CN107931600B - A kind of method of cysteine-modifying copper nano-particle - Google Patents
A kind of method of cysteine-modifying copper nano-particle Download PDFInfo
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- CN107931600B CN107931600B CN201711229994.4A CN201711229994A CN107931600B CN 107931600 B CN107931600 B CN 107931600B CN 201711229994 A CN201711229994 A CN 201711229994A CN 107931600 B CN107931600 B CN 107931600B
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
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Abstract
The invention belongs to chemical material technical fields, a kind of method for specifically disclosing cysteine-modifying copper nano-particle includes the following steps: (1) ingredient: preparing the raw material of following mass fraction: 129.9-173.2 parts of toluene, 40-60 parts of sour water compound, 100-200 parts of copper nanoparticle, 118.3-236.7 parts of ethyl alcohol；(2) it mixes: sour water compound is dissolved in toluene；(3) oil bath: the mixture oil bath heating 3-4h in step (2) obtains oligomer polyamide-L-cysteine ligand；(4) modified: in ethanol by copper nanoparticle dispersion, ligand obtained in step (3) to be added and stirs 2-3h, so that it is carried out surface to nanometer copper particle modified, form the alcohol suspension of Nanometer Copper；(5) volatilize: the alcohol suspension of Nanometer Copper obtained, which is put into draught cupboard, in step (4) makes ethyl alcohol volatilize；(6) it dries；(7) it crushes.Improve stability and dispersibility of the copper nanoparticle in polyamide based material.
Description
Technical field
The present invention relates to chemical technology fields, and in particular to a kind of method of cysteine-modifying copper nano-particle.
Background technique
Dielectric material is also known as dielectric, is the insulating materials of electricity, requires material mainly for the manufacture of capacitors dielectrics
Resistivity it is high, dielectric constant is big.There are many dielectric material type, and important has rutile porcelain, the combined oxidation containing titanium dioxide
Object ceramics, such as calcium titanate, magnesium titanate, barium titanate.
With the development that electronic equipment in recent years is with rapid changepl. never-ending changes and improvements, widely used capacitor to high energy storage, miniaturization and
Environmentally friendly direction is developed.Although ceramic dielectric material has very excellent dielectric properties, multi-layer ceramics electricity
Container needs screen electrode to carry out cofiring in the fabrication process, and energy consumption is big, complex process, and the flexibility of this dielectric material
Difference, when being subjected to mechanical impact or violent temperature change, there may be crackles, affect the use of capacitor.In polymer
Middle that a small amount of conducting particles is added to the percolation threshold close to material, can increase sharply its dielectric constant.
Copper powder have good electric conductivity and price on advantage, but with conventional precious metal electrode material, compared with there are one
A obvious disadvantage, superfine cupper powder are easily oxidized, and partial size is smaller more oxidizable, in sky under the copper powder room temperature greater than 500nm
It can be stabilized in gas, and the copper powder less than 500nm can aoxidize in air, be easier to be oxidized at high temperature.Improve copper
The antioxidative main path of powder is the surface coating modification of copper powder, i.e., copper powder is coated one layer of other substance, protects copper powder
Not oxidized during the sintering process, copper powder interconnects to form an entirety after sintering.Common method of modifying is by copper powder
One layer of silver is coated, such metal powder had not only had good electric conductivity but also inoxidizability with higher, and higher cost, changed
Performance after property is also not satisfactory.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of cysteine-modifying copper nano-particle, change made from this method
Property copper nanoparticle improves stability and dispersibility in polyamide based material.
In order to achieve the above objectives, base case of the invention is as follows: a kind of method of cysteine-modifying copper nano-particle,
Include the following steps:
(1) ingredient: prepare the raw material of following mass fraction: 130-175 parts of toluene, 40-60 parts of sour water compound, Nanometer Copper
100-200 parts of powder, 125-245 parts of ethyl alcohol, wherein sour water compound is L-cysteine, oligomeric polyamide, to toluic acid sour water
Compound, wherein L-cysteine, oligomeric polyamide, be 1:1:1.1-1.3 to the molar ratio of toluic acid sour water compound；
(2) it mixes: sour water compound being dissolved in toluene, mixture is obtained；
(3) oil bath: the mixture oil bath heating 3-4h in step (2) obtains oligomer polyamide-L-cysteine and matches
Body；
(4) modified: in ethanol by copper nanoparticle dispersion, ligand obtained in step (3) to be added and stirs 2-3h, makes it
Surface is carried out to nanometer copper particle to be modified, and forms the alcohol suspension of Nanometer Copper；
(5) volatilize: the alcohol suspension of Nanometer Copper obtained, which is put into draught cupboard, in step (4) makes ethyl alcohol volatilize；
(6) it dries: product obtained in step (5) being dried, blocky modified Nano copper is obtained；
(7) it crushes；Blocky modified Nano copper powder in step (6) is broken, obtain powdered modified Nanometer Copper.
