CN104772472B - nano metal material preparing method and nano metal material prepared by same - Google Patents
nano metal material preparing method and nano metal material prepared by same Download PDFInfo
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- CN104772472B CN104772472B CN201410015483.2A CN201410015483A CN104772472B CN 104772472 B CN104772472 B CN 104772472B CN 201410015483 A CN201410015483 A CN 201410015483A CN 104772472 B CN104772472 B CN 104772472B
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Abstract
The invention discloses a nano metal material preparing method and a nano metal material prepared by the same. The nano metal material preparing method comprises the following steps that one metal trinitride or a plurality of metal trinitrides is/are placed in a closed environment; a driving energy is employed to stimulate the metal trinitride to carry out detonation reaction; then rapid cooling processing is carried out to obtain the nano metal material. The metal trinitrides adopt silver azide, copper azide, zinc azide, lead azide, gold azide, zirconium azide or cerium azide; the nano metal material is nano metal or nano metal alloy; when one metal trinitride is used, the nano metal material is the nano metal; when a plurality of metal trinitrides are used, the nano metal material is the nano metal alloy. The nano metal material is prepared by the nano metal material preparing method. The invention has the advantages that the preparing method is simple, the cost is low, rapid production can be realized, and the energy-saving environmental protection concept can be realized at the same time.
Description
Technical field
The present invention relates to the manufacture method and nano metal material of a kind of nano metal material, more particularly to one kind uses metal
Azido compound is preparing the method and its obtained nano metal material of nano metal material.
Background technology
Nano metal or nano metal alloy all have its application on numerous areas, for example, urge Ru industrial
Agent or conduction material, or the such as pharmaceutical carrier of engineering in medicine or biomarker developer, therefore, nano metal or nm of gold
Category alloy is widely studied and developed.The preparation method of general nano metal or nano metal alloy can using chemical gas-phase method,
The method such as coprecipitation or ball-milling method.
The chemical gas-phase method be by the heated decomposition of a compound containing metal after, or after heated reaction, and formed
Nano metal or nano metal alloy.So, the compound containing metal used in the chemical gas-phase method need to have volatility
Or the characteristic of easy carburation by evaporation, or using high-energy the compound for containing metal need to be made to switch to gas phase, therefore, the chemical gaseous phase
The compound containing metal that is somebody's turn to do used in method is easily limited, it is impossible to extensively prepare various nano metals or nano metal is closed
Gold, and do not meet the environmentally friendly concept of current energy-conservation using high-energy.
In view of above-mentioned, still a need to develop a kind of method that low cost and processing procedure simply prepare nano metal, with
Needed for meeting dealer.
The content of the invention
The first object of the present invention is to provide a kind of method that low cost and processing procedure simply prepare nano metal material.
The method that the present invention prepares nano metal material, comprising below step：By one or more metal azides
(metalazide) in being placed in a closed environment；A driving energy (drivingenergy) is bestowed, to excite the metal nitrine chemical combination
Thing carries out the process of detonation reaction (detonation)；Then, the cooling for carrying out rapidly is processed, you can obtain the nano metal
Material；The metal azide be silver azide, copper azide, Azide zinc, lead azide, Azide gold, Azide zirconium or
Azide cerium；The nano metal material is nano metal or nano metal alloy；When using a kind of metal azide, this is received
Rice metal material is nano metal；And when using various metals azido compound, the nano metal material is nano metal alloy.
Detonation reaction in the present invention refers to the metal azide and is decomposed or atom recombination, while companion
There are a large amount of exergonic chemical reaction processes.
The metal azide is the material of high-energy-density, when bestowing a driving energy to it, it is possible to provide the closed loop
The condition of border high temperature and high pressure.The preparation method of the metal azide can be by the way of conventional, for example, using alkali metal
Azido compound carries out metal displacement reaction and is formed with Yin Yuan, Tong Yuan, zinc source, lead source, Jin Yuan, zirconium source or cerium source.It is preferred that
The alkali metal azide is sodium azide.The silver-colored source is such as, but not limited to AgNO3Or AgCl etc.；The copper source for example but does not limit
In Cu (NO3)2Or CuCl2Deng；The zinc source is such as, but not limited to Zn (NO3)2Or ZnCl2Deng；The lead source is such as, but not limited to Pb
(NO3)2Or PbCl2；The Jin Yuan is such as, but not limited to Au (NO3)2Or AuCl2Deng；The zirconium source is such as, but not limited to Zr (NO3)2、Zr
(NO3)4Or ZrCl4Deng；The cerium source is such as, but not limited to Ce (NO3)3Or Ce (NO3)4Deng.
