CN109047792A - A method of quickly preparing copper nanoparticle - Google Patents
A method of quickly preparing copper nanoparticle Download PDFInfo
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- CN109047792A CN109047792A CN201811267219.2A CN201811267219A CN109047792A CN 109047792 A CN109047792 A CN 109047792A CN 201811267219 A CN201811267219 A CN 201811267219A CN 109047792 A CN109047792 A CN 109047792A
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- Prior art keywords
- copper
- copper nanoparticle
- nanoparticle
- adjuvant
- sample
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of methods for quickly preparing copper nanoparticle, it uses soluble copper salt and adjuvant for raw material, after adding deionized water dissolving, 200~300 DEG C are heated to, constant temperature, deionized water is gradually evaporated in heating and thermostatic process, mixed liquor is set to be concentrated into jelly, then redox reaction occurs rapidly, generate reducibility gas and copper ion is reduced to copper nanoparticle, and copper nanoparticle is wrapped to form flue dust by the gas generated；Released flue dust and filtering are collected, i.e. acquisition target product copper nanoparticle.The present invention prepares copper nanoparticle by single step reaction, and raw material is simple, process is short, at low cost, reaction initiation temperature is low, is suitble to large-scale production.
Description
Technical field
The invention belongs to powder metallurgical technologies, and in particular to a kind of preparation method of copper nanoparticle.
Background technique
Copper nanoparticle has the characteristics that dimensional effect, face effect and macro quanta tunnel effect, because its is unique physical
Matter and chemical property and be widely used in powder metallurgy components, advanced lubrication oil additive, catalyst and electric slurry etc.
Field.Simultaneously as copper is base metal, price is more cheap compared with the noble metals such as gold, silver, thus development copper nanoparticle has
Important theory significance and practical application value.
In recent years, domestic researcher has carried out largely in the preparation of nano copper particle powder and application aspect
Research, and achieve more significant achievement.Such as the Qin wins (Beijing University of Chemical Technology's journal, 2006,33 (6): 86-88) and uses
KBH4As reducing agent, and complexing agent EDTA, dispersing agent PVP (polyvinylpyrrolidone) is added, passes through liquid-phase reduction CuSO4, system
Obtain the copper powder of partial size about 28.4nm.Liquid phase method is current laboratory and what is be industrially widely used prepare polymolecularity Ultramicro-powder
Method, it is good, with high purity that product has many advantages, such as uniformity, but liquid phase method reaction process process is complex, equipment investment compared with
High, reaction condition needs strict control.Ding et al. (Journal of Alloys and Compounds, 1996,234 (L1-
L3): 11) using mechanochemical reaction by CuCl2, Na and NaCl carry out high-energy ball milling, prepared the nanometer that partial size is less than 50nm
Copper powder.Mechanical Method simple process, yield are big, but the disadvantage is that the production time is longer, is easily mixed into impurity, and grain shape is uneven
It is even, internal to have stress.Chinese patent CN102586800A discloses a kind of method that electrolysis method prepares copper nanoparticle, using metal
Copper is electrolyte as anode, Organic Alcohol, and being added and dissolving in the ammonium salt of electrolyte is electrolyte, is made under certain process conditions
Copper nanoparticle.This method is at low cost, but is not suitable for large-scale production, and powder reuniting is serious and apparent density is higher.
To sum up, at present in terms of preparing copper nanoparticle there are still many problems, these problems are largely affected
Application of the copper nanoparticle in every field.Therefore, exploring new preparation method and improvement process equipment is to widen copper nanoparticle
Application field and the key for improving quality.
Summary of the invention
The purpose of the present invention is to provide a kind of new methods for quickly preparing copper nanoparticle.
To realize goal of the invention, the present invention adopts the following technical scheme:
A method of copper nanoparticle quickly being prepared, it is characterized in that: it uses soluble copper salt and adjuvant for raw material, adds
Deionized water dissolving is simultaneously uniformly mixed, and obtains mixed liquor；The mixed liquor is heated to 200~300 DEG C, constant temperature, in heating and
Deionized water is gradually evaporated in thermostatic process, and mixed liquor is made to be concentrated into jelly, and vigorous oxidation reduction reaction then occurs rapidly
(in more than ten seconds time can fully reacting) generates reducibility gas and copper ion is simultaneously reduced to copper nanoparticle, and generate
Copper nanoparticle is wrapped to form flue dust by gas；Released flue dust and filtering are collected, i.e. acquisition target product copper nanoparticle.
Further, the molar ratio of the adjuvant and the soluble copper salt is 1.5~3.Adjuvant and soluble copper
The ratio of salt is an important factor for influencing product component: the dosage of adjuvant is excessively high, and the product of generation is CuO；The use of adjuvant
Measure too low, the product of generation is Cu and Cu2The mixture of O.
