CN104690295B - The method for preparing monodisperse superfine particle - Google Patents
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Abstract
A kind of method for preparing monodisperse superfine particle, is related to the method that single dispersion metal simple substance or metallic oxide ultra fine particle are prepared with microwave irradiation aerosol droplets.Microwave processes are carried out to polydispersed aerosol drop, micron-sized aerosol is broken into sub-micron or nanoscale aerosol, and then obtain monodispersed ultra-fine grain.By changing species, carrier gas type, the microwave power of presoma, single dispersion metal, alloy, metal oxide particle can be obtained.The Ultra-fine-particle Size prepared, morphology controllable, favorable dispersibility, particle diameter has simple to operate, environmental protection in 10 1000 nanometer ranges, whole technique, the advantages of cost is relatively low.
Description
Technical field
The present invention provides a kind of method for preparing monodisperse superfine particle.Specifically, the present invention relates to use microwave irradiation
Aerosol droplets are come the method for preparing single dispersion metal simple substance or metallic oxide ultra fine particle.
Background technology
Monodisperse particles refer to shape and constitute the very narrow particle swarm of homogeneous and particle diameter distribution.Height monodisperse superfine
Granule-morphology unification, in the same size, crystal formation are consistent, are the premises for carrying out nano material basic research and application study.Single dispersing
The overall performance of particle reach unanimity, for people's research material performance provide it is convenient, also in many such as instrument parameter marks
The aspects such as fixed, colloidal theory checking have a wide range of applications.Ultra-fine monodisperse particles have excellent performance, at present, ultra-fine list
Discrete particles have turned into the effective catalyst of many chemical reactions, decomposition, petroleum cracking for water etc., such as using RuO as
Catalyst is dispersed on the monodisperse particles of CdS, by water decomposition can be hydrogen and oxygen by light irradiation, thus is possible to be applied to
Manufacture solar cell.Monodisperse superfine particle is passed in microexamination, such as photonic crystal, nano-device, drug loading, gas
The aspect such as defeated, separation and catalysis has very big application potential.Can be by self-assembling technique monodisperse superfine particle system
Standby various nano structural materials.
Solid phase method is a kind of traditional pulverization process, has the advantages that low cost, yield be high, preparation process is simple.Solid phase
Method is divided into solid phase mechanical crushing method and solid reaction process.Solid phase mechanical crushing method borrow such as Ball-stirring mill, ball mill, airflow milling,
Various pulverizers such as tower mill, using the mutual grinding between medium and material and the principle of impact, make crushing material, often
For preparing the powder particles of micron-level particle size.Li etc.（Solid State Sciences, 2000, 2(8): 767-772.）
The dispersed preferable, SiO of size uniform is successfully synthesized using solid reaction process at room temperature2、CeO2、SnO2Deng superfine
Grain, and first to it is this at room temperature by solid phase reaction formation ultrafine dust mechanism study.But there is energy consumption in this method
Greatly, particle size distribution is uneven, be easily mixed into impurity, the shortcomings of particulate appearance is irregular, thus less be used to prepare superfine
Grain.
Homogeneous precipitation method is a kind of new technology for preparing monodisperse superfine particle for growing up in recent years.During the method is utilized
Between product the precipitating ion in solution slowly and is uniformly discharged, by the formation speed for controlling precipitating ion in solution
To control the speed of growth of particle.Can prepare the particle of various patterns and particle diameter using homogeneous precipitation method, such as ZnO,
CaCO3、CdS、α-Al2O3、Co3O4、MgO、TiO2、SiO2、Y2O3, the ultra-fine grain such as Ag.Homogeneous precipitation method is to prepare single dispersing
A kind of current techique of grain.Chinese patent CN 101698609A prepare particle diameter with urea as precipitating reagent using homogeneous precipitation method
The yttrium oxide nano-powder of 50-500nm, is used to prepare high transmittance crystalline ceramics.Chinese patent CN 102757053A useizations
Learn the precipitation method, and mating surface activating agent high degree of dispersion effect, prepare the controllable SiO of height single dispersing, uniform particle sizes2It is micro-
Powder.The method has the advantages that cost of material is low, easy to operate, process is simple, but method reaction is relatively slow, and finishing time is long, and
It is difficult to control to particle diameter, pattern and the structure of particle.Except homogeneous precipitation method, the method for preparing monodisperse particles also has high temperature pyrolysis
Method, hydro-thermal method, solvent-thermal method, sol-gel process, microemulsion method, solvent-thermal method, ball-milling method etc..But these methods all exist
The shortcomings of particle size wider distribution, poor dispersion, granule-morphology are difficult to control to.
