CN103476524B - Manufacture the method for the metal nanoparticle with nucleocapsid structure with oxidative stability - Google Patents
Manufacture the method for the metal nanoparticle with nucleocapsid structure with oxidative stability Download PDFInfo
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- CN103476524B CN103476524B CN201280018257.9A CN201280018257A CN103476524B CN 103476524 B CN103476524 B CN 103476524B CN 201280018257 A CN201280018257 A CN 201280018257A CN 103476524 B CN103476524 B CN 103476524B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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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
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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
- B22F1/17—Metallic particles coated with metal
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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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
- B22F2202/00—Treatment under specific physical conditions
- B22F2202/11—Use of irradiation
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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
An aspect of of the present present invention relates to a kind of method that manufacture has the metal nanoparticle with nucleocapsid structure of good oxidation stability, and wherein said method comprises the steps: to heat and stirs core metal precursor solutions; By shell metal precursor solutions with through heating and the core metal precursor solutions stirred mix, and heat and the metal precursor solutions that is uniformly mixed; And utilize radioactive rays to through heating and the metal precursor solutions stirred irradiate. Thus, due to by not using the simple and eco-friendly technique of chemical reducing agent can make maximize yields, so not needing the technique that the reductive agent added removes, and because not carrying out the postheat treatment of particle, institute so that described manufacturing process simply and highly economical.
Description
Technical field
The present invention relates to a kind of method that manufacture has the metal nanoparticle with nucleocapsid structure of excellent oxidation stability.
Background technology
There is the method that multiple manufacture has the metal nanoparticle of nucleocapsid structure. Mainly use with the use of chemical reduction method or the method being manufactured metal nanoparticle by physical sepn big piece of (bulk) metallics.
In order to manufacture metal nanoparticle, it is possible to use utilize the chemical reduction method of chemical reducing agent or the wireless plating technology by changing the reduction potential of metal precursor solutions and synthetic metals nanoparticle. Herein, chemical reducing agent can comprise hydrazine, alcohol, tensio-active agent, citric acid etc. Above-mentioned chemical reducing agent can be used from metal ion or organometallic compound reducing metal, and thus synthesis has the metal nanoparticle of nucleocapsid structure and/or has the metal nanoparticle of alloy structure. This kind of chemosynthesis of the metal nanoparticle of chemical reduction method is used to make to manufacture uniform metal nanoparticle; But, the gathering of metal nanoparticle is tended to extremely strong, thus requires postheat treatment. In addition, owing to using harmful a large amount of reductive agents, so also needing the technique processed by the reductive agent of residual after reacting.
Except chemical reduction method, the synthesis of metal nanoparticle can also comprise: in high temperature, high pressure or the method for synthetic metals nanoparticle under the particular atmosphere that realizes by control synthesis atmosphere; With the method using physical force that bulk metal particle carries out physical sepn. These methods can contribute to manufacturing the nanoparticle of various metal component; But, understand poly-doped impurity and expensive equipment can be needed.
In order to address these problems, ray can be utilized to be irradiated by metal precursor solutions, it is possible to the free radical produced in solution is used for reducing metal precursor.
But, as the result of experiment, useful to irradiation of rays is not enough to guarantee to have the oxidative stability of the metal nanoparticle of nucleocapsid structure. Therefore, urgent needs is studied except using the irradiation of ray to manufacture metal nanoparticle, also improves new departure of the oxidative stability of metal nanoparticle.
Summary of the invention
Technical problem
The aspect of the present invention provides a kind of method being manufactured the metal nanoparticle with nucleocapsid structure with excellent oxidation stability when not using chemical reducing agent by useful to irradiation of rays.
Technical scheme
According to aspects of the present invention, it is provided that a kind of manufacture has the method for the metal nanoparticle with nucleocapsid structure of excellent oxidation stability, and described method comprises: heat and stir core metal precursor solutions; By through heating and the core metal precursor solutions stirred mix with shell metal precursor solutions, and heat and the metal precursor solutions that is uniformly mixed; And utilize ray to through heating and the metal precursor solutions stirred irradiate.
At 30 DEG C��300 DEG C, described core metal precursor solutions can be heated and stir 10��120 minutes.
At 30 DEG C��300 DEG C, the metal precursor solutions of described mixing can be heated and stir 10��120 minutes.
Described ray can comprise one or more rays being selected from electron beam ray, X-ray and gamma-rays, and described ray can have the absorption dose of 10kGy��500kGy.
Described core metal precursor solutions can comprise the ion being selected from one or more following metals: gold and silver, copper, platinum, nickel, zinc, palladium, rhodium, ruthenium, iridium, osmium, tungsten, tantalum, titanium, aluminium, cobalt and iron.
Described core metal precursor solutions can comprise decorating molecule (cappingmolecules).
Described decorating molecule can comprise and is selected from one or more following compounds: the compound with thiol, the compound with carboxyl and have the compound of amido.
Described decorating molecule can comprise and is selected from one or more following compounds with amido: propylamine, butylamine, octylame, decyl amine, n-Laurylamine, cetylamine and oil amine.
Described shell metal precursor solutions can comprise the ion being selected from one or more following metals: gold and silver, copper, platinum, nickel, zinc, palladium, rhodium, ruthenium, iridium, osmium, tungsten, tantalum, titanium, aluminium, cobalt and iron.
The metal being included in described shell metal precursor solutions can have the degree of oxidation lower than the metal being included in described core metal precursor solutions.
Useful effect
According to aspects of the present invention, the method of the metal nanoparticle that a kind of manufacture has nucleocapsid structure is provided, described method makes due to the manufacturing process of simplification to improve and manufactures receipts rate and reduce manufacturing cost, namely the manufacturing process of described simplification does not use the environmentally friendly technology of chemical reducing agent, and it does not need the technique and the postheat treatment that remove the reductive agent of residual.
Especially, owing to utilizing ray to be irradiated by metal precursor solutions after the heat treatment, it is possible to improve the oxidative stability of metal nanoparticle further.
Accompanying drawing explanation
Fig. 1 shows the image of the copper-galactic nucleus-core/shell nanoparticles of the concept embodiment of the present invention analyzed by high resolution transmission electron microscope (HR-TEM);
Fig. 2 shows Elemental redistribution (mapping) image of the copper-galactic nucleus-core/shell nanoparticles of concept embodiment of the present invention;
Fig. 3 shows the spectroscopic analysis result of the energy-dispersive spectroscopy (EDS) of the copper-galactic nucleus-core/shell nanoparticles of concept embodiment of the present invention;
Fig. 4��Fig. 7 shows the element distribution analysis result of the copper-galactic nucleus-core/shell nanoparticles of the concept embodiment of the present invention with the use of angle of elevation annular details in a play not acted out on stage, but told through dialogues scanning transmission electron microscope (HAADF-STEM);
Fig. 8 shows X-ray diffraction (XRD) analytical results of 70 weeks of the copper-galactic nucleus-core/shell nanoparticles of concept embodiment of the present invention;
Fig. 9 shows the element distribution image of the copper-Nano silver grain of comparative example 1;
Figure 10 shows the EDS spectroscopic analysis result of the copper-Nano silver grain of comparative example 1;
Figure 11 shows the image of the copper-Nano silver grain of the comparative example 2 analyzed by HR-TEM; And
Figure 12 shows the EDS spectroscopic analysis result of the copper-Nano silver grain of comparative example 2.
Embodiment
Embodiment according to concept of the present invention, the method manufacturing the metal nanoparticle with nucleocapsid structure with excellent oxidation stability can comprise: heats and stirs core metal precursor solutions; By through heating and the core metal precursor solutions stirred mix with shell metal precursor solutions, and heat and the metal precursor solutions that is uniformly mixed; And utilize ray to through heating and the metal precursor solutions stirred irradiate.
