CN113547132A - Method for preparing nano silver powder by hydrothermal method and nano silver powder - Google Patents
Method for preparing nano silver powder by hydrothermal method and nano silver powder Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention provides a method for preparing nano silver powder by a hydrothermal method, which comprises the following steps: dispersing a silver source in deionized water, adding a pH regulator, and preparing a water reaction system containing silver ions; adding a reducing agent and a pH regulator into deionized water to obtain a reducing agent solution; uniformly stirring the obtained reducing agent solution and the silver ion-containing water reaction system, and adding the mixture into a hydrothermal reaction kettle for reaction to obtain a solid-liquid mixture; and carrying out solid-liquid separation, washing and drying on the solid-liquid mixture to obtain the nano silver powder. The method adopts a hydrothermal method to prepare the nano silver powder, can better control the particle size of the silver powder under the condition of using less crystal form control agent or not using the crystal form control agent, has less product impurities, obtains good reproducibility of the silver powder, can avoid the problems existing in the mechanical method preparation, can be used as a functional material to be correspondingly used in conductive ink, and has potential application in the aspects of catalysis, biomedicine and the like.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a method for preparing nano silver powder by a hydrothermal method and the nano silver powder.
Background
The nano silver powder has unique effects of quantum size, small size, surface and the like, so the nano silver powder has electrical property, magnetic property, catalytic performance, biomedicine, excellent biocompatibility, optical property, sensing property and the like which are superior to those of common materials. With the cross development of science and science, such as nano technology, nano materials, nano biology and the like, the application of nano silver technology products gradually permeates into the daily life of people. Nano silver will have a great influence in the following fields in the next decades: medical diagnostic tools and sensors, drug delivery, alloys, improved body-supporting implants, biosensors and chemical sensors, bioanalytical tools, bio-separation techniques, medical imaging and filtration. Meanwhile, the nano silver can be used as a conductive filler of the ink, and the properties of the nano silver powder, such as surface effect, quantum effect, size effect and the like, greatly improve the conductivity of the ink. The small size and high surface activity of the nano silver powder reduce the curing temperature, and the nano silver powder can be cured at room temperature, so that the nano silver powder has wider application. Therefore, the research on the preparation method of the nano silver powder and the optimization of the preparation process have important significance.
At present, the preparation method of the nano silver powder mainly comprises a mechanical ball milling method, adopts a mechanical device with higher energy to directly carry out high-energy crushing on simple substance block silver or silver particles with larger particle size, and can obtain the nano silver powder by controlling the ball milling environment. Another commonly used method for preparing the nano silver powder is a chemical reduction method, a reducing agent is used for reducing a silver precursor into a silver simple substance, a crystal form control agent is added at the same time, and the reaction conditions are controlled to control the size and the morphology of the silver powder. The existing hydrothermal method for preparing nano silver can cause that the reaction rate can not be controlled when a silver source and a reducing agent are mixed without adding a crystal form control agent, a large amount of silver powder is directly generated before hydrothermal reaction, the size of the nano silver powder is difficult to regulate and control, and the obtained product is not ideal in appearance.
How to better regulate the growth process of the silver powder to obtain the nano silver powder with ideal morphology and uniform particle size distribution, and simultaneously avoid the defects of more impurities, high post-treatment difficulty and the like caused by adding a crystal form control agent, and is a technical problem to be solved in the field.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides the preparation method of the nano silver powder for the conductive ink, the nano silver powder is prepared by a hydrothermal method, the particle size of the silver powder can be better controlled under the condition of using less crystal form control agent or not using the crystal form control agent, the post-treatment process is simplified, the reproducibility of the obtained silver powder is good, the problems in the mechanical preparation can be avoided, the obtained nano silver powder can be used as a functional material and correspondingly used in the conductive ink, and meanwhile, the preparation method has potential application in the aspects of catalysis, biomedicine and the like.
The invention provides a method for preparing nano silver powder by a hydrothermal method, which comprises the following steps:
s1, dispersing a silver source in deionized water, adding a PH regulator, and preparing a water reaction system containing silver ions;
s2, adding a reducing agent and a PH regulator into deionized water to obtain a reducing agent solution;
s3, uniformly stirring the reducing agent solution obtained in the step S2 and the water reaction system containing silver ions in the step S1, and adding the mixture into a hydrothermal reaction kettle for reaction to obtain a solid-liquid mixture;
and S4, carrying out solid-liquid separation, washing and drying on the solid-liquid mixture to obtain the nano silver powder.
