CN111455661A - Preparation method of graphene-coated cotton fabric, product and application of product - Google Patents
Preparation method of graphene-coated cotton fabric, product and application of product Download PDFInfo
- Publication number
- CN111455661A CN111455661A CN202010332313.2A CN202010332313A CN111455661A CN 111455661 A CN111455661 A CN 111455661A CN 202010332313 A CN202010332313 A CN 202010332313A CN 111455661 A CN111455661 A CN 111455661A
- Authority
- CN
- China
- Prior art keywords
- graphene
- cotton fabric
- fabric
- coated
- graphene oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a preparation method of a graphene-coated cotton fabric, a product and application of the graphene-coated cotton fabric.
Description
Technical Field
The invention relates to the technical field of conductive fabrics, in particular to a preparation method of a graphene coated cotton fabric, a product and application thereof.
Background
In the past, fabrics exist as necessities for people's life. The fabric used in common use mainly comprises natural fibers and synthetic fibers. However, the common textile fabric can not meet the requirements of people for a long time, so that the conductive fabric is produced while the social science and technology is developed.
The conductive fabric is an important component of the intelligent textile, and is obtained by combining conductive elements with the textile to endow the fabric with conductive performance. For example, Naeqianji et al use chinlon and metal fiber to make conductive fabric by blending and use in weft knitting knitted sensors. Experimental tests show that the conductive fabric has good air permeability and conductivity. The appearance of the intelligent garment can enable common textiles to get rid of the problem of static electricity, and can be combined with more sensing electronic elements to manufacture the intelligent garment beneficial to human life safety monitoring and related danger protection. At present, the conductive fabric has extremely wide application in the fields of sensors, intelligent clothing, medical treatment and the like.
Graphene is a two-dimensional carbon-based material, has a two-dimensional periodic honeycomb lattice structure consisting of six carbon-membered rings, can be warped into zero-dimensional fullerene, and can be curled into one-dimensional carbon nanotubes or stacked into three-dimensional graphite. Therefore, graphene is a basic unit constituting other graphite materials, and the specific structural morphology of graphene often determines its own performance. According to the research of many scientists, the graphene has the characteristics of being the hardest and thinnest, and has the characteristics of good light transmission, strong electric conductivity, flexibility, good mechanical strength and the like. By virtue of the excellent conductivity of graphene, the antistatic or conductive fabric with excellent performance can be prepared by treating graphene on the fabric through processes such as coating and the like, but the unique six-membered ring structure causes the dispersibility and affinity of graphene to be poor, and the graphene is difficult to combine with other materials.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a graphene coated cotton fabric, a product and application thereof.
One of the technical schemes of the invention is a preparation method of a graphene coated cotton fabric, which comprises the following steps:
(1) pretreating cotton fabrics;
(2) preparing a graphene oxide solution, uniformly dispersing, placing the pretreated cotton fabric into the graphene oxide solution for dipping, taking out after a period of time, and drying;
(3) preparing a reducing agent solution, placing the graphene oxide coated cotton fabric prepared in the step (2) in the reducing agent solution, soaking for a period of time, taking out, and drying to obtain the graphene coated cotton fabric.
Preferably, the step (1) specifically comprises the steps of soaking the cotton fabric in a sodium hydroxide solution at the temperature of 80 ℃ for 2 hours at a constant temperature, taking out the cotton fabric, washing the cotton fabric with clear water, and drying the cotton fabric in an oven at the temperature of 70 ℃.
Preferably, the concentration of the sodium hydroxide solution in the step (1) is 1 mol/L.
The cotton fiber is a natural cellulose fiber, which contains natural impurities such as pectin wax, protein, ash, lignin, pigment and the like, besides, warp yarns can be subjected to sizing treatment in the manufacturing process, part of the impurities can be remained on the surface of the cotton fabric, the coating covering process of the cotton fabric is seriously influenced by the existence of the impurities, and the pretreatment aims to remove various impurities on the surface of the cotton fiber, so that graphene oxide can be smoothly coated on the surface of the cotton fiber in the subsequent coating process, and the effect of improving the coating is achieved.
Sodium hydroxide can not dissolve starch, but can cause the starch to generate violent swelling to increase the molecular distance and loosen the structure, and simultaneously, hydrogen bond combination between the starch and hydroxyl on cotton fiber is damaged, so that the adhesive force of the starch on the cotton fiber is reduced, the capability of separating from the cotton fiber and dissolving in water is improved, the water solubility of the starch is increased, and the starch can be removed by washing. The alkaline solution is used for treating the cotton fabric at high temperature, ester bonds connected with the pectic substance and the cellulose can be hydrolyzed and broken, molecular chains of the pectic substance and the cellulose can be broken, the amide bonds of protein molecules are broken by the alkali to be dissolved, and fatty substances are saponified and dissolved with the alkali. Meanwhile, the processing performance of the cotton fiber treated by the sodium hydroxide is improved, and the adsorption capacity of the graphene oxide is improved.