First, according to the embodiment of concept of the present invention, by utilizing ray metal precursor solutions irradiated and the reduction of described precursor can be manufactured the metal nanoparticle with nucleocapsid structure. But, as the result of experiment, this kind of radiation exposure method can provide metal nanoparticle when not having chemical additive or environmental problem, but described method is not enough to guarantee the oxidative stability of metal nanoparticle.
Therefore, in order to guarantee the oxidative stability of metal nanoparticle, heating and the stirring of core metal precursor solutions can be carried out in advance, then core metal precursor solutions and shell metal precursor solutions be mixed mutually and again its mixture heated and stir.
After core metal precursor solutions and shell metal precursor solutions are mixed mutually, it is heated and when stirring, the metal being included in core metal precursor solutions and the metal alloy being included in shell metal precursor solutions, thus cause manufacturing the metal nanoparticle with nucleocapsid structure.
Not implementing in heat treated situation, the nanoparticle in shell has hole so that they contact air by hole, and thus hole can be easy to oxidized. When metal precursor solutions is heat-treated the fusing point so that its temperature to be increased to shell, the nanoparticle in shell can melt and encapsulate hole completely, thus prevents from completely being easy to oxidized hole and air contact, thus can improve oxidative stability.
Therefore, when being heated by metal precursor solutions and stir and then utilize ray to irradiate, the metal nanoparticle with nucleocapsid structure can realize higher oxidative stability.
When heating and stir core metal precursor solutions, it is possible to be 30 DEG C��300 DEG C by heating and temperature control. When Heating temperature is lower than 30 DEG C, guarantee that the effect of oxidative stability can be not obvious by thermal treatment. When Heating temperature is more than 300 DEG C, alloying can be there is, thus cause manufacturing the decline of receipts rate.
In order to manufacture uniform core-shell structure copolymer nanoparticle, it is necessary to core metal precursor solutions is steadily stirred. In order to make it possible to realize it, it is necessary to stirring technique is carried out the predetermined time cycle. Churning time can be controlled to 10��120 minutes. When churning time is shorter than 10 minutes, it may be difficult to obtain enough homogeneities. When churning time was more than 120 minutes, can affect unfavorablely manufacture receipts rate.
Then, it is possible to by through heating and the core metal precursor solutions stirred mix with shell metal precursor solutions. Thereafter, it is possible to again the mixture of core metal precursor solutions and shell metal precursor solutions is heated and stir. Herein, when the temperature of mixture is increased to the fusing point of shell, the nanoparticle in shell can melt and encapsulate core completely, thus prevents from completely being easy to oxidized core and air contact, thus can improve oxidative stability.
When mixture being heated after core metal precursor solutions is mixed mutually with shell metal precursor solutions and stir, it is possible to be 30 DEG C��300 DEG C by heating and temperature control. When Heating temperature is lower than 30 DEG C, guarantee that the effect of oxidative stability can be not obvious by thermal treatment. When Heating temperature is more than 300 DEG C, alloying can be there is, thus cause manufacturing the decline of receipts rate.
In order to manufacture uniform core-shell structure copolymer nanoparticle, it is necessary to the metal precursor solutions of mixing is steadily stirred. In order to make it possible to realize it, it is necessary to stirring technique is carried out the predetermined time cycle. Churning time can be controlled to 10��120 minutes. When churning time is shorter than 10 minutes, it may be difficult to obtain enough homogeneities. When churning time was more than 120 minutes, can affect unfavorablely manufacture receipts rate.
