CN104690295A - Method for preparing monodispersed ultrafine particles - Google Patents
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Abstract
The invention discloses a method for preparing monodispersed ultrafine particles, and relates to a method for preparing monodispersed metal simple substances or metal oxide ultrafine particles by using microwave irradiation of aerosol droplets. The microwave treatment process is performed for polydispersed aerosol droplets, so that micron-sized aerosol is crushed into submicron-sized or nanometer-sized aerosol so as to obtain the monodispersed ultrafine particles. Monodispersed metal, alloy and metal oxide particles can be obtained by changing the precursor type, the carrier gas type and the microwave power. The prepared ultrathin particles have controllable particle diameters and morphologies and excellent dispersibility; the particle diameters are in a range of 10-1000 nanometers; and the whole process has such advantages as simple operation, environmental protection and lower cost.
Description
Technical field
The invention provides a kind of method preparing monodisperse superfine particle.Specifically, the present invention relates to the method preparing single dispersion metal simple substance or metallic oxide ultra fine particle by microwave irradiation aerosol droplets.
Background technology
Monodisperse particles refers to shape and the homogeneous and particle swarm that domain size distribution is very narrow of composition.Height monodisperse superfine granule-morphology is unified, in the same size, crystal formation consistent, is the prerequisite of carrying out nano material basic research and application study.The overall performance of monodispersed particle reaches unanimity, and for people's research material performance provides conveniently, also has a wide range of applications in many such as instrument parameter demarcation, colloidal theory checking etc.Ultra-fine monodisperse particles has excellent performance, at present, ultra-fine monodisperse particles has become the effective catalyst of many chemical reactions, for the decomposition, petroleum cracking etc. of water, such as RuO is dispersed on the monodisperse particles of CdS as catalyst, can be penetrated water decomposition by illumination is hydrogen and oxygen, is thus likely applied to manufacture solar cell.Monodisperse superfine particle in microexamination, as there is very large application potential the aspects such as photonic crystal, nano-device, drug loading, gas transport, separation and catalysis.Multiple nano structural material can be prepared by self-assembling technique monodisperse superfine particle.
Solid phase method is a kind of traditional pulverization process, has that cost is low, output is high, the simple advantage of preparation technology.Solid phase method is divided into solid phase mechanical crushing method and solid reaction process.Solid phase mechanical crushing method uses the multiple pulverizers such as such as Ball-stirring mill, ball mill, airflow milling, tower mill, utilizes the principle of mutual grinding between medium and material and impact, makes crushing material, be commonly used to the powder particles preparing micron-level particle size.Li etc. (
solid State Sciences, 2000,2 (8): 767-772.) at room temperature adopt solid reaction process successfully synthesize dispersed better, the SiO of size uniform
2, CeO
2, SnO
2deng ultrafine dust, and at room temperature studied by the mechanism of solid phase reaction formation ultrafine dust this first.But the shortcomings such as this method exists, and energy consumption is large, particle size distribution is uneven, be easily mixed into impurity, particulate appearance is irregular, thus less in order to prepare ultrafine dust.
Homogeneous precipitation method is a kind of new technology preparing monodisperse superfine particle grown up in recent years.This method utilizes intermediate product that the precipitating ion in solution slowly and is uniformly discharged, and is controlled the speed of growth of particle by the formation speed controlling precipitating ion in solution.Utilize homogeneous precipitation method can prepare the particle of various pattern and particle diameter, as ZnO, CaCO
3, CdS, α-Al
2o
3, Co
3o
4, MgO, TiO
2, SiO
2, Y
2o
3, the ultra-fine grain such as Ag.Homogeneous precipitation method is a kind of current techique preparing monodisperse particles.Chinese patent CN 101698609A take urea as precipitating reagent, adopts homogeneous precipitation method to prepare the yttrium oxide nano-powder of particle diameter 50-500nm, in order to prepare high permeability crystalline ceramics.Chinese patent CN 102757053A adopts chemical precipitation method, and the high degree of dispersion effect of mating surface activating agent, prepares the SiO that height single dispersing, uniform particle sizes are controlled
2micro mist.This method has the advantages such as cost of material is low, easy and simple to handle, technique is simple, but the reaction of this method is comparatively slow, and finishing time is long, and is difficult to the particle diameter of control particle, pattern and structure.Except homogeneous precipitation method, the method preparing monodisperse particles also has high temperature pyrolytic cracking (HTP), hydro-thermal method, solvent-thermal method, sol-gel process, microemulsion method, solvent-thermal method, ball-milling method etc.But these methods all exist, and particle size distribution is wider, dispersiveness is bad, granule-morphology is difficult to the shortcomings such as control.
