CN113005780A - Multi-layer MXenes electromagnetic shielding fabric and preparation method thereof - Google Patents
Multi-layer MXenes electromagnetic shielding fabric and preparation method thereof Download PDFInfo
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Abstract
The invention provides a multilayer MXenes electromagnetic shielding fabric, which is prepared by sequentially soaking a polydopamine modified fabric in a gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane modified MXenes two-dimensional nanosheet colloidal solution and a gamma-aminopropyltriethoxysilane modified MXenes two-dimensional nanosheet colloidal solution and repeatedly reacting for multiple times, and has important application value in the fields of electromagnetic shielding textiles, functional textiles, wearable textiles, flexible intelligent textiles and the like.
Description
Technical Field
The invention relates to the field of textile fabrics and functional nano materials, in particular to an electromagnetic shielding fabric with multiple layers of MXenes.
Background
The rapid development of current electronic technology and the popularization of wireless devices make electromagnetic pollution become more serious, which not only interferes with the normal functions of electronic components, but also may cause potential harm to human health (ACS Nano,2018,12,5: 4583-. Particularly, with the coming of the 5G and 6G times and the rapid development of wearable intelligent textiles, the importance of fabrics/textiles with certain electromagnetic shielding functions is increasingly prominent.
Transition metal carbides, nitrides and carbonitrides (commonly known as MXenes) were titanium carbide (Ti) discovered since yurygootsi et al 20113C2Tx) The new two-dimensional material is provided. The general formula for these materials is Mn+1XnTx(n ═ 1, 2, or 3), where M is an early transition metal, X is carbon and/or nitrogen, and T is a surface group inherited from the synthesis process, typically-OH, -O, and-F. MXenes are typically produced by selectively etching an atomic layer of a from the MAX phase of ternary carbides or nitrides, where a is primarily a group IIIA and group IVA element. There are more than 70 MAX phases reported so far, and at present 20 MXenes based on Ti, V, Nb, Mo, Ta, Zr, etc. are successfully synthesized. The chemical and structural multifunctionality enables MXenes to have competitive advantages with other two-dimensional nano Materials such as graphene in the aspects of high conductivity, large surface area and the like, and has wide application prospects in various application fields, particularly in the fields of energy conversion and energy storage such as electromagnetic shielding, batteries, supercapacitors and catalysis (Science,2016,353, 1137-.
MXenes two-dimensional materials are also reported in the literature in the field of electromagnetic shielding textiles. The Chinese patent CN202010911800.4 is made by etching MAX phase micron sheet by chemical etching methodPreparing a small layer of MXene dispersion, then dip-coating the fabric material, carrying out gradient arrangement on the multiple layers of MXene-coated fabric material according to the MXene content, and compounding to obtain the MXene-based composite fabric material. The PI fabric is pretreated by the Chinese invention patent CN201911174273.7 and then is subjected to plasma treatment; spraying MXene solution on the surface of the treated PI fabric for reaction; mixing Co3O4Spraying the PANI nanowire solution on the obtained MXene/PI composite material for reaction; the obtained mixed Co3O4the/PANI/MXene/PI composite material is placed in a PDMS solution for processing, and the obtained electromagnetic shielding fabric has excellent conductivity and electromagnetic shielding performance. The MXene solution is sprayed on one side of the pretreated fabric layer by layer and dried in the Chinese patent CN201910223295.1, and then the MXene solution is sprayed on the other side of the fabric layer by layer and dried to obtain the MXene modified fabric. The prepared electromagnetic shielding fabric has good electromagnetic shielding effect and does not influence the comfort of the fabric. The Chinese invention patent CN201910144854.X prepares the MXene-based flexible semitransparent electromagnetic shielding fabric by a layer-by-layer self-assembly method. The Beijing university of chemical industry uses a simple and time-saving dip-dyeing method to directly dip-dye the fabric in PPy/MXene conductive ink and waterproof ink in turn, so that the electromagnetic shielding performance of the fabric with the thickness of 0.42mm and the conductivity of 1000S/m reaches 42dB (preparation of MXene-based electromagnetic shielding fabric and performance research thereof [ D)]Beijing university of chemical industry, 2019). The electromagnetic shielding function of the above fabric needs to be further improved. And the MXenes is not effectively combined with the fabric, and the MXenes can continuously fall off in the daily washing or using process, so that the MXenes fabric has poorer and poorer electromagnetic shielding function.
