CN110760093B - Preparation method of Ti-doped porous barium ferrite/polypyrrole composite conductive film - Google Patents
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Abstract
The invention provides a preparation method of a Ti-doped porous barium ferrite/polypyrrole composite conductive film, which comprises the following steps: s1, preparing a surface-treated PI film; s2, preparing xerogel; s3, preparing a Ti-doped porous barium ferrite composite material; s4, preparing a mixed solution A; s5, adding the Ti-doped porous barium ferrite composite material into the mixed solution A, uniformly mixing, coating the mixture on the PI film prepared in the step S1, airing the PI film under the condition of constant temperature and humidity, and then placing the PI film in low-temperature pyrrole steam for reaction to obtain the conductive film. The invention provides a preparation method of a Ti-doped porous barium ferrite/polypyrrole composite conductive film, and the prepared conductive film has excellent conductivity.
Description
Technical Field
The invention relates to the field of conductive films, in particular to a preparation method of a Ti-doped porous barium ferrite/polypyrrole composite conductive film.
Background
Polyimide (PI) is a polar high polymer material containing imide rings on a main chain, has excellent performances of high and low temperature resistance, corrosion resistance, electric insulation, high dimensional stability, low dielectric constant and the like, and is suitable for being used as a dielectric substrate for developing a thin film capacitor. In the conductive polymer, the polypyrrole amine is widely concerned because of the characteristics of easy synthesis, low price, stable chemical property, adjustable conductivity and the like. In addition, hexaferrite, as a traditional permanent magnetic material, is widely applied to microwave devices, magneto-optical devices, high-density magnetic recording media and the like, but the application of compounding polyimide, polypyrrole and ferrite in the field of conductive materials is not available at present.
Disclosure of Invention
The technical problem to be solved is as follows: the invention aims to provide a preparation method of a Ti-doped porous barium ferrite/polypyrrole composite conductive film, and the prepared conductive film has excellent conductivity.
The technical scheme is as follows: a preparation method of a Ti-doped porous barium ferrite/polypyrrole composite conductive film comprises the following steps:
s1, ultrasonically cleaning a pure PI film in 95% ethanol for 10min, ultrasonically cleaning the pure PI film in distilled water for 10min, soaking the pure PI film in 5mol/L potassium hydroxide for 30min, taking out the pure PI film, cleaning the pure PI film, soaking the pure PI film in 1mol/L hydrochloric acid solution for 2h, and cleaning the pure PI film for later use to obtain a surface-treated PI film;
s2, weighing a proper amount of barium nitrate, ferric nitrate, tetrabutyl titanate and citric acid according to a molar ratio of 1:0.2-1:11-11.8:19, dissolving in distilled water, adding cetyl trimethyl ammonium bromide, uniformly mixing, adjusting the pH value to 7 by using an ammonia water solution, keeping the temperature of a water bath at 80 ℃ for 3 hours to obtain sol with viscosity and fluidity, and heating the sol in an oven at 100 ℃ to form dry gel;
s3, placing the xerogel in a muffle furnace, preserving heat for 1.5h at 210 ℃, then heating to 450 ℃, fully preserving heat for 2h, grinding, heating at the speed of 5-l 0 ℃/min, preserving heat for 3h at 1200-1300 ℃, and obtaining the Ti-doped porous barium ferrite composite material;
s4, dissolving hydroxypropyl methyl cellulose and water-soluble carboxymethyl chitosan into FeCl with the concentration of 5-15 wt% according to the mass ratio of 8-10:13To obtain FeCl containing hydroxypropyl methyl cellulose and water-soluble carboxymethyl chitosan with the mass fraction of 0.8-1%3The aqueous solution of (A) is a mixed solution A;
s5, adding the Ti-doped porous barium ferrite composite material into the mixed solution A, uniformly mixing, coating the mixture on the PI film prepared in the step S1, airing the PI film under the condition of constant temperature and humidity, and then placing the PI film in low-temperature pyrrole steam for reaction to obtain the conductive film.
Further, the concentration of barium ions in the step S2 is 0.5 mol/L.
Further, the cetyltrimethylammonium bromide is added in the step S2 at a concentration of 0.5-1 wt%.
Further, in the step S5, the constant temperature and humidity is 20 ℃, and the air humidity is 65%.
Further, the temperature of the low-temperature pyrrole steam in the step S5 is 0-10 ℃.
Has the advantages that: the invention has the advantages that the barium ferrite is more compact by doping Ti, and the growth of barium ferrite grains is promoted; the polypyrrole-barium ferrite nano compound is generated, a certain bond and action exist between a polymer molecular chain and barium ferrite nano particles, and then the barium ferrite is coated with the polypyrrole by adopting an in-situ compounding technology to form the nano microsphere with a cake-peanut structure, so that the nano microsphere has better conductivity.