Preferably, the step (2) specifically comprises the steps of preparing a graphene oxide solution with the mass fraction of 0.2-0.5%, heating to 80 ℃, soaking the cotton fabric pretreated in the step (1) in the graphene oxide solution for 2 hours at a constant temperature, taking out, and transferring to a 70 ℃ oven for drying to obtain the graphene oxide cotton fabric.
When the pretreated fabric is immersed in a graphene oxide solution at 80 ℃, molecular motion is accelerated under a high-temperature condition, so that the diffusion motion of graphene oxide to the interior of the fabric is enhanced, the graphene oxide can permeate into the fabric structure, the fabric is brownish yellow, and the reduced graphene oxide on the corresponding fabric can be increased and the surface of the fabric is gradually covered by the graphene oxide along with the increase of the concentration of the graphene oxide, so that the fabric is in a saturated state; when the graphene oxide on the surface of the fabric reaches a saturated state or more graphene oxide covers the surface of the fabric, in the subsequent graphene oxide reduction process, the reducing agent is not favorable for carrying out better reduction on the graphene oxide permeating into the fiber, so that the graphene oxide is remained on the surface and in the middle of a carbon layer after reduction, and the conductivity and the sensing performance of the graphene coating cotton fabric are influenced due to the discontinuity of the graphene carbon layer.
Preferably, the prepared graphene oxide solution is treated for 2 hours at 70 ℃ in an ultrasonic cleaning instrument, and then is heated to 80 ℃ for constant-temperature impregnation of the cotton fabric.
The purpose of this operation is in order to disperse graphite oxide, ensures that graphite oxide solution dispersion is even and prevents the graphite oxide reunion, and the graphite oxide solution of reunion can make follow-up coating process appear seriously inhomogeneous, influences the electric conductive property of coating cotton knitted fabric then.
Preferably, the reducing agent in the step (3) is L-ascorbic acid.
In the prior art, GO is reduced by reducing agent reduction, microwave reduction, solvent thermal reduction or catalytic treatment, and the like, so as to obtain Reduced Graphene Oxide (RGO). Wherein the reducing agent is further divided into alcohol reducing agent, phenol reducing agent, hydrazine hydrate and NaBH4And L-ascorbic acid L-ascorbic acid is also called VC, has good solubility and weak acidity, but can be used as a reducing agent to reduce and treat graphene oxide, and compared with the reduction treatment of a toxic hydrazine or hydrazine hydrate reagent, the reduction method is an environment-friendly reduction method.
Preferably, the step (3) specifically comprises the steps of preparing L-ascorbic acid solution with the mass fraction of 1-2%, heating to 80 ℃, putting the graphene oxide cotton fabric prepared in the step (2) into L-ascorbic acid solution, soaking for 2-4 hours at constant temperature, taking out, transferring to a 70 ℃ oven, and drying to obtain the graphene coating cotton fabric.
When the graphene oxide fabric is soaked in L-ascorbic acid solution, graphene oxide in the fabric is reduced into graphene, the fabric is changed from brown yellow to black, the graphene oxide is not conductive, therefore, the reducing agent is reduced at normal temperature and is difficult to permeate into fibers, so that the graphene oxide permeating into the fabric cannot be sufficiently reduced, when the temperature of the reducing agent is increased, the molecular movement rate is increased, L-ascorbic acid is easy to permeate into the fabric, the graphene oxide permeating into the fabric is sufficiently reduced, however, the temperature is too high, the reduction rate is continuously increased, more carbon dioxide is released, and the reduction of the graphene oxide on the surface of the fabric is hindered to a certain extent.
Preferably, the reduction time is 3 h.
Preferably, repeating the step (2) and the step (3) for 2-3 times to obtain the composite graphene coated cotton fabric.
When the number of the initial coating layers of the graphene coated cotton knitted fabric is transited from one layer to two layers, the increase amplitude of the mass per unit area of the coated fabric is small, and when the number of the coating layers is transited to three layers, the increase amplitude is large and is about 0.0039g/cm2. Therefore, the number of graphene coating layers is increased, so thatThe unit area mass in the graphene coated cotton knitted fabric is increased. The repeated preparation of the graphene coating can improve the loading capacity of the cotton fabric graphene, so that the graphene is uniformly attached to the inside and the surface of the cotton fabric from inside to outside, and the conductivity and the sensing performance of the cotton fabric are further improved. Along with the increase of the number of layers of the graphene coating, the thickness change of the graphene coating cotton knitted fabric is larger and larger, the content of graphene in the fabric is more, and meanwhile, the color of the fabric is deepened and is more biased to graphite black.
According to the second technical scheme, the graphene coated cotton fabric is prepared by the preparation method of the graphene coated cotton fabric.
According to the third technical scheme, the graphene coated cotton fabric is applied as a sensor fabric and a conductive fabric.