Thereafter, it is possible to use ray to through heating and the metal precursor solutions stirred irradiate. Herein, ray can comprise and is selected from electron beam ray, X-ray and one or more rays gamma-ray. In addition, it is possible to implement the irradiation of ray by the absorption dose of ray is controlled to 10kGy��500kGy. Useful to irradiation of rays is intended to reduce precursor solution. When absorption dose is less than 10kGy, reducing process may be not enough to suitably form metal nanoparticle. When absorption dose is more than 500kGy, the size of the nanoparticle of manufacture can improve and core and shell may separately be formed, and thus can deteriorate the performance of nanoparticle. Thus it is contemplated that to the size of nanoparticle, it is possible to energy and absorption dose thereof to ray suitably control.
Herein, core metal precursor solutions can comprise the ion being selected from one or more following metals: gold and silver, copper, platinum, nickel, zinc, palladium, rhodium, ruthenium, iridium, osmium, tungsten, tantalum, titanium, aluminium, cobalt and iron.
In addition, shell metal precursor solutions can comprise the ion being selected from one or more following metals: gold and silver, copper, platinum, nickel, zinc, palladium, rhodium, ruthenium, iridium, osmium, tungsten, tantalum, titanium, aluminium, cobalt and iron.
The metal being included in shell metal precursor solutions can have the degree of oxidation lower than the metal being included in core metal precursor solutions. With the metallographic phase ratio being included in core metal precursor solutions, the metal being included in shell metal precursor solutions forming the shell being used for coated core can be difficult to oxidized relatively, make the gathering between the oxidation that can prevent core metal or metal nanoparticle, thus can guarantee the stability of metal nanoparticle further.
In addition, core metal precursor solutions can also comprise decorating molecule. When mixing to encapsulate nanoparticle with core metal precursor solutions by decorating molecule, compared with the situation that core metal precursor solutions only heat-treats to be formed core, can growing particle on nano level, the stability of metal nanoparticle is favourable by this more stablely.
Herein, decorating molecule can comprise and is selected from one or more following compounds: the compound with thiol, the compound with carboxyl and have the compound of amido.
Decorating molecule can comprise and is selected from following at least one: propylamine, butylamine, octylame, decyl amine, n-Laurylamine, cetylamine and oil amine. The compound with amido can be used as the most suitable decorating molecule. Especially, it is contemplated that to when carbocyclic ring length increases, can effectively promote the formation of uniform particle, it is possible to preferably by n-Laurylamine, cetylamine and oil amine for the formation of uniform particle.
Hereinafter, with reference to accompanying drawing, the embodiment of concept of the present invention is described in detail. But, the concept of the present invention can carry out illustrating and should not be construed as limited to described specific embodiments herein in many different forms. But, it is provided that these embodiments so that the present invention is by thorough and complete, and passes on the scope of concept of the present invention to the technician of this area completely.
(example)
By acetylacetonate copper (C5H7CuO2) as core metal precursor solutions, and core metal precursor solutions is heated to 100 DEG C and stirs 30 minutes. Then, the silver-colored precursor solution as shell metal precursor solutions is mixed with it, and mixture is heated to 50 DEG C and stirs 1 hour. Thereafter, utilize electron beam to be irradiated by mixture when 0.1MeV��20MeV, 0.001mA��50mA and 10kGy��500kGy, thus manufactured copper-galactic nucleus-core/shell nanoparticles.
Figure 1A and 1B shows the image of the copper-galactic nucleus-core/shell nanoparticles of the manufacture analyzed by high resolution transmission electron microscope (HR-TEM). As shown, the surperficial of copper nano-particle utilizing Nano silver grain will have 150nm �� 50nm granularity encapsulates the thickness to 60nm �� 10nm.
In addition, Fig. 2 A��2E shows the element distribution image of the copper-galactic nucleus-core/shell nanoparticles of manufacture. As shown, core and shell do not form alloy; But, the copper nano-particle as core is positioned at inside and the Nano silver grain as shell is arranged in the way of encapsulating copper nano-particle, thus forms nucleocapsid structure.
In addition, Fig. 3 shows the spectroscopic analysis result of the energy-dispersive spectroscopy (EDS) of the copper-galactic nucleus-core/shell nanoparticles of manufacture. As shown, copper and the Nano silver grain of manufacture are not oxidized, thus illustrate excellent oxidative stability.