Further, the additional amount of deionized water is not strict with, when not influencing product morphology, but reacting for quickening
Between, deionized water dosage guarantees dissolution.
Further, the filtering can be formed using arbitrary filtering, and such as the present invention is easy to operate, using filter paper
It is filtered.
Further, the soluble copper salt is copper nitrate, copper sulphate, copper chloride or cupric phosphate.
Further, the adjuvant is glycine, urea, citric acid or thiocarbamide.
Gained copper nanoparticle of the invention is Nanoparticulate, partial size in 50~400nm,.
The beneficial effects of the present invention are embodied in:
1, the present invention uses soluble copper salt and adjuvant for raw material, prepares copper nanoparticle, raw material by single step reaction
Simply, process is short, at low cost, the reaction time only need more than ten seconds, reaction initiation temperature it is low, be suitble to large-scale production.
2, method of the invention can control the reaction process of preparation, and then control by the type and proportion of control raw material
The pattern and partial size of powder processed.
3, in method of the invention, related chemical reaction can be completed in a very short period of time and generate a large amount of go back
Originality gas, such as CO, NO, these gases hinder directly contacting for reactant and oxygen, are conducive to copper ion and are reduced into receive
Rice copper particle a, so that step prepares nano metal powder in air atmosphere；Meanwhile the quick release of bulk gas is by nanometer
Copper powder is taken out of to form flue dust, hinders nano-powder and reunites and grow up because caused by specific surface energy is big, to ensure that nanometer
Powder has dispersibility well.
4, method products therefrom purity is high of the invention, high surface activity, large specific surface area, good dispersion.
Detailed description of the invention
Fig. 1 is the TEM photo of gained 2 copper nanoparticle of sample in embodiment 1；
Fig. 2 is the XRD spectrum of products therefrom under different ratio in embodiment 1.
Specific embodiment
It elaborates with reference to the accompanying drawing to the embodiment of the present invention, following embodiments are being with technical solution of the present invention
Under the premise of implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to
Following embodiments.
Embodiment 1: the comparison of products therefrom under different ratio
The present embodiment is with nitrate trihydrate copper (Cu (NO3)2)·3H2O and glycine are raw material, are compared under different ratios of raw materials
The pattern of products therefrom:
Respectively according to adjuvant glycine and soluble copper salt nitrate trihydrate copper (Cu (NO3)2)·3H2The molar ratio of O be 1,
1.5,2,3,3.5, weigh 0.1mol nitrate trihydrate copper (Cu (NO3)2)·3H2O, and the glycine of corresponding mole, then will be former
Material plus deionized water dissolving are simultaneously uniformly mixed, and obtain mixed liquor；Mixed liquor is heated to 230 DEG C, constant temperature, in heating and constant temperature mistake
Deionized water is gradually evaporated in journey, and mixed liquor is made to be concentrated into jelly, and then the more than ten seconds time after water evaporation is sent out rapidly
Violent redox reaction has been given birth to, volume of smoke is released；It collects released flue dust and is filtered by filter paper, that is, obtain
Target product copper nanoparticle is obtained, the sample for being 1,1.5,2,3,3.5 corresponding to the molar ratio of adjuvant and soluble copper salt is distinguished
It is denoted as sample 1, sample 1.5, sample 2, sample 3, sample 3.5.
Transmission electron microscope observing is carried out to the pattern of gained each sample, Fig. 2 is the TEM photo of sample 2.Through characterizing, each sample
All pattern is uniform, is in Nanoparticulate, and surface area is big, good dispersion.And sample 1, sample 1.5, sample 2, sample 3, sample 3.5
Diameter respectively in 90nm or so, 110nm or so, 60nm or so, 200nm or so, 260nm or so, thus, it is possible to find out, lead to
The proportion for crossing regulation raw material, can control the pattern and partial size of powder product.
XRD characterization is carried out to gained each sample, partial results are as shown in Fig. 2, the ingredient of sample 1 is Cu and Cu2The mixing of O
Object, sample 3.5 ingredient be CuO, and the ingredient of sample 1.5, sample 2, sample 3 be pure Cu.As can be seen that adjuvant with can
The ratio of dissolubility mantoquita is an important factor for influencing product component, and the dosage of adjuvant is excessively high or too low, can not all obtain pure
The copper nanoparticle of phase.
Embodiment 2: the comparison of products therefrom under variety classes raw material
The present embodiment prepares copper nanoparticle by the identical method of embodiment 1, and the molar ratio of adjuvant and soluble copper salt is
2, difference is only that: selected adjuvant is respectively the glycine and urea, citric acid, thiocarbamide of embodiment 1, and gained sample is successively marked
It is denoted as sample A, sample B, sample C and sample D.
Transmission electron microscope observing is carried out to the pattern of gained each sample, the results showed that each sample all patterns are uniform, are in nanometer
Granular, surface area is big, good dispersion.And sample A, sample B, sample C and sample D diameter respectively on the left side 65nm or so, 80nm
Right, 75nm or so, 100nm or so, by regulating and controlling the type of raw material, can control the pattern of powder product thus, it is possible to find out
And partial size.
XRD characterization is carried out to gained each sample, the results showed that each sample is all the copper nanoparticle of high-purity.
The above is only exemplary embodiment of the present invention, are not intended to limit the invention, all in spirit of the invention
With any modifications, equivalent replacements, and improvements made within principle etc., should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of method for quickly preparing copper nanoparticle, it is characterised in that: use soluble copper salt and adjuvant for raw material, add
Ionized water is dissolved and is uniformly mixed, and obtains mixed liquor；The mixed liquor is heated to 200~300 DEG C, constant temperature, in heating and perseverance
Deionized water is gradually evaporated during temperature, and mixed liquor is made to be concentrated into jelly, and redox reaction then occurs rapidly, is generated also
Copper ion is simultaneously reduced to copper nanoparticle by originality gas, and copper nanoparticle is wrapped to form flue dust by the gas generated；Collection is released
The flue dust of releasing and filtering, i.e. acquisition target product copper nanoparticle.
2. it is according to claim 1 quickly prepare copper nanoparticle method, it is characterised in that: the adjuvant and it is described can
The molar ratio of dissolubility mantoquita is 1.5~3.
3. the method according to claim 1 or 2 for quickly preparing copper nanoparticle, it is characterised in that: the soluble copper
Salt is copper nitrate, copper sulphate, copper chloride or cupric phosphate.
4. the method according to claim 1 or 2 for quickly preparing copper nanoparticle, it is characterised in that: the adjuvant is
Glycine, urea, citric acid or thiocarbamide.
5. the method according to claim 1 or 2 for quickly preparing copper nanoparticle, it is characterised in that: gained copper nanoparticle is
Nanoparticulate, partial size is in 50~400nm.
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| CN201811267219.2A CN109047792A (en) | 2018-10-29 | 2018-10-29 | A method of quickly preparing copper nanoparticle |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100242680A1 (en) * | 2006-04-18 | 2010-09-30 | Chemnano, Inc. | Process of manufacturing nano-scale powders |
| CN103145198A (en) * | 2013-03-08 | 2013-06-12 | 南昌大学 | Method for producing nanometer structure cobalt tetroxide sub-micron hollow balls |
| CN105798320A (en) * | 2014-12-31 | 2016-07-27 | 中国科学院化学研究所 | Method for preparing nanometer copper powder at low temperature |
| CN106424751A (en) * | 2016-11-18 | 2017-02-22 | 南昌大学 | Preparation method of nano copper powder |
| CN106513696A (en) * | 2015-09-09 | 2017-03-22 | 广州千顺工业材料有限公司 | Micro-nano copper powder and preparation method thereof |
| WO2017143978A1 (en) * | 2016-02-22 | 2017-08-31 | The University Of Hong Kong | Method of producing a porous crystalline material with a highly uniform structure |
-
2018
- 2018-10-29 CN CN201811267219.2A patent/CN109047792A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100242680A1 (en) * | 2006-04-18 | 2010-09-30 | Chemnano, Inc. | Process of manufacturing nano-scale powders |
| CN103145198A (en) * | 2013-03-08 | 2013-06-12 | 南昌大学 | Method for producing nanometer structure cobalt tetroxide sub-micron hollow balls |
| CN105798320A (en) * | 2014-12-31 | 2016-07-27 | 中国科学院化学研究所 | Method for preparing nanometer copper powder at low temperature |
| CN106513696A (en) * | 2015-09-09 | 2017-03-22 | 广州千顺工业材料有限公司 | Micro-nano copper powder and preparation method thereof |
| WO2017143978A1 (en) * | 2016-02-22 | 2017-08-31 | The University Of Hong Kong | Method of producing a porous crystalline material with a highly uniform structure |
| CN106424751A (en) * | 2016-11-18 | 2017-02-22 | 南昌大学 | Preparation method of nano copper powder |
Non-Patent Citations (1)
| Title |
|---|
| A. KUMAR等: "Solution Combustion Synthesis of Metal Nanopowders: Copper and Copper/Nickel Alloys", 《REACTORS, KINETICS, AND CATALYSIS》 * |
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Application publication date: 20181221 |