CN112509813A - PbTiO 23Nano-sheet and PI composite high-temperature dielectric energy storage material and preparation method thereof - Google Patents
PbTiO 23Nano-sheet and PI composite high-temperature dielectric energy storage material and preparation method thereof Download PDFInfo
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- CN112509813A CN112509813A CN202011329969.5A CN202011329969A CN112509813A CN 112509813 A CN112509813 A CN 112509813A CN 202011329969 A CN202011329969 A CN 202011329969A CN 112509813 A CN112509813 A CN 112509813A
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- 238000004146 energy storage Methods 0.000 title claims abstract description 39
- 239000011232 storage material Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000002135 nanosheet Substances 0.000 claims abstract description 53
- 229910003781 PbTiO3 Inorganic materials 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000003989 dielectric material Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000013329 compounding Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 13
- 229940046892 lead acetate Drugs 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 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 7
- NMGYKLMMQCTUGI-UHFFFAOYSA-J diazanium;titanium(4+);hexafluoride Chemical compound [NH4+].[NH4+].[F-].[F-].[F-].[F-].[F-].[F-].[Ti+4] NMGYKLMMQCTUGI-UHFFFAOYSA-J 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 238000010335 hydrothermal treatment Methods 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims 1
- 229910001887 tin oxide Inorganic materials 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 7
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 7
- 239000003990 capacitor Substances 0.000 description 4
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 description 4
- 239000002033 PVDF binder Substances 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920006378 biaxially oriented polypropylene Polymers 0.000 description 2
- 239000011127 biaxially oriented polypropylene Substances 0.000 description 2
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 229920005575 poly(amic acid) Polymers 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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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
- H01G4/18—Organic dielectrics of synthetic material, e.g. derivatives of cellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
The invention discloses PbTiO3A nano-sheet and PI compounded high-temperature dielectric energy storage material and a preparation method thereof belong to the field of dielectric energy storage, and comprise growing PbTiO on the surface of FTO which is conductive3Nanosheet array, PI as dielectric material and PbTiO grown3FTO compounding of the nanosheet array; the high-temperature dielectric energy storage material has great application value in the fields of hybrid vehicles and the like, and the development technology of the high-temperature dielectric energy storage material is relatively lagged behind at present and is limited by the high-temperature resistance and the energy storage density of the material. The invention synthesizes PbTiO through hydrothermal method3Nano sheet array, and in-situ polymerization to obtain PI/PbTiO3The composite material of (1). Compounding not only has high temperatureThe invention has the advantages of simple process and low material cost.
Description
Technical Field
The invention belongs to the field of dielectric energy storage, and particularly provides PbTiO3Nano-sheet and PI composite high-temperature dielectric energy storage material anda preparation method.
Background
At present, countries in the world generally face the problem of energy depletion, and high demand is provided for development of new energy. Clean renewable energy sources such as solar, wind and geothermal are generally intermittent and uncontrollable and therefore need to be collected, stored and converted. The dielectric energy storage capacitor can release stored energy in a very short time to generate large power pulse, so that the dielectric energy storage capacitor has wide application prospect in the aspects of pulse power systems, particularly hybrid electric vehicles, grid-connected photovoltaic power generation and the like.
In practical application, the working conditions of high power and high temperature are often adopted, for example, the working temperature of a capacitor in a hybrid automobile inverter is 140 ℃, and the working temperature in underground oil-gas exploration reaches more than 250 ℃. Therefore, the development of a dielectric material suitable for high temperature is urgently required. At present, a commercial dielectric energy storage capacitor usually adopts a biaxially oriented polypropylene film (BOPP) as a dielectric material, but the energy storage density is only 2-3J/cm3The working temperature which can be endured is below 85 ℃. Polyvinylidene fluoride (PVDF) and its derivatives with higher energy storage density>15 J/cm3). However, PVDF-based ferroelectric polymers also have operating temperatures below 125 ℃.
For composite dielectrics, a high temperature polymer matrix material, a high Curie temperature (T) is selectedC) The ceramic filling material and the construction of a special filling body model are very critical. At present, no literature report or patent publication exists in this respect.
Disclosure of Invention
The present invention provides a PbTiO compound for solving the above problems3A nano-sheet and PI compounded high-temperature medium energy storage material and a preparation method thereof. The invention provides PbTiO with high Curie point (470 ℃)3The nano sheet array and high-temperature polymer polyimide (PI, the working temperature reaches 450 ℃) are compounded to form a high-temperature energy storage dielectric medium, and the energy storage density of the composite material is improved through the two-dimensional regular configuration of the filling body.
PbTiO according to the present invention3The nanosheet array is characterized in that: 1) PbTiO 23Nanosheet size:the length and width of the nanosheet are 10-30 μm, and the thickness is 10-300 nm; 2) PbTiO 23The nano sheet phase is a tetragonal phase; 3) PbTiO 23The nano sheets are orderly arranged in a mode of being vertical to the substrate, and gaps between the nano sheets are 50-20 mu m;
the PbTiO of the invention3The thickness of the high-temperature medium energy storage material compounded by the nanosheet array and the PI is 30-50 microns; the working temperature range is between room temperature and 400 ℃; energy density 14J/cm3The above.
Preparing the PI/PbTiO3The method for preparing the nanosheet array high-temperature composite dielectric material comprises the following steps:
1) in a 50 ml beaker, concentrated hydrochloric acid (36% -38%) was mixed with deionized water at a ratio of 1: 2, and preparing a hydrochloric acid solution. To this was added tetrabutyltitanate of 1.7% by volume fraction, the mixture was stirred and mixed well, and then ammonium hexafluorotitanate of 0.19% by volume fraction was added and stirred again.
2) The solution was transferred to an autoclave, to which an FTO conductive glass was added with the conductive side facing up. Carrying out hydrothermal reaction. After the reaction, the autoclave was cooled to room temperature, and then the FTO substrate was washed with deionized water and then dried. Annealing at 500-600 ℃ for 1-3 h.
3) TiO to be grown on FTO2Adding the nanosheet array into lead acetate aqueous solution with the molar concentration of 5-10 mol/L, and carrying out hydrothermal reaction to obtain PbTiO3A nanosheet array.
4) Will grow PbTiO3And (3) placing the FTO of the nanosheet array on a spin coater, uniformly coating the PI solution added with a certain amount of the defoaming agent, and finally carrying out curing treatment.
The step 1) is to add tetrabutyl titanate with the volume ratio of 1.7 percent and stir for 10 minutes, and add ammonium hexafluorotitanate with the volume ratio of 0.19 percent and stir for 30 minutes.
The step 2) hydrothermal treatment is carried out for 12-14 h at 160-200 ℃.
Said step 2) is dried at 80 ℃. The annealing is carried out at 500-600 ℃ for 2-4 h.
The volume percentage of the lead acetate aqueous solution added in the step 3) is 20-80%, and the temperature is kept at 200-300 ℃ for 1-10 hours.
And 4) rotating the spin coater in the step 4) for 10s at 0.2-0.5 kilo revolutions per minute, and then rotating for 1min at 8.5-9.5 kilo revolutions per minute.
The formula of the PI solution in the step 4) is as follows: a certain amount of m-cresol and 3.2 mass percent (3.19mmol) ODA are respectively added into a 100mL three-neck flask with a mechanical stirring device and a reflux condensing device, mechanical stirring is started until the ODA is completely dissolved in the m-cresol, 8.3 mass percent (3.19mmol) BPADA is added in batches within 2h to ensure that the solid content of the whole solution is about 10 percent, and stirring is continued for 3h to obtain polyamic acid (PAA). Then adding isoquinoline with the volume fraction of 4% under the protection of nitrogen, gradually increasing the temperature to 200 ℃, and preserving the temperature for a period of time to obtain a PI solution.
And 4) curing, namely treating at 40-60 ℃ for 0.5h, and then treating at 80-100 ℃, 140-160 ℃, 190-210 ℃ and 240-260 ℃ for 1h and treating at 280-300 ℃ for 2h respectively.