It is preferred that this prepares this of the method for nano metal material bestows a driving energy step, it is folded at least two kinds metals
Nitrogen compound bestows a driving energy.
It is preferred that the driving energy is a thermal source.The temperature range of the thermal source is not particularly limited, as long as the gold can be excited
Category azido compound carries out detonation reaction.Effectively to excite the metal azide to carry out detonation reaction, this is bestowed
The mode of driving energy will flashpoint that is as quick as possible and can reaching metal azide moment.According to different metal nitrine chemical combination
The characteristic of thing, the speed for bestowing driving energy is also different, it is preferred that the speed is 30 DEG C/min to 100 DEG C/min.
It is preferred that when detonation is reacted, the moment maximum pressure scope of the closed environment is 1GPa to 10GPa.It is preferred that
When detonation is reacted, the moment maximum temperature range of the closed environment is 3,000K to 4,000K.
After detonation reaction, carrying out the mode of rapid cooling process can such as import nitrogen or liquid nitrogen using general fashion
To be lowered the temperature.It is preferred that the flow rates of the nitrogen or liquid nitrogen are 300mL/min to 500mL/min.It is preferred that the drop
The cooling rate scope that temperature is processed is 5 DEG C/s to 10 DEG C/s.
As long as the equipment that the method for preparing nano metal material is used have attemperating unit, cooling fluid gatherer,
The equipment of seal, high temperature resistant and high pressure resistant property all may be used.The equipment can adopt the equipment that art was used in the past
, so repeating no more.
The second object of the present invention is to provide a kind of nano metal material.
Nano metal material of the present invention, is by obtained by a method for preparing nano metal material as above.
It is preferred that the average particle size range of the nano metal material is below 10nm.
The beneficial effects of the present invention is：By bestowing a driving energy to the metal azide, fold the metal
Nitrogen compound itself produces violent chemical change, and is decomposed or recombinated, and carries out rapid cooling process, and obtains nanometer
Metal or nano metal alloy.Preparation method of the present invention is simple, low cost and can quickly produce nano metal material, while meeting energy-conservation
Environmentally friendly concept.
Description of the drawings
Fig. 1 is a mode of appearance analysis chart, illustrates the particle size of the Nano Silver metal material of the present invention；
Fig. 2 is a mode of appearance analysis chart, illustrates the particle size of the nano cerium zirconium alloy material of the present invention；
Fig. 3 is a constituent analysis figure, illustrates the composition of the Nano Silver metal material of the present invention；
Fig. 4 is a constituent analysis figure, illustrates the composition of the nano cerium zirconium alloy material of the present invention；
Fig. 5 is a lattice structure figure, illustrates the lattice structure of the Nano Silver metal material of the present invention；And,
Fig. 6 is a lattice structure figure, illustrates the lattice structure of the nano cerium zirconium alloy material of the present invention.
Specific embodiment
The present invention will be described further with regard to following examples, however, it should be noted that the embodiment is only illustrated saying
Bright use, and it is not necessarily to be construed as the restriction of present invention enforcement.
<Embodiment>
<Embodiment 1>
10 grams of carbonato sodium azide is dissolved in 200 milliliters of distilled water, the Ba (NO of 5wt% are added3)2, connect
, after filtering, collect filtrate, then, filtrate is heated to into 50 DEG C.
After solution temperature it is after 50 DEG C, to be gradually added into the silver nitrate solution of 240 milliliters of 5wt%, and stirs so that precipitate
Average particle size range then, is filtered at 125 μm to 250 μm, and cleans filter cake using distilled water, until filtrate is not present
Barium ions and silver ion.Then, filter cake is placed in after air drying, you can obtain silver azide.
By above-mentioned 1.5 grams of silver azide be placed in one have high temperature resistant, high pressure resistant and attemperating unit equipment it is closed
In environment, and the closed environment is full of into nitrogen, then, using attemperating unit a thermal source is provided, and with the speed of 30 DEG C/min
Temperature from ambient is risen to into 300 DEG C, now, the silver azide moment is heated carries out detonation reaction, and the wink of the closed environment
Between maximum pressure be 5GPa, then, liquid nitrogen is imported with the flow velocity of 300mL/min, by temperature drop to room temperature, and cooling rate
For 5 DEG C/s, you can obtain Nano Silver metal material.
<Embodiment 2>
10 grams of carbonato sodium azide is dissolved in 200 milliliters of distilled water, the Ba (NO of 5wt% are added3)2, connect
, after filtering, collect filtrate, then, filtrate is heated to into 40 DEG C.