Disclosure of Invention
In order to overcome the defects, the invention prepares the multi-layer MXenes electromagnetic shielding fabric.
The invention is realized by the following technical scheme:
the preparation technology of the MXene two-dimensional material is mature, and MXene products with different series, sizes and thicknesses are sold in the current markets of companies such as Jiangsu Xiancheng nanometer material science and technology limited company and Beijing Beike Xin material science and technology limited company.
The surface of the fabric without any modification treatment, especially the chemical fiber fabric, is lack of effective reaction sites. Through modification of dopamine, a certain amount of amino groups are introduced. Putting the fabric into acetone, repeatedly washing with ultrasound, then putting the fabric into a dopamine Tris-HCl buffer solution with the mass fraction of 10%, regulating the pH value to 8.5 at a bath ratio of 1:50, reacting for 24h, taking out, repeatedly washing with ethanol, and drying to prepare the polydopamine modified fabric.
Preparing 1-10% of two MXenes two-dimensional nanosheet colloidal solutions with different transverse average sizes, wherein the transverse average size of one MXenes two-dimensional nanosheet is 0.5-1.5 μm, the transverse average size of the other MXenes two-dimensional nanosheet is 3-6 μm, and the ratio of the transverse average sizes of the two MXenes two-dimensional nanosheets is 2-10.
Adding gamma-aminopropyltriethoxysilane into an MXenes two-dimensional nanosheet colloidal solution with the transverse average size of 0.5-1.5 μm, reacting for 24h, washing, centrifuging, and vacuum drying to obtain the gamma-aminopropyltriethoxysilane modified MXenes two-dimensional nanosheets. Adding gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane into the MXenes two-dimensional nanosheet colloidal solution with the transverse average size of 3-6 μm, reacting for 24h, washing, centrifuging, and drying in vacuum to obtain the gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane modified MXenes two-dimensional nanosheet.
Preparing colloid solutions with the mass fraction of 1-10% from gamma-aminopropyltriethoxysilane modified MXenes two-dimensional nanosheets and gamma- (2, 3-glycidoxy) propyltrimethoxysilane modified MXenes two-dimensional nanosheets respectively, and then soaking the polydopamine modified fabric in the gamma- (2, 3-glycidoxy) propyltrimethoxysilane modified MXenes two-dimensional nanosheet colloid solution and the gamma-aminopropyltriethoxysilane modified MXenes two-dimensional nanosheet colloid solution in sequence for reaction for 30min, wherein the bath ratio is 1: 50; and repeating the sequential soaking reaction process as required, taking out, repeatedly cleaning with deionized water, and vacuum drying to finally obtain the MXenes electromagnetic shielding fabric with 1 layer, 2 layers, 3 layers, 4 layers, 5 layers or more.
The invention has the beneficial effects that: MXenes with different sizes are assembled on the surface of the fabric layer by layer, so that the fabric with excellent functions of electromagnetic shielding, electric conduction, antibiosis, ultraviolet resistance, washing resistance and the like is prepared, and the fabric has important application value in the fields of electromagnetic shielding textiles, functional textiles, wearable textiles, flexible intelligent textiles and the like.
Detailed Description
The invention will be further illustrated with reference to specific embodiments.
Example 1:
bleaching all cotton with plain woven fabric (120 g/m)2) And (2) putting the cotton fabric into acetone, repeatedly washing the cotton fabric by ultrasonic waves, putting the cotton fabric into a dopamine Tris-HCl buffer solution with the mass fraction of 10%, regulating the pH value to 8.5 according to a bath ratio of 1:50, reacting for 24 hours, taking out the cotton fabric, repeatedly washing the cotton fabric by using ethanol, and drying to prepare the polydopamine modified cotton fabric.
Preparing 10 percent of Ti by mass fraction3C2TxTwo-dimensional nanosheet colloidal solution of Ti3C2TxThe two-dimensional nanoplatelets have a transverse average dimension of 1 μm. Adding excessive gamma-aminopropyltriethoxysilane, reacting for 24h, washing off the excessive gamma-aminopropyltriethoxysilane, centrifuging, and vacuum drying to obtain gamma-aminopropyltriethoxysilane modified Ti3C2TxTwo-dimensional nanosheets.
Preparing 10 percent of Ti by mass fraction3C2TxTwo-dimensional nanosheet colloidal solution of Ti3C2TxThe two-dimensional nanoplatelets have a mean lateral dimension of 5 μm. Adding excessive gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, reacting for 24h, washing off excessive gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, centrifuging, and vacuum drying to obtain gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane modified Ti3C2TxTwo-dimensional nanosheets.
Modifying the gamma-aminopropyl triethoxysilane3C2TxTwo-dimensional nanosheet and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane modified Ti3C2TxThe two-dimensional nano sheets are respectively prepared to have the mass fraction of 5 percent200mL of the colloidal solution, and then 4g of polydopamine modified cotton fabric is sequentially soaked in gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane modified Ti3C2TxTwo-dimensional nanosheet colloidal solution and gamma-aminopropyltriethoxysilane modified Ti3C2TxAnd reacting in a two-dimensional nanosheet colloidal solution for 30 min. Repeating the reaction process once again, taking out the Ti, repeatedly cleaning the Ti by using deionized water, and drying the Ti in vacuum to finally prepare the 4-layer Ti3C2TxThe electromagnetic shielding cotton fabric.
Tested, 4 layers of Ti in example 13C2TxThe electromagnetic shielding effect value of the electromagnetic shielding cotton fabric is 59 dB. Even after 50 times of water washing, the electromagnetic shielding effect value is still as high as 51 dB. Far exceeding the electromagnetic shielding effectiveness of most MXenes fabrics in the literature.
For comparison, the raw cotton fabric after washing and drying was immersed in Ti having an average size of 1 μm in the transverse direction3C2TxTwo-dimensional nanosheet colloidal solution and Ti having a transverse average size of 5 μm3C2TxReacting in a two-dimensional nanosheet colloidal solution for 30min at a bath ratio of 1:50, repeating the dipping process for 4 times, taking out, repeatedly cleaning with deionized water, and vacuum drying. The electromagnetic shielding effectiveness values are tested and are respectively 22dB and 28 dB. After 50 water washes, the temperature dropped to 12 and 15. As can be seen from the electromagnetic shielding data: 4 layers of Ti3C2TxThe cotton fabric has excellent electromagnetic shielding performance and washing resistance, and greatly exceeds Ti prepared by a direct dipping method3C2TxTwo-dimensional nano-sheet cotton fabric. This is because of the multiple layers of Ti of different sizes3C2TxThe two-dimensional nano sheets form a multilayer layered structure, so that more interfaces are provided for reflection and scattering of electromagnetic waves, and the electromagnetic shielding performance of the cotton fabric is greatly improved. And relative to the direct impregnation method of Ti3C2TxTwo-dimensional nanosheet and Ti3C2TxBetween two-dimensional nanosheets, Ti3C2TxThe hydrogen bond adsorption between the two-dimensional nano-sheet and the cotton fabric is caused by Ti3C2TxTwo-dimensional nanosheet and Ti3C2TxBetween two-dimensional nanosheets, Ti3C2TxCovalent bond combination exists between the two-dimensional nano-sheets and the cotton fabric, so that Ti on the surface of the cotton fabric can be regulated and controlled through different reaction times3C2TxThe number of the assembled two-dimensional nano sheets is large, and the assembled cotton fabric has excellent washing resistance.
