CN113716533B - Preparation method of intelligent material - Google Patents
Preparation method of intelligent material Download PDFInfo
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- CN113716533B CN113716533B CN202110905302.3A CN202110905302A CN113716533B CN 113716533 B CN113716533 B CN 113716533B CN 202110905302 A CN202110905302 A CN 202110905302A CN 113716533 B CN113716533 B CN 113716533B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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Abstract
The invention provides a preparation method of an intelligent material, which comprises the steps of firstly synthesizing g-C 3 N 4 The intelligent material prepared by coating lithium tantalate in situ by a sol-gel method and matching with a polar dispersant and dispersing in an insulating base liquid has giant electrorheological property, the viscosity is rapidly increased under the action of an electric field, the liquid state is changed into the solid state, and the shearing strength is high. The preparation process is simple, the mass production is easy, the preparation method is economic and environment-friendly, and the prepared electrorheological fluid is used in the fields of automobile industry, aerospace and mechanical manufacturing.
Description
Technical Field
The invention belongs to the field of material science, and relates to a preparation method of an intelligent material.
Background
The intelligent material is a complex material system integrating a material, a structure, an execution system, a control system and a sensing system. The basic material components of the intelligent material are piezoelectric material, shape memory material, optical fibre, electric (magnetic) rheological liquid, magnetostrictive material, etc. it can imitate life system, sense environmental change and change its own one or several performance parameters in real time. Electrorheological fluids (ERFs) are fluids whose rheological properties change reversibly with the change of an applied electric field. The fluid is usually a suspended dispersion, and under the action of an applied electric field, the apparent viscosity of the dispersion increases significantly with the increase of the electric field strength, and when the electric field strength reaches a certain critical value, the fluid undergoes a phase change and is rapidly solidified. g-C3N4 is a typical polymer semiconductor, CN atoms in the structure of the polymer semiconductor form a highly delocalized pi conjugated system through sp2 hybridization, the polymer semiconductor has the characteristics of high mechanical strength, strong chemical stability, high electron mobility and the like, can provide higher dielectricity in an electrorheological system, but has poor current leakage and dispersibility as a disperse phase. The ferroelectric phase lithium tantalate crystal has good mechanical and physical properties, low cost, high dielectric and insulating properties, and is loaded in g-C 3 N 4 The powder is used as a disperse phase and is matched with a polar molecular dispersant, so that more optimal electrorheological properties can be obtained.
Disclosure of Invention
The invention aims to provide a preparation method of an intelligent material, which is characterized by comprising the following steps:
(1) Drying the cyanamide aqueous solution with the mass fraction of 20-40 wt%, crushing and grinding the dried product, then preserving the heat for 3-5 hours at 530-570 ℃ under the protection of inert gas, and obtaining a product g-C after calcining 3 N 4 ；
(2) Lithium hydroxide, tantalum pentoxide and g-C 3 N 4 Adding the powder into deionized water, and adding tantalum pentoxide and g-C 3 N 4 Stirring the powder evenly, transferring the mixed solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, and oxidizing by hydrogenThe lithium concentration is 6 to 12mol/L, the equivalent concentration of the tantalum pentoxide in the suspension is 0.05 to 0.1mol/L, and g-C 3 N 4 The concentration equivalent of the reaction kettle is 0.1 to 0.5g/L, the reaction kettle is screwed and sealed, and the reaction kettle is placed into a constant-temperature oven at the temperature of between 180 and 220 ℃ for standing reaction for 6 to 12 hours; repeatedly cleaning the product with deionized water until the pH value is 7-8; filtering and separating out the precipitate by adopting a centrifuge precipitation or suction filtration device, and drying the precipitate in a drying oven at the temperature of between 50 and 70 ℃ to obtain a final product, namely lithium tantalate load g-C 3 N 4 And (3) powder.
(3) 30-50 parts by mass of lithium tantalate loaded g-C 3 N 4 Adding the powder into 100 parts by mass of insulating base liquid, adding 0.5-1 part by mass of polar molecular additive, and putting the mixed liquid into a planetary ball mill for dispersing and grinding for 6-10 hours to obtain the intelligent electrorheological fluid.
The insulating base fluid comprises silicone oil, transformer oil, mineral oil or a mixture thereof.
The inert gas comprises nitrogen or argon.
The polar molecular additive comprises one of urea, triethanolamine and octylphenol polyoxyethylene ether.
The invention synthesizes g-C firstly 3 N 4 The intelligent material prepared by coating lithium tantalate in situ by a sol-gel method and matching with a polar dispersant in the powder and dispersing in an insulating base liquid has giant electrorheological characteristics, the viscosity is sharply increased under the action of an electric field, the liquid state is changed into the solid state, and the shearing strength is high. Lithium tantalate coated g-C 3 N 4 The post-trim density is closer to a dispersant system, high dispersibility and non-settling property are obtained, the preparation process is simple, the mass production is easy, the method is economic and environment-friendly, and the prepared electrorheological fluid is used in the fields of automobile industry, aerospace and mechanical manufacturing.