Atomization is a kind of effective ways for preparing subparticle.According to the difference of atomizing type, there is electrofluid to drive mist
Change（That is electrojet method）With gas pressure atomization.The aerosol produced by aerosol generator for growing up on this basis
Grain have polydispersion and single dispersing point, polydispersion type aerosol generator gained particle size distribution is wider, and mostly micron order,
Yield is higher, is adapted to batch production.Vibration outlet type aerosol generator can be obtained fine monodisperse particles [Chem. Mater., 2005, 17, 2475-2480；Materials Transactions, 2006, 47（5）,1380-1385].Electricity
Gunite can be also obtained close to monodispersed micron/sub-micron grade particle, and the method process is simple, operated under normal temperature and pressure, cost
Low, but yield is very low, generally 0.5 mL/h-25 mL/h are even lower, this restrict the practical application of the method.
The C of CN 100413589 use usual microwave irradiation mixed metal oxide precursors, the patent to emphasize that presoma is necessary
Contain Mn and Nb, and Te or Sb at least one therein.The essence of the patent is that porous hybrid metal is aoxidized using microwave
Thing precursor is modified, and obtains more excellent aperture, porosity and granule-morphology, reaches activation composite metal catalyst, improves
The purpose of catalyst performance.But mixed-metal oxides particle size is larger obtained in the patent, any microwave is not involved with
The control of particle diameter and final oxide particle size monodispersity to aerosol droplets.
In sum, the method that monodisperse superfine particle is prepared at present all comes with some shortcomings, therefore provides a kind of operation
Simplicity, low cost, can be mass and preparation method that process time is short just seems necessary.This is also of the invention basing oneself upon
Point and starting point.
The content of the invention
The technical problems to be solved by the invention are that conventional technology of preparing synthesis particle is big, it is impossible to obtain ultra-fine rank（1 is micro-
Rice is following）Particle, and bad dispersibility problem, there is provided a kind of new method for preparing monodisperse superfine particle.The method has
Have the advantages that monodisperse superfine metal, alloy, metal oxide particle can be obtained.
In order to solve the above technical problems, present invention use is exactly scheme as follows：One kind prepares single dispersion metal, metal oxygen
The method of compound ultrafine dust, the method is comprised the following steps：
（a）Precursor solution is configured to during slaine is added into polar solvent；The slaine is selected from the nitric acid without Nb
At least one in salt, halogeno salt, hypochlorite, acetate, oxalates or sulfate；
（b）By step（a）In obtained precursor solution be atomized to form aerosol droplets through aerosol generator；
（c）Use microwave generator irradiation steps（b）In the aerosol droplets that obtain, the w-600 of power 400 of microwave irradiation
Kw, -10 minutes 0.01 second microwave action time；
（d）By step（c）It is molten that gained aerosol obtains single dispersing gas into treatment at further 100-1000 DEG C of tube furnace
Glue ultrafine dust, single dispersion metal simple substance, alloy or metallic oxide ultra fine particulate are obtained final product by collecting, and its particle diameter is 10-
1000 nanometers.
