CN113263183B - Nano silver lipid dispersion liquid and preparation method thereof - Google Patents
Nano silver lipid dispersion liquid and preparation method thereof Download PDFInfo
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- CN113263183B CN113263183B CN202110380111.XA CN202110380111A CN113263183B CN 113263183 B CN113263183 B CN 113263183B CN 202110380111 A CN202110380111 A CN 202110380111A CN 113263183 B CN113263183 B CN 113263183B
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Abstract
The invention provides a preparation method of nano silver lipid dispersion liquid, which comprises the following steps: adding the polyalcohol into silver nitrate solution and then adjusting the temperature to 20-25 ℃; dissolving sodium hydroxide in water, sequentially adding PVP powder and a regulator, and adjusting to 20-25 ℃; dissolving polysaccharide in water, stirring and adjusting the temperature to 20-25 ℃; mixing the first solution and the second solution, stirring for 10-20 min, adding the third solution, continuously stirring for 10-20 min, and performing gradient temperature rise; cooling the nano silver feed liquid to room temperature, and washing under the pressure of 0.2-0.6 Mpa; concentrating and centrifuging the nano-silver feed liquid; dispersing the pasty nano silver in an organic solvent to obtain pasty nano silver dispersion liquid, and then carrying out ultrasonic centrifugation; dispersing the pasty nano silver in lipid, and then evaporating under vacuum at the temperature of 90-200 ℃. The invention also provides a nano silver lipid dispersion liquid. The nano silver lipid dispersion liquid has low sintering temperature, uniform particle size and low content of the dispersant.
Description
Technical Field
The invention belongs to the technical field of metal conduction, and particularly relates to a nano silver lipid dispersion liquid and a preparation method thereof.
Background
The heterojunction solar cell is a hybrid solar cell made of a crystalline silicon substrate and an amorphous silicon thin film. The surface electrode metalized silver paste generally uses n-type crystalline silicon as a substrate and amorphous silicon with wide band gaps as an emitter, the battery has a double-sided symmetrical structure, two thin intrinsic amorphous silicon layers are arranged on two sides of the n-type silicon substrate, a p-type amorphous silicon emitter layer is arranged on the front side, and an n-type amorphous silicon film back surface field is arranged on the back side; and depositing a transparent conductive oxide film (TCO) on the amorphous silicon thin layers on the two sides by a sputtering method, finally printing silver paste on the TCO, and drying at low temperature to form the conductive grid.
The heterogeneous solar cell silver paste consists of flake silver powder, dendritic silver powder or submicron silver and nano silver particles, a solvent and resin, and the metallization temperature is less than 200 ℃. Therefore, the silver paste of the heterojunction solar cell needs to be metallized and sintered on TCO at the temperature of below 200 ℃, the silver paste silver powder of the heterojunction solar cell is formed by mixing micron-sized silver powder with large particle size and submicron and nano silver, and the required submicron and nano silver needs to have the advantages of easiness in low-temperature sintering, uniformity in particle size and lower content of a dispersing agent so as to prevent organic matters from blocking the silver powder from being sintered.
Disclosure of Invention
The invention aims to provide a preparation method of nano silver lipid dispersion liquid, the nano silver lipid dispersion liquid prepared by the method has low sintering temperature, uniform particle size and low dispersant content, and meets the requirements of silver paste powder of a heterojunction solar cell.
The second purpose of the invention is to provide a nano silver lipid dispersion liquid.
In order to achieve one of the purposes, the invention adopts the following technical scheme:
a preparation method of nano silver lipid dispersion liquid comprises the following steps:
step one, adding polyalcohol into silver nitrate solution with the mass volume concentration of 10-50 g/L, and adjusting the temperature to 20-25 ℃ to obtain first solution;
step two, sequentially adding PVP powder and a slow-release pH regulator into a sodium hydroxide solution with the mass volume concentration of 3-7 g/L, and adjusting the temperature to 20-25 ℃ to obtain a second solution;
dissolving polysaccharide in water, stirring, and adjusting the temperature to 20-25 ℃ to obtain a third solution;
step four, mixing the first solution and the second solution, stirring for 10-20 min, adding the third solution, continuously stirring for 10-20 min, and performing gradient heating to obtain nano-silver feed liquid;
step five, cooling the nano silver feed liquid to room temperature, and then washing under the pressure of 0.2-0.6 Mpa until the conductivity of the nano silver feed liquid is less than 20 microSiemens;
step six, concentrating and centrifuging the washed nano-silver feed liquid to obtain paste nano-silver;
step seven, dispersing the pasty nano silver in an organic solvent to obtain a pasty nano silver dispersion liquid, and then carrying out ultrasonic centrifugal treatment;
step eight, dispersing the paste-like nano silver subjected to the ultrasonic centrifugal treatment in lipids, and then performing vacuum reduced pressure evaporation at the temperature of 90-200 ℃ to obtain nano silver lipid dispersion liquid.