In addition, Fig. 4��7 show the element distribution analysis result of the copper-galactic nucleus-core/shell nanoparticles of the manufacture with the use of angle of elevation annular details in a play not acted out on stage, but told through dialogues scanning transmission electron microscope (HAADF-STEM). As shown, Nano silver grain encapsulates copper nano-particle completely, thus forms uniform core-shell structure copolymer nanoparticle.
Finally, Fig. 8 shows X-ray diffraction (XRD) analytical results of the copper-galactic nucleus-core/shell nanoparticles of manufacture. As the result of XRD analysis, the copper-Nano silver grain of manufacture is identified as the unoxidized copper-Nano silver grain with face-centered cubic (FCC) crystalline network, and does not produce oxidation peak in the Measuring Time of 70 weeks. By useful to irradiation of rays after being heat-treated by precursor solution, unoxidized copper-Nano silver grain achieves excellent oxidative stability.
(comparative example 1)
By acetylacetonate copper (C5H7CuO2) as core metal precursor solutions, and core metal precursor solutions is heated to 250 DEG C and stirs 30 minutes. Then, the silver-colored precursor solution as shell metal precursor solutions is mixed with it, and mixture is heated to 25 DEG C and stirs 1 hour. Thereafter, utilize electron beam to be irradiated by mixture when 0.1MeV��20MeV, 0.001mA��50mA and 10kGy��500kGy.
Fig. 9 A��9E shows the element distribution image of the copper-Nano silver grain of manufacture. As shown, the accurate shape of not clear identification copper nano-particle. That is, nucleocapsid structure is not formed.
In addition, Figure 10 shows the EDS spectroscopic analysis result of the copper-Nano silver grain of manufacture. Figure 10 supports the copper shape shown in Fig. 9.
(comparative example 2)
By acetylacetonate copper (C5H7CuO2) as core metal precursor solutions, and core metal precursor solutions is heated to 350 DEG C and stirs 30 minutes. Then, the silver-colored precursor solution as shell metal precursor solutions is mixed with it, and mixture is heated to 350 DEG C and stirs 1 hour. Thereafter, utilize electron beam to be irradiated by mixture when 0.1MeV��20MeV, 0.001mA��50mA and 10kGy��500kGy.
Figure 11 shows the image of the copper-Nano silver grain of the manufacture analyzed by HR-TEM. Figure 11 shows the copper-Nano silver grain with the alloy structure not being nucleocapsid structure.
In addition, Figure 12 shows the EDS spectroscopic analysis result of the copper-Nano silver grain of manufacture. Figure 12 supports the shape of the copper-silver alloy shown in Figure 11.
Claims (10)
1. manufacture has a method for the metal nanoparticle with nucleocapsid structure of oxidative stability, and described method comprises:
Heat and stir core metal precursor solutions;
By through heating and the core metal precursor solutions stirred mix with shell metal precursor solutions, and heat and stir through mixing metal precursor solutions; And
Utilize ray to through heating and the metal precursor solutions stirred irradiate.
2. method according to claim 1, wherein heats described core metal precursor solutions at 30 DEG C��300 DEG C and stirs 10��120 minutes.
3. method according to claim 1, wherein heats the described metal precursor solutions through mixing at 30 DEG C��300 DEG C and stirs 10��120 minutes.
4. method according to claim 1, wherein said ray comprises one or more rays being selected from electron beam ray, X-ray and gamma-rays, and
Described ray has the absorption dose of 10kGy��500kGy.
5. method according to claim 1, wherein said core metal precursor solutions comprises the ion being selected from one or more following metals: gold and silver, copper, platinum, nickel, zinc, palladium, rhodium, ruthenium, iridium, osmium, tungsten, tantalum, titanium, aluminium, cobalt and iron.