In above-mentioned technical proposal, it is preferable that slaine be selected from Ag, Au, Cu, Pt, Pd, Fe, Co, Ni, Sn, Sb, Mo, Ti,
In the nitrate of V, W, Mn, Ru, Zr, Ce, Zn or Cr metal, halogeno salt, hypochlorite, acetate, oxalates or sulfate
It is at least one；The weight concentration of metal salt solution is no more than 15.0%；The solvent is one or more polar solvent, including：
At least one in water, ethanol, methyl alcohol, isopropanol, acetone or tetrahydrofuran.
In above-mentioned technical proposal, it is preferable that described solvent is at least one in water or ethanol；Described metal is
At least one in Ag, Cu, Au, Pt, Pd, Fe, Zn, Co, Ni, Sn, Sb, Mo, Ti, V or W.
In above-mentioned technical proposal, it is preferable that the weight concentration of slaine is 0.5-8%.
In above-mentioned technical proposal, it is preferable that the polydispersed aerosol generator is commercialized atomizer, by ultrasound
Or high velocity air crushes the aerosol droplets particle diameter to be formed and is not more than 50 μm.
In above-mentioned technical proposal, it is preferable that the microwave generator power is 800 w-200 kw, microwave action time
- 10 minutes 0.1 second.
In above-mentioned technical proposal, it is preferable that step（d）Aerosol droplets are by tube furnace drying, heat after middle microwave treatment
Other chemical reactions are decomposed or occur, tubular type furnace temperature is 200-800 DEG C, and the residence time is -10 minutes 0.1 second, and carrier gas is sky
Gas, nitrogen, carbon dioxide, hydrogen or its gaseous mixture.
In above-mentioned technical proposal, it is preferable that ultra-fine grain particle size is 50-500 nanometers.
The technical advantage of the preparation method of monodisperse particles of the present invention is mainly reflected in：Metal salt solution is used for preceding
Body is driven, cost is relatively low, and raw material is easy to get.Precursor solution is atomized into droplet using polydispersed aerosol generator, is made several
Nanometer, on this basis by microwave treatment, is converted into it monodispersed to the aerosol droplets of tens microns of distribution wide
Aerosol, the method yield is big, can be mass, take it is few, can make up monodisperse aerosol generator yield poorly, high cost not
Foot, it is also possible to make up the homogeneous precipitation method deficiency that time-consuming.While the treatment by controlling the concentration, tube furnace of precursor solution
The factors such as the residence time of temperature, microwave power and particulate in microwave office and tube furnace can control gained ultrafine dust
Size, pattern and crystal formation.
Another feature of this preparation method is increased on the basis of Conventional aerosol technology prepares polydispersion micro-size particles
One microwave processes is added.Heating using microwave have homogeneous heating, it is quick the characteristics of.Slaine, polar solvent are normal dielectrics
The larger material of number, it is sensitive to microwave, after receiving the energy of microwave, can be rapidly heated to heat decomposition temperature, obtain
Monodisperse superfine metal oxide particle directly thermally decomposes to yield monodisperse superfine metal simple-substance particle, or leads in tube furnace
Enter reducibility gas, such as hydrogen, metal oxide is reduced into metal simple-substance.Its core content is to polydispersed aerosol drop
Microwave processes are carried out, is acted on using the high-efficiency heating of microwave, micron-sized aerosol is broken into sub-micron or nanoscale
Aerosol, and then obtain monodispersed ultrafine dust.By changing the species and carrier gas type of presoma, single dispersing can be obtained and surpassed
Thin metal, alloy, metal oxide particle, achieve preferable technique effect.
Brief description of the drawings
Fig. 1 schemes for the SEM of single dispersing ferric oxide particles obtained in embodiment 1.
Fig. 2 is the XRD of single dispersing ferric oxide particles obtained in embodiment 1.
Fig. 3 schemes for the SEM of single dispersing Argent grain obtained in embodiment 2.
Fig. 4 is the XRD of single dispersing Argent grain obtained in embodiment 2.
Fig. 5 schemes for the DLS of monodisperse superfine Argent grain obtained in embodiment 3.
