CN114672183A - AgNWs/Ti3AlC2Conductive filler, preparation method and application - Google Patents
AgNWs/Ti3AlC2Conductive filler, preparation method and application Download PDFInfo
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- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000945 filler Substances 0.000 title description 5
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims abstract description 120
- 239000000243 solution Substances 0.000 claims abstract description 115
- 239000000843 powder Substances 0.000 claims abstract description 112
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000011231 conductive filler Substances 0.000 claims abstract description 55
- 238000002156 mixing Methods 0.000 claims abstract description 32
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 31
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 30
- 239000011259 mixed solution Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
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- 238000000576 coating method Methods 0.000 claims abstract description 20
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- 239000000463 material Substances 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000013329 compounding Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000001291 vacuum drying Methods 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 142
- 239000007864 aqueous solution Substances 0.000 claims description 28
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 26
- 230000003213 activating effect Effects 0.000 claims description 26
- 238000005260 corrosion Methods 0.000 claims description 23
- 229910017604 nitric acid Inorganic materials 0.000 claims description 23
- 230000001235 sensitizing effect Effects 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
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- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 5
- 239000012535 impurity Substances 0.000 description 10
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
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- 239000002184 metal Substances 0.000 description 7
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- 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
- C08K3/02—Elements
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- C08K2003/0806—Silver
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses AgNWs/Ti3AlC2The conductive filler is composed of AgNWs and Ti3AlC2Formed by compounding AgNWs attached to Ti3AlC2In addition, the mass fraction of AgNWs is 30-80 percent, and Ti3AlC2The mass fraction of (A) is 20-70%. The invention also discloses a preparation method and application of the conductive filler; the preparation method comprises the following steps: preparing silver nitrate alcoholic solution; ti3AlC2Pretreating powder; preparation of Ti3AlC2An alcohol solution; preparing a template agent alcohol solution; mixing the three solutions, heating in water bath, and mechanically stirring; pouring the obtained mixed solution into a reaction kettle, placing the reaction kettle in an oven for heat preservation, and cooling to obtain a reacted material; cleaning and vacuum drying the reacted materials to obtain AgNWs/Ti3AlC2And (3) conductive filler. The conductive filler has excellent conductivity, and can be used for preparingAn anticorrosive coating with excellent anticorrosive performance is prepared.
Description
Technical Field
The invention relates to an anti-corrosive surfaceThe technical field of coating materials, in particular to AgNWs/Ti3AlC2Conductive filler, a preparation method and application thereof in preparing an anti-corrosion coating.
Background
The corrosion of metal materials not only causes great loss to national economy, but also causes serious harm to the environment. At present, the most direct and common method for corrosion protection of metal materials is to apply an anti-corrosion coating on its surface. The addition of functional anti-corrosive fillers is an effective means to further improve the anti-corrosive properties of the coating, and typically includes lamellar fillers to improve shielding properties and fillers to inhibit metal corrosion.
The graphene is a special two-dimensional hexagonal lattice lamellar structure material, has the advantages of excellent conductivity, oxidation resistance, permeability resistance, chemical stability, good mechanical property and the like, and can be well applied to the field of corrosion prevention. The initial association of graphene with metal corrosion protection discovered in 2004 was not obvious, and researchers have focused most of their attention on the unique structure and properties of this new material. Until 2008 researchers found that graphene is impermeable to all gas molecules, it has not demonstrated great potential for use in the field of corrosion protection. Graphene sheets, however, tend to agglomerate and have poor dispersion in the medium, which limits their development.
Ti3AlC2The ceramic material is a novel ternary layered compound ceramic material which is paid much attention in recent years, and has a layered structure and comprehensive excellent properties of metal and ceramic, so that the ceramic material gradually becomes a research hotspot; ti3AlC2The excellent properties of the composite material comprise low density, high elastic modulus and strength, good electric and heat conducting properties, low friction coefficient, excellent thermal stability and oxidation resistance and the like. These properties are such that Ti3AlC2Becomes a conductive filler of the anti-corrosion coating with great potential. However, in order to further improve the corrosion resistance of the coating, Ti is required3AlC2With highly conductive metals to form more dense conductive paths. One-dimensional nanowires (1D NWs) are not affected because they have two quantum confinement directions and oneLimited direction and exhibits better conductivity. The metal silver nanowires (AgNWs) are one of the one-dimensional nanowires, have excellent electrical and thermal properties, and have potential application values in the fields of photoelectric devices, flexible conductors, touch screens and the like.