This base case has the beneficial effect that: material adds function performance when overcoming big composite material economize on electricity loss, height filling
The disadvantages of poor, prepares the high-dielectric composite material of low-dielectric loss, controllable percolation threshold, good weatherability properties energy.
Preferred embodiment one: including the original of following mass fraction as the preferred embodiment of basic scheme, in the step (1)
Material: 120-175 parts of toluene, 50 parts of sour water compound, 100-200 parts of copper nanoparticle, 125-245 parts of ethyl alcohol.Inventor passes through examination
It issues after examination and approval now, material property made from the raw material of above-mentioned mass fraction is preferable.
Preferred embodiment two: preferably one preferred embodiment, oil bath temperature is 130-150 DEG C in step (3).Invention
People is found by experiment that material property made from above-mentioned oil bath temperature is preferable.
Preferred embodiment three: preferably one preferred embodiment, oil bath temperature is 140 DEG C in step (3).Inventor is logical
Overtesting finds that material property made from above-mentioned oil bath temperature is preferable.
Preferred embodiment four: preferably and or preferred embodiment three preferred embodiment, the drying in step (6) is to place
5-8h is dried in vacuum drying oven, drying temperature is 60-80 DEG C.Inventor is found by experiment that, made from above-mentioned drying temperature
Material property is preferable.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail:
A kind of method of cysteine-modifying copper nano-particle, includes the following steps:
(1) ingredient: prepare the raw material of following mass fraction: toluene 170ml, sour water compound 50g, copper nanoparticle 150g,
Ethyl alcohol 220ml, wherein sour water compound is L-cysteine, oligomeric polyamide, to toluic acid sour water compound, wherein half Guang of L-
Propylhomoserin, oligomeric polyamide are 1:1:1.1-1.3 to the molar ratio of toluic acid sour water compound；
(2) it mixes: sour water compound being dissolved in toluene, mixture is obtained；
(3) oil bath: the mixture oil bath heating 3-4h in step (2), oil bath temperature are 140 DEG C, obtain oligomer polyamides
Amine-L-cysteine ligand；
(4) modified: in ethanol by copper nanoparticle dispersion, ligand obtained in step (3) to be added and stirs 2-3h, makes it
Surface is carried out to nanometer copper particle to be modified, and forms the alcohol suspension of Nanometer Copper；
(5) volatilize: the alcohol suspension of Nanometer Copper obtained, which is put into draught cupboard, in step (4) makes ethyl alcohol volatilize；
(6) it dries: obtained be placed in vacuum drying oven in step (5) is dried into 5-8h, drying temperature is 60-80 DEG C,
Obtain blocky modified Nano copper；
(7) it crushes；Blocky modified Nano copper powder in step (6) is broken, obtain powdered modified Nanometer Copper.
The data of other embodiments are as shown in table 1:
Table 1
The performance indicator of modified copper powder and existing modified copper powder as made from above-mentioned preparation method is compared such as 2 institute of table
Show:
Table 2
The performance pair of high-dielectric composite material and existing composite material that the modified Nano copper made from this programme is made
Than as shown in table 3:
Table 3
As can be seen from the above table, when the modified Nano copper powder in the application overcomes big composite material economize on electricity loss, height filling
The disadvantages of material adds function performance poor, prepares the high dielectric of low-dielectric loss, controllable percolation threshold, good weatherability properties energy.
What has been described above is only an embodiment of the present invention, and the common sense such as well known characteristic do not describe excessively herein in scheme.
It should be pointed out that for those skilled in the art, under the premise of not departing from the present invention, can also make several deformations and
It improves, these also should be considered as protection scope of the present invention, these all will not influence the reality of effect and patent that the present invention is implemented
The property used.The scope of protection required by this application should be based on the content of the claims, the specific embodiment etc. in specification
Record the content that can be used for explaining claim.