Fig. 6 schemes for the TEM of single dispersing nickel oxide particle obtained in embodiment 4.
Fig. 7 is the XRD of single dispersing nickel oxide particle obtained in embodiment 4.
Fig. 8 is the cobaltosic oxide TEM figures that the common aerosol method of comparative example 1 is prepared.
Fig. 9 is the TEM figures of the cobaltosic oxide that the microwave radiation technology aerosol processing of embodiment 5 is prepared.
Figure 10 is the XRD that embodiment 5 is obtained monodisperse superfine Argent grain.
Specific embodiment
With reference to specific embodiment, the present invention will be further described, but protection scope of the present invention not limited to this.
Embodiment 1
（1）Weigh 0.2 g Fe (NO3)3（Analysis is pure）It is placed in beaker, adds distilled water diluting to 0.5%, is well mixed
Obtain solution；
（2）Above-mentioned solution is put into the container of aerosol generator, micro-wave oven is opened, microwave power is adjusted to 700 w；
（3）Nitrogen cylinder is opened, the pressure for adjusting aerosol generator is 20 psi, and gas obtained in aerosol generator is molten
Micelle enters in micro-wave oven carries out microwave irradiation, and exposure time is about 26 s；
（4）Enter tube furnace through the particle after microwave action（Temperature is set as 400 DEG C）About 5 s of heat treatment；
（5）Particle after heat treatment is collected on the filter, and the temperature of filter maintains 80 DEG C or so；
（6）The particle that will be collected into is dispersed in ethanol solution, to the test of SEM and XRD, gained single dispersing oxygen
Change iron particle as shown in Figure 1 and Figure 2；
As can be seen that the product obtained by embodiment is iron oxide from XRD, product is can be seen that from SEM figures
Monodispersity is fine.
Embodiment 2
（1）Weigh 0.2 g AgNO3（Analysis is pure）It is placed in beaker, adds a certain amount of distilled water diluting to 0.5%, mixes
Conjunction is uniform to obtain solution；
（2）Above-mentioned solution is put into the container of aerosol generator, micro-wave oven is opened, microwave power is adjusted to 700 w；
（3）Nitrogen cylinder is opened, the pressure for adjusting aerosol generator is 15 psi, and gas obtained in aerosol generator is molten
Micelle enters in micro-wave oven carries out microwave irradiation, and exposure time is about 50 s；
（4）Enter tube furnace through the particle after microwave action（Temperature is set as 400 DEG C）About 5 s of heat treatment；
（5）Particle after heat treatment is collected on the filter, and the temperature of filter maintains 80 DEG C or so；
（6）The particle that will be collected into is dispersed in ethanol solution, and to the test of SEM and XRD, gained single dispersing surpasses
Thin Argent grain is as shown in Figure 3, Figure 4；
As can be seen that the product obtained by embodiment is Ag particles from XRD, product is can be seen that from SEM figures
Very well, the particle diameter of particle is in 150 nm or so for monodispersity.
Embodiment 3
（1）Weigh 0.2 g AgNO3（Analysis is pure）It is placed in beaker, adds a certain amount of distilled water diluting to 0.25%, mixes
Conjunction is uniform to obtain solution；
（2）Above-mentioned solution is put into the container of aerosol generator, micro-wave oven is opened, microwave power is adjusted to 800 w；
（3）Nitrogen cylinder is opened, the pressure for adjusting aerosol generator is 40 psi, and gas obtained in aerosol generator is molten
Micelle enters in micro-wave oven carries out microwave irradiation, and exposure time is about 35 s；
（4）Enter tube furnace through the particle after microwave action（Temperature is set as 400 DEG C）About 4 s of heat treatment；
（5）Particle after heat treatment is collected on the filter, and the temperature of filter maintains 80 DEG C or so；
（6）The particle that will be collected into is dispersed in ethanol solution, and to the test of DLS, test result is as shown in Figure 5
It can be seen that the monodispersity of particle is good, average grain diameter in 97 nm or so, in combination with embodiment 2
It can be seen that changing the concentration of precursor solution, the power of microwave action can effectively control the size and dispersiveness of particle.