Detailed Description
Example 1:
(1) Drying a cyanamide aqueous solution with the mass fraction of 20wt%, crushing and grinding the dried product, then preserving heat for 5 hours at 530 ℃ under the protection of nitrogen, and calcining to obtain a product g-C 3 N 4 ；
(2) Lithium hydroxide, tantalum pentoxide and g-C 3 N 4 Powder additionIn deionized water, tantalum pentoxide and g-C 3 N 4 Uniformly stirring the powder, transferring the mixed solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, wherein the concentration of lithium hydroxide is 6mol/L, the equivalent concentration of tantalum pentoxide in the suspension is 0.05mol/L, and the g-C content is 3 N 4 The concentration equivalent of the reaction kettle is 0.1g/L, the reaction kettle is screwed and sealed, and the reaction kettle is placed into a constant-temperature oven at 180 ℃ for standing reaction for 12 hours; repeatedly cleaning the product with deionized water until the pH value is 7-8; filtering and separating out precipitate by using a centrifuge precipitation or suction filtration device, and drying in a 70 ℃ oven to obtain a final product, namely lithium tantalate load g-C 3 N 4 And (3) powder.
(3) 50 parts by mass of lithium tantalate loaded g-C 3 N 4 Adding the powder into 100 parts by mass of silicone oil, adding 1 part by mass of octylphenol polyoxyethylene ether, and putting the mixed solution into a homogenizer for dispersing for 10 hours to obtain the electrorheological fluid. The electrorheological fluid has good non-settling property, and no obvious settling occurs after sealing for 7 days at normal temperature. Shear strength 75KPa under 3 kV.
Example 2:
(1) Drying a cyanamide aqueous solution with the mass fraction of 30wt%, crushing and grinding the dried product, then preserving heat for 4 hours at 550 ℃ under the protection of argon, and calcining to obtain a product g-C 3 N 4 ；
(2) Lithium hydroxide, tantalum pentoxide and g-C 3 N 4 Adding the powder into deionized water, and adding tantalum pentoxide and g-C 3 N 4 Uniformly stirring the powder, transferring the mixed solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, wherein the concentration of lithium hydroxide is 12mol/L, the equivalent concentration of tantalum pentoxide in the suspension is 0.1mol/L, and the g-C content is 3 N 4 The concentration equivalent of the reaction kettle is 0.5g/L, the reaction kettle is screwed and sealed, and the reaction kettle is placed into a constant-temperature oven at 220 ℃ for standing reaction for 6 hours; repeatedly cleaning the product with deionized water until the pH value is 7-8; filtering and separating out precipitate by adopting a centrifugal machine precipitation or suction filtration device, and drying in a 60 ℃ drying oven to obtain a final product lithium tantalate load g-C 3 N 4 And (3) powder.
(3) 40 parts by mass of lithium tantalate loaded g-C 3 N 4 Adding the powder into 100 parts by mass of mineral oil, and adding 0.8 part by mass of ureaAnd dispersing the mixed solution in a homogenizer for 8 hours to obtain the electrorheological fluid. The electrorheological fluid has good non-settling property, and no obvious settling occurs after sealing for 7 days at normal temperature. Shear strength 61KPa at 3 kV.
Example 3:
(1) Drying a cyanamide aqueous solution with the mass fraction of 40wt%, crushing and grinding the dried product, then preserving heat for 3 hours at 570 ℃ under the protection of nitrogen, and calcining to obtain a product g-C 3 N 4 ；
(2) Lithium hydroxide, tantalum pentoxide and g-C 3 N 4 Adding the powder into deionized water, and adding tantalum pentoxide and g-C 3 N 4 Uniformly stirring the powder, transferring the mixed solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, wherein the concentration of lithium hydroxide is 8mol/L, the equivalent concentration of tantalum pentoxide in the suspension is 0.08mol/L, and the g-C content is 3 N 4 The concentration equivalent of the reaction kettle is 0.3g/L, the reaction kettle is screwed and sealed, and the reaction kettle is placed into a constant-temperature oven at 200 ℃ for standing reaction for 10 hours; repeatedly cleaning the product with deionized water until the pH value is 7-8; filtering and separating out precipitate by adopting a centrifugal machine precipitation or suction filtration device, and drying in a 50 ℃ oven to obtain a final product lithium tantalate loaded g-C 3 N 4 And (3) powder.
(3) 30 parts by mass of lithium tantalate loaded g-C 3 N 4 Adding the powder into 100 parts by mass of transformer oil, adding 0.5 part by mass of triethanolamine, and dispersing the mixed solution in a homogenizer for 6 hours to obtain the electrorheological fluid. The electrorheological fluid has good non-settling property, and no obvious settling occurs after being sealed for 7 days at normal temperature. Shear strength 55KPa at 3 kV.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which may be made by those skilled in the art without departing from the spirit and scope of the present invention as defined in the appended claims.