In view of the above problems and background, the present invention is made by adding Ti3AlC2Compounding with AgNWs to form a complex conductive network, and preparing a high-performance AgNWs/Ti for the anti-corrosion coating3AlC2And (3) conductive filler.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides an AgNWs/Ti3AlC2Conductive filler, preparation method and application thereof, and AgNWs and Ti in conductive filler3AlC2A complex conductive network is formed between the conductive filler and the conductive filler, so that the conductive filler has excellent conductive performance; after the conductive filler is applied to the preparation of an anti-corrosion coating, the anti-corrosion performance of the anti-corrosion coating can be improved.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
AgNWs/Ti3AlC2The conductive filler is composed of AgNWs and Ti3AlC2Formed by compounding AgNWs attached to Ti3AlC2In addition, the mass fraction of AgNWs is 30-80 percent, and Ti3AlC2The mass fraction of (A) is 20-70%.
The invention further provides AgNWs/Ti3AlC2The preparation method of the conductive filler comprises the following steps:
step 1, preparing silver nitrate alcoholic solution;
step 3, utilizing the Ti treated in the step 23AlC2Preparation of Ti from powder3AlC2An alcohol solution;
step 4, preparing a template agent alcoholic solution;
step 5, fully mixing the solutions obtained in the step 1, the step 3 and the step 4, heating in a water bath, and then mechanically stirring to obtain a mixed solution;
step 6, pouring the mixed liquid obtained in the step 5 into a reaction kettle, placing the reaction kettle in an oven for heat preservation for a certain time, and cooling the reaction kettle along with the oven to obtain a reacted material;
step 7, cleaning and vacuum drying the reacted material obtained in the step 6 to obtain dry AgNWs/Ti3AlC2And (3) conductive filler.
Further, in step 1, the specific process for preparing the silver nitrate alcoholic solution comprises: mixing silver nitrate and ethylene glycol, and stirring for 5-20 min to dissolve the silver nitrate in the ethylene glycol to obtain a silver nitrate alcoholic solution; wherein the mass volume ratio of the silver nitrate to the ethylene glycol is (0.4-0.6 g) to (10-30 ml).
Further, in step 2, Ti3AlC2The specific steps of the pretreatment of the powder are as follows:
step 2.1, weighing Ti3AlC2Pouring the powder into aqueous solution of nitric acid, and adding Ti3AlC2Completely immersing the powder in the aqueous solution of nitric acid, and treating Ti with the aqueous solution of nitric acid3AlC2Coarsening the powder for 30-60 min;
step 2.2, hydrochloric acid and SnCl2Mixing the aqueous solutions to form a sensitizing solution, and treating the Ti obtained in step 2.13AlC2The powder is poured into the sensitizing solution and Ti is added3AlC2The powder is completely immersed in the sensitizing solution, and the sensitizing solution is used for treating Ti3AlC2Sensitizing the powder for 30-60 min;
step 2.3, AgNO3Dissolving the Ti in water to prepare an activating solution with the concentration of 0.1-0.5 mol/L, and treating the Ti obtained in the step 2.23AlC2Pouring the powder into activating liquid, and adding Ti3AlC2The powder is completely immersed in the activating solution, and the activating solution is used for Ti3AlC2Powder activationActivating for 1-2 h, and activating the activated Ti3AlC2Washing and drying the powder to obtain pretreated Ti3AlC2And (3) powder.
Further, in step 3, Ti is prepared3AlC2The alcohol solution comprises the following specific processes: ti treated by the step 23AlC2Mixing the powder with ethylene glycol, and stirring for 15-20 min to obtain Ti3AlC2Fully dispersing the powder in ethylene glycol to obtain Ti3AlC2An alcoholic solution.