Embodiment 4
（1）Weigh 0.5 g Ni (NO3)2（Analysis is pure）It is placed in beaker, adds a certain amount of distilled water diluting to 0.5%,
It is well mixed to obtain solution；
（2）Above-mentioned solution is put into the container of aerosol generator, micro-wave oven is opened, microwave power is adjusted to 800 w；
（3）Nitrogen cylinder is opened, the pressure for adjusting aerosol generator is 20 psi, and gas obtained in aerosol generator is molten
Micelle enters in micro-wave oven carries out microwave irradiation, and exposure time is about 50 s；
（4）Enter tube furnace through the particle after microwave action（Temperature is set as 400 DEG C）About 5 s of heat treatment；
（5）Particle after heat treatment is collected on the filter, and the temperature of filter maintains 80 DEG C or so；
（6）The particle that will be collected into is dispersed in ethanol solution, and to the test of TEM and XRD, gained single dispersing surpasses
Thin Argent grain is as shown in Figure 6, Figure 7.
Embodiment 5
（1）Weigh 0.5 g Co (NO3)2（Analysis is pure）It is placed in beaker, adds a certain amount of distilled water diluting to 0.5%,
It is well mixed to obtain solution；
（2）Above-mentioned solution is put into the container of aerosol generator, micro-wave oven is opened, microwave power is adjusted to 800 w；
（3）Nitrogen cylinder is opened, the pressure for adjusting aerosol generator is 20 psi, and gas obtained in aerosol generator is molten
Micelle enters in micro-wave oven carries out microwave irradiation, and exposure time is about 50 s；
（4）Enter tube furnace through the particle after microwave action（Temperature is set as 400 DEG C）About 5 s of heat treatment；
（5）Particle after heat treatment is collected on the filter, and the temperature of filter maintains 80 DEG C or so；
（6）The particle that will be collected into is dispersed in ethanol solution, to the test of TEM and XRD, gained single dispersing four
Co 3 O is as shown in Figure 9, Figure 10.
Comparative example 1
（1）Weigh 0.5 g Co (NO3)2（Analysis is pure）It is placed in beaker, adds a certain amount of distilled water diluting to 0.5%,
It is well mixed to obtain solution；
（2）Above-mentioned solution is put into the container of aerosol generator, nitrogen cylinder is opened, regulation aerosol generator
Pressure is 20 psi, and the aerosol droplets of generation enter tube furnace（Temperature is set as 400 DEG C）About 5 s of heat treatment；
（3）Particle after heat treatment is collected on the filter, and the temperature of filter maintains 80 DEG C or so；
（4）The particle that will be collected into is dispersed in ethanol solution, is tested to TEM, and gained cobaltosic oxide is as schemed
8th, it is shown；
By embodiment 5 and comparative example 1, it can be seen that effect of the microwave to aerosol droplets, can effectively improve system
For the monodispersity for going out particle so that the size of whole system reaches unanimity, and demonstrates the effect of microwave.
Embodiment 6
（1）Weigh 0.2 g Fe (NO3)3（Analysis is pure）It is placed in beaker, adds a certain amount of distilled water diluting to 0.5%,
Add 2ml ethanol solutions（Analysis is pure）It is well mixed to obtain solution；
（2）Above-mentioned solution is put into the container of aerosol generator, micro-wave oven is opened, microwave power is adjusted to 800 w；
（3）Nitrogen cylinder is opened, the pressure for adjusting aerosol generator is 20 psi, and gas obtained in aerosol generator is molten
Micelle enters in micro-wave oven carries out microwave irradiation, and exposure time is about 26 s；
（4）Enter tube furnace through the particle after microwave action（Temperature is set as 400 DEG C）About 5 s of heat treatment.
