CN106493385B - 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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- CN106493385B CN106493385B CN201610932056.XA CN201610932056A CN106493385B CN 106493385 B CN106493385 B CN 106493385B CN 201610932056 A CN201610932056 A CN 201610932056A CN 106493385 B CN106493385 B CN 106493385B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 87
- 229910052709 silver Inorganic materials 0.000 claims abstract description 78
- 239000004332 silver Substances 0.000 claims abstract description 78
- 239000007864 aqueous solution Substances 0.000 claims abstract description 77
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 50
- 238000000926 separation method Methods 0.000 claims abstract description 47
- 238000005406 washing Methods 0.000 claims abstract description 33
- 239000001509 sodium citrate Substances 0.000 claims abstract description 30
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 26
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 25
- 239000013078 crystal Substances 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 22
- 239000007787 solid Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 18
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000002135 nanosheet Substances 0.000 claims description 45
- 239000011259 mixed solution Substances 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 239000002211 L-ascorbic acid Substances 0.000 claims description 7
- 235000000069 L-ascorbic acid Nutrition 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- 239000012279 sodium borohydride Substances 0.000 claims description 7
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 3
- 238000002848 electrochemical method Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000002347 injection Methods 0.000 abstract description 2
- 239000007924 injection Substances 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract 1
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 9
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 230000003595 spectral effect Effects 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000002055 nanoplate Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Classifications
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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
-
- 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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- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of preparation methods of silver-colored triangular nano piece.It adds in 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 of silver electrode is put in mixed liquor with stirring, injection commutation snap time is 280~320s between silver electrode, current density is 0.37~0.74mA/cm240~80min of commutation step current after, sodium citrate aqueous solution and aqueous ascorbic acid 0~4 time are added thereto, and the commutation step current of such as aforementioned similary time is injected between silver electrode every time, obtain reaction solution, later, it carries out separation of solid and liquid, washing and the processing of drying successively to reaction solution, product is made.It has the characteristics of environmentally protective, and product can be made to be extremely easy to be widely used in the fields such as conducting resinl.
Description
Technical Field
The invention relates to a preparation method of silver nanosheets, in particular to a preparation method of silver triangular nanosheets.
Background
Silver is the metal with the best electrical and thermal conductivity, and when silver is in the nanometer scale, silver nanomaterials have unique physical and chemical properties not found in bulk materials. The appearance of these properties depends in turn on factors such as their morphology and size. For the silver nano-sheet, the silver nano-sheet has the advantages of large specific surface area, low surface energy, strong bending resistance, good oxidation resistance and good fluidity, and the sheet-to-sheet contact is realized, so that the contact area is large, and the resistance is low. Therefore, it has attracted much attention and has been used in the field of conductive adhesives and the like. In recent years, a series of methods for preparing silver nanoplates have been developed, such as the article entitled "One-step growth of triangular silver nanoplates with predictible dimensions on a large scale", nanoscal,6,4513(2014) "(" large scale One-step synthesis of size-controllable triangular silver nanoplates ", nano-scale 2014, No. 6, page 4513). The synthesis method reported in the article is a solution method, wherein TSC is used as a surface coating agent, sodium borohydride is used as a reducing agent, silver nitrate is used as a precursor, a seed crystal solution is synthesized in an aqueous solution, and then the prepared seed crystal solution is utilized, ascorbic acid is used as a reducing agent, TSC is used as a coating agent, and acetonitrile is used as a complexing agent, so that the silver nanosheet with a large size is further synthesized. Although the triangular silver nanosheets can be obtained by the method, acetonitrile serving as a silver ion complexing agent is used for controlling the dynamic growth process of the silver nanosheets, and the acetonitrile is a toxic substance which has great harm to human bodies.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a green and environment-friendly preparation method of silver triangular nanosheets.
