CN111618312A - Preparation method of rod-shaped Ag powder, preparation method and application of rod-shaped Ag @ BST core-shell particles - Google Patents
Preparation method of rod-shaped Ag powder, preparation method and application of rod-shaped Ag @ BST core-shell particles Download PDFInfo
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- 239000011258 core-shell material Substances 0.000 title claims abstract description 28
- 239000002245 particle Substances 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000003990 capacitor Substances 0.000 claims abstract description 14
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 13
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 13
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 67
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 23
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 7
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims description 6
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 239000002131 composite material Substances 0.000 abstract description 12
- 238000004146 energy storage Methods 0.000 abstract description 11
- 229910010252 TiO3 Inorganic materials 0.000 abstract description 6
- 239000000945 filler Substances 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 229910052454 barium strontium titanate Inorganic materials 0.000 description 23
- 229920000642 polymer Polymers 0.000 description 5
- 239000004020 conductor Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920013657 polymer matrix composite Polymers 0.000 description 1
- 239000011160 polymer matrix composite Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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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
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/14—Organic dielectrics
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Abstract
The invention discloses a preparation method of rod-shaped Ag powder, a preparation method of rod-shaped Ag @ BST core-shell particles and application of the rod-shaped Ag @ BST core-shell particles; belongs to the technical field of micro-capacitors. The invention aims to solve the problems that when the rodlike nano silver is used as a single filler, when the seepage threshold is reached, the dielectric constant is improved, the breakdown strength is reduced, the dielectric loss is increased, and the energy storage density is reduced, so that the application of the rodlike nano silver in the field of capacitors is limited. The invention takes silver nitrate and polyvinylpyrrolidone as raw materials to prepare rod-shaped nano Ag, and then coats a layer of Ba outside the Ag rod by a sol-gel hydrothermal method0.6Sr0.4TiO3And finally, washing, centrifuging and drying to obtain the rod-shaped Ag @ BST powder. Hair brushThe bright rod-shaped Ag @ BST powder can improve the dielectric constant and simultaneously keep a certain breakdown field intensity, and the novel composite material has good dielectric property and energy storage property and has great potential in the energy storage application fields such as electrostatic capacitors and the like.
Description
Technical Field
The invention belongs to the technical field of micro-capacitors; in particular to a preparation method of rod-shaped Ag; and core-shell particle rod-shaped Ag @ Ba0.6Sr0.4TiO3A preparation method and application of the powder.
Background
With the continuous development of human society and the continuous updating of scientific technology, the demand for energy sources is increasing day by day, and the utilization and storage of energy sources become the fields of close attention of people. The capacitor, as a novel physical energy storage device, has a small volume, high energy storage density and high charging and discharging efficiency, and thus is a hotspot in research on the field of energy storage and utilization. To increase the energy storage density of the polymer aggregate, inorganic ceramics or conductive materials are typically added to the polymer matrix. When the inorganic ceramic filler is added, the dielectric constant of the composite material is increased along with the increase of the content of the filler, however, the dielectric loss of the composite material is increased, and the mechanical property of the composite material is sharply reduced, which seriously influences the service life and the application field of the composite material. When the conductive filler is added into the polymer, the dielectric constant of the polymer is sharply increased and the dielectric loss is also sharply increased when the threshold value is reached.
Core-shell structures are a powerful and versatile strategy to design and fabricate high dielectric composites for energy storage and dielectric applications. The dielectric constant of the composite material can be obviously improved by adding the conductive material into the organic polymer, but a certain amount of conductive materials are communicated with each other to form leakage current, so that the dielectric loss of the composite material is improved.
Disclosure of Invention
The invention provides a preparation method of a rod-shaped Ag powder, a preparation method of a rod-shaped Ag @ BST core-shell particle and application of the rod-shaped Ag @ BST core-shell particle, and aims to solve the problems that when a seepage threshold is reached, the dielectric constant is improved, the breakdown strength is reduced, the dielectric loss is increased, and the energy storage density is further reduced, and the application of the rod-shaped Ag powder in the field of capacitors is limited.