Atomization is a kind of effective ways preparing subparticle.According to the difference of atomizing type, electrofluid is had to drive atomization (i.e. electrojet method) and gas pressure atomization.The aerosol particle that the aerosol generator grown up on this basis produces have polydispersion and single dispersing point, polydispersion type aerosol generator gained particle size distribution is wider, and mostly is micron order, and output is higher, is applicable to batch production.Vibration outlet type aerosol generator can obtain fine monodisperse particles [
chem. Mater., 2005,17,2475-2480;
materials Transactions, 2006,47(5), 1380-1385].Electrojet method also can obtain close to monodispersed micron/sub-micron grade particle, and this method process is simple, and operate under normal temperature and pressure, cost is low, but output is very low, is generally 0.5 mL/h-25 mL/h, even lower, this restrict the practical application of the method.
CN 100413589 C adopts usual microwave irradiation mixed metal oxide precursors, and this patent emphasizes that presoma must contain Mn and Nb, and Te or Sb at least one wherein.The essence of this patent adopts microwave to carry out modification to porous mixed metal oxide precursors, obtains more excellent aperture, porosity and granule-morphology, reach activation composite metal catalyst, improve the object of catalyst performance.But the mixed-metal oxides particle size that this patent system obtains is comparatively large, do not relate to the control of any microwave to the particle diameter of aerosol droplets and final oxide particle size monodispersity.
In sum, the method preparing monodisperse superfine particle at present all comes with some shortcomings, therefore provide a kind of easy and simple to handle, cost is low, can be mass and processing time short preparation method just seems necessary.This is also foothold of the present invention and starting point.
Summary of the invention
Technical problem to be solved by this invention is that the particle of technology of preparing synthesis is in the past large, can not obtain ultra-fine rank (less than 1 micron) particle, and the problem of bad dispersibility, provides a kind of method preparing monodisperse superfine particle newly.The method has the advantage that can obtain monodisperse superfine metal, alloy, metal oxide particle.
For solving the problems of the technologies described above, what the present invention adopted is exactly that scheme is as follows: a kind of method preparing single dispersion metal, metallic oxide ultra fine particulate, and the method comprises the following steps:
A slaine adds in polar solvent and is mixed with precursor solution by (); Described slaine is selected from least one in nitrate, halogeno salt, hypochlorite, acetate, oxalates or the sulfate not containing Nb;
B precursor solution obtained in step (a) is formed aerosol droplets through aerosol generator atomization by ();
(c) by the aerosol droplets obtained in microwave generator irradiation steps (b), the power 400 w-600 kw of microwave irradiation, 0.01 second-10 minutes microwave action time;
D step (c) gained aerosol is entered the further 100-1000 of tube furnace DEG C by () at, process obtains monodisperse aerosol ultrafine dust, and through collecting and obtain single dispersion metal simple substance, alloy or metallic oxide ultra fine particulate, its particle diameter is 10-1000 nanometer.
In technique scheme, preferably, slaine is selected from least one in the nitrate of Ag, Au, Cu, Pt, Pd, Fe, Co, Ni, Sn, Sb, Mo, Ti, V, W, Mn, Ru, Zr, Ce, Zn or Cr metal, halogeno salt, hypochlorite, acetate, oxalates or sulfate; The weight concentration of metal salt solution is no more than 15.0%; Described solvent is one or more polar solvents, comprising: at least one in water, ethanol, methyl alcohol, isopropyl alcohol, acetone or oxolane.