In order to solve the technical problem of the invention, the adopted technical scheme is as follows: the preparation method of the silver triangular nanosheet comprises an electrochemical method, and particularly comprises the following main steps:
step 1, according to the volume ratio of 0.055-0.095 mol/L sodium citrate aqueous solution, 0.08-0.12 mol/L ascorbic acid aqueous solution and 0.49-19 mu mol/L silver nanosheet seed crystal aqueous solution of 1: 1.3-1.7: adding a sodium citrate aqueous solution and an ascorbic acid aqueous solution into a silver nanosheet seed crystal aqueous solution under stirring in a proportion of 100-1000 to obtain a mixed solution;
step 2, firstly placing a pair of silver electrodes in the mixed solution under stirring, and then injecting the reversing step time of 280-320 s and the current density of 0.37-0.74 mA/cm between the silver electrodes2After the reversing step current is 40-80 min, adding the sodium citrate aqueous solution and the ascorbic acid aqueous solution which have the same volume ratio as the step 1 for 0-4 times, and injecting the reversing step current for the same time between the silver electrodes every time to obtain a reaction solution;
and 3, sequentially carrying out solid-liquid separation, washing and drying on the reaction liquid to obtain the silver triangular nanosheets with the side length of 320 nm-2.2 mu m and the thickness of 20-40 nm.
As a further improvement of the preparation method of the silver triangular nanosheet:
preferably, the process for obtaining the silver nanosheet seed crystal comprises the following steps of firstly, mixing 0.075mol/L sodium citrate aqueous solution, 0.1mol/L silver nitrate aqueous solution, 30 wt% hydrogen peroxide, 0.1mol/L sodium borohydride aqueous solution and deionized water according to a volume ratio of 4: 0.1: 0.2: 0.6: 100, adding a sodium citrate aqueous solution, a silver nitrate aqueous solution, hydrogen peroxide and a sodium borohydride aqueous solution into deionized water in sequence, stirring for 1h to obtain a mixed solution, standing the mixed solution for two days, and then carrying out solid-liquid separation, washing and drying on the mixed solution in sequence.
Preferably, the silver electrode is silver wire, and before the silver electrode is placed in the mixed solution, the silver electrode is polished and then cleaned by using chloroform, acetone, ethanol and deionized water.
Preferably, the solid-liquid separation treatment is centrifugal separation, the rotating speed of the centrifugal separation is 4000-8000 r/min, and the time is 5-10 min.
Preferably, the washing treatment is to wash the separated solid substance for 1-3 times by using deionized water or ethanol, and the solid substance separation during washing is centrifugal separation.
Preferably, the drying treatment is drying the cleaned solid at 40-80 ℃.
Compared with the prior art, the beneficial effects are that:
firstly, the prepared product is respectively characterized by using a scanning electron microscope and an X-ray diffractometer, and the result shows that the product is a triangular nanosheet, the side length of the nanosheet is 320 nm-2.2 mu m, and the thickness of the nanosheet is 20-40 nm. The triangular nanosheets are silver triangular nanosheets.
Secondly, the preparation method is scientific and effective. The method not only prepares the product with high side length-to-thickness ratio, namely the silver triangular nanosheet, but also can effectively control the kinetic growth process of the silver nanosheet by controlling the concentration of each raw material solution, the magnitude and time of the reversing step current, adding the sodium citrate aqueous solution and the ascorbic acid aqueous solution and continuing electrolysis, namely obtains the product with larger size and has the characteristics of environmental protection; so that the product can be easily and widely applied to the fields of conductive adhesive and the like.
Drawings
Fig. 1 is one of the results of characterizing the product obtained by the preparation method using a Scanning Electron Microscope (SEM) and an X-ray diffraction (XRD) instrument, respectively. Wherein, the a picture in figure 1 is SEM image of the product, and the b picture is XRD spectrogram of the product; figure 1 shows and confirms that the product is a silver triangular nanoplate with an edge length of about 320 nm.
Fig. 2 is one of the results of characterization of the obtained product using a scanning electron microscope. SEM images showed the product to be approximately 900nm on a side.
Fig. 3 is one of the results of characterization of the obtained product using a scanning electron microscope. The SEM image showed the product to have an edge length of about 1.2 μm.
Fig. 4 is one of the results of characterization of the obtained product using a scanning electron microscope. The SEM image showed the product to have an edge length of about 1.74 μm.
Fig. 5 is one of the results of characterization of the obtained product using a scanning electron microscope. The SEM image showed the product to be about 2.0 μm on a side.
Detailed Description
Preferred embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
First commercially available or manufactured on its own:
an aqueous solution of sodium citrate;
an aqueous ascorbic acid solution;
a silver nanosheet seed crystal aqueous solution;
silver wire as silver electrode.
Wherein,
the process for obtaining the silver nano-sheet seed crystals in the silver nano-sheet seed crystal water solution comprises the following steps of firstly, according to the volume ratio of 0.075mol/L sodium citrate water solution, 0.1mol/L silver nitrate water solution, 30 wt% hydrogen peroxide, 0.1mol/L sodium borohydride water solution and deionized water being 4: 0.1: 0.2: 0.6: 100, sequentially adding a sodium citrate aqueous solution, a silver nitrate aqueous solution, hydrogen peroxide and a sodium borohydride aqueous solution into deionized water, stirring for 1h to obtain a mixed solution, standing the mixed solution for two days, and sequentially carrying out solid-liquid separation, washing and drying on the mixed solution; the solid-liquid separation treatment is centrifugal separation, the rotating speed is 4000-8000 r/min, the time is 5-10 min, the washing treatment is to use deionized water (or ethanol) to wash the separated solid for 1-3 times, the solid separation during washing is centrifugal separation, and the drying treatment is to dry the washed solid at 40-80 ℃.
Before the silver wire is placed in the mixed solution, the silver wire is polished and then cleaned by using chloroform, acetone, ethanol and deionized water.
Then, the process of the present invention is carried out,
example 1
The preparation method comprises the following specific steps:
step 1, according to the volume ratio of 0.055mol/L sodium citrate aqueous solution, 0.12mol/L ascorbic acid aqueous solution and 19 mu mol/L silver nanosheet seed crystal aqueous solution of 1: 1.3: and (1000) adding a sodium citrate aqueous solution and an ascorbic acid aqueous solution into the silver nanosheet seed crystal aqueous solution under stirring to obtain a mixed solution.
And 2, firstly, placing a pair of silver electrodes in the mixed solution under stirring. Then injecting commutation step time of 280s and current density of 0.37mA/cm between silver electrodes2The step current of commutation is 80min, and reaction liquid is obtained.
Step 3, carrying out solid-liquid separation, washing and drying treatment on the reaction solution in sequence; wherein the solid-liquid separation is centrifugal separation, the rotating speed is 4000r/min, the time is 10min, the washing treatment is washing the solid obtained by separation for 1 time by using deionized water (or ethanol), the separation of the solid during washing is centrifugal separation, and the drying treatment is drying the washed solid at 40 ℃. Silver triangular nanosheets were produced as shown in graph a in fig. 1, and as shown by the spectral lines in graph b in fig. 1.
Example 2
The preparation method comprises the following specific steps:
step 1, according to the volume ratio of 0.065mol/L sodium citrate aqueous solution, 0.11mol/L ascorbic acid aqueous solution and 13 mu mol/L silver nanosheet seed crystal aqueous solution of 1: 1.4: 775 adding sodium citrate aqueous solution and ascorbic acid aqueous solution into the stirred silver nanometer sheet seed crystal aqueous solution to obtain mixed solution.
And 2, firstly, placing a pair of silver electrodes in the mixed solution under stirring. Then the step time of the injection commutation between the silver electrodes is 290s, and the current density is 0.46mA/cm2After 70min, the same volume ratio of the aqueous solution of sodium citrate and the aqueous solution of ascorbic acid as in step 1 was added thereto 1 time, and the reverse step current was injected between the silver electrodes for the same time as described above to obtain a reaction solution.
Step 3, carrying out solid-liquid separation, washing and drying treatment on the reaction solution in sequence; wherein the solid-liquid separation is centrifugal separation with the rotation speed of 5000r/min and the time of 9min, the washing is 1 time washing of the solid obtained by separation with deionized water (or ethanol), the separation of the solid during washing is centrifugal separation, and the drying is drying the solid after washing at 50 ℃. Silver triangular nanosheets were produced as shown in fig. 2, and as shown by the spectral lines in the b-diagram in fig. 1.
Example 3
The preparation method comprises the following specific steps:
step 1, according to the volume ratio of 0.075mol/L sodium citrate aqueous solution, 0.10mol/L ascorbic acid aqueous solution and 7 mu mol/L silver nanosheet seed crystal aqueous solution of 1: 1.5: 450, adding the sodium citrate aqueous solution and the ascorbic acid aqueous solution into the silver nanosheet seed crystal aqueous solution under stirring to obtain a mixed solution.
And 2, firstly, placing a pair of silver electrodes in the mixed solution under stirring. Then injecting commutation step time of 300s and current density of 0.55mA/cm between silver electrodes2After 60min, the same volume ratio of the sodium citrate aqueous solution and the ascorbic acid aqueous solution as in step 1 was added thereto 2 times, and a reverse step current was injected between the silver electrodes for the same time as described above each time, to obtain a reaction solution.
Step 3, carrying out solid-liquid separation, washing and drying treatment on the reaction solution in sequence; wherein the solid-liquid separation is centrifugal separation at 6000r/min for 8min, the washing is washing with deionized water (or ethanol) for 2 times, the separation is centrifugal separation, and the drying is drying at 60 deg.C. Silver trigonal nanoplates as shown in fig. 3 and as shown by the spectral lines in the b diagram in fig. 1 were produced.
Example 4
The preparation method comprises the following specific steps:
step 1, according to the volume ratio of 0.085mol/L sodium citrate aqueous solution, 0.09mol/L ascorbic acid aqueous solution and 1 mu mol/L silver nanosheet seed crystal aqueous solution of 1: 1.6: and (5) adding a sodium citrate aqueous solution and an ascorbic acid aqueous solution into the silver nanosheet seed crystal aqueous solution under stirring in a proportion of 250 to obtain a mixed solution.
And 2, firstly, placing a pair of silver electrodes in the mixed solution under stirring. Injecting commutation step time of 310s and current density of 0.64mA/cm between silver electrodes2After 50min, the same volume ratio of the sodium citrate aqueous solution and the ascorbic acid aqueous solution as in step 1 was added thereto 3 times, and a reverse step current was injected between the silver electrodes for the same time as described above each time, to obtain a reaction solution.
Step 3, carrying out solid-liquid separation, washing and drying treatment on the reaction solution in sequence; wherein the solid-liquid separation is centrifugal separation with the rotation speed of 7000r/min and the time of 6min, the washing is 2 times of washing of the solid obtained by separation with deionized water (or ethanol), the separation of the solid during washing is centrifugal separation, and the drying is drying of the solid after washing at 70 ℃. Silver trigonal nanoplates as shown in fig. 4 and as shown by the spectral lines in the b diagram in fig. 1 were produced.
Example 5
The preparation method comprises the following specific steps:
step 1, according to the volume ratio of 0.095mol/L sodium citrate aqueous solution, 0.08mol/L ascorbic acid aqueous solution and 0.49 mu mol/L silver nanosheet seed crystal aqueous solution of 1: 1.7: and (3) adding a sodium citrate aqueous solution and an ascorbic acid aqueous solution into the silver nanosheet seed crystal aqueous solution under stirring in a ratio of 100 to obtain a mixed solution.
