CN106623979A - Preparation method of gold-silver alloy nanoparticles - Google Patents
Preparation method of gold-silver alloy nanoparticles Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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Abstract
The invention discloses a preparation method of gold-silver alloy nanoparticles. The preparation method comprises the following steps: firstly preparing a water soluble starch aqueous solution, a chloroauric acid aqueous solution and a silver nitrate aqueous solution in steps, then adding the chloroauric acid aqueous solution and the silver nitrate aqueous solution into deionized water, and carrying out ultrasonic vibration and mixing to obtain mixed solution of chloroauric acid and silver nitrate; heating the water soluble starch aqueous solution until the boiling state is achieved, then adding the mixed solution of chloroauric acid and silver nitrate, controlling the pH value of a reaction system to be 3.6-4.9 by controlling the addition amount of the mixed solution of chloroauric acid and silver nitrate, then reacting for 10-60 minutes while keeping the boiling state, carrying out centrifugal separation on the obtained reaction liquid, and drying the obtained sediments, thus obtaining the gold-silver alloy nanoparticles. The preparation method disclosed by the invention has the advantages of low cost, simplicity in operation, environment-friendly preparation process and the like. The obtained gold-silver alloy nanoparticles also provide an experimental foundation for subsequent biomarker application research and can be applied to the field of biomedicines.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to one kind prepares electrum using water soluble starch
The method of nano-particle.
Background technology
Gold-silver alloy nanoparticles are different from gold, silver monometallic nanoparticle because of its structure, in optics, chemically and electrically etc.
Field shows unique excellent property, it has also become research emphasis of field of nanometer material technology in recent years.Electrum nanometer
Grain has unique electric property and structure, and avirulent gold-silver alloy nano particle is even more and can be used for biological radiography.Meanwhile, it is high
The free of contamination gold silver nanometer particle of purity is to carbon monoxide(CO)Also there is very high catalysis activity, this also has to removing CO toxicity
There is far-reaching influence.It can be seen that, how to prepare nontoxic, free of contamination gold-silver alloy nano particle becomes the key of every research.
So far, the method for preparing gold-silver alloy nano particle is a lot, and traditional method can be divided into Physical and chemical method.Thing
Requirement of the logos to instrument and equipment is higher, and producing cost is expensive, and the uniformity of granule is poor.Chemical rule is using special
Chemical reaction is preparing gold-silver alloy nano particle.Chemical method flexible operation, can synthesize the electrum nanometer of different-shape
Granule.However, chemistry need to typically introduce chemical reagent to do reducing agent or dispersant, the use of some chemical reagent in the reaction
Certain pollution not only may be caused to environment, and is difficult from gold-silver alloy nano particle surface to remove, this is also to application
Potential risks are brought in biomarker.
In recent years, the green synthesis method of gold-silver alloy nano particle gradually emerged in large numbers, such as by grapefruit skin, Punica granatum L. kind and
The plant extraction liquids such as Cacumen Platycladi substitute chemical reducing agent to realize the green syt of gold-silver alloy nano particle.But existing green
Preparation method exist it is relatively costly, technique it is loaded down with trivial details and synthesis gold-silver alloy nano particle lack of homogeneity, poor dispersion
The problems such as.
In sum, the preparation process of current gold-silver alloy nano particle has environmental pollution, relatively costly, technique
The problems such as gold-silver alloy nano particle lack of homogeneity of loaded down with trivial details and synthesis, poor dispersion.
Water soluble starch is cheap, avirulence, the good dispersion to nano-particle, and does not result in environmental pollution.But
In general nanoparticle synthetic system, water soluble starch is typically considered a kind of dispersant of stable performance, its reduction
Property is usually ignored, and rarely has the report to its reproducibility.(Raveendran etc. is proposed in the basic conditions, is made using glucose
For reducing agent, water soluble starch has synthesized golden nanometer particle of the particle diameter in 6-10nm as protective agent.Raveendran P, Fu
J, Wallen S. A simple and"green"method for the synthesis of Au,Ag,and Au-Ag
alloy nanoparticles[J]. Green Chemistry, 2006, 8(1): 34-38.)(Malathi etc. utilizes water
Soluble starch is dispersant, isoniazid(INH)For reducing agent, the golden nanometer particle of size about 14nm under room temperature, is synthesized.