Further, in the first step, the mass of the polyhydric alcohol is 5-10 times of the mass of the silver nitrate in the silver nitrate solution;
in the first step, the polyol is one or a mixture of more of ethylene glycol, glycerol and diethylene glycol.
Further, in the second step, the mass of the sodium hydroxide, the PVP and the slow-release pH regulator in the sodium hydroxide solution is respectively 0.15-1.5 times, 0.5-1.5 times and 0.7-1.5 times of the mass of the silver nitrate;
the slow release pH regulator is one of ammonium bicarbonate and ammonium carbonate.
Further, in the third step, the mass of the polysaccharide is 2.0 to 3.0 times of the mass of the silver nitrate;
the mass concentration of the third solution is 10-30%;
the polysaccharide is one of glucose, dextroglucose and fructose.
Further, in the fourth step, the mass ratio of the first solution to the second solution to the third solution is 1.62 to 8.72: 1;
the gradient temperature rise process comprises the following steps: after the temperature is raised to 27-32 ℃, 37-42 ℃, 47-52 ℃ and 57-62 ℃, the temperature is kept for 20-30 min, and then the temperature is raised to 70-80 ℃ and kept for 1-2 h.
Further, in the sixth step, the process conditions of the concentration and centrifugation treatment are as follows: the concentration pressure is 0.2-0.6 Mpa, and the concentration time is 1-2 h; the centrifugal speed is 9000-20000 rpm, and the centrifugal time is 25-35 min.
Further, in the seventh step, the mass volume concentration of the paste nano silver dispersion liquid is 150-400 g/L;
the process conditions of the ultrasonic centrifugal treatment are as follows: the ultrasonic time is 10-30 min; the centrifugal speed is 9000-20000 rpm; the centrifugation time is 30-60 min;
the organic solvent is one or two mixed solution of polyhydric alcohol and lipid;
the polyalcohol is one of ethylene glycol, glycerol and diethylene glycol;
the lipid is one of butyl carbitol acetate, butyl acetate, hexanediol ethyl ether acetate, dimethyl oxalate and diethyl oxalate.
Further, in the seventh step, the number of times of the ultrasonic centrifugal treatment is 1 to 7.
Further, in the eighth step, the mass ratio of the lipid to the organic solvent is 1:1 to 7;
the lipid is one of butyl carbitol acetate, butyl acetate, hexanediol ethyl ether acetate, dimethyl oxalate and diethyl oxalate.
In order to achieve the second purpose, the invention adopts the following technical scheme:
the nano silver lipid dispersion liquid is characterized by being prepared by the preparation method.
The invention has the beneficial effects that:
the method adopts PVP and a silver oxide precursor as nucleation aids, prepares nano-silver by in-situ induced nucleation growth, and does not adopt a mode of inducing by adding gold colloid, palladium colloid and the like as seed crystals, thereby avoiding the generation of silver mirrors on the inner wall of the reactor and improving the reaction direct yield; according to the invention, under the condition of gradient temperature rise, the slow-release pH regulator (such as ammonium bicarbonate, ammonium carbonate and the like) slowly releases ammonia, and the ammonia is reduced by polysaccharide weak reducing agents such as glucose and the like, so that the chemical reaction speed is effectively reduced, and the particle size uniformity of the nano silver is improved; according to the invention, the polyhydric alcohol (such as ethylene glycol, glycerol, mono-glycol and the like) is adopted, so that the adsorption effect of PVP organic polymer on the surface of nano-silver is effectively reduced, the solution viscosity of a reduction system is increased, and the diffusion growth rate of silver atoms is reduced, so that the organic content of nano-silver is reduced, and the low-temperature sintering of nano-silver and the uniform growth of the particle size of the nano-silver are promoted; washing the nano-silver dispersion liquid under the pressure of 0.2-0.6 Mpa (for example, filtering by adopting a pressure ceramic membrane with the aperture of 10 nm), purifying impurities and water in the nano-silver dispersion liquid, dispersing the nano-silver in a lipid solvent by a gradient displacement method, and distilling under reduced pressure to remove the lipid solvent to obtain nano-silver lipid dispersion liquid; the nano silver lipid dispersion liquid prepared by the invention has the silver content of 30-80%, the particle size range of 50-100 nm, the organic residue less than 1.5% and the sintering temperature less than 170 ℃, and can be used as a sintering aid additive in preparing heterojunction solar cell silver paste to promote low-temperature sintering to obtain a metalized electrode with good conductivity.