And 2, firstly, placing a pair of silver electrodes in the mixed solution under stirring. Then injecting commutation step time of 320s and current density of 0.74mA/cm between silver electrodes2After 40min, the same volume ratio of the aqueous solution of sodium citrate and the aqueous solution of ascorbic acid as in step 1 was added thereto 4 times, and the reverse step current was injected between the silver electrodes for the same time as described above each time to obtain a reaction solution.
Step 3, carrying out solid-liquid separation, washing and drying treatment on the reaction solution in sequence; wherein the solid-liquid separation is centrifugal separation with rotation speed of 8000r/min and time of 5min, the washing is washing with deionized water (or ethanol) for 3 times, the separation of solid is centrifugal separation, and the drying is drying at 80 deg.C. Silver trigonal nanoplates as shown in fig. 5 and as shown by the spectral lines in the b diagram in fig. 1 were produced.
It is apparent that those skilled in the art can make various modifications and variations to the method for preparing the silver trigonal nanoplatelets of the present invention without departing from the spirit and scope of the present invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.
Claims (5)
1. A preparation method of silver triangular nanosheets comprises an electrochemical method and is characterized by mainly comprising the following steps:
step 1, according to the volume ratio of 0.055-0.095 mol/L sodium citrate aqueous solution, 0.08-0.12 mol/L ascorbic acid aqueous solution and 0.49-19 mu mol/L silver nanosheet seed crystal aqueous solution of 1: 1.3-1.7: 100-1000, adding a sodium citrate aqueous solution and an ascorbic acid aqueous solution into a silver nanosheet seed crystal aqueous solution under stirring to obtain a mixed solution, wherein the process for obtaining the silver nanosheet seed crystal comprises the following steps of firstly, according to a volume ratio of 0.075mol/L sodium citrate aqueous solution, 0.1mol/L silver nitrate aqueous solution, 30 wt% hydrogen peroxide, 0.1mol/L sodium borohydride aqueous solution and deionized water of 4: 0.1: 0.2: 0.6: 100, sequentially adding a sodium citrate aqueous solution, a silver nitrate aqueous solution, hydrogen peroxide and a sodium borohydride aqueous solution into deionized water, stirring for 1h to obtain a mixed solution, standing the mixed solution for two days, and sequentially carrying out solid-liquid separation, washing and drying on the mixed solution;
step 2, firstly placing a pair of silver electrodes in the mixed solution under stirring, and then injecting the reversing step time of 280-320 s and the current density of 0.37-0.74 mA/cm between the silver electrodes2After the reversing step current is 40-80 min, adding the sodium citrate aqueous solution and the ascorbic acid aqueous solution which have the same volume ratio as the step 1 for 0-4 times, and injecting the reversing step current for the same time between the silver electrodes every time to obtain a reaction solution;
and 3, sequentially carrying out solid-liquid separation, washing and drying on the reaction liquid to obtain the silver triangular nanosheets with the side length of 320 nm-2.2 mu m and the thickness of 20-40 nm.
2. The method for preparing silver triangular nanosheets of claim 1, wherein the silver electrode is a silver wire, and is polished and washed with chloroform, acetone, ethanol and deionized water before being placed in the mixed solution.
3. The method for producing a silver trigonal nanosheet according to claim 1, wherein the solid-liquid separation treatment is centrifugal separation at a rotation speed of 4000 to 8000r/min for 5 to 10 min.
4. The method for producing a silver trigonal nanosheet according to claim 1, wherein the washing treatment is washing of the separated solid with deionized water or ethanol for 1 to 3 times, and the separation of the solid during washing is centrifugal separation.
5. The method for preparing silver triangular nanosheets according to claim 1, wherein the drying treatment is drying the washed solid at 40 to 80 ℃.
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| TWI698507B (en) | 2018-12-06 | 2020-07-11 | 財團法人工業技術研究院 | Modified metal nanoplate and conductive paste comprising the same |
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