After solution temperature it is after 40 DEG C, to be gradually added into the lead nitrate solution of 160 milliliters of 5wt%, and stirs so that precipitate
Average particle size range then, is filtered at 125 μm to 250 μm, and cleans filter cake using distilled water, until filtrate is not present
Barium ions and lead ion.Then, filter cake is placed in after air drying, you can obtain lead azide.
By above-mentioned 1.5 grams of lead azide be placed in one have high temperature resistant, high pressure resistant and attemperating unit equipment it is closed
In environment, and the closed environment is full of into nitrogen, then, using attemperating unit a thermal source is provided, and with the speed of 50 DEG C/min
Temperature from ambient is risen to into 280 DEG C, now, the lead azide moment is heated carries out detonation reaction, and the wink of the closed environment
Between maximum pressure be 5GPa, then, liquid nitrogen is imported with the flow velocity of 300mL/min, by temperature drop to room temperature, and cooling rate
For 5 DEG C/s, you can obtain nanometer lead metal material.
<Embodiment 3>
10 grams of carbonato sodium azide is dissolved in 200 milliliters of distilled water, the Ba (NO of 5wt% are added3)2, connect
, after filtering, collect filtrate, then, filtrate is heated to into 50 DEG C.
After solution temperature is for 50 DEG C, the silver nitrate solution of 120 milliliters of 5wt% and the nitric acid of 80 milliliters of 5wt% are gradually added into
Lead solution, and stir so that the average particle size range of precipitate then, is filtered at 125 μm to 250 μm, and uses distillation
Water cleans filter cake, until filtrate does not have barium ions, silver ion and lead ion.Then, filter cake is placed in after air drying, i.e.,
The mixture containing lead azide and silver azide can be obtained.
Above-mentioned 1.5 grams of mixture is placed in into a closed loop with high temperature resistant, high pressure resistant and attemperating unit equipment
In border, and the closed environment is full of into nitrogen, then, using attemperating unit a thermal source is provided, and will with the speed of 50 DEG C/min
Temperature from ambient rises to 210 DEG C, and now, the mixture moment is heated carries out detonation reaction, and the moment of the closed environment is most
Big pressure is 5GPa, then, with the flow velocity of 300mL/min liquid nitrogen is imported, and by temperature drop to room temperature, and cooling rate is 5
DEG C/s, you can obtain Nano Silver metal material.
<Embodiment 4>
10 grams of carbonato sodium azide is dissolved in 200 milliliters of distilled water, the Ba (NO of 5wt% are added3)2, connect
, after filtering, collect filtrate, then, filtrate is heated to into 70 DEG C.
After solution temperature is for 70 DEG C, the zirconium nitrate solution of 100 milliliters of 5wt% and the nitric acid of 100 milliliters of 5wt% are gradually added into
Cerium solution, and stir so that the average particle size range of precipitate then, is filtered at 125 μm to 250 μm, and uses distillation
Water cleans filter cake, until filtrate does not have barium ions, zirconium ion and cerium ion.Then, filter cake is placed in after air drying, i.e.,
The mixture containing Azide zirconium and Azide cerium can be obtained.
Above-mentioned 1.5 grams of mixture is placed in into a closed loop with high temperature resistant, high pressure resistant and attemperating unit equipment
In border, and nitrogen is imported, then, using attemperating unit a thermal source is provided, and with the speed of 100 DEG C/min by temperature from ambient
325 DEG C to 400 DEG C are risen to, now, the silver azide moment is heated carries out detonation reaction, and the moment of the closed environment is maximum
Pressure is 5GPa, then, with the flow velocity of 300mL/min liquid nitrogen is imported, and by temperature drop to room temperature, and cooling rate is 5
DEG C/s, you can obtain nano cerium zirconium alloy material.
<<Detection project>>
1. constituent analysis：The nano cerium zirconium alloy material of the Nano Silver metal material of embodiment 1, and embodiment 4 is placed in into high solution
Analysis type scans transmission electron microscope (label：JEOL；Model：TEM-3010), Inner structural shape and particle size are observed
Distribution, and electron diffraction pattern (DiffractionPattern) of arranging in pairs or groups, to analyze sample in micro organization and crystal structure,
In addition, analyzing its chemical element using its X- luminous energy spectrometer (EnergyDispersiveSpectrometer, abbreviation EDS)
Composition and content.
2. lattice structure is determined：The nano cerium zirconium alloy material of the Nano Silver metal material of embodiment 1, and embodiment 4 is placed in into X
X ray diffractometer x (label：RIGAKU；Model：MiniFlex) measured, analysis condition：The angular range of scanning be -3 ° extremely
150 ° (2 θ), and sweep speed is 0.01 ° to 100 °/min (2 θ).