Embodiment 7
（1）Weigh 0.5 g Cu (NO3)2（Analysis is pure）It is placed in beaker, adds a certain amount of distilled water diluting to 0.5%,
It is well mixed to obtain solution；
（2）Above-mentioned solution is put into the container of aerosol generator, micro-wave oven is opened, microwave power is adjusted to 800 w；
（3）Hydrogen gas cylinder is opened, the pressure for adjusting aerosol generator is 20 psi, and gas obtained in aerosol generator is molten
Micelle enters in micro-wave oven carries out microwave irradiation, and exposure time is about 50 s；
（4）Enter tube furnace through the particle after microwave action（Temperature is set as 700 DEG C）About 5 s of heat treatment；
（5）Particle after heat treatment is collected on the filter, and the temperature of filter maintains 80 DEG C or so.
Embodiment 8
（1）Weigh 5 g Fe (NO3)3（Analysis is pure）It is placed in beaker, adds a certain amount of distilled water diluting to 5%, mixing
It is uniform to obtain solution；
（2）Above-mentioned solution is put into the container of aerosol generator, micro-wave oven is opened, microwave power is adjusted to 5 kw；
（3）Hydrogen gas cylinder is opened, the pressure for adjusting aerosol generator is 20 psi, and gas obtained in aerosol generator is molten
Micelle enters in micro-wave oven carries out microwave irradiation, and exposure time is about 50 s；
（4）Enter tube furnace through the particle after microwave action（Temperature is set as 700 DEG C）About 5 s of heat treatment；
（5）Particle after heat treatment is collected on the filter, and the temperature of filter maintains 80 DEG C or so.
Embodiment 9
（1）Weigh 5 gAgNO3（Analysis is pure）It is placed in beaker, adds a certain amount of distilled water diluting to 6%, is well mixed
Obtain solution；
（2）Above-mentioned solution is put into the container of aerosol generator, micro-wave oven is opened, microwave power is adjusted to 10 kw；
（3）Hydrogen gas cylinder is opened, the pressure for adjusting aerosol generator is 20 psi, and gas obtained in aerosol generator is molten
Micelle enters in micro-wave oven carries out microwave irradiation, and exposure time is about 50 s；
（4）Enter tube furnace through the particle after microwave action（Temperature is set as 700 DEG C）About 5 s of heat treatment；
（5）Particle after heat treatment is collected on the filter, and the temperature of filter maintains 80 DEG C or so.It is collected into
Grain average-size is in 20nm.
Claims (5)
1. a kind of to prepare single dispersion metal, the method for metallic oxide ultra fine particle, the method is comprised the following steps：
A () is configured to precursor solution during slaine is added into polar solvent；The slaine is selected from nitrate, halogen without Nb
For at least one in salt, hypochlorite, acetate, oxalates or sulfate；The slaine be selected from Ag, Au, Cu, Pt, Pd,
The nitrate of Fe, Co, Ni, Ti, Sn, Sb, Mo, V, W, Mn, Ru, Zr, Ce, Zn or Cr metal, halogeno salt, hypochlorite, acetic acid
At least one in salt, oxalates or sulfate；The weight concentration of metal salt solution is no more than 15.0%；The solvent is one kind
Or various polarity solvent, including：At least one in water, ethanol, methyl alcohol, isopropanol, acetone or tetrahydrofuran；
B obtained precursor solution in step (a) is atomized to form aerosol droplets by () through aerosol generator；
C () uses aerosol droplets, the power 400w-600kw of microwave irradiation, microwave action in microwave generator irradiation steps (b)
- 10 minutes 0.01 second time；
D step (c) gained aerosol is obtained single dispersing gas by () into treatment under further 100-1000 degrees Celsius of tube furnace molten
Glue ultra-fine grain, single dispersion metal simple substance, metallic oxide ultra fine particle are obtained final product by collecting, and its particle diameter is 10-1000 nanometers.