Claims (5)
1. a kind of method of cysteine-modifying copper nano-particle, characterized by the following steps:
(1) ingredient: prepare the raw material of following mass fraction: 129.9-173.2 parts of toluene, 40-60 parts of sour water compound, Nanometer Copper
100-200 parts of powder, 118.3-236.7 parts of ethyl alcohol, wherein sour water compound is L-cysteine, oligomeric polyamide, to toluic acid
Sour water compound, wherein L-cysteine, oligomeric polyamide, be 1:1:1.1-1.3 to the molar ratio of toluic acid sour water compound；
(2) it mixes: sour water compound being dissolved in toluene, mixture is obtained；
(3) oil bath: the mixture oil bath heating 3-4h in step (2) obtains oligomer polyamide-L-cysteine ligand；
(4) modified: in ethanol by copper nanoparticle dispersion, ligand obtained in step (3) to be added and stirs 2-3h, make it to receiving
Rice copper particle carries out surface and is modified, and forms the alcohol suspension of Nanometer Copper；
(5) volatilize: the alcohol suspension of Nanometer Copper obtained, which is put into draught cupboard, in step (4) makes ethyl alcohol volatilize；
(6) it dries: product obtained in step (5) being dried, blocky modified Nano copper is obtained；
(7) it crushes；Blocky modified Nano copper powder in step (6) is broken, obtain powdered modified Nanometer Copper.
2. a kind of method of cysteine-modifying copper nano-particle according to claim 1, it is characterised in that: the step
It (1) include the raw material of following mass fraction: 129.9-173.2 parts of toluene, 50 parts of sour water compound, copper nanoparticle 100-200 in
Part, 118.3-236.7 parts of ethyl alcohol.
3. a kind of method of cysteine-modifying copper nano-particle according to claim 2, it is characterised in that: step (3)
Middle oil bath temperature is 130-150 DEG C.
4. a kind of method of cysteine-modifying copper nano-particle according to claim 2, it is characterised in that: step (3)
Middle oil bath temperature is 140 DEG C.
5. a kind of method of cysteine-modifying copper nano-particle according to claim 3 or 4, it is characterised in that: step
(6) drying in, which is located in vacuum drying oven, dries 5-8h, and drying temperature is 60-80 DEG C.
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| CN112126251A (en) * | 2020-09-29 | 2020-12-25 | 镇江强龙新材料科技有限公司 | Preparation method and application of chelating functional nano-silver |
| CN113441711A (en) * | 2021-06-02 | 2021-09-28 | 清远市进田企业有限公司 | High-conductivity high-weather-resistance modified nano-copper process |
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| CN101887767A (en) * | 2010-06-11 | 2010-11-17 | 山东大学 | Method for preparing conductive paste by taking copper powder with surface coverage silver nanostructures as packing |
| CN102416468A (en) * | 2011-11-21 | 2012-04-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nano metal leaf and preparation method thereof |
| CN103540311A (en) * | 2013-10-15 | 2014-01-29 | 上海大学 | Synthetic method of cysteine modified rare earth up-conversion luminescent nanocrystallines |
| CN103608139A (en) * | 2011-02-03 | 2014-02-26 | 美塔罗治疗有限公司 | Surface-modified heavy metal nanoparticles, compositions and uses thereof |
| CN104716311A (en) * | 2015-02-11 | 2015-06-17 | 深圳新宙邦科技股份有限公司 | Tin bisulfide nanosheet composite material, as well as preparation method and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20120055211A (en) * | 2010-11-23 | 2012-05-31 | 한국전자통신연구원 | Method of forming nanowire porous media and the media formed by the method |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101887767A (en) * | 2010-06-11 | 2010-11-17 | 山东大学 | Method for preparing conductive paste by taking copper powder with surface coverage silver nanostructures as packing |
| CN103608139A (en) * | 2011-02-03 | 2014-02-26 | 美塔罗治疗有限公司 | Surface-modified heavy metal nanoparticles, compositions and uses thereof |
| CN102416468A (en) * | 2011-11-21 | 2012-04-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nano metal leaf and preparation method thereof |
| CN103540311A (en) * | 2013-10-15 | 2014-01-29 | 上海大学 | Synthetic method of cysteine modified rare earth up-conversion luminescent nanocrystallines |
| CN104716311A (en) * | 2015-02-11 | 2015-06-17 | 深圳新宙邦科技股份有限公司 | Tin bisulfide nanosheet composite material, as well as preparation method and application thereof |
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Effective date of registration: 20220729 Address after: 511500 first floor of H01, 1st-3rd floor, headquarters building, Tianan Zhigu science and Technology Industrial Park, No. 18, Chuangxing Avenue, high tech Industrial Development Zone, Qingyuan City, Guangdong Province Patentee after: GUANGDONG JUHANG INSTITUTE FOR ADVANCED MATERIALS Co.,Ltd. Address before: 511500 No.19, Tianan Zhigu Exhibition Center, No.18, Chuangxing Avenue, science and Technology Innovation Park, Qingyuan high tech Industrial Development Zone, Guangdong Province Patentee before: GUANGDONG JUHANG INSTITUTE FOR ADVANCED MATERIALS Co.,Ltd. Patentee before: GUANGDONG NANFANG ZHI QUAN PLASTIC TECHNOLOGY Co.,Ltd. |