In technique scheme, preferably, 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 technique scheme, preferably, the weight concentration of slaine is 0.5-8%.
In technique scheme, preferably, described polydispersed aerosol generator is business-like atomizer, pulverizes the aerosol droplets particle diameter formed be not more than 50 μm through ultrasonic or high velocity air.
In technique scheme, preferably, described microwave generator power is 800 w-200 kw, 0.1 second-10 minutes microwave action time.
In technique scheme, preferably, aerosol droplets, thermal decomposition dry through tube furnace or other chemical reactions occur after microwave treatment in step (d), tube furnace temperature is 200-800 DEG C, the time of staying is 0.1 second-10 minutes, and carrier gas is air, nitrogen, carbon dioxide, hydrogen or its gaseous mixture.
In technique scheme, preferably, ultra-fine grain particle size is 50-500 nanometer.
The technical advantage of the preparation method of monodisperse particles of the present invention is mainly reflected in: employing metal salt solution is presoma, and cost is lower, and raw material is easy to get.Utilize polydispersed aerosol generator that precursor solution is atomized into droplet, make the aerosol droplets of a few nanometer to the wide distribution of tens microns, pass through microwave treatment on this basis, it is made to be converted into monodispersed aerosol, this method output is large, can be mass, consuming time few, the deficiency that monodisperse aerosol generator yields poorly, cost is high can be made up, also can make up the deficiency of homogeneous precipitation method length consuming time.The size of gained ultrafine dust, pattern and crystal formation can be controlled by controlling the factors such as the concentration of precursor solution, the treatment temperature of tube furnace, microwave power and the time of staying of particulate in microwave office and tube furnace simultaneously.
Another feature of this preparation method adds one microwave processes on the basis that Conventional aerosol technology prepares polydispersion micro-size particles.Heating using microwave has homogeneous heating, fast feature.Slaine, polar solvent are the materials that dielectric constant is larger; responsive to microwave; after accepting the energy of microwave; can be rapidly heated to heat decomposition temperature; obtain monodisperse superfine metal oxide particle or directly thermal decomposition obtain monodisperse superfine metal simple-substance particle; or reducibility gas is passed in tube furnace, as hydrogen, metal oxide back is become metal simple-substance.Its core content carries out microwave processes to polydispersed aerosol drop, utilizes the high-efficiency heating effect of microwave, makes micron-sized aerosol be broken into sub-micron or nanoscale aerosol, and then obtain monodispersed ultrafine dust.By changing kind and the carrier gas type of presoma, monodisperse superfine metal, alloy, metal oxide particle can be obtained, achieve good technique effect.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the single dispersing ferric oxide particles that embodiment 1 obtains.
Fig. 2 is the XRD figure of the single dispersing ferric oxide particles that embodiment 1 obtains.
Fig. 3 is the SEM figure of the single dispersing Argent grain that embodiment 2 obtains.
Fig. 4 is the XRD figure of the single dispersing Argent grain that embodiment 2 obtains.
Fig. 5 is the DLS figure of the monodisperse superfine Argent grain that embodiment 3 obtains.
Fig. 6 is the TEM figure of the single dispersing nickel oxide particle that embodiment 4 obtains.
Fig. 7 is the XRD figure of the single dispersing nickel oxide particle that embodiment 4 obtains.
Fig. 8 is that the cobaltosic oxide TEM that comparative example 1 common aerosol method is prepared schemes.
Fig. 9 is the TEM figure of the cobaltosic oxide that embodiment 5 microwave radiation technology aerosol processing is prepared.