Detailed Description
The following detailed description of specific embodiments of the invention.
Example 1:
step one, adding 132.5g of glycerol into water to reach a constant volume of 1L, adding 26.5g of silver nitrate to form a silver nitrate solution with a mass volume concentration of 26.5g/L, and adjusting the temperature to 23 ℃ to obtain a first solution. Wherein the mass of the glycerol is 5 times of that of the silver nitrate in the silver nitrate solution.
And step two, dissolving 4.999g of sodium hydroxide in 1L of water, adding 26.5g of PVP and 20g of ammonium bicarbonate in sequence, and adjusting the temperature to 25 ℃ to obtain a second solution.
And step three, dissolving 60g of analytically pure glucose in 540ml of water, stirring and dissolving the solution to be clear, and adjusting the temperature to 25 ℃ to obtain a third solution with the mass concentration of 10%.
And step four, mixing the first solution and the second solution, stirring for 10min, adding the third solution, continuously stirring for 10min, heating to 30 ℃, 40 ℃, 50 ℃ and 60 ℃, uniformly preserving heat for 25min, then continuously heating to 75 ℃, and preserving heat for 1.5h to obtain the nano-silver feed liquid with the particle size of 50 nm.
And step five, cooling the nano-silver feed liquid to room temperature, and washing under the pressure of 0.4Mpa until the conductivity of the nano-silver feed liquid is 15 microSiemens.
And step six, concentrating and centrifuging the washed nano silver feed liquid to obtain 15g of paste nano silver. Wherein the concentration pressure is 0.4Mpa, and the concentration time is 1.5h; the centrifugation speed is 10000rpm, and the centrifugation time is 30min.
And seventhly, dispersing 15g of pasty nano silver in 100g of glycerol, performing ultrasonic treatment for 20min, centrifuging, dispersing the pasty nano silver obtained by centrifuging in a mixed solution of 80g of glycerol and 20g of butyl carbitol acetate, performing ultrasonic treatment for 20min, centrifuging, and dispersing the pasty nano silver obtained by centrifuging in 100g of butyl carbitol acetate solvent. Wherein the centrifugation speed is 10000rpm, and the centrifugation time is 40min.
And step eight, dispersing the paste-shaped nano silver subjected to the ultrasonic centrifugal treatment in 100g of butyl carbitol acetate, and then performing vacuum reduced pressure evaporation at the temperature of 100 ℃ to obtain the nano silver butyl carbitol acetate dispersion liquid.
By using a thermogravimetric analysis method, the nano-silver content in the nano-silver butyl carbitol acetate dispersion liquid is determined to be 30 percent by sampling, the particle size range is 100nm, the organic residue is less than 1.5 percent, and the sintering temperature is 160 ℃.
Example 2:
step one, adding 500g of ethylene glycol into water to a constant volume of 2L, adding 100g of silver nitrate to dissolve and prepare a silver nitrate solution with a mass volume concentration of 50g/L, and adjusting the temperature to 25 ℃ to obtain a first solution. Wherein the mass of the ethylene glycol is 10 times of that of the silver nitrate in the silver nitrate solution.
And step two, dissolving 30g of sodium hydroxide in 10L of water, sequentially adding 150g of PVP powder and 150g of ammonium carbonate, and adjusting the temperature to 25 ℃ to obtain a second solution.
And step three, dissolving 200g of dextroglucose in 467ml of pure water, stirring, and adjusting the temperature to 25 ℃ to obtain a third solution with the mass concentration of 30%.