Detailed Description
Example 1
A preparation method of a Ti-doped porous barium ferrite/polypyrrole composite conductive film comprises the following steps:
s1, ultrasonically cleaning a pure PI film in 95% ethanol for 10min, ultrasonically cleaning the pure PI film in distilled water for 10min, soaking the pure PI film in 5mol/L potassium hydroxide for 30min, taking out the pure PI film, cleaning the pure PI film, soaking the pure PI film in 1mol/L hydrochloric acid solution for 2h, and cleaning the pure PI film for later use to obtain a surface-treated PI film;
s2, weighing a proper amount of barium nitrate, ferric nitrate, tetrabutyl titanate and citric acid according to a molar ratio of 1:0.2:11.8:19, dissolving the barium ions with the concentration of 0.5mol/L in distilled water, adding hexadecyl trimethyl ammonium bromide with the concentration of 0.5 wt%, uniformly mixing, adjusting the pH value to 7 with an ammonia water solution, keeping the temperature of a water bath at 80 ℃ for 3 hours to obtain sol with viscosity and fluidity, and heating the sol in an oven at 100 ℃ to form dry gel;
s3, placing the xerogel in a muffle furnace, preserving heat for 1.5h at 210 ℃, then heating to 450 ℃, fully preserving heat for 2h, grinding, heating at the speed of 5 ℃/min, and preserving heat for 3h at 1200 ℃ to obtain the Ti-doped porous barium ferrite composite material;
s4, dissolving hydroxypropyl methyl cellulose and water-soluble carboxymethyl chitosan into FeCl with the concentration of 5 wt% according to the mass ratio of 10:13To obtain FeCl containing hydroxypropyl methyl cellulose and water-soluble carboxymethyl chitosan with the mass fraction of 0.8 percent3The aqueous solution of (A) is a mixtureMixing the solution A;
s5, adding the Ti-doped porous barium ferrite composite material into the mixed solution A, uniformly mixing, coating the mixture on the PI film prepared in the step S1, airing the PI film at the constant temperature and humidity condition, wherein the temperature is 20 ℃, the air humidity is 65%, then placing the PI film in pyrrole steam at the temperature of 10 ℃ for reaction to obtain the conductive film.
Example 2
A preparation method of a Ti-doped porous barium ferrite/polypyrrole composite conductive film comprises the following steps:
s1, ultrasonically cleaning a pure PI film in 95% ethanol for 10min, ultrasonically cleaning the pure PI film in distilled water for 10min, soaking the pure PI film in 5mol/L potassium hydroxide for 30min, taking out the pure PI film, cleaning the pure PI film, soaking the pure PI film in 1mol/L hydrochloric acid solution for 2h, and cleaning the pure PI film for later use to obtain a surface-treated PI film;
s2, weighing a proper amount of barium nitrate, ferric nitrate, tetrabutyl titanate and citric acid according to a molar ratio of 1:1:11:19, dissolving the barium ions in distilled water, wherein the concentration of the barium ions is 0.5mol/L, adding hexadecyl trimethyl ammonium bromide, the concentration of the hexadecyl trimethyl ammonium bromide is 1 wt%, uniformly mixing, adjusting the pH value to 7 by using an ammonia water solution, keeping the temperature of a water bath at 80 ℃ for 3 hours to obtain sol with viscosity and fluidity, and heating the sol in a drying oven at 100 ℃ to form dry gel;
s3, placing the xerogel in a muffle furnace, preserving heat for 1.5h at 210 ℃, then heating to 450 ℃, fully preserving heat for 2h, grinding, heating at the speed of l0 ℃/min, and preserving heat for 3h at 1300 ℃ to obtain the Ti-doped porous barium ferrite composite material;
s4, dissolving hydroxypropyl methyl cellulose and water-soluble carboxymethyl chitosan into FeCl with the concentration of 15 wt% according to the mass ratio of 8:13To obtain FeCl containing hydroxypropyl methyl cellulose and water-soluble carboxymethyl chitosan with the mass fraction of 1 percent3The aqueous solution of (A) is a mixed solution A;
s5, adding the Ti-doped porous barium ferrite composite material into the mixed solution A, uniformly mixing, coating the mixed solution on the PI film prepared in the step S1, airing the PI film at the constant temperature and humidity condition, wherein the temperature is 20 ℃, the air humidity is 65%, then placing the PI film in pyrrole steam at the temperature of 0 ℃, and reacting to obtain the conductive film.
Example 3
A preparation method of a Ti-doped porous barium ferrite/polypyrrole composite conductive film comprises the following steps:
s1, ultrasonically cleaning a pure PI film in 95% ethanol for 10min, ultrasonically cleaning the pure PI film in distilled water for 10min, soaking the pure PI film in 5mol/L potassium hydroxide for 30min, taking out the pure PI film, cleaning the pure PI film, soaking the pure PI film in 1mol/L hydrochloric acid solution for 2h, and cleaning the pure PI film for later use to obtain a surface-treated PI film;
s2, weighing a proper amount of barium nitrate, ferric nitrate, tetrabutyl titanate and citric acid according to a molar ratio of 1:0.6:11.5:19, dissolving the barium ions with the concentration of 0.5mol/L in distilled water, adding hexadecyl trimethyl ammonium bromide with the concentration of 0.8 wt%, uniformly mixing, adjusting the pH value to 7 with an ammonia water solution, keeping the temperature of a water bath at 80 ℃ for 3 hours to obtain sol with viscosity and fluidity, and heating the sol in an oven at 100 ℃ to form dry gel;
s3, placing the xerogel in a muffle furnace, preserving heat for 1.5h at 210 ℃, then heating to 450 ℃, fully preserving heat for 2h, grinding, heating at the speed of 8 ℃/min, and preserving heat for 3h at 1250 ℃ to obtain the Ti-doped porous barium ferrite composite material;
s4, dissolving hydroxypropyl methyl cellulose and water-soluble carboxymethyl chitosan into FeCl with the concentration of 10 wt% according to the mass ratio of 9:13To obtain FeCl containing hydroxypropyl methyl cellulose and water-soluble carboxymethyl chitosan with the mass fraction of 0.9 percent3The aqueous solution of (A) is a mixed solution A;
s5, adding the Ti-doped porous barium ferrite composite material into the mixed solution A, uniformly mixing, coating the mixed solution on the PI film prepared in the step S1, airing the PI film at the constant temperature and humidity condition, wherein the temperature is 20 ℃, the air humidity is 65%, then placing the PI film in pyrrole steam at the temperature of 5 ℃ for reaction to obtain the conductive film.
Comparative example 1
The procedure of example 1 was repeated except that Ti was not added.
The resistance was measured with a MY-65 digital multimeter and the conductivity was calculated according to the formula σ τ/SR.
| σ(S/m) | |
| Example 1 | 1.921 |
| Example 2 | 1.834 |
| Example 3 | 1.973 |
| Comparative example 1 | 1.62×10-1 |
Claims (5)
1. A preparation method of a Ti-doped porous barium ferrite/polypyrrole composite conductive film is characterized by comprising the following steps:
s1, ultrasonically cleaning a pure PI film in 95% ethanol for 10min, ultrasonically cleaning the pure PI film in distilled water for 10min, soaking the pure PI film in 5mol/L potassium hydroxide for 30min, taking out the pure PI film, cleaning the pure PI film, soaking the pure PI film in 1mol/L hydrochloric acid solution for 2h, and cleaning the pure PI film for later use to obtain a surface-treated PI film;
s2, weighing a proper amount of barium nitrate, ferric nitrate, tetrabutyl titanate and citric acid according to a molar ratio of 1:0.2-1:11-11.8:19, dissolving in distilled water, adding cetyl trimethyl ammonium bromide, uniformly mixing, adjusting the pH value to 7 by using an ammonia water solution, keeping the temperature of a water bath at 80 ℃ for 3 hours to obtain sol with viscosity and fluidity, and heating the sol in an oven at 100 ℃ to form dry gel;
s3, placing the xerogel in a muffle furnace, preserving heat for 1.5h at 210 ℃, then heating to 450 ℃, fully preserving heat for 2h, grinding, heating at the speed of 5-l 0 ℃/min, preserving heat for 3h at 1200-1300 ℃, and obtaining the Ti-doped porous barium ferrite composite material;
s4, dissolving hydroxypropyl methyl cellulose and water-soluble carboxymethyl chitosan into FeCl with the concentration of 5-15 wt% according to the mass ratio of 8-10:13To obtain FeCl containing hydroxypropyl methyl cellulose and water-soluble carboxymethyl chitosan with the mass fraction of 0.8-1%3The aqueous solution of (A) is a mixed solution A;
s5, adding the Ti-doped porous barium ferrite composite material into the mixed solution A, uniformly mixing, coating the mixture on the PI film prepared in the step S1, airing the PI film under the condition of constant temperature and humidity, and then placing the PI film in low-temperature pyrrole steam for reaction to obtain the conductive film.
2. The preparation method of the Ti-doped porous barium ferrite/polypyrrole composite conductive film according to claim 1, characterized in that: the concentration of barium ions in the step S2 is 0.5 mol/L.
3. The preparation method of the Ti-doped porous barium ferrite/polypyrrole composite conductive film according to claim 1, characterized in that: the concentration of cetyltrimethylammonium bromide added in step S2 is 0.5-1 wt%.
4. The preparation method of the Ti-doped porous barium ferrite/polypyrrole composite conductive film according to claim 1, characterized in that: in the step S5, the constant temperature and humidity is 20 ℃, and the air humidity is 65%.
5. The preparation method of the Ti-doped porous barium ferrite/polypyrrole composite conductive film according to claim 1, characterized in that: the temperature of the low-temperature pyrrole vapor in the step S5 is 0-10 ℃.
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| CN102634016B (en) * | 2012-04-05 | 2014-04-16 | 南昌航空大学 | Preparation method of neodymium-lanthanum-doped barium ferrite-polyrrole composite microwave absorbent |
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| "钛掺杂钡铁氧休的制备及吸波性能研究";贾敬国;《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅱ辑》;20131015;第C042-5页 * |
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