Further, in the step S1, the silver source is one or two of silver carbonate, silver sulfate and silver oxalate, and the ratio of the amount of the substance containing silver ions added to the silver source to the total amount of the substance containing deionized water added in the steps S1 and S2 is (0.002-0.02): 1.
further, in the step S2, the reducing agent is one of triethylamine, glucose, ascorbic acid and ferrous sulfate citric acid, and the reducing agent is added in an excess amount relative to the silver ions, and the amount of the reducing agent added is 1 to 3 times of the theoretical amount of the substance capable of reducing the silver ions in the silver source in the step S1.
Preferably, the silver source in step S1 is silver oxalate, and the ratio of the amount of the substance containing silver ions added to the total substance of the deionized water added in steps S1 and S2 is (0.002-0.01): 1; the reducing agent in the step S2 is citric acid, and the dosage of the reducing agent is 1.2-1.5 times of the theoretical substance capable of completely reducing the silver ions in the silver source in the step S1.
Further, the pH regulators added in steps S1 and S2 are both alkaline regulators, which may be one or a mixture of two of ammonia water and sodium hydroxide, and the pH of the aqueous reaction system and the pH of the reducing agent solution are controlled to be 8 to 12.
Preferably, the pH regulators added in the steps S1 and S2 are both ammonia water, and the pH of the water reaction system and the pH of the reducing agent solution are both controlled to be 9-10.
Further, in the step S3, the temperature control manner is to place the hydrothermal reaction kettle in an oven with a certain temperature, and the reaction temperature is controlled at 100 ℃ and 200 ℃ during the reaction process, and the reaction time is 1-10 h.
Preferably, in the step S3, the temperature control manner is to place the hydrothermal reaction kettle in an oven with a certain temperature, control the reaction temperature to 105-.
The invention also provides the nano silver powder, which is prepared by the method for preparing the nano silver powder by the hydrothermal method, wherein the average particle size of the nano silver powder is 20-60nm, and the nano silver powder can be used as a functional phase of conductive ink and has potential application in catalysis and biomedicine.
Further, the burning loss value of the nano silver powder is 0.1-0.2%.
Further, in the step S4, after the solid-liquid separation of the silver particles obtained after the reaction is finished, washing the silver particles for 3 to 5 times with deionized water and/or ethanol, removing surface impurities, and drying to obtain the nano silver powder;
the separation method comprises at least one of filtration, sedimentation, evaporation or centrifugation;
the drying method includes at least one of vacuum drying, natural drying, heat drying and forced air drying.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts a hydrothermal method to prepare the nano silver powder, the silver source used is mainly a silver salt which is slightly soluble or insoluble in water, and the reaction condition is controlled to be alkaline, so that the reaction activity during preliminary mixing can be reduced, the reduction reaction rate is reduced, a large amount of silver powder precipitate is avoided being directly generated during early mixing, and the physical and chemical properties of reactants are changed along with the formation of a high-temperature high-pressure environment in the reaction process, and the reactants start to react; the method can better regulate and control the reaction rate, control the growth process of the silver powder crystal form and has good reaction result reproducibility; namely, by using a silver source with specific properties and controlling the pH, the powder with complete crystal grain development, uniform particle size distribution, less agglomeration and controllable particle size can be obtained under the condition of not adding a crystal form control agent.
(2) According to the invention, a crystal form control agent is not used, few impurities are introduced into the system, and the post-treatment difficulty is reduced; compared with the method using the crystal form control agent, the silver powder obtained by the method has fewer impurities and higher purity by adopting the same post-treatment mode, and the conductive ink obtained as the functional phase has better performance.
(3) The particle size of the prepared silver powder can be regulated and controlled by adjusting the conditions of concentration, reaction temperature, time and the like, the silver powder particles with different shapes can be obtained by controlling the growth process of the crystal form of the silver powder so as to meet different use requirements, and the reaction result has good reproducibility.
(4) The silver powder prepared by the method is nano silver powder, has high crystallinity, a burning loss value of 0.1-0.2%, less impurities and high purity, can be used as a functional phase in conductive ink, reduces the curing temperature of slurry, improves the performance of the conductive ink, and has potential application in the aspects of catalysis, biomedicine and the like.