Further, the template agent alcoholic solution in the step 4 is a PVP template agent alcoholic solution; the preparation process of the PVP template agent alcoholic solution specifically comprises the following steps: mixing a template agent PVP and ethylene glycol, and then placing the mixture in an ultrasonic disperser for ultrasonic dissolution for 10-20 min to obtain a PVP template agent alcohol solution; wherein the mass-volume ratio of PVP to glycol is as follows: (0.6-0.9 g): (10-20 ml).
Further, in the step 5, the water bath heating temperature is 40-60 ℃, and the stirring time is 10-20 min.
Further, the heat preservation temperature in the step 6 is 150-180 ℃, and the heat preservation time is 5-8 hours.
The invention further provides the AgNWs/Ti3AlC2The conductive filler is applied to preparing an anti-corrosion coating.
The invention has the beneficial effects that:
the invention is realized by adding Ti with good chemical stability3AlC2Compounding with AgNWs with high conductivity to form conductive filler with complex multidirectional conductive network; compared with two-dimensional materials such as graphene and the like, the conductive filler has better dispersibility, simple preparation process and low cost, and is more beneficial to practical application and large-scale production. And the conductive filler is compared with single Ti3AlC2The conductivity of the material is improved by 3.22 times.
The conductive filler can be used for preparing an anti-corrosion coating, and the anti-corrosion performance of the anti-corrosion coating is improved by improving the conductivity. When electrochemical corrosion occurs, electrons generated by metal anode reaction are more easily transferred to the surface of the coating through the good conductive effect of the conductive filler, so that cathode reaction is carried out on the surface of the coating, and the anode reaction can be inhibited along with the accumulation of metal ions, so that the purpose of inhibiting metal corrosion is achieved, and the base metal is protected. Moreover, based on the complex multidirectional conductive network of the conductive filler, the coating prepared by the conductive filler has excellent conductivity along all directions, and the anti-corrosion performance of the coating can be obviously improved.
AgNWs/Ti of the invention3AlC2Method for preparing conductive filler by AgNO3As activators, in Ti3AlC2Activating point sites are applied on the surfaces of the particles, and no growth auxiliary agent is required to be added, so that AgNWs can be attached and grown on Ti3AlC2In addition, the preparation process is optimized, the production cost is reduced, and heavy metal ions in the waste liquid are reduced. In addition, the preparation method reduces impurities in the AgNWs growth process, and can prepare silver nanowires with higher purity and better conductivity. The invention is to mix Ti3AlC2Interweaving with AgNWs together, more easily forming the conductive network, improving the conductivity and the anti-corrosion performance of the conductive filler.
Drawings
FIG. 1 is AgNWs/Ti of example 3 of the present invention3AlC2XRD pattern of conductive filler.
FIG. 2 shows AgNWs/Ti of example 3 of the present invention3AlC2SEM image of conductive fillers.
FIG. 3 shows AgNWs/Ti of example 3 of the present invention3AlC2Conductive filler and single Ti3AlC2Conductivity of (a).
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
The invention provides AgNWs/Ti3AlC2Conductive filler consisting of AgNWs and Ti3AlC2Formed by compounding AgNWs attached to Ti3AlC2In addition, the mass fraction of AgNWs is 30-80 percent, and Ti3AlC2The mass fraction of (A) is 20-70%.
The invention further provides AgNWs/Ti3AlC2The preparation method of the conductive filler comprises the following steps:
step 1, preparing a silver nitrate alcoholic solution, which specifically comprises the following steps:
mixing silver nitrate and ethylene glycol, and stirring for 5-20 min to dissolve the silver nitrate in the ethylene glycol to obtain a silver nitrate alcoholic solution; wherein the mass volume ratio of the silver nitrate to the ethylene glycol is (0.4-0.6 g) to (10-30 ml).