Although the direct impregnation method was also repeated 4 times to adsorb Ti3C2TxAnd (3) two-dimensional nanosheet processing. However, it is known that Ti3C2TxThe two-dimensional nano-sheet is negatively charged in water, thus Ti3C2TxThe adsorption amount and the assembly amount of the two-dimensional nano-sheet on the surface of the cotton fabric are certain when the Ti on the surface of the cotton fabric is3C2TxAfter the adsorption capacity of the two-dimensional nanosheets tends to be saturated, Ti is continuously added due to the charge repulsion effect of the same species3C2TxThe difficulty of the adsorption amount of the two-dimensional nanosheets will be multiplied. Therefore, the direct impregnation method has a critical point when the surface of the cotton fabric is Ti3C2TxAfter the adsorption capacity of the two-dimensional nanosheets reaches saturation, the adsorption process is not helpful even if repeated for a plurality of times.
Two most representative strains of gram-negative bacteria and gram-positive bacteria, namely escherichia coli and staphylococcus aureus, are selected as test strains, and the antibacterial effect of the sample is represented by quantitative test by adopting a shaking flask method. The bacteriostasis rate is tested according to a shaking flask method in an American standard ASTM E2149 and a national latest FZ/T73023-2006 standard. The test shows that the raw cotton fabric without any treatment has no bacteriostatic effect on escherichia coli and staphylococcus aureus. 4 layers of Ti in example 13C2TxThe bacteriostasis rates of the electromagnetic shielding cotton fabric to escherichia coli and staphylococcus aureus are respectively 99.99% and 99.65%. It is shown that the cotton fabric of example 1 is excellent in antibacterial property. The uv protection effect of cotton fabric is expressed using the uv protection index (UPF). The raw cotton fabric without any treatment had a UPF value of 6, 4 layers of Ti in example 13C2TxThe electromagnetic shielding cotton fabric has a UPF value as high as 148, which shows that the cotton fabric in the example 1 has excellent ultraviolet resistance.
Example 2:
putting 65%/35% polyester-cotton blended fabric which is not dyed and finished into acetone, repeatedly washing with ultrasound, then putting the fabric into 10% by mass of dopamine Tris-HCl buffer solution, regulating the pH value to 8.5, reacting for 24 hours, taking out, repeatedly washing with ethanol, and drying to prepare the polydopamine modified polyester-cotton blended fabric.
Preparing 10 percent of Nb by mass fraction2C two-dimensional nanosheet colloidal solution, wherein Nb2The average transverse size of the C two-dimensional nanosheet is 1 mu m, excessive gamma-aminopropyltriethoxysilane is added, the reaction is carried out for 24 hours, the excessive gamma-aminopropyltriethoxysilane is washed off, centrifugation and vacuum drying are carried out, and the gamma-aminopropyltriethoxysilane modified Nb is obtained2C, two-dimensional nanosheet.
Preparing 1-10% of Nb by mass fraction2C two-dimensional nanosheet colloidal solution, wherein Nb2The average size of the C two-dimensional nano-sheets in the transverse direction is 4 mu m. Adding excessive gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, reacting for 24h, washing off excessive gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, centrifuging, and vacuum drying to obtain gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane modified Nb2C, two-dimensional nanosheet.
Modifying the gamma-aminopropyltriethoxysilane2C two-dimensional nanosheet and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane modified Nb2Respectively preparing 100mL of colloidal solution with the mass fraction of 10% by using C two-dimensional nano sheets, and sequentially soaking 2g of polydopamine modified polyester-cotton blended fabric in gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane modified Nb2C two-dimensional nanosheet colloidal solution and gamma-aminopropyltriethoxysilane modified Nb2And C, reacting in a two-dimensional nanosheet colloidal solution for 30 min. And after being taken out, the fabric is repeatedly washed by deionized water and dried in vacuum, and finally the 2-layer MXenes electromagnetic shielding polyester-cotton blended fabric is prepared.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications of the present invention are within the scope of the present invention.