Drawings
FIG. 1 is a scanning electron microscope picture of the silver nanoparticles obtained in example 1;
FIG. 2 is a scanning electron microscope picture of the silver nanoparticles obtained in example 2;
FIG. 3 is a scanning electron microscope picture of the silver nanoparticles obtained in example 3;
FIG. 4 is a scanning electron micrograph of the silver powder obtained in the comparative example.
Detailed Description
The present invention is described in further detail below in connection with specific embodiments, which may be embodied in many different forms and should not be construed as limited to the specific embodiments set forth herein. Rather, these embodiments are provided to explain the principles of the invention and its practical application to thereby enable others skilled in the art to understand the invention for various embodiments and with various modifications as are suited to the particular use contemplated.
The invention provides a method for preparing nano silver powder by a hydrothermal method, which comprises the following steps:
s1, dispersing a silver source in deionized water, adding a PH regulator, and preparing a water reaction system containing silver ions;
the silver source used specifically is mainly a silver salt which is slightly soluble or insoluble in water, such as silver carbonate, silver sulfate and silver oxalate, and aims to avoid that the reduction reaction rate is too high during primary mixing, a large amount of silver powder precipitates are directly generated during the previous mixing, and the crystal growth is difficult to regulate and control; the ratio of the amount of the substance containing silver ions in the added silver source to the amount of the substance containing deionized water in the whole reaction system is (0.002-0.02): 1.
s2, adding a reducing agent and a PH regulator into deionized water to obtain a reducing agent solution;
optional reducing agents include triethylamine, glucose, ascorbic acid, ferrous sulfate citric acid, in an amount greater than the amount theoretically required to reduce silver ions, the amount of reducing agent added being 1-3 times, preferably 1.2-1.5 times, the amount of the theoretical species of reducing agent capable of completely reducing silver ions in the silver source in step S1; the theoretical amount of the reducing agent is the amount of the reducing agent required to completely reduce silver ions contained in the solution, assuming that the silver source is completely dissolved.
The pH regulator used in the above steps S1 and S2 is alkaline regulator, which may be one or two of ammonia water and sodium hydroxide, and the pH is adjusted by adding alkaline regulator into the silver ion-containing aqueous solution to control the pH of the final solution to 8-12, and other values not listed in the above range are applicable. The purpose of adding the alkaline regulator is to avoid that the reduction reaction rate is too high during primary mixing, a large amount of silver powder precipitates are directly generated during early mixing, and the crystal growth is difficult to regulate and control. Further preferably, the pH is 9 to 10.
S3, uniformly stirring the reducing agent solution obtained in the step S2 and the water reaction system containing silver ions in the step 1, and adding the mixture into a hydrothermal reaction kettle for reaction to obtain a solid-liquid mixture;
specifically, the hydrothermal reaction kettle is placed in an oven with a certain temperature, and the reaction temperature is controlled to be 100-; the reaction time is 1-10h, such as 1h, 2h, 3h, 4h, 6h, 7h, 8h, 9, 10h, preferably 5-8 h.
S5, carrying out solid-liquid separation, washing and drying on the solid-liquid mixture to obtain nano silver powder;
the separation method of the reaction product includes at least one of filtration, sedimentation, evaporation or centrifugation, preferably centrifugation. Typical but non-limiting combinations are: combinations of filtration and settling, combinations of settling and evaporation, combinations of evaporation and centrifugation, combinations of centrifugation and filtration or combinations of evaporation, centrifugation and filtration, and the like.
The washing method comprises the step of repeatedly washing the nano silver powder for 3-5 times by adopting absolute ethyl alcohol and/or deionized water, and further preferably washing by matching with ultrasonic dispersion.
The drying method includes at least one of vacuum drying, natural drying, heat drying and forced air drying.
The invention also provides nano silver powder which is prepared by the method for preparing the nano silver powder by the hydrothermal method, and the average particle size of the obtained nano silver powder is 20-60 nm. The nano silver powder with different particle diameters can be obtained by regulating and controlling the conditions of concentration, reaction temperature, reaction time and the like according to different requirements so as to meet different application requirements. The obtained silver powder has a burning loss value of 0.1-0.2%, and contains less impurities and has high purity.
