CN113716533A - Preparation method of intelligent material - Google Patents
Preparation method of intelligent material Download PDFInfo
- Publication number
- CN113716533A CN113716533A CN202110905302.3A CN202110905302A CN113716533A CN 113716533 A CN113716533 A CN 113716533A CN 202110905302 A CN202110905302 A CN 202110905302A CN 113716533 A CN113716533 A CN 113716533A
- Authority
- CN
- China
- Prior art keywords
- powder
- preparation
- reaction kettle
- mass
- hours
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention provides a preparation method of an intelligent material, which comprises the steps of firstly synthesizing g-C3N4The 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. The g-C3N4 is a typical polymer semiconductor, CN atoms in the structure of the polymer semiconductor are hybridized by sp2 to form a highly delocalized pi conjugated system, and the polymer semiconductor has the characteristics of high mechanical strength, strong chemical stability, high electron mobility and the like, can provide higher dielectric property 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 and high dielectric propertyAnd excellent insulating property, and lithium tantalate is loaded in g-C3N4The powder is used as a disperse phase and is matched with a polar molecular dispersing agent, so that more optimal electrorheological properties can be expected to 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 a cyanamide aqueous solution with the mass fraction of 20-40 wt%, crushing and grinding the dried product, then preserving heat for 3-5 hours at 530-570 ℃ under the protection of inert gas, and calcining to obtain a product g-C3N4；
(2) Lithium hydroxide, tantalum pentoxide and g-C3N4Adding the powder into deionized water, and adding tantalum pentoxide and g-C3N4Uniformly stirring the powder, transferring the mixed solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, wherein the concentration of lithium hydroxide is 6-12 mol/L, the equivalent concentration of tantalum pentoxide in turbid liquid is 0.05-0.1 mol/L, and the g-C content is3N4The concentration equivalent of the reaction kettle is 0.1-0.5 g/L, the reaction kettle is screwed and sealed, and the reaction kettle is placed in a constant-temperature oven at 180-220 ℃ for standing reaction for 6-12 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 50-70 ℃ to obtain a final product, namely lithium tantalate load g-C3N4And (3) powder.
(3) 30-50 parts by mass of lithium tantalate-loaded g-C3N4Adding 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 octyl phenol polyoxyethylene ether.
The invention firstly synthesizes g-C3N4Powder in-situ coated by sol-gel methodThe lithium tantalate is coated, the polar dispersant is matched, and the intelligent material prepared by dispersing the lithium tantalate in the 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. Lithium tantalate coated g-C3N4The 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 20 wt%, 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-C3N4；
(2) Lithium hydroxide, tantalum pentoxide and g-C3N4Adding the powder into deionized water, and adding tantalum pentoxide and g-C3N4Uniformly 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 is3N4The 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-C3N4And (3) powder.
(3)50 parts by mass of lithium tantalate loaded g-C3N4Adding the powder into 100 parts by mass of silicone oil, adding 1 part by mass of octylphenol polyoxyethylene ether, and dispersing the mixed solution in a homogenizer for 10 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 75KPa at 3 kV.
Example 2:
(1) drying a cyanamide aqueous solution with the mass fraction of 30 wt%, 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-C3N4；
(2) Lithium hydroxide, tantalum pentoxide and g-C3N4Adding the powder into deionized water, and adding tantalum pentoxide and g-C3N4Uniformly 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 is3N4The 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 using a centrifuge precipitation or suction filtration device, and drying in a 60 ℃ oven to obtain the final product, namely lithium tantalate load g-C3N4And (3) powder.
(3)40 parts by mass of lithium tantalate loaded g-C3N4Adding the powder into 100 parts by mass of mineral oil, adding 0.8 part by mass of urea, and 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 being sealed 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 40 wt%, 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-C3N4；
(2) Lithium hydroxide, tantalum pentoxide and g-C3N4Adding the powder into deionized water, and adding tantalum pentoxide and g-C3N4Uniformly 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 is3N4The 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 using a centrifuge precipitation or suction filtration device, and drying in a 50 ℃ oven to obtain the final product, namely lithium tantalate load g-C3N4And (3) powder.
