CN115287040A - Preparation method of anti-static composite material - Google Patents
Preparation method of anti-static composite material Download PDFInfo
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- CN115287040A CN115287040A CN202210939532.6A CN202210939532A CN115287040A CN 115287040 A CN115287040 A CN 115287040A CN 202210939532 A CN202210939532 A CN 202210939532A CN 115287040 A CN115287040 A CN 115287040A
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Abstract
A preparation method of an antistatic composite material comprises the following steps: (1) Respectively dissolving tin tetrachloride pentahydrate and antimony trichloride in a proper amount of absolute ethyl alcohol, and then fully mixing the two dissolved solutions to obtain a tin-antimony mixed solution; (2) Stirring the tin-antimony mixed solution obtained in the step (1) on a magnetic stirrer at constant temperature; (3) carrying out reflux treatment on the tin-antimony mixed solution at about 78 ℃; in conclusion, the invention uses SnCl 4 And SbCl 3 Preparing a precursor by using NaOH or ammonia water as a precipitator and a chemical codeposition method, and calcining the precursor at high temperature to obtain powder; the method is suitable for industrial mass production, but the grain diameter of the obtained powder is wider; low manufacturing cost, easy control and short period.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of an anti-static composite material.
Background
Along with the continuous application of electronic products, electrostatic hazard and electromagnetic pollution are increasingly deepened, ceramics are one of the most important materials in buildings, and the application of the anti-static ceramics not only can play a better decorative role, but also can fundamentally eliminate the hazard of electrostatic and electromagnetic radiation to human bodies in various industries.
Disclosure of Invention
The invention aims to provide a preparation method of an antistatic composite material, which has low manufacturing cost, is easy to control, and is safe and environment-friendly.
In order to solve the technical problems, the invention adopts the following technical scheme: a preparation method of an antistatic composite material comprises the following steps:
(1) Respectively dissolving tin tetrachloride pentahydrate and antimony trichloride in a proper amount of absolute ethyl alcohol, and then fully mixing the two dissolved solutions to obtain a tin-antimony mixed solution;
(2) Stirring the tin-antimony mixed solution obtained in the step (1) on a magnetic stirrer at a constant temperature ranging from 26 ℃ to 33 ℃ for 3 hours;
(3) Carrying out reflux treatment on the tin-antimony mixed solution at about 78 ℃;
(4) Taking the upper layer solution, titrating with a small amount of ammonia water, keeping a proper pH value within the range of 2-7, carrying out full alcoholysis reaction on the solution until a light yellow sol solution is formed, and then repeatedly washing with absolute ethyl alcohol to remove chloride ions in the solution;
(5) Carrying out rotary evaporation treatment by using a rotary evaporator;
(6) And then calcining to obtain the antimony doped tin oxide powder.
Preferably, the electrical resistivity of the antimony-doped tin oxide powder obtained in step (6) is measured by using a resistivity resistance meter.
Preferably, the resistivity resistance instrument comprises a base platform and a resistance meter, wherein a polyacrylate pipe is fixed on the base platform, two metal rods are arranged in the polyacrylate pipe, the antimony-doped tin oxide powder is located between the two metal rods, the two metal rods are respectively connected with the electronic watch through conducting wires, and a weight block is placed on the metal rod above the metal rods.
Preferably, the method for measuring the resistivity of the antimony doped tin oxide powder by using a resistivity resistance meter comprises the following steps: adding the prepared antimony-doped tin oxide powder into a polyacrylate tube, then inserting an upper metal rod above the antimony-doped tin oxide powder, placing a weight block, and calculating the resistivity of the antimony-doped tin oxide powder according to the following formula; the resistivity calculation formula is as follows: p = RS/H, where p is the volume resistivity (Ω · cm), R is the metal rod resistance (Ω), S is the cross-sectional area (cm) of the polyacrylate tube, and H is the height (cm) of the antimony doped tin oxide powder.
Preferably, the percentage content of antimony trichloride in step (1) is 6%, and the pH value in step (4) is 2.
Compared with the prior art, the invention has the beneficial effects that: the invention selects antimony doped tin dioxide (ATO) nano conductive powder as antistatic functional powder, and prepares the ATO conductive powder by alkoxide hydrolysis. ATO is a short for the analog bonded Tin Dioxide, which belongs to the N-type semiconductor. Antimony Doped Tin Oxide (ATO) is Sb & lt 3+ & gt which replaces Sn & lt 2+ & gt in a Tin dioxide crystal lattice, and simultaneously replaces gaps in a crystal structure to form electron holes, so that the electron holes are converted into an N-type semiconductor transparent conductive material with good conductivity; compared with other transparent conductive and heat-insulating materials such as nano Indium Tin Oxide (ITO), fluorine-doped silicon dioxide (FTO), aluminum-doped zinc oxide (AZO) and the like, ATO has more excellent transparency, laser absorption performance, meteorological performance, conductivity, light transmission, infrared absorption, chemical stability and the like.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a process flow diagram of a method for preparing an antistatic composite material according to the present invention;
FIG. 2 is a schematic diagram of a resistivity-resistivity tool;
FIG. 3 is a graph showing the relationship between different amounts of antimony chloride and the volume resistivity of the powder;
FIG. 4 is a graph showing the relationship between the pH of the solution and the volume resistivity of the powder.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The present invention will be described in further detail with reference to examples.
The specific embodiment of the preparation method of the antistatic composite material provided by the invention comprises the following steps:
as shown in fig. 1, a preparation method of an antistatic composite material comprises the following steps:
(1) Respectively dissolving tin tetrachloride pentahydrate and antimony trichloride in a proper amount of absolute ethyl alcohol, and then fully mixing the two dissolved solutions to obtain a tin-antimony mixed solution;
(2) Stirring the tin-antimony mixed solution obtained in the step (1) on a magnetic stirrer at a constant temperature ranging from 26 ℃ to 33 ℃ for 3 hours;
(3) Carrying out reflux treatment on the tin-antimony mixed solution at about 78 ℃;
(4) Titrating the upper solution with a small amount of ammonia water, keeping a proper pH value within the range of 2-7, carrying out full alcoholysis reaction on the solution until a pale yellow sol solution is formed, and then repeatedly washing the solution with absolute ethyl alcohol to remove chloride ions in the solution;
(5) Carrying out rotary evaporation treatment by using a rotary evaporator;
(6) And then calcining to obtain the antimony doped tin oxide powder.
And (3) measuring the resistivity of the antimony-doped tin oxide powder obtained in the step (6) by using a resistivity resistance meter, wherein the resistivity resistance meter comprises a base table and a resistance meter, a polyacrylate pipe is fixed on the base table, two metal rods are arranged in the polyacrylate pipe, the antimony-doped tin oxide powder is positioned between the two metal rods, the two metal rods are respectively connected with an electronic watch through conducting wires, and a weight block is placed on the metal rod above the antimony-doped tin oxide powder, as shown in fig. 2.
The method for measuring the resistivity of the antimony doped tin oxide powder by using the resistivity resistance instrument comprises the following steps: adding the prepared antimony-doped tin oxide powder into a polyacrylate tube, then inserting an upper metal bar above the antimony-doped tin oxide powder, placing a weight block, and calculating the resistivity of the antimony-doped tin oxide powder according to the following formula; the resistivity calculation formula is as follows: p = RS/H, where p is the volume resistivity (Ω · cm), R is the metal rod resistance (Ω), S is the cross-sectional area (cm) of the polyacrylate tube, and H is the height (cm) of the antimony doped tin oxide powder.
Determining the influence of the proportion of the tin tetrachloride pentahydrate and the antimony trichloride on the conductivity of the antimony-doped tin oxide powder in the step (1) through a comparison experiment; 0.2g of antimony trichloride, 0.4g of antimony trichloride, 0.8g of antimony trichloride, 1.2g of antimony trichloride, 2.0g of antimony trichloride and 2.4g of antimony trichloride, namely the percentage content of the antimony trichloride is 1% -12%, the six kinds of antimony trichloride and 20g of tin tetrachloride pentahydrate are dissolved in a proper amount of absolute ethanol solution, then the pH values of the solutions are adjusted to be 1.0, 1.5, 2.0, 3.0, 4.0, 5.0 and 6.0 respectively, and experiments are carried out according to the preparation methods to prepare different antimony-doped tin oxide powders.
Then measuring the resistivity of the antimony doped tin oxide powder by using a resistivity resistance meter according to the method, calculating the resistivity of different antimony doped tin oxide powders, and drawing a chart as shown in figure 3, wherein as shown in figure 3, the conductivity of the powder is not always improved along with the increase of the addition of antimony trichloride, and the resistivity of the powder just begins to be improved along with SbCl 3 The volume resistivity of the powder is rapidly reduced when the adding amount is less than 4 percent, and the volume resistivity is minimum when the adding amount reaches about 6 percent, so the best value of the mass content of the antimony trichloride is about 6 percent in the aspect of conductivity.
When the adding amount of antimony trichloride is continuously increased, the volume resistivity of the powder is increased. For analysis reasons, on one hand, antimony which can be contained in a tin dioxide crystal lattice is limited, excessive antimony enters the crystal lattice to destroy a partial crystal lattice structure of the tin dioxide, so that the movement of a current carrier is hindered, and the conductivity of the powder is reduced, on the other hand, the higher the content of antimony element is, the higher the concentration of corresponding trivalent antimony ions is, the trivalent antimony ions can eliminate electrons generated by high-valence antimony ions, namely, the concentration of free current carriers is reduced, so that the resistance of the powder is increased. In addition, the color of the powder also becomes darker along with the increase of the doping amount of the antimony.
In the process of preparing the powder, the pH value of the solution in the step (4) determines the state of a reaction product, and the final powder has great influence on various properties. The method comprises the steps of taking antimony trichloride content as 6%, changing the PH values of precipitation reactions to prepare powder with the PH values of 1.0, 1.5, 2.0, 3.0, 4.0, 5.0 and 6.0 respectively, measuring the volume resistivity of each sample respectively, and obtaining the relation between the volume resistance of the powder and the PH as shown in figure 4, wherein when the PH value is less than 2, the volume resistivity is reduced along with the increase of the value, because when the PH value is too small, snCl 4 Can not be completely reacted to form Sn (OH) 4 Sn and Sb can not form colloid completely according to proper proportion after the reaction is finished, and when the pH value is equal to>2, the volume resistivity increases with increasing PH, especially when PH is high>4, the pH value is increased sharply, because Sn and Sb are precipitated rapidly when the pH value is high, and are crystallized by themselves, and crystals grow rapidly, so that the volume resistivity of the conductive powder is high; when PH =2 is about, the absolute value of Zeta potential of the powder is closest to zero, sedimentation is most easy to occur, and the reaction generation rate is relatively low, so that the phenomenon of coarsening of self-nucleating particles of a precipitation product cannot occur, and the performance of the generated conductive powder is best when PH = 2.
It should be noted that, in this document, terms such as "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The preparation method of the antistatic composite material is characterized by comprising the following steps of:
(1) Respectively dissolving tin tetrachloride pentahydrate and antimony trichloride in a proper amount of absolute ethyl alcohol, and then fully mixing the two dissolved solutions to obtain a tin-antimony mixed solution;
(2) Stirring the tin-antimony mixed solution obtained in the step (1) on a magnetic stirrer at a constant temperature ranging from 26 ℃ to 33 ℃ for 3 hours;
(3) Carrying out reflux treatment on the tin-antimony mixed solution at about 78 ℃;
(4) Titrating the upper solution with a small amount of ammonia water, keeping a proper pH value within the range of 2-7, carrying out full alcoholysis reaction on the solution until a pale yellow sol solution is formed, and then repeatedly washing the solution with absolute ethyl alcohol to remove chloride ions in the solution;
(5) Carrying out rotary evaporation treatment by using a rotary evaporator;
(6) And then calcining to obtain the antimony doped tin oxide powder.
2. The preparation method of the antistatic composite material as claimed in claim 1, wherein the resistivity of the antimony-doped tin oxide powder obtained in the step (6) is measured by a resistivity resistance meter.
3. The method according to claim 2, wherein the resistivity meter comprises a base and a resistance meter, a polyacrylate tube is fixed on the base, two metal rods are arranged in the polyacrylate tube, the antimony-doped tin oxide powder is located between the two metal rods, the two metal rods are respectively connected with an electronic watch through conducting wires, and a weight is placed on the metal rod above the two metal rods.
4. The preparation method of the antistatic composite material as claimed in claim 3, wherein the method for measuring the resistivity of the antimony-doped tin oxide powder by using a resistivity resistance meter comprises the following steps: adding the prepared antimony-doped tin oxide powder into a polyacrylate tube, then inserting an upper metal bar above the antimony-doped tin oxide powder, placing a weight block, and calculating the resistivity of the antimony-doped tin oxide powder according to the following formula; the resistivity calculation formula is as follows: p = RS/H, where p is the volume resistivity (Ω · cm), R is the metal rod resistance (Ω), S is the cross-sectional area (cm) of the polyacrylate tube, and H is the height (cm) of the antimony doped tin oxide powder.
5. The method for preparing the antistatic composite material as claimed in claim 1, wherein the percentage of antimony trichloride in step (1) is 6%, and the pH value in step (4) is 2.
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| CN103553120A (en) * | 2013-10-30 | 2014-02-05 | 华南理工大学 | Preparation method for antimony-doped tin oxide powder |
| CN104263056A (en) * | 2014-09-25 | 2015-01-07 | 广西大学 | Preparation method of tin antimony oxide organic nano paste |
| CN106986331A (en) * | 2017-04-14 | 2017-07-28 | 盐城工学院 | A kind of graphene tin-antiomony oxide composite conducting material and preparation method thereof |
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2022
- 2022-08-05 CN CN202210939532.6A patent/CN115287040A/en active Pending
Patent Citations (12)
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| JPH0952712A (en) * | 1995-08-17 | 1997-02-25 | Mitsubishi Materials Corp | Production of fine powder of antimony-doped tin oxide and transparent conductive coating material |
| CN1357509A (en) * | 2000-12-14 | 2002-07-10 | 成都亿安方博低维材料科技有限公司 | Transparent conductive nano Sb:SnO2 fine powder |
| CN1317803A (en) * | 2001-05-29 | 2001-10-17 | 华东理工大学 | Process for preparing light-colour electrically conductive Sb-dopped SnO2 powder |
| CN1746112A (en) * | 2005-07-20 | 2006-03-15 | 哈尔滨工业大学 | Nanometer conductive calcium carbonate and its production thereof |
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| CN106986331A (en) * | 2017-04-14 | 2017-07-28 | 盐城工学院 | A kind of graphene tin-antiomony oxide composite conducting material and preparation method thereof |
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