6. method according to claim 1, wherein said core metal precursor solutions comprises decorating molecule.
7. method according to claim 6, wherein said decorating molecule comprises and is selected from one or more following compounds: the compound with thiol, the compound with carboxyl and have the compound of amido.
8. method according to claim 6, wherein said decorating molecule comprises and is selected from one or more following compounds with amido: propylamine, butylamine, octylame, decyl amine, n-Laurylamine, cetylamine and oil amine.
9. method according to claim 1, wherein said shell metal precursor solutions comprises the ion being selected from one or more following metals: gold and silver, copper, platinum, nickel, zinc, palladium, rhodium, ruthenium, iridium, osmium, tungsten, tantalum, titanium, aluminium, cobalt and iron.
10. method according to claim 1, the degree of oxidation of the metal being wherein included in described shell metal precursor solutions is lower than the degree of oxidation of the metal being included in described core metal precursor solutions.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020110033755A KR101329081B1 (en) | 2011-04-12 | 2011-04-12 | Method for manufacturing metal nanoparticle of core-shell structure having excellent oxidation stability |
| KR10-2011-0033755 | 2011-04-12 | ||
| PCT/KR2012/002225 WO2012141439A2 (en) | 2011-04-12 | 2012-03-27 | Method for manufacturing metal nanoparticles having a core-shell structure with good oxidation stability |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103476524A CN103476524A (en) | 2013-12-25 |
| CN103476524B true CN103476524B (en) | 2016-06-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201280018257.9A Expired - Fee Related CN103476524B (en) | 2011-04-12 | 2012-03-27 | Manufacture the method for the metal nanoparticle with nucleocapsid structure with oxidative stability |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US20140020508A1 (en) |
| JP (1) | JP2014514451A (en) |
| KR (1) | KR101329081B1 (en) |
| CN (1) | CN103476524B (en) |
| DE (1) | DE112012001664T5 (en) |
| WO (1) | WO2012141439A2 (en) |
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| KR20140058893A (en) * | 2012-11-07 | 2014-05-15 | 삼성정밀화학 주식회사 | Method of preparing nano particles having core-shell structure and nano particles prepared from the same |
| CN104190919B (en) * | 2014-09-01 | 2017-05-17 | 中国科学院长春应用化学研究所 | Platinum nano particle and preparation method thereof |
| CN104985193A (en) * | 2015-07-24 | 2015-10-21 | 天津大学 | Alloy nano-particle preparation method based on protein reduction method |
| CN106378448B (en) * | 2016-09-20 | 2019-03-19 | 杨海波 | A kind of nickel powder silver clad surface for circuit brake material is modified |
| CN109093110B (en) * | 2017-06-20 | 2021-09-07 | 华邦电子股份有限公司 | Composite material and method for producing same |
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2011
- 2011-04-12 KR KR1020110033755A patent/KR101329081B1/en active IP Right Grant
-
2012
- 2012-03-27 DE DE112012001664.5T patent/DE112012001664T5/en not_active Withdrawn
- 2012-03-27 CN CN201280018257.9A patent/CN103476524B/en not_active Expired - Fee Related
- 2012-03-27 WO PCT/KR2012/002225 patent/WO2012141439A2/en active Application Filing
- 2012-03-27 JP JP2014505061A patent/JP2014514451A/en active Pending
- 2012-03-27 US US14/009,544 patent/US20140020508A1/en not_active Abandoned
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Also Published As
| Publication number | Publication date |
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| WO2012141439A2 (en) | 2012-10-18 |
| US20140020508A1 (en) | 2014-01-23 |
| DE112012001664T5 (en) | 2014-02-06 |
| JP2014514451A (en) | 2014-06-19 |
| KR20120116169A (en) | 2012-10-22 |
| KR101329081B1 (en) | 2013-11-14 |
| WO2012141439A3 (en) | 2013-01-10 |
| CN103476524A (en) | 2013-12-25 |
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