And step four, mixing the first solution and the second solution, stirring for 20min, adding the third solution, continuously stirring for 20min, heating to 32 ℃, 42 ℃, 52 ℃ and 62 ℃, uniformly preserving heat for 30min, then continuously heating to 80 ℃, and preserving heat for 2h to obtain the nano-silver material liquid with the particle size of 100 nm.
And step five, cooling the nano-silver feed liquid to room temperature, and then washing under the pressure of 0.6Mpa until the conductivity of the nano-silver feed liquid is 18 microSiemens.
And step six, concentrating and centrifuging the washed nano silver feed liquid to obtain 40g of paste nano silver. Wherein the concentration pressure is 0.6Mpa, and the concentration time is 2h; the centrifugation speed is 20000rpm, and the centrifugation time is 35min.
And seventhly, dispersing 40g of pasty nano silver in 100g of ethylene glycol, performing ultrasonic treatment for 20min, centrifuging, dispersing the pasty nano silver obtained by centrifuging in a mixed solution of 60g of ethylene glycol and 40g of butyl acetate, performing ultrasonic treatment for 30min, centrifuging, dispersing the pasty nano silver obtained by centrifuging in a mixed solution of 40g of ethylene glycol and 60g of butyl acetate, performing ultrasonic treatment for 30min, and dispersing the pasty nano silver obtained by centrifuging in 100g of butyl acetate solvent. Wherein the centrifugation speed is 10000rpm, and the centrifugation time is 40min.
And step eight, dispersing the paste-like nano silver subjected to the ultrasonic centrifugal treatment in 100g of butyl acetate, and then performing vacuum reduced pressure evaporation at the temperature of 200 ℃ to obtain the nano silver butyl acetate dispersion liquid.
The content of nano silver in the nano silver butyl acetate dispersion liquid is 80 percent, the particle size range is 50nm, the organic residue is less than 1.2 percent, and the sintering temperature is 120 ℃ by using a thermogravimetric analysis method for sampling and determining.
Example 3:
step one, 480g of diethylene glycol is added into water to be constant volume to 6L, 60g of silver nitrate is added to be dissolved to prepare silver nitrate solution with mass volume concentration of 10g/L, and then the temperature is adjusted to 20 ℃ to obtain first solution. Wherein the mass of the mono-glycol is 8 times of that of the silver nitrate in the silver nitrate solution.
And step two, dissolving 90g of sodium hydroxide in 13L of water, sequentially adding 30g of PVP30 powder and 42g of ammonium carbonate, and adjusting the temperature to 20 ℃ to obtain a second solution.
And step three, dissolving 150g of fructose in 600ml of water, stirring, and adjusting the temperature to 20 ℃ to obtain a third solution with the mass concentration of 20%.
And step four, mixing the first solution and the second solution, stirring for 15min, adding the third solution, continuously stirring for 15min, heating to 27 ℃, 37 ℃, 47 ℃ and 57 ℃, uniformly preserving heat for 25min, and then continuously heating to 70 ℃, preserving heat for 1h to obtain the nano-silver material liquid with the particle size of 80 nm.
And step five, cooling the nano-silver feed liquid to room temperature, and then washing under the pressure of 0.2Mpa until the conductivity of the nano-silver feed liquid is less than 16 micro Siemens.
And step six, concentrating and centrifuging the washed nano silver feed liquid to obtain 30g of paste nano silver. Wherein the concentration pressure is 0.2Mpa, and the concentration time is 1h; the centrifugation speed was 9000rpm and the centrifugation time was 25min.
Dispersing 30g of pasty nano silver in 100g of diethylene glycol, performing ultrasonic treatment for 30min, centrifuging, dispersing the pasty nano silver obtained by centrifuging in a mixed solution of 80g of diethylene glycol and 20g of hexanediol ethyl ether acetate, performing ultrasonic treatment for 15min, centrifuging, dispersing the pasty nano silver obtained by centrifuging in a mixed solution of 60g of diethylene glycol and 40g of hexanediol ethyl ether acetate, performing ultrasonic treatment for 30min, centrifuging, dispersing the pasty nano silver obtained by centrifuging in a mixed solution of 40g of diethylene glycol and 60g of hexanediol ethyl ether acetate, performing ultrasonic treatment for 10min, and centrifuging; dispersing the paste nano silver obtained by centrifugation in a mixed solution of 20g of mono-glycol and 80g of hexanediol ethyl ether acetate, performing ultrasonic treatment for 30min, centrifuging, and dispersing the paste nano silver obtained by centrifugation in 100g of hexanediol ethyl ether acetate solvent. Wherein the centrifugal speed is 9000rpm, and the centrifugal time is 30min.