The technical effects of the invention are as follows: the invention synthesizes PbTiO through hydrothermal method3Nano sheet array, and in-situ polymerization to obtain PI/PbTiO3The composite material of (1). The composite material not only has high-temperature working capacity, but also has high energy storage performance, and in addition, the invention also has the advantages of simple process and low material cost. The working temperature is between room temperature and 400 ℃; energy storage density: 14J/cm3The method has important significance in the field of high-temperature dielectric energy storage.
Drawings
FIG. 1 shows PI/PbTiO3Schematic representation of a nanoplate array composite.
FIG. 2 shows PI/PbTiO3Surface scanning electron microscope picture of nano sheet array composite material
FIG. 3 shows PI/PbTiO3Dielectric constant frequency curve of nano-sheet array composite material
Detailed Description
Example 1
Aiming at the problems in the prior art, the invention provides PbTiO3Compounding of nanosheet array and PIThe high temperature medium energy storage material and the preparation method.
Preparation of the PbTiO3The method for preparing the high-temperature medium energy storage material compounded by the nanosheet array and the PI comprises the following steps:
1) 13 ml of hydrochloric acid and 17 ml of deionized water were mixed in a beaker, and then 1.7% by volume of tetrabutyl titanate was added. The mixture was stirred for 10 minutes, then 0.19% volume fraction ammonium hexafluorotitanate was added, and stirred for another 30 minutes. The solution was then transferred to an autoclave and subjected to hydrothermal treatment at 160 ℃ for 12 hours. In a teflon lined cylindrical autoclave, there is a piece of FTO with its conductive side facing up. After the autoclave was cooled to room temperature, the FTO substrate was washed with deionized water and then dried at 80 ℃. The obtained TNS array film was annealed at 500 ℃ for 2 hours.
2) Using lead acetate aqueous solution with the molar concentration of 5mol/L as a medium and TiO2Adding 50 volume percent of hydrothermal reaction solution, namely lead acetate aqueous solution, into the nanosheet array serving as a template, and preserving the temperature at 200 ℃ for 4 hours to obtain PbTiO3A nanosheet array.
3) Will grow PbTiO3And (3) placing the FTO of the nanosheet array on a spin coater, uniformly coating the PI solution, and rotating at 0.2 kilorevolutions per minute for 10s and then at 8.5 kilorevolutions per minute for 1 min. Finally, the mixture is cured at 40 ℃ for 0.5h, then at 80 ℃, 140 ℃, 190 ℃ and 240 ℃ for 1h and at 280 ℃ for 2 h. The final results are shown in fig. 1 and 2.
The resulting measured dielectric constant (1 kHz) was 21 (as shown in FIG. 3), and the energy storage density was 14.8J/cm3The temperature range is from room temperature to 400 ℃.
Example 2
Preparation of the PbTiO3The method for preparing the high-temperature medium energy storage material compounded by the nanosheet array and the PI comprises the following steps:
1) 16 ml of hydrochloric acid and 21 ml of deionized water were mixed in a beaker, and then 1.7% by volume of tetrabutyl titanate was added. The mixture was stirred for 10 minutes, then 0.19% volume fraction ammonium hexafluorotitanate was added, and stirred for another 30 minutes. The solution was then transferred to an autoclave and subjected to a hydrothermal treatment at 180 ℃ for 13 hours. In a teflon lined cylindrical autoclave, there is a piece of FTO with its conductive side facing up. After the autoclave was cooled to room temperature, the FTO substrate was washed with deionized water and then dried at 80 ℃. The obtained TNS array film was annealed at 550 ℃ for 3 hours.
2) Using TiO as medium and lead acetate solution with the molar concentration of 6 mol/L2Adding 60 volume percent of hydrothermal reaction solution, namely lead acetate aqueous solution, into the nanosheet array serving as a template, and preserving the temperature at 250 ℃ for 5 hours to obtain PbTiO3A nanosheet array.
3) Will grow PbTiO3And (3) placing the FTO of the nanosheet array on a spin coater, uniformly coating the PI solution, and rotating at 0.3 kilorevolutions per minute for 10s and then at 9 kilorevolutions per minute for 1 min. Finally, the mixture is cured at 50 ℃ for 0.5h, then at 90 ℃, 150 ℃, 200 ℃ and 250 ℃ for 1h and at 290 ℃ for 2 h. As shown in fig. 1 and 2.
The final measured dielectric constant (1 kHz) was 24, and the energy storage density was 14.5J/cm3The temperature range is from room temperature to 400 ℃.
Example 3
Preparation of the PbTiO3The method for preparing the high-temperature medium energy storage material compounded by the nanosheet array and the PI comprises the following steps:
1) 18 ml of hydrochloric acid and 24 ml of deionized water were mixed in a beaker, and then 1.7% by volume of tetrabutyl titanate was added. The mixture was stirred for 10 minutes, then 0.19% volume fraction ammonium hexafluorotitanate was added, and stirred for another 30 minutes. The solution was then transferred to an autoclave and subjected to a hydrothermal treatment at 200 ℃ for 14 hours. In a teflon lined cylindrical autoclave, there is a piece of FTO with its conductive side facing up. After the autoclave was cooled to room temperature, the FTO substrate was washed with deionized water and then dried at 80 ℃. The obtained TNS array film was annealed at 600 ℃ for 4 hours.
2) Using TiO as medium and lead acetate solution with the molar concentration of 7 mol/L2Adding 70 volume percent of hydrothermal reaction solution, namely lead acetate aqueous solution, into the nano-sheet array serving as a template, and preserving the temperature at 300 DEG CAfter 6 hours, PbTiO is obtained3A nanosheet array.
3) Will grow PbTiO3And (3) placing the FTO of the nanosheet array on a spin coater, uniformly coating the PI solution, and rotating at 0.4 kilorevolutions per minute for 10s and then at 9.5 kilorevolutions per minute for 1 min. Finally, the mixture is cured at 60 ℃ for 0.5h, then at 100 ℃, 160 ℃, 200 ℃ and 260 ℃ for 1h and at 300 ℃ for 2 h. As shown in fig. 1 and 2.
The final measured dielectric constant (1 kHz) was 18, and the energy storage density was 14.2J/cm3The temperature range is from room temperature to 390 ℃.
Claims (10)
1. PbTiO 23The nano-sheet and PI compounded high-temperature medium energy storage material is characterized in that PbTiO grows on the conductive surface of FTO3Nanosheet array, PI as dielectric material and PbTiO grown3And (4) FTO compounding of the nanosheet array.
2. PbTiO according to claim 13The nano-sheet and PI compounded high-temperature medium energy storage material is characterized in that the PbTiO is3The length and the width of the nanosheet are both 10-30 mu m, and the thickness is 10-300 nm; PbTiO 23The nano sheet phase is a tetragonal phase; PbTiO 23The nano sheets are orderly arranged in a mode of being vertical to the substrate, and gaps between the nano sheets are 50-20 mu m.
3. PbTiO according to claim 13The nanosheet and PI compounded high-temperature medium energy storage material is characterized in that the thickness of the nanosheet and PI compounded high-temperature medium energy storage material is 30-50 micrometers.
4. PbTiO 23The method for preparing the high-temperature medium energy storage material compounded by the nanosheets and the PI comprises the following steps:
1) adding tetrabutyl titanate into a reaction container filled with dilute hydrochloric acid, uniformly stirring, then adding ammonium hexafluorotitanate, and stirring again;
2) transferring the solution in the step 1) into a polytetrafluoroethylene-lined cylindrical autoclave with an FTO (fluorine-doped tin oxide) with a conductive surface facing upwards, and carrying out hydrothermal treatment;
3) after the high-pressure kettle is cooled to room temperature, washing the FTO substrate by deionized water, and then drying;
4) annealing the FTO obtained in the step 3) at 500-600 ℃ for 1-3 h to obtain the grown TiO2FTO of the array;
5) preparing lead acetate aqueous solution with the molar concentration of 1-10 mol/L, and adding the lead acetate aqueous solution into the TiO-grown material obtained in the step 4)2Adding lead acetate aqueous solution into FTO of the array, and preserving the temperature to obtain PbTiO3A nanosheet array;
6) will grow PbTiO3And (3) placing the FTO of the nanosheet array on a spin coater, uniformly coating the PI solution, and finally carrying out curing treatment.
