CN114160785A - Preparation method of nano-silver solution with controllable mild conditions - Google Patents
Preparation method of nano-silver solution with controllable mild conditions Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000002245 particle Substances 0.000 claims abstract description 30
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 23
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 23
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 23
- 239000001509 sodium citrate Substances 0.000 claims abstract description 18
- 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 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 17
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 16
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 16
- 239000012498 ultrapure water Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000003223 protective agent Substances 0.000 claims abstract description 7
- 229910052709 silver Inorganic materials 0.000 claims abstract description 6
- 239000004332 silver Substances 0.000 claims abstract description 6
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 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 30
- 229960005070 ascorbic acid Drugs 0.000 claims description 15
- 235000010323 ascorbic acid Nutrition 0.000 claims description 15
- 239000011668 ascorbic acid Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 7
- 239000008103 glucose Substances 0.000 claims description 7
- 239000012279 sodium borohydride Substances 0.000 claims description 7
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 7
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- 238000009826 distribution Methods 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 4
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- 239000000243 solution Substances 0.000 description 24
- 239000000203 mixture Substances 0.000 description 17
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- 238000002156 mixing Methods 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 235000013570 smoothie Nutrition 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 108010039918 Polylysine Proteins 0.000 description 1
- 206010052428 Wound Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
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- 239000012535 impurity Substances 0.000 description 1
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- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920000656 polylysine Polymers 0.000 description 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000014599 transmission of virus Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000029663 wound healing Effects 0.000 description 1
Images
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
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- 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 discloses a nano silver solution with controllable particle size under the mild condition at room temperature, which is prepared by taking ultrapure water as a solvent, silver nitrate as a silver source, sodium citrate as a protective agent, polyvinylpyrrolidone as a dispersing agent and a reducing agent with a certain concentration, and has good dispersibility, spherical shape and agglomeration prevention, and the particle size of the nano silver solution is about 60 nm. The nano silver solution has good dispersibility, controllable particle size distribution and spherical shape. The invention designs the preparation method of the nano silver solution which has low requirement on equipment, simple process, mild reaction condition, simple and convenient operation, is suitable for large-scale production and has good product performance.
Description
Technical Field
The invention belongs to the technical field of new nano materials, and particularly relates to a preparation method of a nano silver solution with controllable room temperature and mild conditions.
Background
Nanotechnology is the most promising new technology in the 21 st century, combines biological principles with physical and chemical processes to generate nanoparticles with specific functions, is widely applied to the fields of information, biology, medicine, chemical industry, aerospace, energy, national defense and the like, and has huge market potential. In recent years, metal nanoparticles have attracted much attention because of their unique magnetic, electronic configuration, optical, and other properties. The nano silver material has stable physical and chemical properties, has excellent properties in the aspects of electricity, optics, catalysis and the like, and is widely applied to the fields of biomedicine, ceramic materials, environment-friendly materials, coatings and the like. More importantly, few nano-silver can generate strong bactericidal action, broad-spectrum sterilization and no drug resistance, can promote the healing of wounds, the growth of cells and the repair of damaged cells, has no toxic reaction and no irritation reaction to skin, and opens up a broad prospect for widely applying nano-silver to antibiosis.
The nano silver has the particle size distribution of 1-100 nm, the atomic arrangement is represented as a 'medium state' between a solid and molecules, the specific surface area is extremely large, and the nano silver has a surface effect, a small-size effect and a macroscopic quantum tunnel effect, so that the surface activity of the nano silver is enhanced, and meanwhile, the nano silver has very strong penetrating power and antibacterial capability. Therefore, the nano silver solution with the controllable particle size can be applied to daily life, such as masks, clothes and the like, and can play a strong role in sterilization and disinfection.
AgNPs are synthesized by different physical and chemical methods such as a sol-gel method, a solvent-thermal synthesis method, a chemical reduction method, a laser ablation method, an inert gas condensation method and the like, the principle of the physical method is simple, and the obtained product has few impurities and good quality, but has higher requirements on instruments and equipment and high production cost. Chemical methods are simpler, but have higher requirements on the control of the particle size, and the particle size is controlled by variable factors with different conditions.
