CN114799196A - Method for improving cubic purity of silver nano - Google Patents
Method for improving cubic purity of silver nano Download PDFInfo
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- CN114799196A CN114799196A CN202210332003.XA CN202210332003A CN114799196A CN 114799196 A CN114799196 A CN 114799196A CN 202210332003 A CN202210332003 A CN 202210332003A CN 114799196 A CN114799196 A CN 114799196A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 38
- 239000004332 silver Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000012528 membrane Substances 0.000 claims abstract description 14
- 238000000967 suction filtration Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 4
- 239000010931 gold Substances 0.000 claims description 33
- 229910052737 gold Inorganic materials 0.000 claims description 33
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 32
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 26
- 239000002105 nanoparticle Substances 0.000 claims description 24
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 20
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 16
- 229960005070 ascorbic acid Drugs 0.000 claims description 16
- 235000010323 ascorbic acid Nutrition 0.000 claims description 16
- 239000011668 ascorbic acid Substances 0.000 claims description 16
- 239000003638 chemical reducing agent Substances 0.000 claims description 14
- 239000003093 cationic surfactant Substances 0.000 claims description 12
- -1 gold ion Chemical class 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 239000012279 sodium borohydride Substances 0.000 claims description 8
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001000 micrograph Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000746 purification Methods 0.000 abstract description 13
- 239000012535 impurity Substances 0.000 abstract description 10
- 239000002042 Silver nanowire Substances 0.000 abstract description 9
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000010970 precious metal Substances 0.000 abstract description 2
- 230000035040 seed growth Effects 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical group [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- 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 belongs to the field of precious metal nano materials, and discloses a method for improving cubic purity of silver nano. The large-size silver nanocubes prepared by the prior art can generate a large amount of independently nucleated silver nanowire impurities, and the impurities can seriously influence the uniformity of the silver nanocubes as the SERS substrate. Aiming at the problem, the invention provides a purification method which is simple and convenient to operate, low in cost and capable of being processed in a large scale. The method firstly utilizes a seed growth method to prepare a large batch of silver nano cubes. And then filtering the prepared silver nanocubes by using filter membranes with proper pore diameters and layers, so that the silver nanocubes can pass through the filter membranes, and the silver nanowire impurities can be attached to the filter membranes due to the large length, thereby obtaining the high-purity silver nanocubes. The flexible and simple suction filtration purification method opens up a new way for improving the purity of the silver nano cube, and the high-purity silver nano cube has wide application prospect in the fields of electronics, medical treatment, biology, food safety and the like.
Description
Technical Field
The invention relates to the field of precious metal nano materials, in particular to a method for improving cubic purity of silver nano.
Background
The silver nanocube has strong and unique surface plasmon resonance (LSPR) characteristics in a visible spectrum region, has a cubic structure with sharp edges and vertex angles, can generate strong electromagnetic field enhancement, has remarkable optical signal enhancement performance and catalysis performance, and has wide application in the aspects of biomedicine, chemical catalysis, ceramic materials, wastewater treatment, high-performance electrode materials and the like. At present, several methods for preparing silver nanocubes have been proposed, and the most common method is synthesis of a polyol system, but the method has the disadvantages of complicated steps, high reaction temperature, use of organic reagents and the like. The other simpler method is water phase synthesis, which includes the first preparation of small size nanometer monocrystal gold seed and the subsequent growth of silver on the surface to obtain nanometer cubic gold-silver core-shell structure. Because the volume of the gold core is smaller, the whole gold-silver core-shell nano cube still shows the LSPR characteristic of the silver cube. However, the large-sized silver nanocubes prepared by this method have many impurities such as silver nanowires, and thus the size of the silver nanocubes is limited to 50nm or less.
Disclosure of Invention
In view of the disadvantages of the prior art, in order to break through the limitation described in the background art and further obtain high-purity silver cubes, we propose a method for improving the purity of silver nanocubes.
The technical scheme of the invention is as follows:
a method for improving the purity of silver nano-cubic comprises the following steps:
(1) rapidly adding a strong reducing agent into the mixed solution of the gold ion solution and the cationic surfactant to prepare gold nanoparticles with the size of about 1-3 nm;
(2) adding the gold nanoparticles prepared in the step (1) into a solution mixed with a gold ion solution, a cationic surfactant and a reducing agent to prepare gold nanoparticles with the size of 10 nm;
(3) reducing silver ions to the 10nm gold nanoparticles prepared in the step (2) by using a mixture of a reducing agent and a cationic surfactant under the condition of 60 ℃ water bath, namely adding the gold nanoparticles prepared in the step (2) into the cationic surfactant, stirring for 15 minutes under the condition of 60 ℃ water bath, simultaneously adding a mixed solution of a silver nitrate solution and the reducing agent at the speed of 0.4mL/min by using a syringe pump to prepare a silver nanocube, stopping the reaction after the reaction is carried out for a period of time, and centrifuging and dispersing the silver ions in a 20mM hexadecyltrimethylammonium chloride solution;
(4) performing suction filtration on the initial silver nano cubic sample in the step (3) by using a filter cup and a vacuum pump;
(5) and (5) adsorbing the silver cube purified in the step (4) on a silicon chip to obtain a scanning electron microscope image.
Further, in the step (1), the gold ion solution is chloroauric acid, the cationic surfactant is cetyl trimethyl ammonium bromide, and the strong reducing agent is sodium borohydride; wherein the concentrations of chloroauric acid, hexadecyl trimethyl ammonium bromide and sodium borohydride are 0.25mM, 100mM and 10mM respectively; the volume ratio of chloroauric acid, hexadecyl trimethyl ammonium bromide and sodium borohydride is 25: 25: 3.
further, in the step (2), the gold ion solution is chloroauric acid, the cationic surfactant is hexadecyltrimethylammonium chloride, and the reducing agent is ascorbic acid; wherein the concentrations of the chloroauric acid, the hexadecyltrimethylammonium chloride and the ascorbic acid are 0.5mM, 200mM and 100mM respectively; the volume ratio of the chloroauric acid, the hexadecyltrimethylammonium chloride, the ascorbic acid and the 3nm gold nanoparticles prepared in the step (1) is 40: 40: 30: 1.
further, the silver ion solution in the step (3) is silver nitrate, and the reducing agent is ascorbic acid; the concentrations of silver nitrate, ascorbic acid and hexadecyl trimethyl ammonium chloride are respectively 2mM, 10mM and 42.5 mM; the volume ratio of silver nitrate, hexadecyl trimethyl ammonium chloride, ascorbic acid and the 10nm gold nanoparticles prepared in the step (2) is 6000: 8000: 3000: 19.
further, the amount of the gold nanoparticles in the step (3) is 38-900 mu L.
Further, the reaction time in the step (3) is 4-8 hours.
Further, the size of the silver nano cube prepared in the step (3) is 28-70 nm.
Further, the centrifugation time in the step (3) is 15min, and the rotating speed is 4000rpm-10000 rpm.
Further, the suction filtration time in the step (4) was 15 seconds.
Further, the specific step of suction filtration in the step (4) is to select the number of filter membrane layers to be 1-3, and the aperture of the filter membrane is 0.2 μm.
Compared with the prior art, the invention has the following advantages:
1. the invention does not need complex instruments and equipment, has simple and convenient operation and low cost, is beneficial to popularization and can be produced in large batch;
2. the impurities of the silver nanowires in the silver cubes are removed, and the limitation of preparing the large-size silver nano cubes due to a large amount of impurities is broken;
3. opens up a new way for improving the purity of the noble metal nano-particles, and the high-purity noble metal nano-particles have wide application prospect in the fields of electronics, medical treatment, biology, food safety and the like.
Drawings
FIG. 1 is a schematic diagram of a suction filtration purification method according to the present invention;
FIG. 2 is a scanning electron microscope photograph of silver nanocubes obtained without purification in example 1;
FIG. 3 is a scanning electron microscope photograph of the silver nanocubes obtained by filtration in example 2 using a filter having a pore size of 0.2 μm with one layer, two layers and three layers, respectively.
Detailed Description
The invention is described in more detail below with reference to specific examples, without limiting the scope of the invention. Unless otherwise specified, the experimental methods adopted by the invention are all conventional methods, and experimental equipment, materials, reagents and the like used in the experimental method can be obtained from commercial sources.
In the prior art, a large amount of independently nucleated silver nanowire impurities can appear when large-size silver nanocubes are prepared, and the impurities can seriously influence the uniformity of the silver nanocubes as an SERS substrate. Aiming at the problem, the invention provides a purification method which is simple and convenient to operate, low in cost and capable of being processed in a large scale. The method comprises the following specific operation that firstly, a seed growth method is utilized to prepare a large batch of silver nano cubes. And then filtering the prepared silver nanocubes by using filter membranes with proper pore diameters and layers, so that the silver nanocubes can pass through the filter membranes, and the silver nanowire impurities can be attached to the filter membranes due to the large length, thereby obtaining the high-purity silver nanocubes. The flexible and simple suction filtration purification method opens up a new way for improving the purity of the silver nano cube, and the high-purity silver nano cube has wide application prospect in the fields of electronics, medical treatment, biology, food safety and the like.
Example 1
(1) Firstly, adding 5mL of 0.25mM chloroauric acid solution into 5mL of 100mM hexadecyl trimethyl ammonium bromide solution, quickly adding 0.6mL of 10mM freshly prepared sodium borohydride aqueous solution, and violently stirring for 2 minutes to obtain gold nanoparticles with the size of about 3 nm;
(2) adding 6mL of 0.5mM chloroauric acid solution into 6mL of 200mM hexadecyltrimethylammonium chloride solution, then adding 4.5mL of 100mM ascorbic acid solution, and finally adding 150 μ L of the 3nm gold nanoparticles prepared in the step (1), and stirring for 15 minutes to obtain gold nanoparticles with the size of about 10 nm;
(3) mu.L of the gold nanoparticles prepared in step (2) was added to 10mL of a 20mM cetyltrimethylammonium chloride solution, and after stirring for 15 minutes under a water bath condition at 60 ℃, 12mL of a 2mM silver nitrate solution and 6mL of a mixed solution of 10mM ascorbic acid and 6mL of 80mM cetyltrimethylammonium chloride were simultaneously added at a rate of 0.4mL/min using a syringe pump. After the injection is finished, the reaction is continued for 8 hours, silver nano cubes with the size of 70nm are prepared, and the silver nano cubes are centrifuged at the rotating speed of 4000rpm for 15min and dispersed in 8mL of 20mM hexadecyl trimethyl ammonium chloride solution;
(4) adsorbing the unpurified silver nanocubes in the step (3) on a silicon wafer to obtain a scanning electron microscope image 2.
Example 2
(1) Firstly, adding 5mL of 0.25mM chloroauric acid solution into 5mL of 100mM hexadecyl trimethyl ammonium bromide solution, quickly adding 0.6mL of 10mM freshly prepared sodium borohydride aqueous solution, and violently stirring for 2 minutes to obtain gold nanoparticles with the size of about 3 nm;
(2) adding 6mL of 0.5mM chloroauric acid solution into 6mL of 200mM hexadecyltrimethylammonium chloride solution, then adding 4.5mL of 100mM ascorbic acid solution, and finally adding 150 μ L of the 3nm gold nanoparticles prepared in the step (1), and stirring for 15 minutes to obtain gold nanoparticles with the size of about 10 nm;
(3) mu.L of the gold nanoparticles prepared in step (2) was added to 10mL of a 20mM cetyltrimethylammonium chloride solution, and after stirring for 15 minutes under a water bath condition at 60 ℃, 12mL of a 2mM silver nitrate solution and 6mL of a mixed solution of 10mM ascorbic acid and 6mL of 80mM cetyltrimethylammonium chloride were simultaneously added at a rate of 0.4mL/min using a syringe pump. After the injection is finished, the reaction is continued for 8 hours, silver nano cubes with the size of 70nm are prepared, and the silver nano cubes are centrifuged at the rotating speed of 4000rpm for 15min and dispersed in 8mL of 20mM hexadecyl trimethyl ammonium chloride solution;
4) using a filter cup and a vacuum pump, selecting one layer, two layers and three layers of filter membranes with the aperture of 0.2 mu m, and carrying out suction filtration and purification on the initial silver nano cubic sample for 15 s;
(5) and (4) adsorbing the purified silver nano cube in the step (4) on a silicon chip to obtain a scanning electron microscope image 3.
According to example 1, it can be seen that the silver nanocube sample which is not subjected to the filtration purification treatment contains more silver nanowire impurities. From the example 2, it can be known that, when the filtration purification is performed on the silver nanocube with the diameter of 70nm by adopting a single-layer filter membrane with the aperture of 0.2 μm, a part of the silver nanowires can not be removed; when three filter membranes with the aperture of 0.2 mu m are adopted for filtration and purification, although the silver nanowires are completely removed, a part of silver nanocubes are also left on the filter membranes, so that the silver nanocubes have certain loss; the yield and the purification effect are considered, relatively good purification effect can be obtained by adopting two layers of filter membranes with the aperture of 0.2 mu m, and the purity can reach more than 90 percent.
The above description is only about the purification of the invention by using 70nm silver nanocube, and is not intended to limit the invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the invention, and these modifications and variations should be regarded as the protection scope of the invention.
Claims (10)
1. A method for improving the purity of silver nano-cubic is characterized by comprising the following steps:
(1) rapidly adding a strong reducing agent into the gold ion solution and the cationic surfactant mixed solution to prepare gold nanoparticles with the size of 1-3 nm;
(2) adding the gold nanoparticles prepared in the step (1) into a solution mixed with a gold ion solution, a cationic surfactant and a reducing agent to prepare gold nanoparticles with the size of 10 nm;
(3) reducing silver ions to the 10nm gold nanoparticles prepared in the step (2) by using a mixture of a reducing agent and a cationic surfactant under the condition of 60 ℃ water bath, namely adding the gold nanoparticles prepared in the step (2) into the cationic surfactant, stirring for 15 minutes under the condition of 60 ℃ water bath, simultaneously adding a mixed solution of a silver nitrate solution and the reducing agent at the speed of 0.4mL/min by using a syringe pump to prepare a silver nanocube, stopping the reaction after the reaction is carried out for a period of time, and centrifuging and dispersing the silver ions in a 20mM hexadecyltrimethylammonium chloride solution;
(4) performing suction filtration on the initial silver nano cubic sample in the step (3) by using a filter cup and a vacuum pump;
(5) and (5) adsorbing the silver cube purified in the step (4) on a silicon chip to obtain a scanning electron microscope image.
2. The method for improving the nano cubic purity of silver according to claim 1, wherein in the step (1), the gold ion solution is chloroauric acid, the cationic surfactant is cetyl trimethyl ammonium bromide, and the strong reducing agent is sodium borohydride; wherein the concentrations of chloroauric acid, hexadecyl trimethyl ammonium bromide and sodium borohydride are 0.25mM, 100mM and 10mM respectively; the volume ratio of chloroauric acid, hexadecyl trimethyl ammonium bromide and sodium borohydride is 25: 25: 3.
3. the method for improving the nano cubic purity of silver according to claim 1, wherein in the step (2), the gold ion solution is chloroauric acid, the cationic surfactant is cetyltrimethylammonium chloride, and the reducing agent is ascorbic acid; wherein the concentrations of the chloroauric acid, the hexadecyltrimethylammonium chloride and the ascorbic acid are 0.5mM, 200mM and 100mM respectively; the volume ratio of the chloroauric acid, the hexadecyltrimethylammonium chloride, the ascorbic acid and the 3nm gold nanoparticles prepared in the step (1) is 40: 40: 30: 1.
4. the method for improving the nano cubic purity of silver according to claim 1, wherein the silver ion solution in the step (3) is silver nitrate, and the reducing agent is ascorbic acid; the concentrations of silver nitrate, ascorbic acid and hexadecyl trimethyl ammonium chloride are respectively 2mM, 10mM and 42.5 mM; the volume ratio of silver nitrate, hexadecyl trimethyl ammonium chloride, ascorbic acid and the 10nm gold nanoparticles prepared in the step (2) is 6000: 8000: 3000: 19.
5. the method for improving the cubic purity of silver nanoparticles as claimed in claim 1, wherein the amount of the gold nanoparticles in the step (3) is 38 to 900 μ L.
6. The method for improving the nano cubic purity of silver according to claim 1, wherein the reaction time in the step (3) is 4 to 8 hours.
7. The method for improving the purity of the silver nanocube according to claim 1, wherein the size of the prepared silver nanocube in the step (3) is 28 to 70 nm.
8. The method for improving the cubic purity of silver nanoparticles as claimed in claim 1, wherein the centrifugation time in step (3) is 15min and the rotation speed is 4000rpm to 10000 rpm.
9. The method for improving the nano-cubic purity of silver according to claim 1, wherein the suction filtration time in the step (4) is 15 s.
10. The method for improving the cubic purity of silver nanoparticles as claimed in claim 1, wherein the filtration in step (4) comprises selecting 1 to 3 filtration membrane layers with a pore size of 0.2 μm.
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US20050056118A1 (en) * | 2002-12-09 | 2005-03-17 | Younan Xia | Methods of nanostructure formation and shape selection |
CN108723385A (en) * | 2018-06-07 | 2018-11-02 | 大连民族大学 | A kind of monocrystalline silver nanoparticle ball aqueous phase preparation method |
KR102270806B1 (en) * | 2020-10-28 | 2021-06-28 | 금오공과대학교 산학협력단 | The process for producing silver nanocube and silver nanocube produced using the same |
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Non-Patent Citations (2)
Title |
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