The XRD figure of Figure 10 to be embodiment 5 be obtained monodisperse superfine Argent grain.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described, but protection scope of the present invention is not limited thereto.
embodiment 1
(1) 0.2 g Fe (NO is taken
3)
3(analyzing pure) is placed in beaker, adds distilled water diluting to 0.5%, mixes to obtain solution;
(2) above-mentioned solution is put in the container of aerosol generator, open micro-wave oven, make microwave power be adjusted to 700 w;
(3) open nitrogen cylinder, the pressure regulating aerosol generator is 20 psi, and the particulate that aerosol generator obtains enters in micro-wave oven and carries out microwave irradiation, and exposure time is about 26 s;
(4) particle after microwave action enters tube furnace (temperature is set as 400 DEG C) heat treatment about 5 s;
(5) particle after heat treatment is collected on the filter, and the temperature of filter maintains about 80 DEG C;
(6) by the particle dispersion collected in ethanol solution, in order to the test of SEM and XRD, gained single dispersing ferric oxide particles is as shown in Figure 1 and Figure 2;
As can be seen from XRD figure, the product obtained by embodiment is iron oxide, can find out that the monodispersity of product is fine from SEM figure.
embodiment 2
(1) 0.2 g AgNO is taken
3(analyzing pure) is placed in beaker, adds a certain amount of distilled water diluting to 0.5%, mixes to obtain solution;
(2) above-mentioned solution is put in the container of aerosol generator, open micro-wave oven, make microwave power be adjusted to 700 w;
(3) open nitrogen cylinder, the pressure regulating aerosol generator is 15 psi, and the particulate that aerosol generator obtains enters in micro-wave oven and carries out microwave irradiation, and exposure time is about 50 s;
(4) particle after microwave action enters tube furnace (temperature is set as 400 DEG C) heat treatment about 5 s;
(5) particle after heat treatment is collected on the filter, and the temperature of filter maintains about 80 DEG C;
(6) by the particle dispersion collected in ethanol solution, in order to the test of SEM and XRD, gained monodisperse superfine Argent grain is as shown in Figure 3, Figure 4;
As can be seen from XRD figure, the product obtained by embodiment is Ag particle, and can find out that from SEM figure the monodispersity of product is fine, the particle diameter of particle is at about 150 nm.
embodiment 3
(1) 0.2 g AgNO is taken
3(analyzing pure) is placed in beaker, adds a certain amount of distilled water diluting to 0.25%, mixes to obtain solution;
(2) above-mentioned solution is put in the container of aerosol generator, open micro-wave oven, make microwave power be adjusted to 800 w;
(3) open nitrogen cylinder, the pressure regulating aerosol generator is 40 psi, and the particulate that aerosol generator obtains enters in micro-wave oven and carries out microwave irradiation, and exposure time is about 35 s;
(4) particle after microwave action enters tube furnace (temperature is set as 400 DEG C) heat treatment about 4 s;
(5) particle after heat treatment is collected on the filter, and the temperature of filter maintains about 80 DEG C;
(6) by the particle dispersion collected in ethanol solution, in order to the test of DLS, test result is as shown in Figure 5
As can be seen from the figure, the monodispersity of particle is good, and average grain diameter is at about 97 nm, and the size that 2 can find out the change concentration of precursor solution in conjunction with the embodiments simultaneously, the power of microwave action effectively can control particle is with dispersed.
embodiment 4
(1) 0.5 g Ni (NO is taken
3)
2(analyzing pure) is placed in beaker, adds a certain amount of distilled water diluting to 0.5%, mixes to obtain solution;
(2) above-mentioned solution is put in the container of aerosol generator, open micro-wave oven, make microwave power be adjusted to 800 w;
(3) open nitrogen cylinder, the pressure regulating aerosol generator is 20 psi, and the particulate that aerosol generator obtains enters in micro-wave oven and carries out microwave irradiation, and exposure time is about 50 s;
(4) particle after microwave action enters tube furnace (temperature is set as 400 DEG C) heat treatment about 5 s;
(5) particle after heat treatment is collected on the filter, and the temperature of filter maintains about 80 DEG C;
(6) by the particle dispersion collected in ethanol solution, in order to the test of TEM and XRD, gained monodisperse superfine Argent grain is as shown in Figure 6, Figure 7.