Compared with the prior art, the invention has the following beneficial effects:
graphene has excellent electrical properties, but due to the unique six-membered ring structure, graphene is poor in dispersibility and affinity, and is difficult to combine with other materials. The graphene oxide is used as an important oxide of graphene, has oxygen-containing functional groups such as carboxyl, hydroxyl and the like, has good dispersion stability in water and partial organic solvents, can be perfectly combined with hydroxyl on cotton fabric cellulose to form hydrogen bonds, is adsorbed on cotton fabric, and is finally reduced to obtain the graphene composite cotton fabric.
Before the graphene oxide coating is carried out, the cotton fabric is pretreated under the high-temperature condition, impurities on the surface of the cotton fabric are removed, meanwhile, the surface of the cotton fabric is pretreated, the diffusion of graphene oxide to the interior of the cotton fabric is promoted, the loading capacity of the graphene oxide is increased, the loading capacity of each layer of graphene oxide is strictly controlled, each layer of graphene oxide coating is prepared, namely, the graphene oxide coating is subjected to reducing agent reduction and then the next layer of graphene oxide coating is attached, the loading capacity of the graphene is improved to the maximum extent, the graphene oxide in the interior and on the surface of the cotton fabric is fully reduced, the continuity of graphene carbon layers in the interior and on the surface of the cotton fabric is guaranteed, the prepared graphene coated cotton fabric has excellent conductivity and sensing performance, and the sensitivity of the cotton fabric as a sensor material is improved.
Drawings
Fig. 1 is an appearance analysis diagram of graphene-coated cotton fabric prepared in example 1 of effect verification example 1;
fig. 2 is a surface topography diagram observed by a scanning electron microscope of the graphene-coated cotton fabric prepared in example 1 in effect verification example 2;
fig. 3 is a thickness test chart of the graphene-coated cotton fabric prepared in example 1 of effect verification example 3;
fig. 4 is a thickness test chart of the graphene-coated cotton fabric prepared in example 2 of the effect verification example 3;
fig. 5 is a graph illustrating the effect of the graphene oxide concentration of the graphene-coated cotton fabric prepared in example 1 and example 2 on the mass per unit area of the coated fabric in effect verification example 4;
fig. 6 is a graph showing the effect of the number of coating layers of the graphene-coated cotton fabric prepared in example 1 on the mass per unit area of the coated fabric in effect verification example 4;
fig. 7 is a graph showing effects of the graphene oxide concentration of the graphene-coated cotton fabric prepared in examples 1 and 2 on the graphene-coated cotton knitted fabric Rs in effect verification example 5;
fig. 8 is a graph of the effect of reduction time on graphene-coated cotton fabric Rs for the graphene-coated cotton fabric prepared in example 3;
FIG. 9 is a graph of the sensing performance of 0.2% C-RGO1 (1% +2h) graphene coated cotton fabric prepared in example 3;
FIG. 10 is a graph of the sensing performance of 0.2% C-RGO1 (1% +3h) graphene coated cotton fabric prepared in example 3;
FIG. 11 is a graph of the sensing performance of 0.5% C-RGO1 (1% +3h) graphene coated cotton fabric in effect validation example 6;
FIG. 12 is a graph of the sensing performance of 0.5% C-RGO2 (1% +3h) graphene coated cotton fabric in effect verification example 6;
FIG. 13 is a graph of the sensing performance of 0.5% C-RGO2 (1% +3h) graphene coated cotton fabric in effect verification example 6
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
Used in the following examples of the present invention are graphene oxides prepared by the classical "Hummers" method.
Example 1
(1) Pretreatment of cotton fabric: a8 cm by 8cm sample of cotton knitted fabric was weighed and recorded as M0. Weigh 4g of NaOH solid, pour into a 400ml beaker, and go to the beakerAdding water to 100ml, uniformly stirring by a magnetic stirrer to obtain 1 mol/L NaOH solution, putting the NaOH solution into a water bath kettle at 80 ℃, soaking a cotton knitted fabric sample into the NaOH solution, taking out the sample after 2 hours, washing the sample in water for 3 times to ensure that NaOH in the cotton knitted fabric sample is washed clean, putting the sample into a 70 ℃ oven for drying, weighing again after drying, and marking as M1。
(2) Preparing a graphene oxide solution: 0.4g of graphene oxide powder is weighed by an electronic scale, poured into a beaker, and 200ml of water is injected into the beaker, treated for 2 hours at 70 ℃ by an ultrasonic cleaner, and then transferred into a water bath kettle at 80 ℃.
(3) Preparing a graphene oxide cotton fabric: soaking the cotton fabric pretreated in the step (1) into the graphene oxide beaker solution prepared in the step (2), keeping a water bath at a constant temperature of 80 ℃, soaking for 2 hours, taking out, placing in a 70 ℃ drying oven, drying, and taking out, wherein the mark is 0.2% C-GO.
(4) Preparing the graphene coated cotton fabric, namely weighing 1g of L-ascorbic acid by using an electronic scale, pouring the weighed ascorbic acid into a beaker, then injecting water into the beaker to 100ml, stirring the ascorbic acid by using a magnetic stirrer, accelerating the dissolution of L-ascorbic acid to obtain L-ascorbic acid solution with the concentration of 1%, then placing the L-ascorbic acid solution into a water bath kettle at the temperature of 80 ℃, then soaking 0.2% of C-GO1 into L-ascorbic acid for reduction for 2h, taking out the fabric after reduction, transferring the fabric into an oven for drying at the temperature of 70 ℃, and weighing the weight as M and marking as 0.2% of C-RGO1 (1% +2h)2。
(5) Preparing a multilayer graphene coating cotton fabric: and (5) repeating the step (3) and the step (4) to obtain 0.2% of C-RGO2 (1% +2h) of the two-layer graphene coated cotton fabric and 0.2% of C-RGO3 (1% +2h) of the three-layer graphene coated cotton fabric.
Example 2
The difference from example 1 is that the mass fraction of the graphene oxide solution is 0.5%, and the prepared graphene-coated cotton fabric is 0.5% of C-RGO1 (1% +2h), 0.5% of C-RGO2 (1% +2h) and 0.5% of C-RGO3 (1% +2 h).
Effect test example 1
Appearance analysis was performed on the graphene-coated cotton fabric prepared in example 1, as shown in fig. 1, wherein, a is a pretreated fabric, b is 0.2% C-GO, C is 0.2% C-RGO1 (1% +2h), d is 0.2% C-RGO3 (1% +2h), it can be found that the fabric is white after pretreatment, when the fabric is immersed in a graphene oxide solution, the graphene oxide will penetrate into the fabric structure, so that the fabric is brownish yellow, and when the graphene oxide fabric is immersed in a L-ascorbic acid solution, the graphene oxide in the fabric is reduced to graphene, so that the fabric is changed from brownish yellow to black, and when the number of coating layers is increased, the content of graphene coated on the fabric is increased, so that the fabric is darkened, and is more biased towards graphite black.
Effect test example 2
The change of the surface morphology of the graphene-coated cotton fabric prepared in example 1 after coating was observed by using a S-4800 field emission scanning electron microscope produced by hitachi corporation, and the result is shown in fig. 2, in which, a is the morphology of the fiber of the pretreated pure cotton fabric magnified 1000 times, b is the morphology of the fiber of 0.2% C-GO after the cotton fabric is soaked in the GO dispersion for 2 hours, C is the morphology of the sample of 0.2% C-RGO1 (1% +2 hours) magnified 1000 times, and d is the morphology of the sample of 0.2% C-RGO3 (1% +2 hours) magnified 2500 times. Comparing the graph b with the graph a, the treated surface fiber surface layer of the cotton fabric is already provided with a GO coating layer, but the fiber coating rate is not very high. As can be seen from the graph c, a graphene coating layer is formed on the surface of the cotton fabric through the coating treatment, and the coating layer has a large number of folds and a rough surface. It can be seen from fig. d that the graphene sheet layer has been uniformly coated on the surface of the cotton fiber. Observing the graphs c and d, the fact that the cotton fibers are not cracked or the surfaces of the cotton fibers are damaged after the VC is subjected to long-time reduction treatment is found, and the fact that the graphene sheet layers have good coating and protecting effects on the cotton fibers is also proved.
Effect test example 3
The thickness of the knitted fabric is related to the basis weight, bulkiness, rigidity and flexibility, wear resistance, warmth retention, air permeability, and the like of the fabric. The graphene-coated cotton fabrics prepared in examples 1 and 2 were therefore tested for thickness according to the GB/T3820-1997 Standard for determination of the thickness of textiles and textile products.
The verification method comprises the following steps: the sample is placed on the reference plate, a certain pressure is applied to the sample by the pressure foot, and then the distance between the area of the pressure foot contacting the sample and the reference plate is measured, namely the thickness of the sample.
During experimental test, the area of the presser foot is set to be 2000mm2The pressurizing pressure was 200cN, the pressurizing time was 30s, and 5 sets of data were measured for each sample, and the average value was taken. The results of the experiment are shown in FIGS. 3 and 4.
For the graphene coated cotton knitted fabric, the thickness value change of the coated fabric indirectly represents the content of the graphene coated in the coated cotton knitted fabric. In fig. 3 and 4, the abscissa is the graphene-coated cotton knitted fabric sample, the ordinate is the corresponding thickness, and the slope of the broken line reflects the magnitude of the change rate of the thickness. Observing the line graph, the change rate of the thickness of the coated fabric is small and about 0.48% when the number of coating layers of the graphene coated fabric is changed from one layer to two layers, and the change rate of the thickness of the fabric is large and about 1.91% when the number of coating layers is changed to three layers. Therefore, with the increase of the number of graphene coating layers, the thickness of the graphene-coated cotton knitted fabric is changed more and more, and the content of graphene in the fabric is increased.