step 2.1, weighing 0.1-0.5 g of Ti3AlC2Pouring the powder into a certain amount of nitric acid aqueous solution, and enabling Ti to be contained3AlC2Completely immersing the powder in the aqueous solution of nitric acid, and treating Ti with the aqueous solution of nitric acid3AlC2Coarsening the powder for 30-60 min;
the nitric acid aqueous solution is prepared by mixing nitric acid and water according to the volume ratio of 1: 1-4, and uniformly mixing;
step 2.2, adding hydrochloric acid and SnCl according to the volume ratio of 1-4: 12Mixing the aqueous solutions to form a sensitizing solution, and treating the Ti obtained in step 2.13AlC2The powder is poured into the sensitizing solution and Ti is added3AlC2The powder is completely immersed in the sensitizing solution, and the sensitizing solution is used for treating Ti3AlC2Sensitizing the powder for 30-60 min;
step 2.3, AgNO3Dissolving the Ti in water to prepare an activating solution with the concentration of 0.1-0.5 mol/L, and treating the Ti obtained in the step 2.23AlC2The powder is poured into the activating liquid,and make Ti3AlC2The powder is completely immersed in the activating solution, and the activating solution is used for Ti3AlC2Activating the powder for 1-2 h, and activating the activated Ti3AlC2Washing and drying the powder to obtain pretreated Ti3AlC2And (3) powder.
Step 3, utilizing the Ti prepared in the step 23AlC2Preparation of Ti from powder3AlC2An alcohol solution; the specific process is as follows: ti treated by the step 23AlC2Mixing the powder with 5-15 ml of ethylene glycol, and fully stirring for 15-20 min by using a mechanical stirrer to ensure that Ti is formed3AlC2The powder is fully dispersed in glycol to obtain Ti3AlC2An alcoholic solution.
Step 4, preparing the PVP template agent alcoholic solution, which comprises the following specific steps:
mixing a template agent PVP and ethylene glycol, and then placing the mixture in an ultrasonic disperser for ultrasonic dissolution for 10-20 min to obtain a PVP template agent alcohol solution; wherein the mass-volume ratio of PVP to ethylene glycol is (0.6-0.9 g): (10-20 ml).
And 5, fully mixing the solutions obtained in the steps 1, 3 and 4, then placing the mixed solution in a water bath, heating to 40-60 ℃, and mechanically stirring for 10-20 min to obtain a mixed solution.
Step 6, pouring the mixed solution obtained in the step 5 into a 100ml polytetrafluoroethylene reaction kettle, placing the reaction kettle in a drying oven for heat preservation, setting the heat preservation temperature to be 150-180 ℃, and keeping the heat preservation time for 5-8 h to ensure that the Ag nano-wires are aligned with the Ti nano-wires3AlC2Is fully grown, and is cooled to room temperature along with the furnace to obtain a reacted material (AgNWs/Ti)3AlC2Powder mixture solution);
step 7, firstly, acetone solution with 2-3 times volume is adopted to react the AgNWs/Ti obtained in the step 63AlC2Cleaning the powder mixed solution, centrifuging the powder mixed solution in a centrifugal machine with the speed of 5000-7000 r/min for 10-15 min, pouring off the yellow ethylene glycol impurity solution on the upper layer, adding deionized water, centrifuging and cleaning again, and repeating the steps for 3-4 times repeatedly to remove the redundant ethylene glycolAlcohol, PVP and other impurities; finally, putting the completely cleaned solid and liquid in an oven at 80-120 ℃ for baking for 4h to obtain the dried AgNWs/Ti3AlC2And (3) conductive filler.
The invention also provides AgNWs/Ti3AlC2The application of the conductive filler comprises the following specific steps: the AgNWs/Ti3AlC2The conductive filler can be used to prepare an anti-corrosion coating.
Example 1
Step 1, preparing silver nitrate alcoholic solution: weighing 0.4g of solid silver nitrate, putting the solid silver nitrate into a beaker, weighing 10ml of ethylene glycol solution, adding the ethylene glycol solution, and fully stirring for 5min by adopting a mechanical stirrer to fully dissolve the silver nitrate in the ethylene glycol solution.