embodiment 5
(1) 0.5 g Co (NO is taken
3)
2(analyzing pure) is placed in beaker, adds a certain amount of distilled water diluting to 0.5%, mixes to obtain solution;
(2) above-mentioned solution is put in the container of aerosol generator, open micro-wave oven, make microwave power be adjusted to 800 w;
(3) open nitrogen cylinder, the pressure regulating aerosol generator is 20 psi, and the particulate that aerosol generator obtains enters in micro-wave oven and carries out microwave irradiation, and exposure time is about 50 s;
(4) particle after microwave action enters tube furnace (temperature is set as 400 DEG C) heat treatment about 5 s;
(5) particle after heat treatment is collected on the filter, and the temperature of filter maintains about 80 DEG C;
(6) by the particle dispersion collected in ethanol solution, in order to the test of TEM and XRD, gained single dispersing cobaltosic oxide is as shown in Figure 9, Figure 10.
comparative example 1
(1) 0.5 g Co (NO is taken
3)
2(analyzing pure) is placed in beaker, adds a certain amount of distilled water diluting to 0.5%, mixes to obtain solution;
(2) put in the container of aerosol generator by above-mentioned solution, open nitrogen cylinder, the pressure regulating aerosol generator is 20 psi, and the aerosol droplets of generation enters tube furnace (temperature is set as 400 DEG C) heat treatment about 5 s;
(3) particle after heat treatment is collected on the filter, and the temperature of filter maintains about 80 DEG C;
(4) by the particle dispersion collected in ethanol solution, in order to TEM test, gained cobaltosic oxide as Fig. 8, shown in;
By embodiment 5 and comparative example 1, the effect of microwave to aerosol droplets can be found out, can effectively improve the monodispersity preparing particle, the size of whole system be reached unanimity, demonstrates the effect of microwave.
embodiment 6
(1) 0.2 g Fe (NO is taken
3)
3(analyzing pure) is placed in beaker, adds a certain amount of distilled water diluting to 0.5%, adds 2ml ethanolic solution (analyzing pure) and mixes to obtain solution;
(2) above-mentioned solution is put in the container of aerosol generator, open micro-wave oven, make microwave power be adjusted to 800 w;
(3) open nitrogen cylinder, the pressure regulating aerosol generator is 20 psi, and the particulate that aerosol generator obtains enters in micro-wave oven and carries out microwave irradiation, and exposure time is about 26 s;
(4) particle after microwave action enters tube furnace (temperature is set as 400 DEG C) heat treatment about 5 s.
embodiment 7
(1) 0.5 g Cu (NO is taken
3)
2(analyzing pure) is placed in beaker, adds a certain amount of distilled water diluting to 0.5%, mixes to obtain solution;
(2) above-mentioned solution is put in the container of aerosol generator, open micro-wave oven, make microwave power be adjusted to 800 w;
(3) open hydrogen gas cylinder, the pressure regulating aerosol generator is 20 psi, and the particulate that aerosol generator obtains enters in micro-wave oven and carries out microwave irradiation, and exposure time is about 50 s;
(4) particle after microwave action enters tube furnace (temperature is set as 700 DEG C) heat treatment about 5 s;
(5) particle after heat treatment is collected on the filter, and the temperature of filter maintains about 80 DEG C.
embodiment 8
(1) 5 g Fe (NO are taken
3)
3(analyzing pure) is placed in beaker, adds a certain amount of distilled water diluting to 5%, mixes to obtain solution;
(2) above-mentioned solution is put in the container of aerosol generator, open micro-wave oven, make microwave power be adjusted to 5 kw;
(3) open hydrogen gas cylinder, the pressure regulating aerosol generator is 20 psi, and the particulate that aerosol generator obtains enters in micro-wave oven and carries out microwave irradiation, and exposure time is about 50 s;
(4) particle after microwave action enters tube furnace (temperature is set as 700 DEG C) heat treatment about 5 s;
(5) particle after heat treatment is collected on the filter, and the temperature of filter maintains about 80 DEG C.
embodiment 9
(1) 5 gAgNO are taken
3(analyzing pure) is placed in beaker, adds a certain amount of distilled water diluting to 6%, mixes to obtain solution;
(2) above-mentioned solution is put in the container of aerosol generator, open micro-wave oven, make microwave power be adjusted to 10 kw;
(3) open hydrogen gas cylinder, the pressure regulating aerosol generator is 20 psi, and the particulate that aerosol generator obtains enters in micro-wave oven and carries out microwave irradiation, and exposure time is about 50 s;
(4) particle after microwave action enters tube furnace (temperature is set as 700 DEG C) heat treatment about 5 s;
(5) particle after heat treatment is collected on the filter, and the temperature of filter maintains about 80 DEG C.Collect particle mean size at 20nm.