And step eight, dispersing the paste-like nano silver subjected to ultrasonic centrifugal treatment in 100g of hexanediol ethyl ether acetate, and then performing vacuum reduced pressure evaporation at the temperature of 150 ℃ to obtain a nano silver hexanediol ethyl ether acetate dispersion liquid.
The content of the nano-silver in the nano-silver hexanediol ether acetate dispersion liquid is 60 percent, the particle size range is 70nm, the organic residue is less than 1.3 percent, and the sintering temperature is 140 ℃ by using thermogravimetric analysis method for sampling and determining.
Example 4:
step one, adding 480g of diethylene glycol into pure water to a constant volume of 2.66L, adding 80g of silver nitrate to prepare a silver nitrate solution with a mass volume concentration of 30g/L, and adjusting the temperature to 22 ℃ to obtain a first solution. Wherein the mass of the mono-glycol is 6 times of that of the silver nitrate in the silver nitrate solution.
And step two, dissolving 40g of sodium hydroxide in 10L of water, sequentially adding 80g of PVP powder and 80g of ammonium carbonate, and adjusting the temperature to 23 ℃ to obtain a second solution.
And step three, dissolving 200g of fructose in 600ml of water, stirring, and adjusting the temperature to 23 ℃ to obtain a third solution with the mass concentration of 25%.
And step four, mixing the first solution and the second solution, stirring for 18min, adding the third solution, continuously stirring for 15min, heating to 28 ℃, 38 ℃, 48 ℃ and 58 ℃, uniformly preserving heat for 22min, and then continuously heating to 77 ℃ and preserving heat for 1h to obtain the nano-silver feed liquid with the particle size of 82 nm.
And step five, cooling the nano-silver feed liquid to room temperature, and then washing under the pressure of 0.4Mpa until the conductivity of the nano-silver feed liquid is less than 15 micro Siemens.
And step six, concentrating and centrifuging the washed nano silver feed liquid to obtain 35g of paste nano silver. Wherein the concentration pressure is 0.2Mpa, and the concentration time is 1.2h; the centrifugation speed is 10000rpm, and the centrifugation time is 25min.
Dispersing 35g of pasty nano silver in 100g of diethylene glycol, performing ultrasonic treatment for 30min, centrifuging, dispersing the pasty nano silver obtained by centrifuging in a mixed solution of 80g of diethylene glycol and 20g of hexanediol ethyl ether acetate, performing ultrasonic treatment for 15min, centrifuging, dispersing the pasty nano silver obtained by centrifuging in a mixed solution of 60g of diethylene glycol and 40g of hexanediol ethyl ether acetate, performing ultrasonic treatment for 30min, centrifuging, dispersing the pasty nano silver obtained by centrifuging in a mixed solution of 40g of diethylene glycol and 60g of hexanediol ethyl ether acetate, performing ultrasonic treatment for 10min, and centrifuging; dispersing the paste nano silver obtained by centrifugation in a mixed solution of 20g of diethylene glycol and 80g of hexanediol ethyl ether acetate, performing ultrasonic treatment for 30min, centrifuging, and dispersing the paste nano silver obtained by centrifugation in 100g of hexanediol ethyl ether acetate solvent. Wherein the centrifugal speed is 9000rpm, and the centrifugal time is 30min.
And step eight, dispersing the paste-shaped nano silver subjected to the ultrasonic centrifugal treatment in 100g of hexanediol ethyl ether acetate, and then performing vacuum reduced pressure evaporation at the temperature of 150 ℃ to obtain the nano silver hexanediol ethyl ether acetate dispersion liquid.
The content of nano-silver in the nano-silver hexanediol ether acetate dispersion liquid is 90 percent, the particle size range is 55nm, the organic residue is less than 1.2 percent, and the sintering temperature is 110 ℃ by using thermogravimetric analysis method for sampling and determining.
Although the embodiments of the present invention have been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the embodiments of the present invention.
