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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
nano metal
metal material
azide
nano
metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201410015483.2A
Other languages
Chinese (zh)
Other versions
CN104772472A (en
Inventor
王浡生
林岳辉
徐嘉泽
潘建亮
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lin Yuehui
Original Assignee
Xian Zitangsheng Skill Ltd Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian Zitangsheng Skill Ltd Co filed Critical Xian Zitangsheng Skill Ltd Co
Priority to CN201410015483.2A priority Critical patent/CN104772472B/en
Publication of CN104772472A publication Critical patent/CN104772472A/en
Application granted granted Critical
Publication of CN104772472B publication Critical patent/CN104772472B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

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

Prepare the method and its obtained nano metal material of nano metal material
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.
CN201410015483.2A 2014-01-14 2014-01-14 nano metal material preparing method and nano metal material prepared by same Expired - Fee Related CN104772472B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410015483.2A CN104772472B (en) 2014-01-14 2014-01-14 nano metal material preparing method and nano metal material prepared by same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410015483.2A CN104772472B (en) 2014-01-14 2014-01-14 nano metal material preparing method and nano metal material prepared by same

Publications (2)

Publication Number Publication Date
CN104772472A CN104772472A (en) 2015-07-15
CN104772472B true CN104772472B (en) 2017-04-12

Family

ID=53614408

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410015483.2A Expired - Fee Related CN104772472B (en) 2014-01-14 2014-01-14 nano metal material preparing method and nano metal material prepared by same

Country Status (1)

Country Link
CN (1) CN104772472B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116082105B (en) * 2023-04-07 2023-07-11 中国万宝工程有限公司 Copper azide lead azide carbon fiber composite initiating explosive and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
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

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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 *

Also Published As

Publication number Publication date
CN104772472A (en) 2015-07-15

Similar Documents

Publication Publication Date Title
Hammond et al. Ionic liquids and deep eutectics as a transformative platform for the synthesis of nanomaterials
Soofivand et al. Silver chromate and silver dichromate nanostructures: sonochemical synthesis, characterization, and photocatalytic properties
Chen et al. An evolution from 3D face-centered-cubic ZnSnO3 nanocubes to 2D orthorhombic ZnSnO3 nanosheets with excellent gas sensing performance
EP1844884B1 (en) Silver particle powder and process for producing the same
EP1844883B1 (en) Silver particle powder and process for producing the same
Xu et al. Nanosized Cu2O/PEG400 composite hollow spheres with mesoporous shells
Benhammada et al. Green synthesis of CuO nanoparticles using Malva sylvestris leaf extract with different copper precursors and their effect on nitrocellulose thermal behavior
Zinatloo-Ajabshir et al. Preparation and characterization of nanocrystalline praseodymium oxide via a simple precipitation approach
AU2009241334B2 (en) A process for the preparation of silver nano particles
EP3159078A1 (en) Silver-coated copper nanowire and preparation method therefor
DE102006032590A1 (en) Hydrothermal process for the production of nano- to microscale particles
Kundu et al. Microwave assisted swift synthesis of ZnWO4 nanomaterials: material for enhanced photo-catalytic activity
Soofivand et al. Simple and facile synthesis of Ag2CrO4 and Ag2Cr2O7 micro/nanostructures using a silver precursor
CN105381813A (en) Preparation method of carbon and nitrogen doped niobium (V) pentoxide nano sheet and application of nano sheet as photocatalyst
US10464136B2 (en) Preparation method of copper nano-structures
CN1696060A (en) Method for preparing Nano powder of alumina from industrial waste
WO2011129562A2 (en) Method for the mass production of silver nanoparticles having a uniform size
JP4248857B2 (en) Method for producing silver fine particles
Romano et al. The role of operating conditions in the precipitation of magnesium hydroxide hexagonal platelets using NaOH solutions
Mao et al. Selective synthesis of morphology and species controlled La2O3: Eu3+ and La2O2Co3: Eu3+ phosphors by hydrothermal method
CN104772472B (en) nano metal material preparing method and nano metal material prepared by same
CN1237006C (en) In2O3 and ITO monodisperse nano powder hydrothermal preparation method
Li et al. Synthesis and characterization of magnesium hydroxide using a bubbling setup
Hua et al. Preparation of KMgF3 and Eu-doped KMgF3 nanocrystals in water-in-oil microemulsions
Mohammadikish et al. Synthesis and optical band gap determination of CuO nanoparticles from salen-based infinite coordination polymer nanospheres

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
EXSB Decision made by sipo to initiate substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20171226

Address after: Taiwan County, Pingtung, China

Patentee after: Lin Yuehui

Address before: Kaohsiung City, Taiwan, China

Co-patentee before: Lin Yuehui

Patentee before: Xian Zitangsheng skill limited company

Co-patentee before: Xu Jiaze

Co-patentee before: Pan Jianliang

TR01 Transfer of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20170412

Termination date: 20210114

CF01 Termination of patent right due to non-payment of annual fee