Claims (8)
1. prepare a method for single dispersion metal, metallic oxide ultra fine particle, the method comprises the following steps:
A slaine adds in polar solvent and is mixed with precursor solution by (); Described slaine is selected from least one in nitrate, halogeno salt, hypochlorite, acetate, oxalates or the sulfate not containing Nb;
B precursor solution obtained in step (a) is formed aerosol droplets through aerosol generator atomization by ();
C () uses aerosol droplets in microwave generator irradiation steps (b), the power 400 w-600 kw of microwave irradiation, 0.01 second-10 minutes microwave action time;
D step (c) gained aerosol is entered the further 100-1000 of tube furnace degree Celsius by () under, process obtains monodisperse aerosol ultra-fine grain, through collecting and obtain single dispersion metal simple substance, alloy or metallic oxide ultra fine particle, its particle diameter is 10-1000 nanometer.
2. the method preparing monodisperse superfine particle according to claim 1, is characterized in that slaine is selected from least one in the nitrate of Ag, Au, Cu, Pt, Pd, Fe, Co, Ni, Ti, Sn, Sb, Mo, V, W, Mn, Ru, Zr, Ce, Zn or Cr metal, halogeno salt, hypochlorite, acetate, oxalates or sulfate; The weight concentration of metal salt solution is no more than 15.0%; Described solvent is one or more polar solvents, comprising: at least one in water, ethanol, methyl alcohol, isopropyl alcohol, acetone or oxolane.
3. the method preparing monodisperse superfine particle according to claim 2, is characterized in 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, Ti, Sn, Sb, Mo, V or W.
4. the method preparing monodisperse superfine particle according to claim 2, is characterized in that the weight concentration of slaine is 0.5-8%.
5. the method preparing monodisperse superfine particle according to claim 1, is characterized in that described polydispersed aerosol generator is business-like atomizer, pulverizes the aerosol droplets particle diameter formed be not more than 50 μm through ultrasonic or high velocity air.
6. the method preparing monodisperse superfine particle according to claim 1, is characterized in that described microwave generator power is 400 w-600 kw, 0.1 second-10 minutes microwave action time.
7. the method preparing monodisperse superfine particle according to claim 1, to it is characterized in that in step (d) after microwave treatment that aerosol is dry through tube furnace, thermal decomposition or other chemical reactions occur, tube furnace temperature is 200-1000 degree Celsius, the time of staying is 0.1 second-10 minutes, and carrier gas is air, nitrogen, carbon dioxide, hydrogen or its gaseous mixture.
8. the method preparing monodisperse superfine particle according to claim 1, is characterized in that Ultra-fine-particle Size is 10-1000 nanometer.
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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 |
| CN109863113A (en) * | 2016-08-18 | 2019-06-07 | 阿弗拉科技有限责任公司 | The method of particle is synthesized in the presence of solid phase |
| CN111842924A (en) * | 2020-07-16 | 2020-10-30 | 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 |
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| CN111842924A (en) * | 2020-07-16 | 2020-10-30 | 西安交通大学 | Microwave-assisted metal nanoparticle preparation method and system |
| CN114425055A (en) * | 2020-10-15 | 2022-05-03 | 武汉工程大学 | Silicon dioxide loaded multi-metal nano-particles, preparation method and antibacterial application thereof |
| CN114425055B (en) * | 2020-10-15 | 2024-04-19 | 武汉工程大学 | Silica supported multi-metal nano-particle, preparation method and antibacterial application thereof |
| 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 |
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