CN106493385A - The preparation method of silver-colored triangular nano piece - Google Patents
The preparation method of silver-colored triangular nano piece Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of silver-colored triangular nano piece.It adds sodium citrate aqueous solution and aqueous ascorbic acid in the Nano silver piece crystal seed aqueous solution under stirring, obtain mixed liquor, then, first a pair of silver electrode are put in mixed liquor with stirring, it is 0.37～0.74mA/cm for 280～320s, electric current density to inject the snap time that commutates then between silver electrode2Commutation 40～80min of step current after, it is added to sodium citrate aqueous solution and aqueous ascorbic acid 0～4 time, and inject the commutation step current of such as aforementioned same time every time between silver electrode, obtain reactant liquor, afterwards, carry out the process of solid-liquid separation, washing and drying to reactant liquor successively, product is obtained.The characteristics of it has environmental protection, can make product be extremely easy to be widely used in the fields such as conducting resinl.
Description
Technical field
The present invention relates to a kind of preparation method of Nano silver piece, especially a kind of preparation method of silver-colored triangular nano piece.
Background technology
Silver is the best metal of electric conductivity and heat conductivity, and when silver is in nanoscale, silver nano material has block
The unexistent unique physics of body material and chemical property.The embodiment of these properties be largely dependent upon again its pattern with
The factors such as size.For Nano silver piece, due to specific surface area big, surface energy is low, anti-deflect strong ability, good in oxidation resistance,
Belong to face to contact between good fluidity, and piece and piece, contact area is big, resistance is relatively low.Therefore, cause people widely to close
Note, and applied in fields such as conducting resinls.In recent years, people have developed a series of sides for preparing Nano silver piece
Method, such as entitled " One-step growth of triangular silver nanoplates with predictable
(" the controllable triangle of extensive one-step synthesis size of sizes on a large scale ", nanoscal, 6,4513 (2014)
Nano silver piece ",《Nanoscale》Page 4513 of 6th phase in 2014) article.The synthetic method that reports in this article is solwution method,
Its first using TSC be surface capping agents, sodium borohydride be reducing agent, silver nitrate be presoma, in aqueous synthesis crystal seed molten
Liquid, recycles the seed-solution that configured, with ascorbic acid as reducing agent, TSC as covering, acetonitrile as chelating agent, further
Synthesize larger-size Nano silver piece.Though this method can obtain triangular silver nanosheet, but also exist and receive to control silver
The Growth kinetics process of rice piece, has used the acetonitrile as silver ion complexation agent, and acetonitrile be a kind of to person injury compared with
The deficiency of big Toxic.
Content of the invention
The technical problem to be solved in the present invention is to overcome weak point of the prior art, there is provided a kind of silver of environmental protection
The preparation method of triangular nano piece.
For solve the present invention technical problem, the technical scheme for being adopted for：The preparation method of silver-colored triangular nano piece includes
Electrochemical process, particularly key step are as follows：
Step 1, according to the sodium citrate aqueous solution of 0.055～0.095mol/L, the ascorbic acid of 0.08～0.12mol/L
The volume ratio of the Nano silver piece crystal seed aqueous solution of aqueous solution and 0.49～19 μm of ol/L is 1：1.3～1.7：100～1000 ratio
Example, sodium citrate aqueous solution and aqueous ascorbic acid is added in the Nano silver piece crystal seed aqueous solution under stirring, is mixed
Liquid；
Step 2, first puts a pair of silver electrode in mixed liquor with stirring, injection commutation snap time then between silver electrode
It is 0.37～0.74mA/cm for 280～320s, electric current density2Commutation 40～80min of step current after, be added to
Volume ratio identical sodium citrate aqueous solution and aqueous ascorbic acid 0～4 time in step 1, and note between silver electrode every time
Enter such as the commutation step current of aforementioned same time, obtain reactant liquor；
Step 3, carries out the process of solid-liquid separation, washing and drying successively to reactant liquor, and it is 320nm～2.2 μ that the length of side is obtained
M, thickness are the silver-colored triangular nano piece of 20～40nm.