The method for preparing the above-mentioned silver nanoparticles according to the present invention will be described below with reference to specific examples, and it will be understood by those skilled in the art that the following examples are only specific examples of the method for preparing the above-mentioned silver nanoparticles according to the present invention, and are not intended to limit the entirety thereof.
Example 1
Adding 10g of silver oxalate into 150g of deionized water, adding an ammonia water solution into the silver oxalate to adjust the pH value to 9, and fully stirring and dispersing; dissolving 1.5g of triethylamine into 150g of deionized water to prepare a reducing agent solution, adding an ammonia water solution into the reducing agent solution to adjust the pH value to 9, and fully stirring; pouring a reducing agent solution into a silver ion-containing solution, uniformly mixing and transferring the solution into a hydrothermal reaction kettle; setting the hydrothermal reaction temperature at 150 ℃, reacting for 5h, after the reaction is finished, taking out reaction liquid after the hydrothermal kettle is cooled to room temperature, carrying out solid-liquid separation on the reaction liquid, washing for 5 times by using deionized water and ethanol, removing surface impurities, and drying for 2h in an oven at 80 ℃ to obtain the silver powder.
Fig. 1 is a scanning electron microscope picture of the silver nanoparticles obtained in example 1, showing the magnification of SEMMAG: the grain size observed under 100.0kx is small, the size is nm level (the large scale in the figure is 500nm, and the one-tenth small scale in the figure is 50nm), and the obtained nano silver powder particles are proved to have smaller particle size (less than 100nm), good uniformity, good dispersibility and high crystallization degree.
Example 2
Adding 10g of silver carbonate into 100g of deionized water, adding an ammonia water solution into the silver carbonate to adjust the pH value to 9, and fully stirring and dispersing; dissolving 1.5g of triethylamine into 100g of deionized water to prepare a reducing agent solution, adding an ammonia water solution into the reducing agent solution to adjust the pH value to 9, and fully stirring; pouring a reducing agent solution into a silver ion-containing solution, uniformly mixing and transferring the solution into a hydrothermal reaction kettle; setting the hydrothermal reaction temperature at 105 ℃, reacting for 8 hours, after the reaction is finished, taking out reaction liquid after the hydrothermal kettle is cooled to room temperature, carrying out solid-liquid separation on the reaction liquid, washing for 3 times by using deionized water and ethanol, removing surface impurities, and drying in an oven at 80 ℃ for 2 hours to obtain the silver powder.
Fig. 2 is a scanning electron microscope picture of the silver nanoparticles obtained in example 2, showing that the magnification SEMMAG: the grain size observed under 100.0kx is small, the size is nm level (the large scale in the figure is 500nm, and the one-tenth small scale in the figure is 50nm), and the obtained nano silver powder particles are proved to have smaller particle size (less than 100nm), good uniformity, good dispersibility and high crystallization degree.
Example 3
Adding 10g of silver oxalate into 150g of deionized water, adding an ammonia water solution into the silver oxalate to adjust the pH value to 10, and fully stirring and dispersing; dissolving 15g of ferrous sulfate into 150g of deionized water to prepare a reducing agent solution, adding an ammonia water solution into the reducing agent solution to adjust the pH value to 10, and fully stirring; pouring a reducing agent solution into a silver ion-containing solution, uniformly mixing and transferring the solution into a hydrothermal reaction kettle; setting the hydrothermal reaction temperature at 120 ℃, reacting for 6 hours, after the reaction is finished, taking out reaction liquid after the hydrothermal kettle is cooled to room temperature, carrying out solid-liquid separation on the reaction liquid, washing for 4 times by using deionized water and ethanol, removing surface impurities, and drying in an oven at 80 ℃ for 2 hours to obtain the silver powder.
Fig. 3 is a scanning electron microscope picture of the silver nanoparticles obtained in example 3, showing the magnification SEMMAG: the grain size observed under 100.0kx is small, the size is nm level (the large scale in the figure is 500nm, and the one-tenth small scale in the figure is 50nm), and the obtained nano silver powder particles are proved to have smaller particle size (less than 100nm), good uniformity, good dispersibility and high crystallization degree.
Example 4
Adding 10g of silver oxalate into 150g of deionized water, adding an ammonia water solution into the silver oxalate to adjust the pH value to 12, and fully stirring and dispersing; dissolving 10g of ferrous sulfate into 150g of deionized water to prepare a reducing agent solution, adding an ammonia water solution into the reducing agent solution to adjust the pH value to 12, and fully stirring; pouring a reducing agent solution into a silver ion-containing solution, uniformly mixing and transferring the solution into a hydrothermal reaction kettle; setting the hydrothermal reaction temperature at 200 ℃, reacting for 1h, after the reaction is finished, taking out reaction liquid after the hydrothermal kettle is cooled to room temperature, carrying out solid-liquid separation on the reaction liquid, washing for 4 times by using deionized water and ethanol, removing surface impurities, and drying in an oven at 80 ℃ for 2h to obtain the silver powder.
Example 5
Adding 10g of silver oxalate into 15g of deionized water, adding an ammonia water solution into the silver oxalate to adjust the pH value to 8, and fully stirring and dispersing; dissolving 30g of ferrous sulfate into 15g of deionized water to prepare a reducing agent solution, adding an ammonia water solution into the reducing agent solution to adjust the pH value to 8, and fully stirring; pouring a reducing agent solution into a silver ion-containing solution, uniformly mixing and transferring the solution into a hydrothermal reaction kettle; setting the hydrothermal reaction temperature at 170 ℃, reacting for 10h, after the reaction is finished, taking out reaction liquid after the hydrothermal kettle is cooled to room temperature, carrying out solid-liquid separation on the reaction liquid, washing for 3 times by using deionized water and ethanol, removing surface impurities, and drying in an oven at 80 ℃ for 2h to obtain the silver powder.
Example 6
Adding 10g of silver oxalate into 30g of deionized water, adding an ammonia water solution into the silver oxalate to adjust the pH value to 8, and fully stirring and dispersing; dissolving 20g of ferrous sulfate into 30g of deionized water to prepare a reducing agent solution, adding an ammonia water solution into the reducing agent solution to adjust the pH value to 11, and fully stirring; pouring a reducing agent solution into a silver ion-containing solution, uniformly mixing and transferring the solution into a hydrothermal reaction kettle; setting the hydrothermal reaction temperature at 110 ℃, reacting for 9h, after the reaction is finished, taking out reaction liquid after the hydrothermal kettle is cooled to room temperature, carrying out solid-liquid separation on the reaction liquid, washing for 3 times by using deionized water and ethanol, removing surface impurities, and drying in an oven at 80 ℃ for 2h to obtain the silver powder.
The experimental comparison shows that: in the following comparative example, silver powder was prepared without using a hydrothermal reaction, and the morphology of the silver powder prepared in the comparative example was compared with that of the silver powder prepared in examples 1 to 3.
Comparative example
Adding 10g of silver sulfate into 150g of deionized water, and fully stirring and dispersing; dissolving 1.5g of triethylamine into 150g of deionized water to prepare a reducing agent solution; adding an ammonia water solution into the silver sulfate to adjust the pH value to 9, and fully stirring; and adding a reducing agent solution into the silver ion-containing solution in the stirring process, heating the reaction solution to 80 ℃, stirring to reduce silver ions, cooling the reaction solution after the reaction is finished, separating solid from liquid of the reaction solution, washing with deionized water and ethanol to remove surface impurities, and drying in an oven at 80 ℃ for 2 hours to obtain the silver powder.
Fig. 4 is a scanning electron microscope image of the silver powder obtained in the comparative example, magnification SEMMAG: the grain size observed at 30.0kx is large, on the order of μm (large scale in the figure is 2 μm, and one-tenth small scale is 0.2 μm), and is not a nanoscale silver powder; compared with fig. 1 to 3, the shapes are irregular and the sizes are not uniform.
Although examples 1 to 6 and comparative examples all used the same post-treatment, the silver powder obtained by the present invention had less impurity residue, had a burnout value of 0.1 to 0.2%, had a high purity, and was used as a functional material in conductive inks to obtain conductive inks having a better performance. In the comparative example, a crystal form control agent is not used, a hydrothermal method is not used, the obtained silver powder is not nano silver powder, the grain size is large, the appearance is irregular, the size is not uniform, and the use requirement of the conductive ink cannot be met.
Claims (10)
1. A method for preparing nano silver powder by a hydrothermal method is characterized by comprising the following steps:
s1, dispersing a silver source in deionized water, adding a PH regulator, and preparing a water reaction system containing silver ions;
s2, adding a reducing agent and a PH regulator into deionized water to obtain a reducing agent solution;
s3, uniformly stirring the reducing agent solution obtained in the step S2 and the water reaction system containing silver ions in the step S1, and adding the mixture into a hydrothermal reaction kettle for reaction to obtain a solid-liquid mixture;
and S4, carrying out solid-liquid separation, washing and drying on the solid-liquid mixture to obtain the nano silver powder.
2. The hydrothermal method for producing silver nanopowder according to claim 1, wherein in step S1, the silver source is one or a mixture of two of silver carbonate, silver sulfate and silver oxalate, and the ratio of the amount of the substance containing silver ions added to the silver source to the total amount of the substance of deionized water added in steps S1 and S2 is (0.002-0.02): 1.
3. the hydrothermal method for preparing silver nanopowder according to claim 1, wherein in step S2, the reducing agent is one of triethylamine, glucose, ascorbic acid, ferrous sulfate and citric acid, and the reducing agent is added in an excess amount relative to the silver ions, wherein the amount of the reducing agent added is 1-3 times of the theoretical amount of the material capable of reducing the silver ions in the silver source in step S1.
4. The hydrothermal method for producing silver nanopowder according to claim 1, wherein the silver source in step S1 is silver oxalate, and the ratio of the amount of the substance containing silver ions added to the silver oxalate to the total amount of the substance containing deionized water added in steps S1 and S2 is (0.002-0.01): 1; the reducing agent in the step S2 is citric acid, and the dosage of the reducing agent is 1.2-1.5 times of the theoretical substance capable of completely reducing the silver ions in the silver source in the step S1.
5. The hydrothermal method for preparing silver nanopowder according to claim 1, wherein the pH regulators added in steps S1 and S2 are alkaline regulators, which can be one or a mixture of ammonia water and sodium hydroxide, and the pH of the aqueous reaction system and the pH of the reducing agent solution are controlled to be 8-12.
6. The hydrothermal method for preparing silver nanopowder according to claim 1, wherein the pH regulators added in steps S1 and S2 are ammonia water, and the pH of the aqueous reaction system and the pH of the reducing agent solution are controlled to be 9-10.
7. The method for preparing silver nanoparticles according to claim 1, wherein in step S3, the temperature is controlled by placing the hydrothermal reaction kettle in an oven at a certain temperature, and the reaction temperature is controlled at 100-200 ℃ during the reaction, and the reaction time is 1-10 h.
8. The hydrothermal method for preparing silver nanoparticles as claimed in claim 1, wherein in the step S3, the reaction temperature is controlled to be 105-150 ℃ and the reaction time is controlled to be 5-8 h.
9. A silver nanopowder obtained by a hydrothermal process for the preparation of silver nanopowder according to any one of claims 1 to 9, said silver nanopowder having an average particle size of 20 to 60 nm.
10. The silver nanopowder according to claim 9, wherein the silver powder has a burning loss value of 0.1 to 0.2%.
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| CN115401209A (en) * | 2022-09-02 | 2022-11-29 | 陕西煤业化工技术研究院有限责任公司 | Preparation method of nano silver powder with controllable particle size |
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| CN101554664A (en) * | 2009-05-20 | 2009-10-14 | 广东风华高新科技股份有限公司 | Method for preparing nano-scale silver powder |
| US20110256383A1 (en) * | 2010-04-01 | 2011-10-20 | Bayer Materialscience Ag | Polymer material comprising a polymer and silver nanoparticles dispersed herein |
| CN109822106A (en) * | 2019-02-23 | 2019-05-31 | 北京氦舶科技有限责任公司 | A kind of preparation method and applications of flake silver powder |
| CN110834100A (en) * | 2019-12-09 | 2020-02-25 | 成都市天甫金属粉体有限责任公司 | Preparation method of flaky porous silver powder |
| CN111168083A (en) * | 2020-02-24 | 2020-05-19 | 深圳先进技术研究院 | Preparation method of nano silver powder |
| CN112570728A (en) * | 2020-12-10 | 2021-03-30 | 长沙新材料产业研究院有限公司 | Flaky silver powder and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115401209A (en) * | 2022-09-02 | 2022-11-29 | 陕西煤业化工技术研究院有限责任公司 | Preparation method of nano silver powder with controllable particle size |
| CN115401209B (en) * | 2022-09-02 | 2024-03-26 | 陕西煤业化工技术研究院有限责任公司 | Preparation method of granularity-controllable nano silver powder |
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