Malathi S, Ezhilarasu T, Abiraman T, et al. One pot green synthesis of Ag, Au
and Au–Ag alloy nanoparticles using isonicotinic acid hydrazide and starch
[J].Carbohydrate Polymers, 2014, 111: 734-743.)As water soluble starch only makees dispersant, also need
It is possible to additionally incorporate other reducing agents, therefore exist that preparation system is complicated, preparation process is loaded down with trivial details and the nanoparticle dispersibility of gained
The technical problems such as difference.But if water soluble starch can both make reducing agent in synthetic system, dispersant can be done again, that is by letter
Chemical combination architectonical, it is easier to which realization is commercially produced.
For problem present in the studies above, applicant is based on state natural sciences fund(11404210), to water-soluble
Property starch green syt gold-silver alloy nano particle has done further exploration.
The content of the invention
The invention aims in solving above-mentioned nanoparticle preparation process as environmental pollution, preparation cost are high,
Preparation process is loaded down with trivial details and the technical problem such as gold-silver alloy nanoparticles bad dispersibility for preparing and one kind for providing are using water-soluble
Property starch prepares the green synthesis method of electrum nanometer.In the preparation method, water soluble starch is used as dispersant,
It is used as reducing agent, and need not separately plus by any other chemical assistant synthesizes nanometer gold silver alloying pellet, therefore there is preparation
Process is simple, mild condition, environmental friendliness and the advantages of without chemical agent residue are gold-silver alloy nano particle in biomedicine
The application in field is laid a good foundation.
The know-why of the present invention
Water soluble starch simultaneously as reducing agent and dispersant, respectively by the gold ion and nitric acid in gold chloride under water bath condition
Silver ion in silver is reduced into gold atom and silver atoms simultaneously, and then gold atom is combined by metallic bond with silver atoms, forms gold
Silver alloy nano-particle.
Technical scheme
A kind of preparation method of gold-silver alloy nano particle, specifically includes following steps:
(1), water soluble starch is dissolved in deionized water 0.4-1.0mol/L is obtained, the water solublity of preferred 0.58mol/L forms sediment
Amidin;
Described water soluble starch is amylose, and its molecular formula is C12H22O11, molecular weight is 342.30;
(2), gold chloride dissolution of crystals is formed in deionized water 0.05-0.12mol/L, the gold chloride water of preferred 0.1mol/L
Solution;
Silver nitrate crystal is dissolved in deionized water and forms 0.01-0.03mol/L, the silver nitrate of preferred 0.01mol/L is water-soluble
Liquid;
Aqueous solution of chloraurate and silver nitrate aqueous solution are added separately in deionized water, after sonic oscillation is mixed, 1min is obtained
To gold chloride and silver nitrate mixed liquor, described sonic oscillation, which controls frequency for 25KHz;
The consumption of aqueous solution of chloraurate, silver nitrate aqueous solution and deionized water in gold chloride and silver nitrate mixed liquor, by gold chloride
With gold ion in silver nitrate mixed liquor:Silver ion:The mol ratio of deionized water is 1:20-35:2.52×108Ratio calculate,
It is preferred that gold ion:Silver ion:The mol ratio of deionized water is 1:25-30:2.52×108;
(3), by step(1)The water soluble starch aqueous solution of gained is heated to boiling and keeps 1-60min, so that water soluble starch is molten
Liquid is fully hydrolyzed, and the gold chloride and silver nitrate mixed liquor for then obtaining step (2) is added to the water soluble starch solution of boiling
In, reaction system is protected all the time by controlling the addition of gold chloride and silver nitrate mixed liquor to control the pH value of reaction system
Hold reducing condition such that it is able to ensure that gold chloride and silver nitrate mixed liquor are reduced completely, when the pH value of reaction system is 3.6-
Stop adding gold chloride and silver nitrate mixed liquor when 4.9, keep under fluidized state, carrying out reaction 10-60min, reaction will after terminating
Gained reactant liquor centrifugation, obtains final product gold-silver alloy nano particle after gained sediment is dried.
And the water soluble starch in the preparation method of the present invention is used as dispersant, reducing agent is also served as, at present, there is not yet
Not only dispersant had been done with regard to water soluble starch but also make reducing agent to synthesize the report of gold-silver alloy nano particle.