5. A PbTiO according to claim 43The method for preparing the high-temperature medium energy storage material compounded by the nanosheets and the PI is characterized in that the volume ratio of the dilute hydrochloric acid and the tetrabutyl titanate in the step 1) is 120: 1 to 60: 1, the ratio of the dilute hydrochloric acid solution to the ammonium hexafluorotitanate is 60-240 ml/g.
6. A PbTiO according to claim 43The method for preparing the high-temperature medium energy storage material compounded by the nanosheets and the PI is characterized in that the hydrothermal treatment in the step 2) is carried out for 12-14 hours at 160-200 ℃.
7. A PbTiO according to claim 43The method for preparing the high-temperature medium energy storage material compounded by the nanosheets and the PI is characterized in that the step 2) is carried out drying at 80 ℃, and the step 4) is carried out annealing at 500-600 ℃ for 2-4 h.
8. A PbTiO according to claim 43The method for preparing the high-temperature medium energy storage material compounded by the nanosheets and the PI is characterized in that the lead acetate added in the step 5) accounts for 20-80% of the whole solution, and the solution is kept at the temperature of 200-300 ℃ for 1-10 hours.
9. A PbTiO according to claim 43The method for preparing the high-temperature medium energy storage material compounded by the nanosheets and the PI is characterized in that in the step 6), the spin coater rotates at 0.2-0.5 kilorevolutions per minute for 10s, and then rotates at 8.5-9.5 kilorevolutions per minute for 1 min.
10. A PbTiO according to claim 43The method for preparing the high-temperature medium energy storage material compounded by the nanosheets and the PI is characterized in that the step 6) is performed with curing treatment for 0.5 hour at the temperature of 40-60 ℃, and then the treatment is performed for 1 hour at the temperature of 80-100 ℃, 140-160 ℃, 190-210 ℃ and 240-260 ℃ and for 2 hours at the temperature of 280-300 ℃.
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|---|---|---|---|---|
| JPH02225358A (en) * | 1989-02-23 | 1990-09-07 | Matsushita Electric Works Ltd | Complex dielectric material |
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| CN102925979A (en) * | 2012-11-08 | 2013-02-13 | 浙江大学 | Method for preparing perovskite lead titanate crystal nanosheet |
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| CN107056087A (en) * | 2017-04-20 | 2017-08-18 | 清华大学 | A kind of preparation method of the thin dielectric film with titanic oxide nanorod array |
-
2020
- 2020-11-24 CN CN202011329969.5A patent/CN112509813B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02225358A (en) * | 1989-02-23 | 1990-09-07 | Matsushita Electric Works Ltd | Complex dielectric material |
| CN102779651A (en) * | 2012-07-31 | 2012-11-14 | 中国科学院化学研究所 | Preparation method of ultra-thin inorganic/organic composite dielectric layer material for supercapacitor |
| CN102925979A (en) * | 2012-11-08 | 2013-02-13 | 浙江大学 | Method for preparing perovskite lead titanate crystal nanosheet |
| CN103253699A (en) * | 2013-06-07 | 2013-08-21 | 浙江大学 | Self-assembled structure of perovskite/lead titanate nanosheet and preparation method thereof |
| CN107056087A (en) * | 2017-04-20 | 2017-08-18 | 清华大学 | A kind of preparation method of the thin dielectric film with titanic oxide nanorod array |
Non-Patent Citations (1)
| Title |
|---|
| 简刚等: "用于高介电复合材料的全包裹 Ag@TiO2 填充颗粒的制备", 《无机材料学报》 * |
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