(3)30 parts by massg-C of lithium tantalate3N4Adding 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 can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (5)
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 a cyanamide aqueous solution with the mass fraction of 20-40 wt%, crushing and grinding the dried product, then preserving heat for 3-5 hours at 530-570 ℃ under the protection of inert gas, and calcining to obtain a product g-C3N4；
(2) Lithium hydroxide, tantalum pentoxide and g-C3N4Adding the powder into deionized water, and adding tantalum pentoxide and g-C3N4Uniformly stirring the powder, transferring the mixed solution into a hydrothermal reaction kettle with a polytetrafluoroethylene inner container, wherein the concentration of lithium hydroxide is 6-12 mol/L, the equivalent concentration of tantalum pentoxide in turbid liquid is 0.05-0.1 mol/L, and the g-C content is3N4The concentration equivalent of the reaction kettle is 0.1-0.5 g/L, the reaction kettle is screwed and sealed, and the reaction kettle is placed in a constant-temperature oven at 180-220 ℃ for standing reaction for 6-12 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 50-70 ℃ to obtain a final product, namely lithium tantalate load g-C3N4And (3) powder.
(3) 30-50 parts by mass of lithium tantalate-loaded g-C3N4Powder addingAdding the mixture 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.
2. A method for preparing a smart material as claimed in claim 1, wherein the insulating base fluid comprises silicone oil, transformer oil, mineral oil or a mixture thereof.
3. A method of manufacturing a smart material as claimed in claim 1, wherein the inert gas comprises nitrogen or argon.
4. The method of claim 1, wherein the polar molecular additive comprises one of urea, triethanolamine, and polyoxyethylene octylphenol ether.
5. The intelligent material prepared by the preparation method of the intelligent material according to any one of claims 1 to 4 has giant electrorheological property, the viscosity is rapidly 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110905302.3A CN113716533B (en) | 2021-08-04 | 2021-08-04 | Preparation method of intelligent material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110905302.3A CN113716533B (en) | 2021-08-04 | 2021-08-04 | Preparation method of intelligent material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113716533A true CN113716533A (en) | 2021-11-30 |
| CN113716533B CN113716533B (en) | 2022-11-18 |
Family
ID=78675248
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110905302.3A Active CN113716533B (en) | 2021-08-04 | 2021-08-04 | Preparation method of intelligent material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113716533B (en) |
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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113716533B (en) | 2022-11-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101179385B1 (en) | Composition for dispersing of particle, composition having particle dispersed therein, process for producing the same, and sintered compact of anatase titanium oxide | |
| CN101089164B (en) | Polar molecule type electric rheologic liquid | |
| Li et al. | Synthesis of (La+ Nb) co-doped TiO2 rutile nanoparticles and dielectric properties of their derived ceramics composed of submicron-sized grains | |
| CN107057809B (en) | Electrorheological fluid with high breakdown resistance and preparation method thereof | |
| CN110372977B (en) | Ferromagnetic composite polymer nano film and preparation method thereof | |
| CN108892503B (en) | High-electrocaloric-effect thin film material and preparation method thereof | |
| CN101423244A (en) | Method for preparing tin doped barium titanate nano powder | |
| CN113716533B (en) | Preparation method of intelligent material | |
| CN1123551C (en) | Nanometer grade tetragonal-phase barium titanate powder and its prepn. | |
| Zhao et al. | A new organic/inorganic hybrid with high electrorheological activity | |
| CN111995780B (en) | Preparation method of in-situ polymerization high-dielectric film based on modified barium titanate nanowire | |
| CN113511673A (en) | Preparation method of high-axial-ratio and high-dispersion barium titanate powder | |
| CN103755958B (en) | A kind of preparation method of polyimides/CaCu 3 Ti 4 O coated with silver nano particle composite material | |
| Huang et al. | Preparation and characterization of conductive polyaniline/zirconia nanoparticles composites | |
| CN109553127B (en) | Sodium bismuth titanate nanowire prepared by hydrothermal method and preparation method thereof | |
| CN113087514B (en) | Lead-free multiferroic material with relaxor ferroelectric property and preparation method thereof | |
| CN107603712B (en) | Flower-like polyaniline nanoparticle electrorheological fluid and preparation method thereof | |
| CN101575544B (en) | Surface modified titanium-calcium oxyoxalate electrorheological fluid and preparation method thereof | |
| CN101805176A (en) | Method for reducing sintering temperature of high dielectric ceramic material | |
| CN101525151B (en) | Manufacturing technique for high-purity electronic grade strontium titanate | |
| CN113755229A (en) | C3N4/TiO2Nano composite particle electric rheologic liquid and its preparing method | |
| CN114773645B (en) | Dielectric flexible film and preparation method thereof | |
| CN113845964A (en) | Preparation method of electrorheological fluid | |
| CN108706626A (en) | A kind of SrTiO3The preparation method of nano material | |
| Anas et al. | Influence of Zirconium (Zr4+) Substitution on the Crystal Structure and Optical and Dielectric Properties of Sr0. 8Mg0. 2 (Sn1–x Zr x) O3 Ceramics |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |