxide heterogeneous structural nano line composite sensitive material, ethylene glycol sensor and preparation method |
| CN111842924A (en) * | 2020-07-16 | 2020-10-30 | 西安交通大学 | Microwave-assisted metal nanoparticle preparation method and system |
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