Claims (10)
1. The preparation method of the nano silver lipid dispersion liquid is characterized by comprising the following steps:
step one, adding polyalcohol into silver nitrate solution with the mass volume concentration of 10-50 g/L, and adjusting the temperature to 20-25 ℃ to obtain first solution;
step two, sequentially adding PVP powder and a slow-release pH regulator into a sodium hydroxide solution with the mass volume concentration of 3-7 g/L, and adjusting the temperature to 20-25 ℃ to obtain a second solution;
the slow release pH regulator is one of ammonium bicarbonate and ammonium carbonate;
dissolving monosaccharide in water, stirring, and adjusting the temperature to 20-25 ℃ to obtain a third solution;
step four, mixing the first solution and the second solution, stirring for 10-20 min, adding the third solution, continuously stirring for 10-20 min, and performing gradient heating to obtain nano-silver feed liquid;
the gradient temperature rise process comprises the following steps: after the temperature is raised to 27-32 ℃, 37-42 ℃, 47-52 ℃ and 57-62 ℃, the temperature is kept for 20-30 min, and then the temperature is raised to 70-80 ℃ and kept for 1-2 h;
step five, cooling the nano-silver feed liquid to room temperature, and then washing under the pressure of 0.2-0.6 Mpa until the conductivity of the nano-silver feed liquid is less than 20 micro siemens;
step six, concentrating and centrifuging the washed nano silver feed liquid to obtain paste nano silver;
step seven, dispersing the pasty nano silver in an organic solvent to obtain pasty nano silver dispersion liquid, and then carrying out ultrasonic centrifugal treatment;
and step eight, dispersing the paste-like nano silver subjected to the ultrasonic centrifugal treatment in lipid, and then performing vacuum reduced pressure evaporation at the temperature of 90-200 ℃ to obtain nano silver lipid dispersion liquid.
2. The method according to claim 1, wherein in the first step, the mass of the polyol is 5 to 10 times of the mass of the silver nitrate in the silver nitrate solution;
in the first step, the polyol is one or a mixture of more of ethylene glycol, glycerol and diethylene glycol.
3. The method according to claim 1, wherein in the second step, the mass of the sodium hydroxide, the mass of the PVP and the mass of the pH adjustor are respectively 0.15 to 0.3 times, 0.5 to 1.5 times and 0.7 to 1.5 times the mass of the silver nitrate in the silver nitrate solution.
4. The method according to any one of claims 1 to 3, wherein in step three, the mass of the monosaccharide is 2.0 to 3.0 times the mass of the silver nitrate in the silver nitrate solution;
the mass concentration of the third solution is 10-30%;
the monosaccharide is one of glucose and fructose.
5. The production method according to any one of claims 1 to 3, wherein in step four, the mass ratio of the first solution to the second solution to the third solution is 1.62 to 8.72:1.
6. the preparation method according to any one of claims 1 to 3, wherein in the sixth step, the process conditions of the concentration and centrifugation treatment are as follows: the concentration pressure is 0.2-0.6 Mpa, and the concentration time is 1-2 h; the centrifugal speed is 9000-20000 rpm, and the centrifugal time is 25-35 min.
7. The preparation method according to any one of claims 1 to 3, wherein in the seventh step, the mass volume concentration of the paste-like nano silver dispersion liquid is 150 to 400g/L;
the process conditions of the ultrasonic centrifugal treatment are as follows: the ultrasonic time is 10-30 min; the centrifugal speed is 9000-20000 rpm; the centrifugation time is 30-60 min;
the organic solvent is polyalcohol or lipid or a mixed solution of polyalcohol and lipid; the polyalcohol is one of ethylene glycol, glycerol and diethylene glycol;
the lipid is one of butyl carbitol acetate, butyl acetate, hexanediol ethyl ether acetate, dimethyl oxalate and diethyl oxalate.
8. The method according to claim 7, wherein in the seventh step, the number of times of the ultrasonic centrifugation treatment is 1 to 7.
9. The method according to any one of claims 1 to 3, wherein the mass ratio of the lipid to the organic solvent is 1:1 to 7;
the lipid is one of butyl carbitol acetate, butyl acetate, hexanediol ethyl ether acetate, dimethyl oxalate and diethyl oxalate.
10. A nano silver lipid dispersion, characterized in that the nano silver lipid dispersion is prepared by the preparation method of any one of claims 1 to 9.
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