Claims (7)
1. A multilayer MXenes electromagnetic shielding fabric, comprising: (1) preparing a polydopamine modified fabric; (2) preparing a gamma-aminopropyltriethoxysilane modified MXenes two-dimensional nanosheet; (3) preparing a gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane modified MXenes two-dimensional nanosheet; (4) preparing colloid solutions with the mass fraction of 1-10% from gamma-aminopropyltriethoxysilane modified MXenes two-dimensional nanosheets and gamma- (2, 3-glycidoxy) propyltrimethoxysilane modified MXenes two-dimensional nanosheets respectively, and then soaking the polydopamine modified fabric in the gamma- (2, 3-glycidoxy) propyltrimethoxysilane modified MXenes two-dimensional nanosheet colloid solution and the gamma-aminopropyltriethoxysilane modified MXenes two-dimensional nanosheet colloid solution in sequence for reaction for 30min, wherein the bath ratio is 1: 50; (5) and (4) repeating the process of the sequential soaking reaction in the step (4) as required, taking out, repeatedly washing with deionized water, and drying in vacuum to prepare the multi-layer MXenes electromagnetic shielding fabric.
2. The multi-layer MXenes electromagnetic shielding fabric as claimed in claim 1, wherein the polydopamine modified fabric is prepared by the following steps: putting the fabric into acetone, carrying out ultrasonic repeated cleaning, then putting the fabric into a dopamine Tris-HCl buffer solution with the mass fraction of 10%, regulating the pH value to 8.5 at a bath ratio of 1:50, reacting for 24h, taking out, and repeatedly cleaning and drying by using ethanol.
3. The multi-layer MXenes electromagnetic shielding fabric according to claim 1, wherein the preparation method of the gamma-aminopropyltriethoxysilane modified MXenes two-dimensional nanosheets is as follows: preparing MXenes two-dimensional nanosheet colloidal solution with the mass fraction of 1-10%, adding gamma-aminopropyltriethoxysilane, reacting for 24h, washing, centrifuging, and vacuum drying.
4. The multi-layer MXenes electromagnetic shielding fabric according to claim 1, wherein the γ - (2, 3-epoxypropoxy) propyltrimethoxysilane modified MXenes two-dimensional nanosheets are prepared by the following steps: preparing MXenes two-dimensional nanosheet colloidal solution with the mass fraction of 1-10%, adding gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, reacting for 24h, washing, centrifuging and vacuum drying.
5. The multi-layer MXenes electromagnetic shielding fabric according to claim 1 or 3, wherein the MXenes two-dimensional nanosheets in step (2) have a transverse average size of 0.5-1.5 μm.
6. The multi-layer MXenes electromagnetic shielding fabric according to claim 1 or 4, wherein the MXenes two-dimensional nanosheets in step (3) have a transverse average size of 3-6 μm, and the MXenes two-dimensional nanosheets in step (3) have a transverse average size 2-10 times that of the MXenes two-dimensional nanosheets in step (2).
7. A multilayered MXenes electromagnetically shielding fabric obtained by the process of claim 1.
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| CN114318852A (en) * | 2022-01-07 | 2022-04-12 | 苏州大学 | Intelligent fireproof textile based on nano composite material and preparation method thereof |
| CN114672992A (en) * | 2022-03-21 | 2022-06-28 | 苏州经贸职业技术学院 | Function-lasting cotton fabric and preparation method thereof |
| CN114775267A (en) * | 2022-04-12 | 2022-07-22 | 南通大学 | Electromagnetic shielding non-woven fabric and preparation method thereof |
| CN114855443A (en) * | 2022-05-23 | 2022-08-05 | 江南大学 | Preparation method of flexible electromagnetic shielding fabric |
| CN115787283A (en) * | 2021-09-10 | 2023-03-14 | 北京服装学院 | Preparation method and application of infrared stealth fabric |
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