Effect test example 4
Mass analysis of the graphene-coated cotton fabric prepared in example 1 and example 2 is shown in fig. 5. Observing fig. 5, it can be easily found that the coated cotton fabric obtained by the high GO concentration treatment in the experimental process has a larger mass increase per unit area than that of the low GO concentration under the same and unchanged other conditions. When the graphene oxide coating is applied to the cotton knitted fabric, the GO concentration is increased, so that the GO can enter a cotton fabric structure. More graphene oxide is coated on the cotton knitted fabric, so that the mass of the graphene coated cotton knitted fabric per unit area is larger.
FIG. 6 is a graph showing the influence of the number of coating layers on the mass per unit area of the coated fabric in the graphene-coated cotton fabric prepared in example 1, and it can be found from FIG. 6 that when the number of coating layers of the graphene-coated cotton fabric is initially transited from one layer to two layers, the mass per unit area of the coated fabric is increased to a small extent, and when the number of coating layers is transited to three layers, the mass per unit area of the coated fabric is increased to a large extentAbout 0.0039g/cm2. Therefore, the increase of the number of the graphene coating layers can also increase the mass per unit area in the graphene-coated cotton knitted fabric.
Effect test example 5
The surface specific resistance (Rs) is an index for measuring the conductivity of the fabric, and thus the conductivity test was performed on the graphene-coated cotton fabric prepared in example 1 and example 2.
The testing principle is that two electrodes of the CAT digital multimeter are pressed on the surface of the fabric by a certain pressure, the distance between the electrodes is kept to be 1cm in the test, and the resistance value between the two electrodes is recorded after the numerical value is stable. The sheet specific resistance is generally expressed using the following formula:
Rs＝R*(L/b) (1)
wherein, R represents the resistance value measured by the two electrodes, L represents the width of the electrode, the value is 0.05cm, b represents the distance of the electrode, the value is 1 cm., and the substitution is simplified to obtain:
Rs＝0.05R
the results are shown in fig. 7, which analyzes that the Rs value of graphene coated cotton knitted fabric decreases rapidly and the conductive performance of the coated fabric is better as GO concentration increases under otherwise the same conditions. In addition, under the same other conditions and with different coating layers, the Rs value of the graphene-coated cotton knitted fabric is reduced along with the increase of the coating layers, and then the coated fabric shows better conductivity.
Example 3
Similar to example 1, except that the reduction time is 2h, 3h and 4h, respectively, the prepared graphene-coated cotton fabric is 0.2% of C-RGO1 (1% +2h), 0.2% of C-RGO1 (1% +3h) and 0.2% of C-RGO1 (1% +4h), and the effect of the reduction time on the graphene-coated cotton knitted fabric Rs is verified, and the result is shown in FIG. 8. The coated fabric Rs is significantly affected by the reduction time within three hours prior to the reduction time, with longer reduction times giving lower Rs for the coated fabric. However, after three hours of reduction, this effect gradually diminished or disappeared, and the Rs value hardly changed. The reason for this may be that after three hours of the reduction treatment, the graphene oxide present on the graphene oxide fabric can almost default to be completely reduced to graphene, and then in the subsequent time, the conductivity of the fabric does not change significantly with the increase of the reduction time.
The prepared 0.2% C-RGO1 (1% +2h), 0.2% C-RGO1 (1% +3h) were subjected to a sensing performance test;
the graphene-coated cotton knitted fabric is stretched and deformed at a fixed stretching rate of 2%, the resistance of the fabric per centimeter is changed along with the stretching, and the sensitivity of the fabric as a sensor is evaluated through sensing performance detection. The sensitivity formula is given below:
GF＝(R1/R0)/(L1/L0)
wherein GF represents the strain sensitive coefficient, R1 represents the resistance change value, R0 represents the initial resistance value, L1 represents the yarn length change value, and L0 represents the initial yarn length.
Referring to AATCC76-2011 textile surface resistance test method, before an experiment, a strong tensile tester parameter is set at a computer end, the tensile cycle is 5, the tensile rate is fixed to be 2%, the clamping distance is 100mm, and the tensile speed is 10 mm/min. After the connection of the inspection instrument is faultless, the electric meter pen clamps the fabric, the two ends of the fabric are fixed, the clamping distance between the two electrodes is 10mm, the interface of the instrument is adjusted, and the test is started. After the test is finished, the experimental data is derived, the resistance value of the fabric at the original length and the topmost end of the fabric after being stretched is taken, if 1 is the resistance value of the original length, and 2 is the resistance value of the fabric under the state of stretching to the top, and the steps are repeated in sequence.
The experimental data obtained are plotted in FIGS. 9-10. Under the premise of the same other conditions, the resistance value of each unit centimeter of the fabric is reduced along with the prolonging of the VC reduction time, and the sensing performance of the corresponding cloth sample is improved.
Example 4
The difference from example 2 is that the reduction time is 3h, and the prepared graphene-coated cotton fabric is 0.5% of C-RGO1 (1% +3h), 0.5% of C-RGO2 (1% +3h) and 0.5% of C-RGO3 (1% +3 h).