In order to solve the technical problems, the preparation method of the rod-shaped Ag powder comprises the following steps:
step one, taking ethylene glycol, heating to 160-170 ℃ while stirring, and preserving heat for 1-2 h;
step two, adding sodium chloride, and continuing to perform heat preservation reaction for 20-40 min;
adding a glycol solution of polyvinylpyrrolidone, dropwise adding the glycol solution of silver nitrate when the reaction temperature rises to 160-170 ℃, heating to 180-190 ℃ after dropwise adding, and carrying out heat preservation reaction for 1-2 h;
washing and centrifuging for at least 3 times by using an ethanol solution with the volume concentration of 95%, and drying to obtain rod-shaped silver powder; the whole process is carried out under stirring.
Further limiting, 100mL-140mL of ethylene glycol is taken in the first step; adding 0.002g-0.007g of sodium chloride in the second step; the glycol solution of polyvinylpyrrolidone added in the step three is prepared by dissolving 3.5-4 g of polyvinylpyrrolidone in 70-80 mL of glycol and uniformly mixing; the ethylene glycol solution of silver nitrate added dropwise in the third step is prepared by dissolving 1.5-2 g of silver nitrate in 70-80 mL of ethylene glycol and mixing uniformly, and the adding speed is 140-150 mL/min.
Further limiting, the centrifugation speed in the fourth step is 3000r/min-5000 r/min.
Further limiting, the drying temperature in the fourth step is 80-100 ℃.
The preparation method of the rod-shaped Ag @ BST core-shell particle is completed by the following steps:
step 1, dissolving barium acetate and strontium acetate in acetic acid, and stirring for 30min-1h at 40-50 ℃ to obtain a solution A;
step 2, dissolving tetrabutyl titanate in absolute ethyl alcohol, and stirring for 30min-1h at room temperature to obtain a solution B;
step 3, dropwise adding the solution B into the solution A at room temperature, and stirring for 1-2 h at room temperature to obtain BST sol;
step 4, adding the rod-shaped Ag powder prepared by the method into the BST sol obtained in the step 3, and carrying out ultrasonic treatment for 2-3 h at the temperature of 60-80 ℃;
and step 5, washing and centrifuging for at least 3 times by using an ethanol solution with the volume concentration of 95%, and drying to obtain the Ag @ BST xerogel.
Step 6, adding a KOH solution into a stainless steel kettle with a polytetrafluoroethylene lining, then adding the Ag @ BST xerogel obtained in the step 5, then placing the dried gel into a drying oven, reacting for 10-12 h at 120-130 ℃, and naturally cooling to room temperature;
and 7, washing and centrifuging for at least 3 times by using an ethanol solution with the volume concentration of 95%, and drying to obtain the rod-shaped Ag @ BST core-shell particles.
Further limiting, 1.5g to 2g of barium acetate and 0.5g to 1g of strontium acetate are mixed and dissolved in 10mL to 20mL of acetic acid in the step 1; dissolving 3g-4g of tetrabutyl titanate in 5mL-10mL of absolute ethyl alcohol in the step 2; in the step 4, the adding amount of the rod-shaped Ag powder is 3.5g-4 g; step 6A stainless steel kettle lined with polytetrafluoroethylene is filled with 25mL-35mL of KOH solution with the concentration of 6M-8M.
Further defined, the centrifugation rate in step 5 is 3000r/min to 4000 r/min.
Further limiting, the drying temperature in the step 5 is 80-100 ℃.
Further defined, the centrifugation rate in step 7 is 3000r/min to 4000 r/min.
Further limiting, the drying temperature in the step 7 is 80-100 ℃.
The rod-shaped Ag @ BST core-shell particles prepared by the method are used as a filler of a high dielectric composite material and used for manufacturing a micro capacitor.
According to the method, after the rodlike nano silver and the barium strontium titanate are compounded, the insulating layer is introduced to effectively reduce the contact between the conductive materials, the path of the charge carriers is normalized, the occurrence of large-range leakage current is prevented, and the dielectric loss is effectively reduced while the dielectric constant of the composite material is improved.
The high dielectric rod-shaped Ag @ Ba prepared by the invention0.6Sr0.4The TiO core-shell particles are applied to the preparation of embedded micro-capacitors, can effectively increase the compatibility of the embedded micro-capacitors with the main board polymer,and effectively improve the capacitance, storage capacity and conductivity of the capacitor, and provides a new technology for the development of the micro embedded capacitor.
The invention relates to a rod-shaped Ag @ Ba0.6Sr0.4TiO3The powder can improve the dielectric constant and keep a certain breakdown field strength, and the novel composite material has good dielectric property and energy storage property and has great potential in the energy storage application fields such as electrostatic capacitors and the like.
The high dielectric rod-shaped Ag @ Ba prepared by the invention0.6Sr0.4Core-shell particles of TiO with Ba0.6Sr0.4The TiO-coated rodlike nano silver is used as a filler, so that the contact between conductive fillers can be reduced, the leakage current is reduced, the dielectric loss is reduced, and the dielectric property of the material is improved.
Drawings
FIG. 1 is a scanning electron micrograph of a rod-shaped Ag powder;
FIG. 2 is a transmission electron micrograph of rod-like Ag @ Ba0.6Sr0.4TiO core-shell particles.
Detailed Description
Example 1:
the rod-shaped Ag powder used in this example was prepared by the following procedure:
step one, taking 100mL of glycol, heating the reaction temperature to 160 ℃ at a heating rate of 5 ℃/min under stirring, and keeping the temperature for 1 h;
step two, then adding 0.002g of sodium chloride, and continuing to perform heat preservation reaction for 30 min;
thirdly, adding a glycol solution of polyvinylpyrrolidone, dropwise adding the glycol solution of silver nitrate at a dropwise adding speed of 144mL/min when the temperature rises to 160 ℃ after the reaction, and reacting for 1h under the condition of heat preservation;
in the third step, 3.5g of polyvinylpyrrolidone is dissolved in 70mL of glycol and is uniformly mixed to prepare the glycol solution of polyvinylpyrrolidone, and 1.5g of silver nitrate is dissolved in 70mL of glycol and is uniformly mixed to prepare the glycol solution of silver nitrate;
step four, washing and centrifuging for 3 times by using an ethanol solution with the volume concentration of 95%, and drying for 10 hours at 80 ℃ to obtain rod-shaped silver powder;
wherein, the whole process is carried out under stirring, and the stirring speed is 8000 r/min.
The rod-shaped Ag powder is shown in FIG. 1.
The average length of the rod-shaped nano Ag is 10 μm, and the average diameter is 200 nm.
In this embodiment, the rod-shaped Ag @ Ba0.6Sr0.4TiO3The method of the core-shell particle is completed by the following steps:
step 1, dissolving 1.5g of barium acetate and 0.5g of strontium acetate in 10mL of acetic acid, and stirring at the temperature of 40 ℃ at the speed of 7000r/min for 30min to obtain a solution A;
step 2, dissolving 3g of tetrabutyl titanate in 5mL of absolute ethyl alcohol, and stirring at the speed of 7000r/min for 30min at room temperature to obtain a solution B;
step 3, dropwise adding the solution B into the solution A at room temperature, and stirring at 7000r/min for 1h at room temperature to obtain BST sol;
step 4, adding 3.5g of the rod-shaped Ag powder prepared in the embodiment into the BST sol obtained in the step 3, and performing ultrasonic treatment for 2 hours at the temperature of 60 ℃;
step 5, washing and centrifuging for 3 times by using an ethanol solution with the volume concentration of 95%, and drying for 10h at 80 ℃ to obtain a dry gel of Ag @ BST;
step 6, adding 25mL of KOH solution with the concentration of 6M into a stainless steel kettle with a polytetrafluoroethylene lining, then adding the Ag @ BST xerogel obtained in the step 5, then placing the dried gel into an oven, reacting for 10 hours at 120 ℃, and naturally cooling to room temperature;
step 7, washing and centrifuging for 3 times by using an ethanol solution with the volume concentration of 95%, and drying for 10h at 80 ℃ to obtain a rod-shaped Ag @ Ba0.6Sr0.4TiO3Core-shell particles.
The rod-shaped Ag @ BST core-shell particles are shown in FIG. 2.
The high-dielectric polymer matrix composite is obtained by adopting the rod-shaped Ag @ BST core-shell particles as a filler and compounding the rod-shaped Ag @ BST core-shell particles with a polyvinylidene fluoride matrix, and at the moment, the composite can provide a higher dielectric constant and has excellent mechanical property and processability, so that an embedded micro capacitor is manufactured and can be well embedded into a circuit board, the area of the circuit board is greatly reduced, the running speed and stability of a product are improved, and the cost is reduced.
Example 2:
the rod-shaped Ag powder used in this example was prepared by the following procedure:
step one, taking 120mL of glycol, heating the reaction temperature to 160 ℃ at a heating rate of 5 ℃/min under stirring, and keeping the temperature for 1 h;
step two, then adding 0.005g of sodium chloride, and continuing to perform heat preservation reaction for 20 min;
thirdly, adding a glycol solution of polyvinylpyrrolidone, dropwise adding a glycol solution of silver nitrate at a dropping speed of 150mL/min when the temperature rises to 165 ℃ after the reaction, and reacting for 2 hours while keeping the temperature;
in the third step, 4g of polyvinylpyrrolidone is dissolved in 75mL of glycol and is uniformly mixed to prepare the glycol solution of polyvinylpyrrolidone, and 2g of silver nitrate is dissolved in 80mL of glycol and is uniformly mixed to prepare the glycol solution of silver nitrate;
step four, washing and centrifuging for 3 times by using an ethanol solution with the volume concentration of 95%, and drying for 10 hours at the temperature of 95 ℃ to obtain rod-shaped silver powder;
wherein the whole process is carried out under stirring, the stirring speed is 8000r/min, and the centrifugation speed in the step 5 is 3000 r/min; the centrifugation rate in step 7 was 3000 r/min.
The method for preparing the rod-shaped Ag @ BST core-shell particles in the implementation is completed by the following steps:
step 1, dissolving 2g of barium acetate and 1g of strontium acetate in 15mL of acetic acid, and stirring at 45 ℃ at a rate of 7000r/min for 1h to obtain a solution A;
step 2, dissolving 4g of tetrabutyl titanate in 10mL of absolute ethyl alcohol, and stirring at the speed of 7000r/min for 1h at room temperature to obtain a solution B;
step 3, dropwise adding the solution B into the solution A at room temperature, and stirring at 7000r/min for 1h at room temperature to obtain BST sol;
step 4, adding 4g of the rod-shaped Ag powder prepared in the embodiment into the BST sol obtained in the step 3, and performing ultrasonic treatment for 3 hours at 80 ℃;
step 5, washing and centrifuging for 3 times by using an ethanol solution with the volume concentration of 95%, and drying for 10h at 100 ℃ to obtain a dry gel of Ag @ BST;
step 6, putting 30mL of KOH solution with the concentration of 8M into a stainless steel kettle with a polytetrafluoroethylene lining, then adding the Ag @ BST xerogel obtained in the step 5, then putting the dried gel into an oven, reacting for 12h at 130 ℃, and naturally cooling to room temperature;
step 7, washing and centrifuging for 3 times by using an ethanol solution with the volume concentration of 95%, and drying for 10h at 90 ℃ to obtain a rod-shaped Ag @ Ba0.6Sr0.4TiO3Core-shell particles.
Wherein, the whole process is carried out under stirring, the stirring speed is 7000r/min, and the centrifugation speed in the step 5 is 4000 r/min; the centrifugation rate in step 7 was 4000 r/min.
Claims (10)
1. The preparation method of the rod-shaped Ag powder is characterized by comprising the following steps:
step one, taking ethylene glycol, heating to 160-170 ℃ while stirring, and preserving heat for 1-2 h;
step two, adding sodium chloride, and continuing to perform heat preservation reaction for 20-40 min;
adding a glycol solution of polyvinylpyrrolidone, dropwise adding the glycol solution of silver nitrate when the reaction temperature rises to 160-170 ℃, heating to 180-190 ℃ after dropwise adding, and carrying out heat preservation reaction for 1-2 h;
and step four, washing and centrifuging for at least 3 times by using an ethanol solution with the volume concentration of 95%, and drying to obtain the rod-shaped silver powder.
2. The method for preparing rod-like Ag powder according to claim 1, wherein the first step is performed by taking 100mL-140mL of ethylene glycol and the second step is performed by adding 0.002g-0.007g of sodium chloride.
3. The method for preparing rod-shaped Ag powder according to claim 2, wherein the solution of polyvinylpyrrolidone in ethylene glycol added in step three is prepared by dissolving 3.5-4 g polyvinylpyrrolidone in 70-80 mL ethylene glycol and mixing.
4. The method for preparing the rod-shaped Ag powder according to claim 3, wherein the dropwise addition of the silver nitrate solution in the third step is performed by dissolving 1.5g to 2g of silver nitrate in 70mL to 80mL of ethylene glycol and mixing the solution uniformly, and the dropping speed is 140mL/min to 150 mL/min.
5. The method for preparing rod-like Ag powder according to any of claims 1-4, wherein the centrifugation rate in step four is 3000r/min-5000 r/min; the drying temperature is 80-100 ℃.
6. The preparation method of the rod-shaped Ag @ BST core-shell particles is characterized in that the preparation method of the rod-shaped Ag @ BST core-shell particles is completed through the following steps:
step 1, dissolving barium acetate and strontium acetate in acetic acid, and stirring for 30min-1h at 40-50 ℃ to obtain a solution A;
step 2, dissolving tetrabutyl titanate in absolute ethyl alcohol, and stirring for 30min-1h at room temperature to obtain a solution B;
step 3, dropwise adding the solution B into the solution A at room temperature, and stirring for 1-2 h at room temperature to obtain BST sol;
step 4, adding the rod-shaped Ag powder prepared by the method of any one of claims 1 to 5 into the BST sol obtained in the step 3, and carrying out ultrasonic treatment at the temperature of 60-80 ℃ for 2-3 h;
step 5, washing and centrifuging for at least 3 times by using an ethanol solution with the volume concentration of 95%, and drying to obtain Ag @ BST xerogel;
step 6, adding a KOH solution into a stainless steel kettle with a polytetrafluoroethylene lining, then adding the Ag @ BST xerogel obtained in the step 5, then placing the dried gel into a drying oven, reacting for 10-12 h at 120-130 ℃, and naturally cooling to room temperature;
and 7, washing and centrifuging for at least 3 times by using an ethanol solution with the volume concentration of 95%, and drying to obtain the rod-shaped Ag @ BST core-shell particles.
7. The method for preparing rod-shaped Ag @ BST core-shell particles according to claim 6, wherein 1.5g to 2g of barium acetate and 0.5g to 1g of strontium acetate are mixed and dissolved in 10mL to 20mL of acetic acid in step 1; in step 2, 3g to 4g of tetrabutyl titanate is dissolved in 5mL to 10mL of absolute ethyl alcohol.
8. The method for preparing rod-shaped Ag @ BST core-shell particles according to claim 7, wherein the amount of the rod-shaped Ag powder added in the step 4 is 3.5g to 4 g; step 6A stainless steel kettle lined with polytetrafluoroethylene is filled with 25mL-35mL of KOH solution with the concentration of 6M-8M.
9. The process for the preparation of rod-shaped Ag @ BST core-shell particles according to any one of claims 6 to 8, characterized in that the centrifugation rate in step 5 is 3000r/min to 4000 r/min; in the step 5, the drying temperature is 80-100 ℃; in the step 7, the centrifugal rate is 3000r/min-4000 r/min; in step 7, the drying temperature is 80-100 ℃.
10. Rod-shaped Ag @ BST core-shell particles prepared by the method of any one of claims 6 to 8 are used for fabricating micro-capacitors.
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| CN112973686A (en) * | 2021-03-02 | 2021-06-18 | 大连工业大学 | Method for enhancing photocatalytic performance of heterostructure composite material through pyroelectric effect and application |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5453908A (en) * | 1994-09-30 | 1995-09-26 | Texas Instruments Incorporated | Barium strontium titanate (BST) thin films by holmium donor doping |
| CN101712784A (en) * | 2009-10-29 | 2010-05-26 | 西安交通大学 | Nuclear shell structured packing/polymer-based composite material and preparation method thereof |
| CN103639423A (en) * | 2013-12-27 | 2014-03-19 | 哈尔滨理工大学 | Nano-Ag-coated aluminum silicate nuclear shell particle, and preparation method and application thereof |
| CN103951976A (en) * | 2014-05-22 | 2014-07-30 | 哈尔滨理工大学 | Nano core-shell particle/polyimide (PI) composite film, and preparation method and application thereof |
| CN104496463A (en) * | 2014-11-21 | 2015-04-08 | 中国计量学院 | Surfactant assisted in situ co-precipitation method for preparing core-shell structure nano powder |
| CN104841946A (en) * | 2015-04-23 | 2015-08-19 | 深圳先进技术研究院 | Silver nanorod and preparing method thereof |
| CN108031838A (en) * | 2017-12-25 | 2018-05-15 | 畅的新材料科技（上海）有限公司 | A kind of preparation method of M@N core-shell structured nanomaterials |
| CN108314078A (en) * | 2018-02-08 | 2018-07-24 | 西北工业大学 | A kind of preparation method of hollow ball-shape barium-strontium titanate powder material |
-
2020
- 2020-04-28 CN CN202010349859.9A patent/CN111618312B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5453908A (en) * | 1994-09-30 | 1995-09-26 | Texas Instruments Incorporated | Barium strontium titanate (BST) thin films by holmium donor doping |
| CN101712784A (en) * | 2009-10-29 | 2010-05-26 | 西安交通大学 | Nuclear shell structured packing/polymer-based composite material and preparation method thereof |
| CN103639423A (en) * | 2013-12-27 | 2014-03-19 | 哈尔滨理工大学 | Nano-Ag-coated aluminum silicate nuclear shell particle, and preparation method and application thereof |
| CN103951976A (en) * | 2014-05-22 | 2014-07-30 | 哈尔滨理工大学 | Nano core-shell particle/polyimide (PI) composite film, and preparation method and application thereof |
| CN104496463A (en) * | 2014-11-21 | 2015-04-08 | 中国计量学院 | Surfactant assisted in situ co-precipitation method for preparing core-shell structure nano powder |
| CN104841946A (en) * | 2015-04-23 | 2015-08-19 | 深圳先进技术研究院 | Silver nanorod and preparing method thereof |
| CN108031838A (en) * | 2017-12-25 | 2018-05-15 | 畅的新材料科技（上海）有限公司 | A kind of preparation method of M@N core-shell structured nanomaterials |
| CN108314078A (en) * | 2018-02-08 | 2018-07-24 | 西北工业大学 | A kind of preparation method of hollow ball-shape barium-strontium titanate powder material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112973686A (en) * | 2021-03-02 | 2021-06-18 | 大连工业大学 | Method for enhancing photocatalytic performance of heterostructure composite material through pyroelectric effect and application |
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