Chinese patent 201010148262.4 discloses a method for preparing water-soluble nano silver, which comprises dissolving silver salt and protective agent in water at 30-60 deg.C under stirring, adjusting pH, adding reducing agent into the reaction system after the solution system is clear and transparent for 5-20 min, and continuously stirring for 5-30 min.
Chinese patent 201410344102.5 discloses a method for preparing nano-silver sol, which comprises mixing silver nitrate solution or silver ammonia solution with polylysine aqueous solution, stirring and reacting at 500-100 deg.C for 30-180 min to obtain nano-silver sol.
Chinese patent 201410850968.3 discloses a method for preparing and storing colorless nano silver sol by low temperature technology, which comprises dissolving silver source in water, mixing uniformly, freezing, and pulverizing to obtain silver-containing raw material smoothie. Then dissolving the reducing agent in water, uniformly mixing, freezing and crushing to obtain the smoothie containing the reducing agent. Mixing the obtained ice sand containing the silver raw material with the ice sand containing the reducing agent, and grinding to obtain nano silver ice crystals.
The above invention requires temperature and pH adjustment within specific ranges, and is not suitable for large-scale industrial production.
Disclosure of Invention
The invention aims to provide a method for preparing a nano silver solution, which has the advantages of low requirement on equipment, simple process, mild reaction condition, simple and convenient operation, suitability for large-scale production and good product performance, aiming at the problems in the background technology.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a nano-silver solution with controllable mild conditions comprises the steps of taking ultrapure water as a solvent, 99.95% of high-grade pure silver nitrate as a silver source, sodium citrate (TSC) as a protective agent, polyvinylpyrrolidone (PVP, K30) as a dispersing agent, ascorbic acid, glucose or sodium borohydride as a reducing agent, sequentially adding 0.05mol/L silver nitrate 50 mu L, 0.075mol/L sodium citrate (TSC) 0.3-0.8 mL and 0.0175mol/L polyvinylpyrrolidone (PVP, K30) 0.3-1.0 mL into 50mL of ultrapure water at room temperature, stirring the solution system for 3min at a rotating speed of 400r/min, adding 0.1mol/L reducing agent 0.2-0.5 mL into a reaction system, continuously stirring for 30min for reaction, and preparing the nano-silver solution with good dispersibility and agglomeration prevention, wherein the particle size of the nano-silver solution is about 60nm, the nano-silver solution has good dispersibility, the particle size distribution can be controlled, and the shape of the nano silver is spherical.
Further, the molar ratio of The Sodium Citrate (TSC) to the silver nitrate is 9-24: 1.
Furthermore, the molar ratio of the polyvinylpyrrolidone (PVP, K30) to the silver nitrate is 2.1-7: 1.
Further, the molar ratio of the reducing agent to the silver nitrate is 8-20: 1.
The invention has the beneficial effects that:
the invention systematically studies the reduction action and mechanism of reducing agents such as sodium borohydride, glucose, ascorbic acid and the like on silver nitrate, controls the nucleation size, shape and speed of nano-silver by adjusting the type and dosage of the reducing agents, and the obtained nano-silver solution has high stable dispersion performance, has no obvious agglomeration and sedimentation phenomenon within three months, has the average grain diameter of the nano-silver of about 60nm, and is diluted by ultrapure water with the blending concentration to prevent the influence of ions in water.
The invention has low preparation cost, low energy consumption, no generation of toxic and harmful wastes and meets the requirement of green production. Low requirement on equipment, simple process, mild reaction condition, simple and convenient operation, suitability for large-scale production and good product performance.
The preparation process is simple, the precise regulation and control of the particle size and the shape of the nano silver particles can be realized, and the product can be used for antibacterial medical materials for wound healing and the like, antibacterial textiles and shoes and socks, and can act on the mask to more effectively inhibit the transmission of viruses.