Claims (3)
1. The preparation method of the intelligent material is characterized by comprising the following steps of:
the preparation method comprises the following steps:
(1) Drying the cyanamide aqueous solution with the mass fraction of 20-40 wt%, crushing and grinding the dried product, then preserving the heat for 3-5 hours at 530-570 ℃ under the protection of inert gas, and calcining to obtain the product g-C 3 N 4 ；
(2) Lithium hydroxide, tantalum pentoxide and g-C 3 N 4 Adding the powder into deionized water, and adding tantalum pentoxide and g-C 3 N 4 The powder is evenly stirred, and then the mixed solution is transferred into a hydrothermal reaction kettle with a polytetrafluoroethylene liner, the concentration of lithium hydroxide is 6 to 12mol/L, the equivalent concentration of tantalum pentoxide in suspension is 0.05 to 0.1mol/L, and the g-C content is 3 N 4 The concentration equivalent of the reaction kettle is 0.1 to 0.5g/L, the reaction kettle is screwed and sealed, and the reaction kettle is put into a constant-temperature oven with the temperature of 180 to 220 ℃ for standing reaction for 6 to 12 hours; repeatedly cleaning the product with deionized water until the pH value is 7-8; filtering and separating out the precipitate by adopting a centrifuge precipitation or suction filtration device, and drying the precipitate in a drying oven at the temperature of between 50 and 70 ℃ to obtain a final product, namely lithium tantalate load g-C 3 N 4 And (3) powder.
(3) 30-50 parts by mass of lithium tantalate loaded g-C 3 N 4 Adding the powder into 100 parts by mass of insulating base liquid, adding 0.5-1 part by mass of polar molecular additive, and putting the mixed liquid into a planetary ball mill for dispersing and grinding for 6-10 hours to obtain intelligent electrorheological fluid; the insulating base fluid comprises silicone oil, transformer oil, mineral oil or a mixture thereof; the polar molecular additive comprises one of urea, triethanolamine and octyl phenol polyoxyethylene ether.
2. A method of claim 1, wherein the inert gas comprises nitrogen or argon.
3. The intelligent material prepared by the preparation method of the intelligent material according to any one of claims 1 to 2 has giant electrorheological property, the viscosity is sharply increased under the action of an electric field and is changed from a liquid state to a solid state, and the prepared electrorheological fluid is used in the fields of automobile industry, aerospace and mechanical manufacturing.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1533078A (en) * | 1976-08-30 | 1978-11-22 | Tokyo Shibaura Electric Co | Method of manufacturing single crystal lithium tantalate adapted for application of surface waves and piezoelectricity |
| US20060169196A1 (en) * | 2003-03-06 | 2006-08-03 | Shin-Etsu Chemical Co., Ltd. | Method for producing lithium tantalate crystal |
| CN101225545A (en) * | 2007-10-25 | 2008-07-23 | 宁夏东方钽业股份有限公司 | Method for preparing near-stoichiometric lithium tantalate crystals |
| CN102943244A (en) * | 2012-11-26 | 2013-02-27 | 中国民用航空飞行学院 | Preparation method for LiTaO3 film through ion beam enhanced deposition (IBED) |
| CN103787415A (en) * | 2014-01-23 | 2014-05-14 | 上海海事大学 | Method for preparing lithium tantalate nano-powder by adopting solvothermal method |
| CN104163454A (en) * | 2014-09-01 | 2014-11-26 | 中山大学 | Preparing method of lithium tantalate crystal |
-
2021
- 2021-08-04 CN CN202110905302.3A patent/CN113716533B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1533078A (en) * | 1976-08-30 | 1978-11-22 | Tokyo Shibaura Electric Co | Method of manufacturing single crystal lithium tantalate adapted for application of surface waves and piezoelectricity |
| US20060169196A1 (en) * | 2003-03-06 | 2006-08-03 | Shin-Etsu Chemical Co., Ltd. | Method for producing lithium tantalate crystal |
| CN101225545A (en) * | 2007-10-25 | 2008-07-23 | 宁夏东方钽业股份有限公司 | Method for preparing near-stoichiometric lithium tantalate crystals |
| CN102943244A (en) * | 2012-11-26 | 2013-02-27 | 中国民用航空飞行学院 | Preparation method for LiTaO3 film through ion beam enhanced deposition (IBED) |
| CN103787415A (en) * | 2014-01-23 | 2014-05-14 | 上海海事大学 | Method for preparing lithium tantalate nano-powder by adopting solvothermal method |
| CN104163454A (en) * | 2014-09-01 | 2014-11-26 | 中山大学 | Preparing method of lithium tantalate crystal |
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