Table 1
The data of Fig. 1, Fig. 3 and Fig. 5 for being drawn from embodiment 1, the present invention preparation method can prepare 10nm really with
The silver metal material of lower nano-scale.From the data of Fig. 2, Fig. 4 and Fig. 6 of embodiment 4, the preparation method of the present invention can be prepared really
Go out below 10nm nano cerium zirconium alloy materials.In sum, by bestowing a driving energy to the metal azide, the gold is made
Category azido compound itself produces violent chemical change, and is decomposed or recombinated, and carries out rapid cooling process, and obtains
Obtain nano metal or nano metal alloy.Preparation method of the present invention is simple, low cost and can quickly produce nano metal material, while meeting
The environmentally friendly concept of energy-conservation, does not require the use of the expensive devices such as general plasma-based or laser, and cost benefit and innovation can be reached really
Purpose.
Claims (9)
1. a kind of method for preparing nano metal material, it is characterised in that comprising below step：By one or more metal nitrine
Compound is placed in a closed environment；A driving energy is bestowed, to excite the metal azide to carry out the process of detonation reaction,
When detonation is reacted, the moment maximum pressure scope of the closed environment is 1GPa to 10GPa；Then, carry out at cooling rapidly
Reason, you can obtain the nano metal material；The metal azide is silver azide, copper azide, lead azide, Azide
Gold, Azide zirconium or Azide cerium；The nano metal material is nano metal or nano metal alloy；When using a kind of metal nitrine
During compound, the nano metal material is nano metal；And when using various metals azido compound, the nano metal material is to receive
Rice metal alloy.
2. the method for preparing nano metal material according to claim 1, it is characterised in that：This bestows a driving energy step,
It is that a driving energy is bestowed at least two kinds metal azides.
3. the method for preparing nano metal material according to claim 1, it is characterised in that：The driving energy is a thermal source.
4. the method for preparing nano metal material according to claim 1, it is characterised in that：When detonation is reacted, this is closed
The moment maximum temperature range of environment is 3,000K to 4,000K.
5. the method for preparing nano metal material according to claim 1, it is characterised in that：The cooling rate that the cooling is processed
Scope is 5 DEG C/s to 10 DEG C/s.
6. the method for preparing nano metal material according to claim 1, it is characterised in that：The metal azide be by
One alkali metal azide carries out metal displacement reaction and is formed with Yin Yuan, Tong Yuan, lead source, Jin Yuan, zirconium source or cerium source.
7. the method for preparing nano metal material according to claim 6, it is characterised in that：The alkali metal azide is
Sodium azide.
8. a kind of nano metal material, is the method institute for preparing nano metal material by any one of just like claim 1 to 7
It is obtained.
9. nano metal material according to claim 8, it is characterised in that：The average particle size range of the nano metal material is
Below 10nm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102728853A (en) * | 2012-06-11 | 2012-10-17 | 仇晓丰 | Production technique for high-purity nanoscale metal magnesium powder |
| CN102744420A (en) * | 2012-06-20 | 2012-10-24 | 中国科学院宁波材料技术与工程研究所 | Preparation method of magnetic nanometer particles with adjustable and controllable particle diameter |
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| US7967891B2 (en) * | 2006-06-01 | 2011-06-28 | Inco Limited | Method producing metal nanopowders by decompositon of metal carbonyl using an induction plasma torch |
| JP2010222622A (en) * | 2009-03-23 | 2010-10-07 | Nagoya Institute Of Technology | Method of synthecizing transition metal nano particle |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102728853A (en) * | 2012-06-11 | 2012-10-17 | 仇晓丰 | Production technique for high-purity nanoscale metal magnesium powder |
| CN102744420A (en) * | 2012-06-20 | 2012-10-24 | 中国科学院宁波材料技术与工程研究所 | Preparation method of magnetic nanometer particles with adjustable and controllable particle diameter |
Non-Patent Citations (2)
| Title |
|---|
| DETONATION OF MOLECULAR PRECURSORS AS A TOOL FOR THE ASSEMBLY OF NANO-SIZED MATERIALS;ZHENPING ZHU;《Modern Physics Letters B》;20031231;第17卷(第29-30期);1477、1489 * |
| The Generation Of Nanoscale Metal Particles From Metal Azides: A High Resolution Electron Microscopic Study;P. J. Herley et. al.;《Atoms, Molecules and Clusters, Phys.》;19931231;第26卷;159-161 * |
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