step 2.1, weigh 0.1g Ti3AlC2Pouring the powder into a certain amount of nitric acid aqueous solution, and enabling Ti to be contained3AlC2Completely immersing the powder in the aqueous solution of nitric acid, and using the aqueous solution of nitric acid to treat Ti3AlC2Coarsening the powder for 30 min;
the nitric acid aqueous solution is prepared by mixing nitric acid and water according to the volume ratio of 1: 1, uniformly mixing to obtain the product;
step 2.2, mixing the raw materials in a volume ratio of 1: 1 reacting hydrochloric acid and SnCl2Mixing the aqueous solutions to form a sensitizing solution, and treating the Ti obtained in step 2.13AlC2The powder is poured into the sensitizing solution and Ti is added3AlC2The powder is completely immersed in the sensitizing solution, and the sensitizing solution is used for treating Ti3AlC2Sensitizing the powder for 30 min;
step 2.3, AgNO3Dissolving the Ti powder in water to prepare an activating solution with the concentration of 0.1mol/L, and treating the Ti powder obtained in the step 2.23AlC2Pouring the powder into activating solution, and adding Ti3AlC2The powder is completely immersed in the activating solution to utilize activityChemical solution to Ti3AlC2Activating the powder for 1 h; then Ti after activation treatment is added3AlC2Washing and drying the powder to obtain pretreated Ti3AlC2And (3) powder.
Step 3, preparing Ti3AlC2Alcoholic solution: ti treated by the step 23AlC2Adding the powder into ethylene glycol, wherein the volume of the ethylene glycol is 5ml, and stirring with a mechanical stirrer for 15min to obtain Ti3AlC2Fully dispersed in ethylene glycol to obtain Ti3AlC2An alcoholic solution.
Step 4, preparing a PVP template agent alcoholic solution: 0.6g of PVP is weighed into a beaker, 10ml of ethylene glycol is weighed and added, and the PVP alcohol solution is placed in an ultrasonic disperser for ultrasonic dissolution for 10 min.
And 5, fully mixing the solutions obtained in the steps 1, 3 and 4, placing the mixed solution in a water bath kettle, heating to 40 ℃, and mechanically stirring for 10min to obtain a mixed solution.
Step 6, transferring the mixed solution obtained in the step 5 into a 100mL polytetrafluoroethylene reaction kettle, putting the reaction kettle into an oven for heat preservation, setting the heat preservation temperature to be 150 ℃, and the heat preservation time to be 5 hours so as to ensure that the Ag nano-wires are aligned to the Ti nano-wires3AlC2Is fully grown, and is cooled to room temperature along with the furnace to obtain a reacted material (AgNWs/Ti)3AlC2Powder mixed liquid);
step 7, taking out the prepared AgNWs/Ti3AlC2Mixing the powder with 2 times volume of acetone solution to AgNWs/Ti3AlC2Cleaning the powder mixed solution, placing the powder mixed solution in a centrifugal machine with the speed of 5000r/min for centrifuging for 10min, and pouring off the yellow ethylene glycol impurity solution on the upper layer. Adding deionized water, performing centrifugal cleaning again, and repeating for 3 times to remove excessive ethylene glycol, PVP and other impurities; finally, putting the completely cleaned solid and liquid in an oven at 80 ℃ for baking for 4 hours to obtain the dried AgNWs/Ti3AlC2And (3) conductive filler.
Example 2
Step 1, preparing silver nitrate alcoholic solution: weighing 0.6g of solid silver nitrate, putting the solid silver nitrate into a beaker, weighing 30ml of ethylene glycol solution, adding the ethylene glycol solution, and fully stirring the mixture for 20min by adopting a mechanical stirrer so as to fully dissolve the silver nitrate in the ethylene glycol solution.
step 2.1, weigh 0.5g Ti3AlC2Pouring the powder into a certain amount of nitric acid aqueous solution, and enabling Ti to be contained3AlC2The powder is completely immersed in the nitric acid aqueous solution, and the nitric acid aqueous solution is utilized to treat Ti3AlC2Coarsening the powder for 60 min;
the nitric acid aqueous solution is prepared by mixing nitric acid and water according to the volume ratio of 1: 4, uniformly mixing to obtain the product;
step 2.2, according to the volume ratio of 4:1 reacting hydrochloric acid and SnCl2Mixing the aqueous solutions to form a sensitizing solution, and treating the Ti obtained in step 2.13AlC2The powder is poured into the sensitizing solution and Ti is added3AlC2The powder is completely immersed in the sensitizing solution, and the sensitizing solution is used for treating Ti3AlC2Sensitizing the powder for 60 min;
step 2.3, AgNO3Dissolving in water to prepare an activating solution with the concentration of 0.5mol/L, and treating the Ti obtained by the step 2.23AlC2Pouring the powder into activating solution, and adding Ti3AlC2The powder is completely immersed in the activating solution, and the activating solution is used for Ti3AlC2Activating the powder for 2 h; then Ti after activation treatment is added3AlC2Washing and drying the powder to obtain pretreated Ti3AlC2And (3) powder.
Step 3, preparing Ti3AlC2Alcoholic solution: ti treated by the step 23AlC2Adding the powder into ethylene glycol, wherein the volume of the ethylene glycol is 15ml, and mechanically stirringStirring thoroughly for 20min to obtain Ti3AlC2Fully dispersed in ethylene glycol to obtain Ti3AlC2An alcoholic solution.
Step 4, preparing a PVP template agent alcoholic solution: 0.9g of PVP is weighed into a beaker, 20ml of ethylene glycol is weighed and added, and the PVP alcohol solution is placed in an ultrasonic disperser for ultrasonic dissolution for 20 min.
And 5, fully mixing the solutions obtained in the steps 1, 3 and 4, placing the mixed solution in a water bath kettle, heating to 60 ℃, and mechanically stirring for 20min to obtain a mixed solution.
Step 6, transferring the mixed solution obtained in the step 5 into a 100mL polytetrafluoroethylene reaction kettle, putting the reaction kettle into an oven for heat preservation, setting the heat preservation temperature to be 180 ℃, and the heat preservation time to be 8 hours so as to ensure that the Ag nano-wires are aligned to the Ti nano-wires3AlC2Is fully grown, and is cooled to room temperature along with the furnace to obtain a reacted material (AgNWs/Ti)3AlC2Powder mixed liquid);
step 7, taking out the prepared AgNWs/Ti3AlC2And (3) cleaning the mixed solution by using an acetone solution with the volume 3 times that of the mixed solution, centrifuging the mixed solution in a 7000r/min centrifugal machine for 15min, and pouring off the upper yellow glycol impurity solution. And adding deionized water, performing centrifugal cleaning again, and repeating for 4 times to remove excessive impurities such as ethylene glycol and PVP. Finally, putting the completely cleaned solid and liquid in a 120 ℃ oven for baking for 10h to obtain the dried AgNWs/Ti3AlC2And (3) conductive filler.
Example 3
Step 1, preparing silver nitrate alcoholic solution: weighing 0.5g of solid silver nitrate, putting the solid silver nitrate into a beaker, weighing 20ml of ethylene glycol solution, adding the ethylene glycol solution, and fully stirring the mixture for 10min by adopting a mechanical stirrer so as to fully dissolve the silver nitrate in the ethylene glycol solution.
step 2.1, weigh 0.3g Ti3AlC2Pouring the powder into a certain amount of nitric acid aqueous solution, and enabling Ti to be contained3AlC2The powder is completely immersed in the nitric acid aqueous solution, and the nitric acid aqueous solution is utilized to treat Ti3AlC2Coarsening the powder for 40 min;
the nitric acid aqueous solution is prepared by mixing nitric acid and water according to the volume ratio of 1: 2, uniformly mixing to obtain the product;
step 2.2, according to the volume ratio of 3: 1 reacting hydrochloric acid and SnCl2Mixing the aqueous solutions to form a sensitizing solution, and treating the Ti obtained in step 2.13AlC2The powder is poured into the sensitizing solution and Ti is added3AlC2The powder is completely immersed in the sensitization treatment liquid, and the sensitization treatment liquid is utilized to treat Ti3AlC2Sensitizing the powder for 40 min;
step 2.3, AgNO3Dissolving the Ti powder in water to prepare an activating solution with the concentration of 0.3mol/L, and treating the Ti powder obtained in the step 2.23AlC2Pouring the powder into activating solution, and adding Ti3AlC2The powder is completely immersed in the activating solution, and the activating solution is used for Ti3AlC2Activating the powder for 1.5 h; then Ti after activation treatment is added3AlC2Washing and drying the powder to obtain pretreated Ti3AlC2Powder body
Step 3, preparing Ti3AlC2Alcoholic solution: ti treated by the step 23AlC2Adding the powder into ethylene glycol with a volume of 10ml, and stirring with a mechanical stirrer for 15min to obtain Ti3AlC2Fully dispersed in ethylene glycol to obtain Ti3AlC2An alcoholic solution.
Step 4, preparing a PVP template agent alcoholic solution: 0.8g of PVP is weighed and placed in a beaker, 15ml of ethylene glycol is weighed and added, and the PVP alcohol solution is placed in an ultrasonic disperser for ultrasonic dissolution for 15 min.
And 5, fully mixing the solutions obtained in the steps 1, 3 and 4, placing the mixed solution in a water bath kettle, heating to 50 ℃, and mechanically stirring for 15min to obtain a mixed solution.
Step 6, transferring the mixed solution obtained in the step 5 into a 100mL polytetrafluoroethylene reaction kettle, putting the reaction kettle into an oven for heat preservation, setting the heat preservation temperature to be 160 ℃, and the heat preservation time to be 6 hours so as to ensure that the Ag nano-wires are aligned to the Ti nano-wires3AlC2Is fully grown, and is cooled to room temperature along with the furnace to obtain a reacted material (AgNWs/Ti)3AlC2Powder mixture solution);
step 7, taking out the prepared AgNWs/Ti3AlC2And (3) cleaning the mixed solution by using an acetone solution with the volume being 3 times that of the mixed solution, centrifuging the mixed solution in a 6000r/min centrifugal machine for 12min, and pouring off the yellow ethylene glycol impurity solution on the upper layer. And adding deionized water, performing centrifugal cleaning again, and repeating for 4 times to remove excessive impurities such as ethylene glycol, PVP and the like. Finally, putting the completely cleaned solid and liquid in a baking oven at 100 ℃ for baking for 8 hours to obtain the dried AgNWs/Ti3AlC2And (3) conductive filler.
AgNWs/Ti obtained in example 3 of the present invention as shown in FIG. 13AlC2XRD pattern of conductive filler; as can be seen from FIG. 1, except for Ti3AlC2Besides the diffraction peak, the diffraction peak of Ag can be obviously observed, which shows that the simple substance of Ag is successfully reduced, and AgNWs/Ti is successfully prepared3AlC2The conductive filler was compounded, and other impurity peaks were not detected in addition thereto.
AgNWs/Ti obtained in example 3 of the present invention as shown in FIG. 23AlC2SEM images of conductive fillers; as can be seen from FIG. 2, Ti3AlC2Interweaving with AgNWs to form a conductive network in multiple directions. FIG. 3 shows AgNWs/Ti obtained in example 3 of the present invention3AlC2Conductive filler and single Ti3AlC2Conductivity of (a). As can be seen from FIG. 3, AgNWs/Ti of the present invention3AlC2The conductivity of the conductive filler is obviously higher than that of single Ti3AlC2The electrical conductivity of (a); with Ti alone3AlC2Compared with the material, the AgNWs/Ti of the invention3AlC2The conductivity of the conductive filler is improved3.22 times, and is a conductive filler for an anti-corrosion coating with better application prospect.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. AgNWs/Ti3AlC2The conductive filler is characterized by consisting of AgNWs and Ti3AlC2Formed by compounding AgNWs attached to Ti3AlC2In addition, the mass fraction of AgNWs is 30-80 percent, and Ti3AlC2The mass fraction of (A) is 20-70%.
2. The AgNWs/Ti of claim 13AlC2The preparation method of the conductive filler is characterized by comprising the following steps:
step 1, preparing silver nitrate alcoholic solution;
step 2, Ti3AlC2Pretreating powder: for Ti3AlC2The powder is sequentially subjected to coarsening, sensitization, activation, washing and drying treatment to obtain pretreated Ti3AlC2Powder;
step 3, utilizing the Ti treated in the step 23AlC2Preparation of Ti from powder3AlC2An alcohol solution;
step 4, preparing a template agent alcoholic solution;
step 5, mixing the solutions obtained in the step 1, the step 3 and the step 4, heating in a water bath, and then mechanically stirring to obtain a mixed solution;
step 6, pouring the mixed liquid obtained in the step 5 into a reaction kettle, placing the reaction kettle in an oven for heat preservation for a certain time, and cooling the reaction kettle along with the oven to obtain a reacted material;
step 7, cleaning and vacuum drying the reacted material obtained in the step 6 to obtain dry AgNWs/Ti3AlC2And (3) conductive filler.
3. An AgNWs/Ti according to claim 23AlC2The preparation method of the conductive filler is characterized in that in the step 1, the specific process of preparing the silver nitrate alcoholic solution is as follows: mixing silver nitrate and ethylene glycol, and stirring for 5-20 min to dissolve the silver nitrate in the ethylene glycol to obtain a silver nitrate alcoholic solution; wherein the mass volume ratio of the silver nitrate to the ethylene glycol is (0.4-0.6 g) to (10-30 ml).
4. An AgNWs/Ti according to claim 23AlC2The preparation method of the conductive filler is characterized in that in the step 2, Ti3AlC2The pretreatment of the powder comprises the following specific steps:
step 2.1, weighing Ti3AlC2Pouring the powder into aqueous solution of nitric acid, and adding Ti3AlC2Completely immersing the powder in the aqueous solution of nitric acid, and treating Ti with the aqueous solution of nitric acid3AlC2Coarsening the powder for 30-60 min;
step 2.2, hydrochloric acid and SnCl2Mixing the aqueous solutions to form a sensitizing solution, and treating the Ti obtained in step 2.13AlC2The powder is poured into the sensitizing solution and Ti is added3AlC2The powder is completely immersed in the sensitizing solution, and the sensitizing solution is used for treating Ti3AlC2Sensitizing the powder for 30-60 min;
step 2.3, AgNO3Dissolving the Ti in water to prepare an activating solution with the concentration of 0.1-0.5 mol/L, and treating the Ti obtained in the step 2.23AlC2Pouring the powder into activating liquid, and adding Ti3AlC2The powder is completely immersed in the activating solution, and the activating solution is used for Ti3AlC2Activating the powder for 1-2 h, and activating the activated Ti3AlC2Washing and drying the powder to obtain pretreated Ti3AlC2And (3) powder.
5. An AgNWs/Ti according to claim 23AlC2The preparation method of the conductive filler is characterized in that in the step 3, Ti is prepared3AlC2The specific process of the alcoholic solution is as follows: ti treated by the step 23AlC2Mixing the powder with ethylene glycol, and stirring for 15-20 min to obtain Ti3AlC2Fully dispersing the powder in ethylene glycol to obtain Ti3AlC2An alcoholic solution.
6. An AgNWs/Ti according to claim 23AlC2The preparation method of the conductive filler is characterized in that the alcoholic solution of the template agent in the step 4 is an alcoholic solution of a PVP template agent; the preparation process of the PVP template agent alcoholic solution specifically comprises the following steps: mixing a template agent PVP and ethylene glycol, and then placing the mixture in an ultrasonic disperser for ultrasonic dissolution for 10-20 min to obtain a PVP template agent alcohol solution; wherein the mass-volume ratio of PVP to ethylene glycol is (0.6-0.9 g): (10-20 ml).
7. An AgNWs/Ti according to claim 23AlC2The preparation method of the conductive filler is characterized in that in the step 5, the water bath heating temperature is 40-60 ℃, and the stirring time is 10-20 min.
8. An AgNWs/Ti according to claim 23AlC2The preparation method of the conductive filler is characterized in that the heat preservation temperature in the step 6 is 150-180 ℃, and the heat preservation time is 5-8 hours.
9. The AgNWs/Ti of claim 13AlC2Use of an electrically conductive filler, characterized in that the AgNWs/Ti3AlC2The conductive filler is used for preparing an anti-corrosion coating.
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| YI LIU ETAL.: "Electromagnetic and microwave absorption properties of Ti3SiC2/AgNWs/ acrylic acid resin composite coatings with FSS incorporation", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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