Drawings
FIG. 1 is a TEM image of a nano-silver solution of the present invention (TSC 0.3-0.8 mL (0.075 mol/L));
FIG. 2 is a TEM image of a nano-silver solution of the present invention (ascorbic acid 0.5mL (0.1 mol/L));
fig. 3 is a particle size distribution diagram of the nano silver solution prepared by the present invention.
Detailed Description
The following description of the embodiments of the present invention is provided in order to better understand the present invention for those skilled in the art with reference to the accompanying drawings. It is to be expressly noted that in the following description, a detailed description of known functions and designs will be omitted when it may obscure the subject matter of the present invention.
The invention discloses a preparation method of a nano-silver solution with controllable mild conditions, which comprises the steps of sequentially adding 50 mu L (0.05 mol/L) of silver nitrate, 0.3-0.8 mL (0.075 mol/L) of sodium citrate (TSC) and 0.3-1.0 mL (0.0175 mol/L) of polyvinylpyrrolidone into 50mL of ultrapure water, rapidly stirring at a rotation speed of 400r/min, uniformly dispersing, adding one of 0.2-0.5 mL (0.1 mol/L) of ascorbic acid, 0.2 mL (0.1 mol/L) of sodium borohydride or 0.2 mL (0.1M) of glucose after 3 minutes, and continuously stirring for 30 minutes.
Examples 1-8 test materials were added in the amounts shown in the table below.
Example 1
50 mu L (0.05 mol/L) of silver nitrate, 0.3 mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone are sequentially added into 50mL of ultrapure water, the mixture is rapidly stirred and uniformly dispersed at the rotating speed of 400r/min, 0.2 mL (0.1 mol/L) of ascorbic acid is added after 3 minutes, and the mixture is continuously stirred for 30 minutes.
Example 2
50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone are sequentially added into 50mL of ultrapure water, the mixture is rapidly stirred and uniformly dispersed at the rotating speed of 400r/min, 0.2 mL (0.1 mol/L) of ascorbic acid is added after 3 minutes, and the mixture is continuously stirred for 30 minutes.
Example 3
50 mu L (0.05 mol/L) of silver nitrate, 0.8 mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone are sequentially added into 50mL of ultrapure water, the mixture is rapidly stirred and uniformly dispersed at the rotating speed of 400r/min, 0.2 mL (0.1 mol/L) of ascorbic acid is added after 3 minutes, and the mixture is continuously stirred for 30 minutes.
Example 4
50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.3 mL (0.0175 mol/L) of polyvinylpyrrolidone are sequentially added into 50mL of ultrapure water, the mixture is rapidly stirred and uniformly dispersed at the rotating speed of 400r/min, 0.2 mL (0.1 mol/L) of ascorbic acid is added after 3 minutes, and the mixture is continuously stirred for 30 minutes.
Example 5
50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 1.0 mL (0.0175 mol/L) of polyvinylpyrrolidone are sequentially added into 50mL of ultrapure water, the mixture is rapidly stirred and uniformly dispersed at the rotating speed of 400r/min, 0.2 mL (0.1 mol/L) of ascorbic acid is added after 3 minutes, and the mixture is continuously stirred for 30 minutes.
Example 6
50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone are sequentially added into 50mL of ultrapure water, the mixture is rapidly stirred and uniformly dispersed at the rotating speed of 400r/min, 0.5mL (0.1 mol/L) of ascorbic acid is added after 3 minutes, and the mixture is continuously stirred for 30 minutes.
Example 7
50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone are sequentially added into 50mL of ultrapure water, the mixture is rapidly stirred and uniformly dispersed at the rotating speed of 400r/min, 0.2 mL (0.1 mol/L) of sodium borohydride is added after 3 minutes, and the mixture is continuously stirred for 30 minutes.
Example 8
50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone are sequentially added into 50mL of ultrapure water, the mixture is rapidly stirred and uniformly dispersed at the rotating speed of 400r/min, 0.2 mL (0.1 mol/L) of glucose is added after 3 minutes, and the stirring is continued for 30 minutes.
The particle size distribution, average particle size and polydispersity index test results of the nano-silver solutions of examples 1-8 are shown in the following table:
in examples 1, 2 and 3, sodium citrate (TSC) (0.075 mol/L) is used as a variable, the effect of the TSC as a protective agent is obvious, the particle size gradually decreases with the increase of the volume of the TSC solution, but after the TSC reaches a certain volume, the dispersibility becomes poor with the increase of the volume of the TSC solution, the particle size tends to increase slightly, and the agglomeration phenomenon of nano silver particles is obvious. From the TEM image of fig. 1, it is known that the TSC as the protective agent has a great influence on the shape of the nano-silver, and when the volume of the TSC is 0.5mL, the sphericity and dispersibility of the nano-silver are optimal, and the average particle size is about 56.71 nm.
In examples 2, 4 and 5, the dispersion agent PVP had a certain effect on the particle size and the dispersion uniformity, with 0.3-1.0 mL (0.0175 mol/L) of polyvinylpyrrolidone (K30) as the variable. With the increase of the dispersing agent, the particle size of the nano silver particles has an optimal PVP usage amount, so that the particle size distribution of the nano silver is more balanced. When the volume of PVP is 0.6mL, the polydispersity index of the nano silver solution is the smallest, namely the particle size distribution is the narrowest. In examples 2 and 6, with 0.2-0.5 mL (0.1 mol/L) of ascorbic acid as a variable, it can be seen from the TEM image of fig. 2 that the shape of the nano-silver is changed from spherical to strip with the increase of ascorbic acid, and the average particle diameter and the polydispersity index of the nano-silver solution are increased.
In examples 2, 7 and 8, it was found that the polydispersity index of the nano-silver solution prepared from glucose was the smallest, but the average particle size was larger, and the average particle size of the nano-silver prepared from sodium borohydride was the largest, using ascorbic acid 0.2 (0.1 mol/L), sodium borohydride 0.2 mL (0.1 mol/L) and glucose 0.2 mL (0.1M) as the reducing agents, respectively.
According to the invention, the particle size distribution, the average particle size and the polydispersity index of the nano silver solution are closely related to the types and the dosages of the protective agent, the dispersing agent and the reducing agent, 50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone are sequentially added into 50mL of ultrapure water, the mixture is rapidly stirred and uniformly dispersed at the rotating speed of 400r/min, 0.2 mL (0.1 mol/L) of ascorbic acid is added after 3 minutes, and the mixture is continuously stirred for 30 minutes to prepare the spherical nano silver solution with good dispersibility and narrow particle size distribution.
It is to be understood that the above-described embodiments are only a few, and not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (4)
1. A preparation method of a nano-silver solution with controllable mild conditions is characterized by comprising the following steps: the method comprises the steps of taking ultrapure water as a solvent, 99.95% silver nitrate as a silver source, sodium citrate as a protective agent, polyvinylpyrrolidone as a dispersing agent, ascorbic acid, glucose or sodium borohydride as a reducing agent, sequentially adding 50 mu L of silver nitrate of 0.05mol/L, 0.3-0.8 mL of sodium citrate of 0.075mol/L and 0.3-1.0 mL of polyvinylpyrrolidone of 0.0175mol/L into 50mL of ultrapure water at room temperature, stirring for 3min at the rotating speed of 400r/min, adding 0.2-0.5 mL of reducing agent of 0.1mol/L, continuously stirring and reacting for 30min to obtain the spherical nano-silver solution with the particle size of 60 nm.
2. The preparation method of the nano-silver solution with the controllable mild condition according to claim 1, wherein the molar ratio of the sodium citrate to the silver nitrate is 9-24: 1.
3. The preparation method of the nano-silver solution with controllable mild conditions according to claim 1, wherein the molar ratio of the polyvinylpyrrolidone to the silver nitrate is 2.1-7: 1.
4. The preparation method of the nano-silver solution with the controllable mild condition according to claim 1, wherein the molar ratio of the reducing agent to the silver nitrate is 8-20: 1.
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| CN115846648A (en) * | 2022-12-13 | 2023-03-28 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | High-activity spherical silver powder with cracking-shaped rough surface structure and preparation method thereof |
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