2. it is according to claim 1 to prepare single dispersion metal, the method for metallic oxide ultra fine particle, it is characterised in that institute
The solvent stated is at least one in water or ethanol；Described metal be Ag, Cu, Au, Pt, Pd, Fe, Zn, Co, Ni, Ti, Sn,
At least one in Sb, Mo, V or W.
3. it is according to claim 1 to prepare single dispersion metal, the method for metallic oxide ultra fine particle, it is characterised in that gold
The weight concentration for belonging to salting liquid is 0.5-8%.
4. it is according to claim 1 to prepare single dispersion metal, the method for metallic oxide ultra fine particle, it is characterised in that institute
Aerosol generator is stated for commercialized atomizer, it is little to crush the aerosol droplets particle diameter to be formed by ultrasound or high velocity air
In 50 μm.
5. it is according to claim 1 to prepare single dispersion metal, the method for metallic oxide ultra fine particle, it is characterised in that step
Suddenly aerosol dries, thermally decomposes or occurs other chemical reactions by tube furnace after microwave treatment in (d), and tubular type furnace temperature is
200-1000 degrees Celsius, the residence time is -10 minutes 0.1 second, and carrier gas is air, nitrogen, carbon dioxide, hydrogen or its mixing
Gas.
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| CN107855539A (en) * | 2017-11-16 | 2018-03-30 | 武汉工程大学 | A kind of method for preparing superfine metal and metal oxide |
| CN107934922A (en) * | 2017-12-13 | 2018-04-20 | 武汉工程大学 | A kind of microwave radiation technology aerosol prepares nanometer TeO2Method |
| CN111842924B (en) * | 2020-07-16 | 2022-06-07 | 西安交通大学 | Microwave-assisted metal nanoparticle preparation method and system |
| CN112958014A (en) * | 2020-10-23 | 2021-06-15 | 武汉市格勒特新材料有限公司 | Method for producing superfine nano silver-based metal composite antibacterial agent by microwave-assisted aerosol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791704A (en) * | 2010-03-25 | 2010-08-04 | 江苏大学 | Method for preparing nano silver |
| CN102784926A (en) * | 2012-07-16 | 2012-11-21 | 太原理工大学 | Method for preparing spherical nano-silver particles |
| CN102887541A (en) * | 2011-07-21 | 2013-01-23 | 北京化工大学 | Preparation method of phthalocyanine sensitized TiO2 nano-particle by microwave-hydrothermal method |
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| US4784686A (en) * | 1987-04-24 | 1988-11-15 | The United States Of America As Represented By The United States Department Of Energy | Synthesis of ultrafine powders by microwave heating |
| CN100335434C (en) * | 2002-07-19 | 2007-09-05 | Ppg工业俄亥俄公司 | Article having nano-scaled structures and a process for making such article |
| EP1693107A1 (en) * | 2005-02-11 | 2006-08-23 | Rohm And Haas Company | Method for preparing mixed-metal oxide catalysts and the catalysts produced thereby |
| CN101426610A (en) * | 2005-06-08 | 2009-05-06 | 丰田发动机工程及制造北美公司 | Metal oxide nanoparticles and process for producing the same |
| US20070160899A1 (en) * | 2006-01-10 | 2007-07-12 | Cabot Corporation | Alloy catalyst compositions and processes for making and using same |
| FI20060428L (en) * | 2006-05-03 | 2007-11-04 | Esko Kauppinen | Surface-modified aerosol particles, method and device for their production and powders and dispersions containing said particles |
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| CN101791704A (en) * | 2010-03-25 | 2010-08-04 | 江苏大学 | Method for preparing nano silver |
| CN102887541A (en) * | 2011-07-21 | 2013-01-23 | 北京化工大学 | Preparation method of phthalocyanine sensitized TiO2 nano-particle by microwave-hydrothermal method |
| CN102784926A (en) * | 2012-07-16 | 2012-11-21 | 太原理工大学 | Method for preparing spherical nano-silver particles |
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