Further improvement as the preparation method of silver-colored triangular nano piece：
Preferably, the process for obtaining Nano silver piece crystal seed is, first according to the sodium citrate aqueous solution of 0.075mol/L,
The body of the silver nitrate aqueous solution of 0.1mol/L, the hydrogen peroxide of 30wt%, the sodium borohydride aqueous solution of 0.1mol/L and deionized water
Product is than being 4：0.1：0.2：0.6：100 ratio, successively by sodium citrate aqueous solution, silver nitrate aqueous solution, hydrogen peroxide and boron hydrogen
Change stirring 1h after sodium water solution is added in deionized water, obtain mixed liquid, then liquid to be mixed stands two days later, solid-liquid is carried out successively to which
The process for separating, washing and dry.
Preferably, silver electrode is filamentary silver, before being placed in mixed liquor, first sanding and polishing, reuse chloroform,
The cleaning of acetone, ethanol and deionized water.
Preferably, solid-liquid separation is processed as centrifugation, and its rotating speed is 4000～8000r/min, the time is 5～10min.
Preferably, carrying out washing treatment is, using deionized water or ethanol, isolated solids are carried out with 1～3 time clear
Wash, it is centrifugation to separate solids during cleaning.
Preferably, the solids after dried is by cleaning are placed at 40～80 DEG C and dry.
Beneficial effect relative to prior art is：
First, obtained product is characterized using scanning electron microscope and X-ray diffractometer respectively, from its result,
Product is triangle nanometer sheet, and its length of side is 320nm～2.2 μm, thickness is 20～40nm.Triangle nanometer sheet is received for silver-colored triangle
Rice piece.
Second, preparation method science, effectively.With high length of side product silver triangle with thickness ratio has not only been obtained
Nanometer sheet, can also pass through concentration, the size of commutation step current and the time for controlling each material solution, and add sodium citrate
Aqueous solution and aqueous ascorbic acid and continue electrolysis effectively to control the Growth kinetics process of Nano silver piece, that is, obtain more
Large-sized product, the characteristics of more have environmental protection；So that product is extremely easy to be widely used in the fields such as conducting resinl.
Description of the drawings
Fig. 1 is that product obtained in preparation method is carried out using scanning electron microscope (SEM) and X-ray diffraction (XRD) instrument respectively
One of result of sign.Wherein, the XRD spectra that a figures in Fig. 1 are the SEM image of product, b figures are product；Fig. 1 shows and demonstrate,proves
Real silver-colored triangular nano piece of the product for the length of side about 320nm.
Fig. 2 is to one of result that obtained product is characterized using scanning electron microscope.SEM image shows the side of product
Long about 900nm.
Fig. 3 is to one of result that obtained product is characterized using scanning electron microscope.SEM image shows the side of product
Long about 1.2 μm.
Fig. 4 is to one of result that obtained product is characterized using scanning electron microscope.SEM image shows the side of product
Long about 1.74 μm.
Fig. 5 is to one of result that obtained product is characterized using scanning electron microscope.SEM image shows the side of product
Long about 2.0 μm.
Specific embodiment
Below in conjunction with the accompanying drawings the optimal way of the present invention is described in further detail.
Buy from market first or be voluntarily obtained：
Sodium citrate aqueous solution；
Aqueous ascorbic acid；
Nano silver piece crystal seed aqueous solution；
Filamentary silver as silver electrode.
Wherein,
The acquisition process of the Nano silver piece crystal seed in Nano silver piece crystal seed aqueous solution is, first according to the Fructus Citri Limoniae of 0.075mol/L
Acid sodium aqueous solution, the silver nitrate aqueous solution of 0.1mol/L, the hydrogen peroxide of 30wt%, the sodium borohydride aqueous solution of 0.1mol/L and go
The volume ratio of ionized water is 4：0.1：0.2：0.6：100 ratio, successively by sodium citrate aqueous solution, silver nitrate aqueous solution, double
Oxygen water and sodium borohydride aqueous solution add in deionized water after stirring 1h, obtain mixed liquid, then liquid mix standing be two days later, to its according to
The secondary process for carrying out solid-liquid separation, washing and drying；Solid-liquid separation therein is processed as centrifugation, its rotating speed be 4000～
8000r/min, time are 5～10min, and carrying out washing treatment is isolated solids to be carried out using deionized water (or ethanol)
The cleaning of 1～3 time, during cleaning separate solids be centrifugation, dried be by cleaning after solids be placed in 40～80
Dry at DEG C.
Before being placed in mixed liquor, first sanding and polishing reuses chloroform, acetone, ethanol and deionized water to filamentary silver
Cleaning.
Then,
Embodiment 1
Prepared concretely comprises the following steps：
Step 1, according to the sodium citrate aqueous solution of 0.055mol/L, the aqueous ascorbic acid of 0.12mol/L and 19 μ
The volume ratio of the Nano silver piece crystal seed aqueous solution of mol/L is 1：1.3：1000 ratio, by sodium citrate aqueous solution and Vitamin C
Aqueous acid is added in the Nano silver piece crystal seed aqueous solution under stirring, obtains mixed liquor.
Step 2, first puts a pair of silver electrode in mixed liquor with stirring.Injection commutation snap time then between silver electrode
It is 0.37mA/cm for 280s, electric current density2Commutation step current 80min, obtain reactant liquor.
Step 3, carries out the process of solid-liquid separation, washing and drying successively to reactant liquor；Wherein, solid-liquid separation be processed as from
The heart is separated, and its rotating speed is 4000r/min, the time is 10min, and carrying out washing treatment is to isolated using deionized water (or ethanol)
Solids carry out the cleaning of 1 time, it is centrifugation to separate solids during cleaning, dried be by cleaning after solids put
Dry at 40 DEG C.It is obtained as shown in a figures in Fig. 1, and the silver-colored triangular nano piece as shown in the spectral line in the b figures in Fig. 1.
Embodiment 2
Prepared concretely comprises the following steps：
Step 1, according to the sodium citrate aqueous solution of 0.065mol/L, the aqueous ascorbic acid of 0.11mol/L and 13 μ
The volume ratio of the Nano silver piece crystal seed aqueous solution of mol/L is 1：1.4：775 ratio, by sodium citrate aqueous solution and ascorbic acid
Aqueous solution is added in the Nano silver piece crystal seed aqueous solution under stirring, obtains mixed liquor.
Step 2, first puts a pair of silver electrode in mixed liquor with stirring.Injection commutation snap time then between silver electrode
It is 0.46mA/cm for 290s, electric current density2Commutation step current 70min after, be added to and volume ratio phase in step 1
With sodium citrate aqueous solution and aqueous ascorbic acid 1 time, and between silver electrode the injection such as aforementioned same time commutation rank
Jump electric current, obtains reactant liquor.
Step 3, carries out the process of solid-liquid separation, washing and drying successively to reactant liquor；Wherein, solid-liquid separation be processed as from
The heart is separated, and its rotating speed is 5000r/min, the time is 9min, and carrying out washing treatment is to isolated using deionized water (or ethanol)
Solids carry out the cleaning of 1 time, it is centrifugation to separate solids during cleaning, dried be by cleaning after solids put
Dry at 50 DEG C.It is obtained as shown in Fig. 2 and the silver-colored triangular nano piece as shown in the spectral line in the b figures in Fig. 1.
Embodiment 3
Prepared concretely comprises the following steps：
Step 1, according to the sodium citrate aqueous solution of 0.075mol/L, the aqueous ascorbic acid of 0.10mol/L and 7 μ
The volume ratio of the Nano silver piece crystal seed aqueous solution of mol/L is 1：1.5：450 ratio, by sodium citrate aqueous solution and ascorbic acid
Aqueous solution is added in the Nano silver piece crystal seed aqueous solution under stirring, obtains mixed liquor.
Step 2, first puts a pair of silver electrode in mixed liquor with stirring.Injection commutation snap time then between silver electrode
It is 0.55mA/cm for 300s, electric current density2Commutation step current 60min after, be added to and volume ratio phase in step 1
With sodium citrate aqueous solution and aqueous ascorbic acid 2 times, and inject such as the aforementioned same time between silver electrode every time
Commutation step current, obtains reactant liquor.
Step 3, carries out the process of solid-liquid separation, washing and drying successively to reactant liquor；Wherein, solid-liquid separation be processed as from
The heart is separated, and its rotating speed is 6000r/min, the time is 8min, and carrying out washing treatment is to isolated using deionized water (or ethanol)
Solids carry out the cleaning of 2 times, it is centrifugation to separate solids during cleaning, dried be by cleaning after solids put
Dry at 60 DEG C.It is obtained as shown in figure 3, and the silver-colored triangular nano piece as shown in the spectral line in the b figures in Fig. 1.
Embodiment 4
Prepared concretely comprises the following steps：
Step 1, according to the sodium citrate aqueous solution of 0.085mol/L, the aqueous ascorbic acid of 0.09mol/L and 1 μ
The volume ratio of the Nano silver piece crystal seed aqueous solution of mol/L is 1：1.6：250 ratio, by sodium citrate aqueous solution and ascorbic acid
Aqueous solution is added in the Nano silver piece crystal seed aqueous solution under stirring, obtains mixed liquor.
Step 2, first puts a pair of silver electrode in mixed liquor with stirring.Injection commutation snap time then between silver electrode
It is 0.64mA/cm for 310s, electric current density2Commutation step current 50min after, be added to and volume ratio phase in step 1
With sodium citrate aqueous solution and aqueous ascorbic acid 3 times, and inject such as the aforementioned same time between silver electrode every time
Commutation step current, obtains reactant liquor.
Step 3, carries out the process of solid-liquid separation, washing and drying successively to reactant liquor；Wherein, solid-liquid separation be processed as from
The heart is separated, and its rotating speed is 7000r/min, the time is 6min, and carrying out washing treatment is to isolated using deionized water (or ethanol)
Solids carry out the cleaning of 2 times, it is centrifugation to separate solids during cleaning, dried be by cleaning after solids put
Dry at 70 DEG C.It is obtained as shown in figure 4, and the silver-colored triangular nano piece as shown in the spectral line in the b figures in Fig. 1.
Embodiment 5
Prepared concretely comprises the following steps：
Step 1, according to the sodium citrate aqueous solution of 0.095mol/L, the aqueous ascorbic acid of 0.08mol/L and 0.49 μ
The volume ratio of the Nano silver piece crystal seed aqueous solution of mol/L is 1：1.7：100 ratio, by sodium citrate aqueous solution and ascorbic acid
Aqueous solution is added in the Nano silver piece crystal seed aqueous solution under stirring, obtains mixed liquor.
Step 2, first puts a pair of silver electrode in mixed liquor with stirring.Injection commutation snap time then between silver electrode
It is 0.74mA/cm for 320s, electric current density2Commutation step current 40min after, be added to and volume ratio phase in step 1
With sodium citrate aqueous solution and aqueous ascorbic acid 4 times, and inject such as the aforementioned same time between silver electrode every time
Commutation step current, obtains reactant liquor.
Step 3, carries out the process of solid-liquid separation, washing and drying successively to reactant liquor；Wherein, solid-liquid separation be processed as from
The heart is separated, and its rotating speed is 8000r/min, the time is 5min, and carrying out washing treatment is to isolated using deionized water (or ethanol)
Solids carry out the cleaning of 3 times, it is centrifugation to separate solids during cleaning, dried be by cleaning after solids put
Dry at 80 DEG C.It is obtained as shown in figure 5, and the silver-colored triangular nano piece as shown in the spectral line in the b figures in Fig. 1.
Obviously, those skilled in the art can carry out various changes to the preparation method of the silver-colored triangular nano piece of the present invention
With modification without departing from the spirit and scope of the present invention.So, if these modifications and modification to the present invention belong to the present invention
Within the scope of claim and its equivalent technologies, then the present invention is also intended to comprising these changes and modification.
Claims (6)
1. a kind of preparation method of silver-colored triangular nano piece, including electrochemical process, it is characterised in that key step is as follows：
Step 1, the ascorbic acid according to the sodium citrate aqueous solution of 0.055～0.095mol/L, 0.08～0.12mol/L are water-soluble
The volume ratio of the Nano silver piece crystal seed aqueous solution of liquid and 0.49～19 μm of ol/L is 1：1.3～1.7：100～1000 ratio, will
Sodium citrate aqueous solution and aqueous ascorbic acid are added in the Nano silver piece crystal seed aqueous solution under stirring, obtain mixed liquor；
Step 2, first puts a pair of silver electrode in mixed liquor with stirring, and then between silver electrode, injection commutation snap time is
280～320s, electric current density are 0.37～0.74mA/cm2Commutation 40～80min of step current after, be added to and step
Volume ratio identical sodium citrate aqueous solution and aqueous ascorbic acid 0～4 time in rapid 1, and injection between silver electrode every time
Such as the commutation step current of aforementioned same time, reactant liquor is obtained；
Step 3, carries out the process of solid-liquid separation, washing and drying successively to reactant liquor, and it is 320nm～2.2 μm, thickness that the length of side is obtained
Spend the silver-colored triangular nano piece for 20～40nm.
2. the preparation method of silver-colored triangular nano piece according to claim 1, is characterized in that the mistake for obtaining Nano silver piece crystal seed
Cheng Wei, first according to the sodium citrate aqueous solution of 0.075mol/L, the silver nitrate aqueous solution of 0.1mol/L, the hydrogen peroxide of 30wt%,
The volume ratio of the sodium borohydride aqueous solution and deionized water of 0.1mol/L is 4：0.1：0.2：0.6：100 ratio, successively by lemon
Lemon acid sodium aqueous solution, silver nitrate aqueous solution, hydrogen peroxide and sodium borohydride aqueous solution stir 1h after adding in deionized water, are mixed
Liquid, then liquid to be mixed standing is two days later, carries out the process of solid-liquid separation, washing and drying to which successively.
3. the preparation method of silver-colored triangular nano piece according to claim 1, is characterized in that silver electrode, for filamentary silver, is being put
Before in the mixed liquor, first sanding and polishing reuses the cleaning of chloroform, acetone, ethanol and deionized water.
4. the preparation method of silver-colored triangular nano piece according to claim 1 and 2, is characterized in that solid-liquid separation is processed as being centrifuged
Separate, its rotating speed is 4000～8000r/min, the time is 5～10min.
5. the preparation method of silver-colored triangular nano piece according to claim 1 and 2, it is characterized in that carrying out washing treatment be using go from
Sub- water or ethanol carry out the cleaning of 1～3 time to isolated solids, and it is centrifugation to separate solids during cleaning.
6. the preparation method of silver-colored triangular nano piece according to claim 1 and 2, it is characterized in that dried be by cleaning after
Solids be placed at 40～80 DEG C dry.
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| CN109270052A (en) * | 2018-11-15 | 2019-01-25 | 云南大学 | A kind of uric acid detection method based on silver nanoparticle triangular plate |
| CN109500405A (en) * | 2019-01-17 | 2019-03-22 | 鲁东大学 | A kind of preparation method of triangle Nano silver piece |
| US10913865B2 (en) | 2018-12-06 | 2021-02-09 | Industrial Technology Research Institute | Modified metal nanoplate and conductive paste comprising the same |
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