Effect test example 6
The sensor performance test was performed on the 0.5% C-RGO1 (1% +3h), 0.5% C-RGO2 (1% +3h), and 0.5% C-RGO3 (1% +3h) graphene coated cotton fabric prepared in example 4 according to the method described in example 3, and the experimental data obtained were plotted in FIGS. 11-13.
From fig. 10 to 11, it can be seen that the resistance of the knitted fabric monotonously increases at the time of stretching and monotonously decreases at the time of recovery. The reason for this is that the longitudinal stretching of the knitted fabric causes the sinking arc section of the yarn in the loop to shift toward the loop column, resulting in an increase in the length resistance in the test direction. On the other hand, however, longitudinal stretching of the fabric also results in increased pressure at the point of the hook junction between adjacent loops, resulting in decreased electrical resistance. From the test results, the former had a significant effect on the electrical resistance of the fabric. In addition, the number of coating layers is the same, the reduction time is the same, after the GO is treated in different concentrations, the resistance values of the two cloth samples per centimeter are periodically changed under the fixed stretching state of 2%, but the resistance value of the fabric treated by the 0.5% GO coating layer per centimeter is lower than that of the fabric treated by the 0.2% GO solution, namely the sensing performance of the fabric is increased along with the increase of the GO concentration.
As can be seen from fig. 12 to 13, when the graphene-coated cotton knitted fabric is under a fixed tension of 2% under the same other conditions, the resistance per centimeter decreases and the sensing performance increases as the number of coating layers increases.
Note: in the sensing performance curve graph, partial data are irregular or the regularity is not obvious, because the interference of factors such as human, experimental materials and equipment exists in the experimental coating process, the graphene coating on the coated cotton knitted fabric has partial unevenness, the resistance value on the same cloth sample possibly has overlarge difference, and even if a plurality of experiments are adopted, the sensing performance on the cloth sample cannot be prevented from having partial errors due to methods such as averaging of a plurality of groups of data.
Example 5
The same as example 1 except that the concentration of L-ascorbic acid was 1.5%, and the prepared graphene-coated cotton fabric was 0.2% C-RGO1 (1.5% +2h), 0.2% C-RGO2 (1.5% +2h), and 0.2% C-RGO3 (1.5% +2h), respectively.
Example 6
The difference from example 2 is that the concentration of L-ascorbic acid is 1.5%, and the prepared graphene-coated cotton fabric is 0.5% C-RGO1 (1.5% +2h), 0.5% C-RGO2 (1.5% +2h), and 0.5% C-RGO3 (1.5% +2h), respectively.
Comparative example 1
The difference from example 1 is that the pretreatment of the cotton fabric is carried out without addition of sodium hydroxide. The appearance, quality, thickness, conductivity and sensing performance of the graphene oxide-coated cotton fabric are tested, and the reason that the graphene oxide-coated cotton fabric is not subjected to sodium hydroxide treatment and is not beneficial to the subsequent adhesion of graphene oxide in the interior and on the surface of the cotton fabric is found that the performances of the graphene oxide-coated cotton fabric are far inferior to those of the graphene oxide-coated cotton fabric prepared in example 1 in all aspects.
Comparative example 2
The difference from example 1 is that after the first graphene oxide impregnation and drying, the reduction treatment is not performed, but the second graphene oxide solution impregnation and drying is directly performed, followed by the reduction with a reducing agent. The appearance, quality, thickness, conductivity and sensing performance of the graphene coated cotton fabric are tested, and the fact that the graphene coated cotton fabric prepared in the embodiment 1 is far inferior in performance in all aspects is found because the graphene oxide inside the graphene coated cotton fabric is covered due to the fact that the graphene oxide is not reduced after primary impregnation and is directly subjected to secondary impregnation, so that the graphene oxide cannot be fully reduced in the reduction process, the continuity of the graphene inside the graphene is poor, and the conductivity and sensing performance test of the graphene is affected.
Comparative example 3
The difference from example 1 is that the L-ascorbic acid solution has the temperature of 50 ℃ and 100 ℃, respectively, and the appearance, quality, thickness, conductivity and sensing performance tests show that the solution is far inferior to the graphene-coated cotton fabric prepared in example 1 in all aspects of performance, because the graphene oxide inside and on the surface of the cotton fabric cannot be sufficiently reduced due to the fact that the temperature is too low and the molecular motion is not severe, and when the temperature is too high, the reaction rate is too fast, so that more carbon dioxide is released to hinder the reduction of the graphene oxide on the surface of the fabric, and the reduction degree of the graphene oxide on the surface of the cotton fabric is affected due to the fact that the temperature is too high or too low.
It should be noted that the above examples are only for illustrating the technical idea and features of the present invention, and the purpose thereof is to enable others to understand the content of the present invention and to implement the present invention, and thus the protection scope of the present invention is not limited thereby. All equivalent changes or improvements made according to the spirit of the invention should be covered within the scope of the invention.