The technique effect of the present invention
A kind of preparation method of the gold-silver alloy nano particle of the present invention, due to water soluble starch used in preparation process conveniently
Be easy to get, cheap, and no toxicity, therefore the preparation method has preparation cost low, and preparation process is simple to operate, prepares
The advantages of Cheng Huanbao.
Further, it is prepared by the preparation method of a kind of gold-silver alloy nano particle of the invention, water soluble starch used
During except the effect for dispersant, while which is also as reducing agent, the reducing agent such as sodium citrate that replaces using in the past,
The chemical reagent such as sodium borohydride, mercaptan, oleyl amine, i.e., without the need for separately adding other chemical assistants synthesize nanometer gold silver alloying pellet.
Therefore the preparation method has simple to operate, and is not in other poisonous reducing agents, therefore prepared electrum nanometer
Particle surface will not produce the advantage of toxic chemical residual, also provide experiment base to the applied research of subsequent bio labelling
Plinth..
Further, the gold-silver alloy nano particle obtained by a kind of preparation method of gold-silver alloy nano particle of the invention is produced
Raw absworption peak scope produces obvious plasmon resonance signal, can be applicable to biomedicine field in 420-500nm.
Description of the drawings
In Fig. 1, embodiment 1 after correspondence response time respectively 10min, 20min, 30min, 40min, 50min, 60min
The uv-visible absorption spectra of the gold-silver alloy nano particle of sampling gained(UV-Vis)Figure;
The transmission electron microscope of resulting gold-silver alloy nano particle when the response time is 10min in Fig. 2, embodiment 1
(TEM)Figure;
The power spectrum of resulting gold-silver alloy nano particle when the response time is 10min in Fig. 3, embodiment 1(EDX)Figure;
In Fig. 4, embodiment 2, the correspondence response time is respectively sampling after 10min, 20min, 30min, 40min, 50min, 60min
The uv-visible absorption spectra of the gold-silver alloy nano particle of gained(UV-Vis)Figure;
The transmission electron microscope of resulting gold-silver alloy nano particle when the response time is 60min in Fig. 5, embodiment 2
(TEM)Figure;
The power spectrum of resulting gold-silver alloy nano particle when the response time is 60min in Fig. 6, embodiment 2(EDX)Figure.
Specific embodiment
It is combined below by specific embodiments and the drawings that the present invention will be further described, those skilled in the art should
The understanding, embodiment and accompanying drawing are intended merely to more fully understand the present invention, are not used to make any restriction.
Water soluble starch(C12H22O11, AR, 500g)
Gold chloride crystal (HAuCl4•3H2O, AR,1g)
Silver nitrate crystal (AgNO3 , GR,25g)
Above medicine is purchased from Aladdin reagent company limited.
In each embodiment, glass container used will be washed with chloroazotic acid first, be made after then deionized water is rinsed well
With.
Embodiment 1
A kind of preparation method of gold-silver alloy nano particle, specifically includes following steps:
(1), in beaker 1,5g water soluble starchs are dissolved in 25mL deionized waters the water soluble starch water that 0.58mol/L is obtained
Solution;
Described water soluble starch is amylose, and its molecular formula is C12H22O11, molecular weight is 342.30;
(2), in beaker 2,1g gold chlorides dissolution of crystals is formed in 25mL deionized waters the aqueous solution of chloraurate of 0.1mol/L;
In beaker 3, the silver nitrate that 0.085g silver nitrate crystals are dissolved in formation 0.01mol/L in 50ml deionized waters is water-soluble
Liquid;
30 mL deionized waters are initially charged in beaker 4, subsequently 20 μ L aqueous solution of chloraurate and 5 mL silver nitrate aqueous solutions are added successively
Enter in the deionized water of beaker 4, control frequency be 25KHz ultrasound condition sonic oscillation 1min mixed after, obtain chlorine
Auric acid and silver nitrate mixed liquor;
The consumption of aqueous solution of chloraurate, silver nitrate aqueous solution and deionized water in above-mentioned gold chloride and silver nitrate mixed liquor, by chlorine
Gold ion in aqueous solution of chloraurate in auric acid and silver nitrate mixed liquor:Silver ion in silver nitrate aqueous solution:Deionized water mole
Than for 1:25:2.52×108Ratio calculate;
(3), by 25ml steps(1)The water soluble starch aqueous solution of gained is put into flask 5, is heated to boiling, keeps fluidized state
25min;
Then the gold chloride and silver nitrate mixed liquor for step (2) being obtained is added to the water soluble starch solution of above-mentioned boiling
In, the pH value of reaction system is controlled by the addition of control gold chloride and silver nitrate mixed liquor, when the pH value of reaction system
Stop adding gold chloride and silver nitrate mixed liquor for 4.15, keep reaction 10-60min being carried out under fluidized state, respectively in reaction
10min, 20min, 30min, 40min, 50min, 60min are sampled, respectively will reactant liquor control obtained by the correspondence differential responses time
Rotating speed is that 8000rpm is centrifuged 10min, and correspondence differential responses time gained sediment is controlled temperature to be dried at 40-50 DEG C
The gold-silver alloy nano particle of correspondence differential responses time is obtained final product after 10min.
Analyze from the result of sampling, it can be deduced that with the increase in response time, the color of the reactant liquor of gained is by purple
Color is gradually converted into brown;
Using Japanese Shimadzu Corporation UV-2600 types ultraviolet spectrophotometer respectively to above-mentioned reaction 10min, 20min, 30min,
After reactant liquor centrifugation obtained by 40min, 50min, 60min, the electrum nanometer of gained is measured uv-visible absorption spectra
Situation, the uv-visible absorption spectra of gained(UV-Vis)Figure as shown in figure 1, as can be seen from Figure 1 its absworption peak by
490nm or so is gradually blue shifted to 430nm or so, has been indicated above gold ion and has been completely reduced first, the content of subsequent silver atoms
Gradually increase.The absworption peak scope that gold-silver alloy nano particle is produced produces obvious plasma resonance letter in 420-500nm
Number, further biologic applications can be done.
Using the JEM-2100F type Flied emission transmission electron microscopes of NEC company to obtained by above-mentioned reaction 10min
Electrum nanometer measure, the TEM of gained figure is as shown in Fig. 2 as can be seen from Figure 2 gained electrum nanometer
Grain is presented class ball-type.Gold-silver alloy nano particle sample obtained by remaining 20min, 30min, 40min, 50min, 60min
Pattern it is similar with the pattern of the gold-silver alloy nano particle sample that 10min is obtained, its average diameter is 17.6nm or so.
Electrum obtained by above-mentioned reaction 10min is received using 60 type energy disperse spectroscopies of NEC company EDAX Falcon s
Rice grain is measured, and the EDX collection of illustrative plates of gained is as shown in figure 3, can significantly find out the electrum of reaction gained from Fig. 3
Secondly the main component of nano-particle is gold element Au, is silver Ag and copper Cu, copper Cu therein be copper mesh used by test into
Point, it is not impurity that gold-silver alloy nano particle is included.
Embodiment 2
A kind of preparation method of gold-silver alloy nano particle, specifically includes following steps:
(1), in beaker 6,5g water soluble starchs are dissolved in 25ml deionized waters the water soluble starch water that 0.58mol/L is obtained
Solution;
Described water soluble starch is amylose, and its molecular formula is C12H22O11, molecular weight is 342.30;
(2), in beaker 7,1g gold chlorides dissolution of crystals is formed in 25mL deionized waters the aqueous solution of chloraurate of 0.1mol/L;
In beaker 8, the silver nitrate that 0.085g silver nitrate crystals are dissolved in formation 0.01mol/L in 50ml deionized waters is water-soluble
Liquid;
30 mL deionized waters are initially charged in beaker 9, subsequently again by 16.66 μ L aqueous solution of chloraurate and 5 mL silver nitrate aqueous solutions
Sequentially add in deionized water, control frequency of vibration be 25KHz ultrasound condition sonic oscillation 1min mixed after, obtain chlorine
Auric acid and silver nitrate mixed liquor;
The consumption of aqueous solution of chloraurate, silver nitrate aqueous solution and deionized water in gold chloride and silver nitrate mixed liquor, by mixed liquor
Gold ion in middle aqueous solution of chloraurate:Silver ion in silver nitrate aqueous solution:The mol ratio of deionized water is 1:30:2.52×108
Ratio calculate;
(3), by 25ml steps(1)The water soluble starch aqueous solution of gained is put into flask 10, is heated to boiling, keeps fluidized state
25min, the gold chloride and silver nitrate mixed liquor for then obtaining step (2) are added in the water soluble starch solution of boiling, are led to
Cross the addition of control gold chloride and silver nitrate mixed liquor to control the pH value of reaction system, when the pH value of reaction system is 4.23
Stop adding gold chloride and silver nitrate mixed liquor, keep carrying out reaction 10-60min under fluidized state, respectively reaction 10min,
20min, 30min, 40min, 50min, 60min are sampled, and reactant liquor obtained by the correspondence differential responses time is controlled rotating speed respectively and is
8000rpm is centrifuged 10min, and correspondence differential responses time gained sediment is controlled temperature to be dried after 10min i.e. at 40-50 DEG C
The gold-silver alloy nano particle of differential responses time must be corresponded to.
Analyze from the result of sampling, it can be deduced that with the increase in response time, the color of the reactant liquor of gained is by purple
Color is gradually converted into brown;
Using Japanese Shimadzu Corporation UV-2600 types ultraviolet spectrophotometer respectively to above-mentioned reaction 10min, 20min, 30min,
After reactant liquor centrifugation obtained by 40min, 50min, 60min, the electrum nanometer of gained is measured uv-visible absorption spectra
Situation, the uv-visible absorption spectra of gained(UV-Vis)Figure as shown in figure 4, as can be seen from Figure 4 its absworption peak by
490nm or so is gradually blue shifted to 430nm or so, has been indicated above gold ion and has been completely reduced first, the content of subsequent silver atoms
Gradually increase.The absworption peak scope that gold-silver alloy nano particle is produced produces obvious plasma resonance letter in 420-500nm
Number, further biologic applications can be done.
Using the JEM-2100F type Flied emission transmission electron microscopes of NEC company to obtained by above-mentioned reaction 60min
Electrum nanometer measure, the TEM of gained figure is as shown in figure 5, as can be seen from Figure 4 gained electrum nanometer
Grain is presented class ball-type.Gold-silver alloy nano particle sample obtained by remaining 10min, 20min, 30min, 40min, 50min
Pattern it is similar with the pattern of the gold-silver alloy nano particle sample that 60min is obtained, its average diameter is 15.8nm or so.
Electrum obtained by above-mentioned reaction 60min is received using 60 type energy disperse spectroscopies of NEC company EDAX Falcon s
Rice grain is measured, and the EDX collection of illustrative plates of gained is as shown in fig. 6, can significantly find out the electrum of reaction gained from Fig. 6
Secondly the main component of nano-particle is gold element Au, is silver Ag and copper Cu, copper Cu therein be copper mesh used by test into
Point, it is not impurity that gold-silver alloy nano particle is included.
Although above-described embodiment simply lists laboratory scale reaction, it will be understood by those skilled in the art that this
The method of invention is equally applicable to plant-scale reaction.
In sum, the invention provides a kind of method of utilization water soluble starch preparation gold-silver alloy nano particle.It is logical
Cross the molar ratio of gold ion and silver ion in regulation and control gold chloride and silver nitrate mixed liquor, preferred gold ion and silver ion mole
Than from 1:25 to 1:30, the response time, the gold-silver alloy nano particle of final gained showed 420- from 10 to 60min
Plasma resonance absorption peak between 500nm, the molar ratio of two kinds of elements of gold, silver which is included can also accordingly 1:
0.1-1:Adjust between 2.8, that is, control molar ratio and the response time of two kinds of elements of gold, silver, so that it may to obtain having not
With gold silver proportioning, the gold-silver alloy nano particle of different plasmon resonance signals.And the gold-silver alloy nano particle of gained is ball
Shape, good dispersion, particle size uniformity, its average-size are about 15.8-17.6nm or so.
The above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, on the premise of without departing from the technology of the present invention principle, some improvement and modification can also be made, these improve and become
Type also should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of gold-silver alloy nano particle, it is characterised in that specifically include following steps:
(1), by water soluble starch be dissolved in deionized water be obtained 0.4-1.0mol/L water soluble starch aqueous solution;
Described water soluble starch is amylose, and its molecular formula is C12H22O11, molecular weight is 342.30;
(2), gold chloride dissolution of crystals is formed in deionized water the aqueous solution of chloraurate of 0.05-0.12mol/L;
Silver nitrate crystal is dissolved in deionized water the silver nitrate aqueous solution for forming 0.01-0.03mol/L;
Aqueous solution of chloraurate and silver nitrate aqueous solution are added separately in deionized water, after sonic oscillation is mixed, 1min is obtained
To gold chloride and silver nitrate mixed liquor;
The consumption of aqueous solution of chloraurate, silver nitrate aqueous solution and deionized water in gold chloride and silver nitrate mixed liquor, by gold chloride
With gold ion in silver nitrate mixed liquor:Silver ion:The mol ratio of deionized water is 1:20-35:2.52×108Ratio calculate;
(3), by step(1)The water soluble starch aqueous solution of gained is heated to boiling and keeps 1-60min, so that water soluble starch is molten
Liquid is fully hydrolyzed, and the gold chloride and silver nitrate mixed liquor for then obtaining step (2) is added to the water soluble starch solution of boiling
In, reaction system is protected all the time by controlling the addition of gold chloride and silver nitrate mixed liquor to control the pH value of reaction system
Hold reducing condition such that it is able to ensure that gold chloride and silver nitrate mixed liquor are reduced completely, when the pH value of reaction system is 3.6-
Stop adding gold chloride and silver nitrate mixed liquor when 4.9, keep under fluidized state, reacting 10-60min, react gained after terminating
Reactant liquor centrifugation, obtains final product gold-silver alloy nano particle after gained sediment is dried.
2. a kind of preparation method of gold-silver alloy nano particle as claimed in claim 1, it is characterised in that step(1)In it is water-soluble
Property amidin concentration be 0.58mol/L;
Step(2)The concentration of middle aqueous solution of chloraurate is 0.1mol/L;
The concentration of silver nitrate aqueous solution is 0.01mol/L;
The consumption of aqueous solution of chloraurate, silver nitrate aqueous solution and deionized water in gold chloride and silver nitrate mixed liquor, by gold chloride
With gold ion in silver nitrate mixed liquor:Silver ion:The mol ratio of deionized water is 1:25-30:2.52×108Ratio calculate;
Step(3)It is middle by step(1)The water soluble starch aqueous solution of gained is heated to boiling and keeps 25min, when reaction system
Stop adding gold chloride and silver nitrate mixed liquor when pH value is 4.15-4.23.
3. a kind of preparation method of gold-silver alloy nano particle as claimed in claim 2, it is characterised in that step(2)Middle chlorine gold
The consumption of aqueous solution of chloraurate, silver nitrate aqueous solution and deionized water in acid and silver nitrate mixed liquor, by gold chloride and silver nitrate
Gold ion in mixed liquor:Silver ion:The mol ratio of deionized water is 1:25:2.52×108Ratio calculate;
Step(3)In stop adding gold chloride and silver nitrate mixed liquor when the pH value of reaction system is 4.15.
4. a kind of preparation method of gold-silver alloy nano particle as claimed in claim 2, it is characterised in that step(2)Middle chlorine gold
The consumption of aqueous solution of chloraurate, silver nitrate aqueous solution and deionized water in acid and silver nitrate mixed liquor, by gold chloride and silver nitrate
Gold ion in mixed liquor:Silver ion:The mol ratio of deionized water is 1:30:2.52×108Ratio calculate;
Step(3)In stop adding gold chloride and silver nitrate mixed liquor when the pH value of reaction system is 4.23.
5. a kind of preparation method of the gold-silver alloy nano particle as described in claim 1,2,3 or 4, it is characterised in that step
(2)Described in sonic oscillation, which controls frequency for 25KHz.
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CN112743097A (en) * | 2020-12-17 | 2021-05-04 | 北京科技大学 | Preparation method of fully alloyed monodisperse gold-silver alloy nanoparticles |
CN116020453A (en) * | 2022-10-09 | 2023-04-28 | 西北工业大学 | Gold-silver nano alloy and ultra-clean preparation method and application thereof |
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