Claims (10)
1. A preparation method of a graphene coated cotton fabric is characterized by comprising the following steps:
(1) pretreating cotton fabrics;
(2) preparing a graphene oxide solution, uniformly dispersing, placing the pretreated cotton fabric into the graphene oxide solution for dipping, taking out after a period of time, and drying;
(3) preparing a reducing agent solution, placing the graphene oxide coated cotton fabric prepared in the step (2) in the reducing agent solution, soaking for a period of time, taking out, and drying to obtain the graphene coated cotton fabric.
2. The preparation method of the graphene-coated cotton fabric according to claim 1, wherein the step (1) specifically comprises the steps of soaking the cotton fabric in a sodium hydroxide solution at a temperature of 80 ℃ for 2 hours at a constant temperature, taking out the cotton fabric, washing the cotton fabric with clear water, and drying the cotton fabric in an oven at a temperature of 70 ℃.
3. The method for preparing graphene-coated cotton fabric according to claim 2, wherein the concentration of the sodium hydroxide solution in the step (1) is 1 mol/L.
4. The preparation method of the graphene coated cotton fabric according to claim 1, wherein the step (2) specifically comprises the steps of preparing a graphene oxide solution with the mass fraction of 0.2-0.5%, heating to 80 ℃, soaking the cotton fabric pretreated in the step (1) in the graphene oxide solution at a constant temperature for 2 hours, taking out, and transferring to a 70 ℃ oven for drying to obtain the graphene oxide cotton fabric.
5. The preparation method of the graphene coated cotton fabric according to claim 4, wherein the prepared graphene oxide solution is treated in an ultrasonic cleaning instrument at 70 ℃ for 2 hours, and then heated to 80 ℃ for constant temperature impregnation of the cotton fabric.
6. The method for preparing graphene-coated cotton fabric according to claim 1, wherein the reducing agent in step (3) is L-ascorbic acid.
7. The preparation method of the graphene-coated cotton fabric according to claim 6, wherein the step (3) specifically comprises the steps of preparing L-ascorbic acid solution with the mass fraction of 1-2%, heating to 80 ℃, putting the graphene oxide cotton fabric prepared in the step (2) into L-ascorbic acid solution, soaking at a constant temperature for 1-4 hours, taking out, transferring to a 70 ℃ oven, and drying to obtain the graphene-coated cotton fabric.
8. The preparation method of the graphene-coated cotton fabric according to any one of claims 1 to 7, wherein the step (2) and the step (3) are repeated for 2 to 3 times to obtain the composite graphene-coated cotton fabric.
9. Graphene coated cotton fabric prepared according to the method for preparing graphene coated cotton fabric according to any one of claims 1-8.
10. Use of the graphene coated cotton fabric according to claim 9 as a sensor fabric, a conductive fabric.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010332313.2A CN111455661B (en) | 2020-04-24 | 2020-04-24 | Preparation method of graphene-coated cotton fabric, product and application of product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010332313.2A CN111455661B (en) | 2020-04-24 | 2020-04-24 | Preparation method of graphene-coated cotton fabric, product and application of product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111455661A true CN111455661A (en) | 2020-07-28 |
| CN111455661B CN111455661B (en) | 2023-02-03 |
Family
ID=71675138
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010332313.2A Active CN111455661B (en) | 2020-04-24 | 2020-04-24 | Preparation method of graphene-coated cotton fabric, product and application of product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111455661B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112189945A (en) * | 2020-09-25 | 2021-01-08 | 电子科技大学 | Gait monitoring insole based on pressure sensor |
| CN112656409A (en) * | 2021-01-08 | 2021-04-16 | 嘉兴学院 | Textile ion sensor and preparation method and application thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20140138536A (en) * | 2013-05-23 | 2014-12-04 | 동국대학교 산학협력단 | Conductive fibers and preparation method thereof |
| CN105088749A (en) * | 2015-08-28 | 2015-11-25 | 东华大学 | Graphene/cotton cloth flexible conducting fabric and preparing method of graphene/cotton cloth flexible conducting fabric |
| CN104328653B (en) * | 2014-10-11 | 2016-06-08 | 江南大学 | A kind of graphene oxide derivative is for the method for multifunctional finish of textiles |
| WO2017063241A1 (en) * | 2015-10-13 | 2017-04-20 | 江南大学 | Method for preparing conductive fabric by using oxidized graphene electrochemical reduction |
| WO2018146592A1 (en) * | 2017-02-09 | 2018-08-16 | Indian Institute Of Science | Reduced grapheneoxide nanomaterial coated cotton fabric as a heating device and method therefore |
| CN109295694A (en) * | 2018-09-29 | 2019-02-01 | 上海工程技术大学 | A method of promoting cotton fiber electric conductivity |
| JP2019060067A (en) * | 2017-09-26 | 2019-04-18 | 東レ株式会社 | Method for producing graphene-coated fabric and graphene-coated fabric |
| CN110093775A (en) * | 2018-08-30 | 2019-08-06 | 东华大学 | A kind of preparation method of the uvioresistant cotton fabric of conductive energy |
| CN110344241A (en) * | 2019-07-23 | 2019-10-18 | 安徽工程大学 | A kind of preparation method of super-hydrophobic Electromagnetically shielding fabrics |
-
2020
- 2020-04-24 CN CN202010332313.2A patent/CN111455661B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20140138536A (en) * | 2013-05-23 | 2014-12-04 | 동국대학교 산학협력단 | Conductive fibers and preparation method thereof |
| CN104328653B (en) * | 2014-10-11 | 2016-06-08 | 江南大学 | A kind of graphene oxide derivative is for the method for multifunctional finish of textiles |
| CN105088749A (en) * | 2015-08-28 | 2015-11-25 | 东华大学 | Graphene/cotton cloth flexible conducting fabric and preparing method of graphene/cotton cloth flexible conducting fabric |
| WO2017063241A1 (en) * | 2015-10-13 | 2017-04-20 | 江南大学 | Method for preparing conductive fabric by using oxidized graphene electrochemical reduction |
| WO2018146592A1 (en) * | 2017-02-09 | 2018-08-16 | Indian Institute Of Science | Reduced grapheneoxide nanomaterial coated cotton fabric as a heating device and method therefore |
| JP2019060067A (en) * | 2017-09-26 | 2019-04-18 | 東レ株式会社 | Method for producing graphene-coated fabric and graphene-coated fabric |
| CN110093775A (en) * | 2018-08-30 | 2019-08-06 | 东华大学 | A kind of preparation method of the uvioresistant cotton fabric of conductive energy |
| CN109295694A (en) * | 2018-09-29 | 2019-02-01 | 上海工程技术大学 | A method of promoting cotton fiber electric conductivity |
| CN110344241A (en) * | 2019-07-23 | 2019-10-18 | 安徽工程大学 | A kind of preparation method of super-hydrophobic Electromagnetically shielding fabrics |
Non-Patent Citations (2)
| Title |
|---|
| 张松林 等: "氧化石墨烯多层膜在棉织物上的层层组装及其电磁屏蔽性能", 《东华大学学报（自然科学版）》 * |
| 贾栋等: "石墨烯/棉布复合材料的制备、表征及应用", 《印染助剂》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112189945A (en) * | 2020-09-25 | 2021-01-08 | 电子科技大学 | Gait monitoring insole based on pressure sensor |
| CN112656409A (en) * | 2021-01-08 | 2021-04-16 | 嘉兴学院 | Textile ion sensor and preparation method and application thereof |
| CN112656409B (en) * | 2021-01-08 | 2022-03-01 | 嘉兴学院 | Textile ion sensor and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111455661B (en) | 2023-02-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111455661B (en) | Preparation method of graphene-coated cotton fabric, product and application of product | |
| CN106521744B (en) | Reduced graphene oxide conductive elastic composite yarn and preparation method thereof | |
| Yan et al. | A highly sensitive strain sensor based on a carbonized polyacrylonitrile nanofiber woven fabric | |
| JP5264150B2 (en) | Carbon fiber strand and method for producing the same | |
| Frank et al. | High-performance PAN-based carbon fibers and their performance requirements | |
| CN108680095B (en) | Flexible strain transducer and preparation method thereof based on carbon nano-fiber yarn woven fabric | |
| Varesano et al. | Improving electrical performances of wool textiles: synthesis of conducting polypyrrole on the fiber surface | |
| JP4392432B2 (en) | Method for producing carbonized fabric | |
| Yang et al. | Conductive and durable CNT-cotton ring spun yarns | |
| EP0451263B1 (en) | Linear carbonaceous fiber with improved elongatability | |
| CN113607309A (en) | Stretchable calotropis gigantea fiber graphene flexible sensor | |
| CN108517571A (en) | A kind of preparation method of conduction regenerated silk fibroin nano fibrous membrane | |
| Hossain et al. | Durability of smart electronic textiles | |
| Zhang et al. | A flexible strain sensor based on conductive TPU/CNTs‐Gr composites | |
| Yan et al. | Anisotropy of resistance-type strain sensing networks based on aligned carbon nanofiber membrane | |
| CN113047041B (en) | Composite material of nano-cellulose/fiber fabric and preparation method thereof | |
| Luo et al. | Preparation and tensile conductivity of carbon nanotube/polyurethane nanofiber conductive films based on the centrifugal spinning method | |
| EP3763856A1 (en) | Carbon fiber and method for manufacturing same | |
| Nasouri et al. | Effects of diameter and surface area of electrospun nanocomposite fibers on electromagnetic interference shielding | |
| JP4392433B2 (en) | Method for producing carbonized fabric | |
| CN114739280B (en) | Multi-element nano carbon fiber yarn strain sensor and preparation method thereof | |
| CN101586308B (en) | Method for preparing polyacrylonitrile-based flame-retardant fiber | |
| Özen et al. | Comprehensive performance characterization of conductive fabric made of reduced graphene oxide (rGO) | |
| He et al. | An electrically stable and mechanically robust stretchable fiber conductor prepared by dip-coating silver nanowires on porous elastomer yarn | |
| JPH054463B2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |