CN114068065B - Conductive material for temperature sensor and use thereof - Google Patents
Conductive material for temperature sensor and use thereof Download PDFInfo
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Abstract
The invention discloses a conductive material for a temperature sensor and application thereof; the conductive material comprises modified graphene, a binder, a surfactant and a solvent; the preparation method comprises the following steps: and uniformly mixing the binder, the surfactant and the solvent under the stirring action, adding the modified graphene, and continuously stirring to obtain the conductive material. The modified graphene is prepared from 3, 4-dimethoxyphenyl isocyanate modified graphene oxide; the modified graphene prepared by the invention has good dispersibility and stability, and can be used as a component of a conductive material, so that the conductive material has excellent conductivity and flexibility, and the surface of a substrate material can be coated with the modified graphene, so that the substrate material has excellent fatigue resistance.
Description
Technical Field
The invention belongs to the field of conductive materials, and particularly relates to a conductive material for a temperature sensor and application thereof.
Background
In the current technical development, the temperature sensor has wide application value in various fields such as production, life and the like. Common sensors can be classified into contact type and non-contact type according to different measurement modes. The sensitivity of the conventional contact temperature sensor needs to be improved, and the application range is narrow. The non-contact temperature sensor has high intrinsic noise and is greatly influenced by the outside. The temperature sensor also has wide application in real-time fluorescence quantitative PCR instruments.
Graphene is a new carbonaceous material with a two-dimensional structure, and has excellent electrical, thermal and mechanical properties. Therefore, various signals can be sensed through the change of the conductivity of the graphene, and the device has high sensitivity due to the high charge mobility of the graphene. The surface of the graphene oxide has a large number of oxygen-containing groups, has good solvent solubility and polymer affinity, and has excellent electrical, thermal and mechanical properties, so that the graphene oxide is a very promising material in the field of sensor preparation.
Disclosure of Invention
The invention aims to provide a conductive material with good conductivity and flexibility.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a conductive material comprises modified graphene, a binder, a surfactant and a solvent;
the modified graphene is prepared from 3, 4-dimethoxyphenyl isocyanate modified graphene oxide.
According to the invention, 3, 4-dimethoxyphenyl isocyanate is adopted to modify graphene oxide to prepare modified graphene, and the modified graphene is used as a component of a conductive material to further prepare a temperature sensor; the prepared conductive material has excellent conductivity, and the conductive material is coated on the surface of a substrate material, so that the substrate material has better fatigue resistance, repeated bending deformation is realized, and the conductive material still has good conductivity; the reason may be that other atoms are introduced into the structure of the graphene, so that the interlayer spacing of the graphene can be increased, the physical and chemical properties of the graphite are improved, the original physical and chemical properties of the graphene cannot be damaged, and the solubility and the dispersibility of the graphene in an organic solvent or water are obviously improved; the modified graphene is used as a component of a conductive material, so that the modified graphene has excellent dispersibility, and is used as a component of the conductive material, so that the conductivity of the conductive material is improved; the conductive material is coated on the surface of the base material, so that the base material still has excellent conductivity after being subjected to multiple cycles of bending deformation, namely excellent fatigue resistance.
Another object of the present invention is to provide a modified graphene having excellent dispersibility and stability in a solvent.
Preferably, the modified graphene is 1-8 parts by weight, the binder is 5-15 parts by weight, the surfactant is 0.02-0.8 part by weight, and the solvent is 10-30 parts by weight.
Preferably, the binder is one or a mixture of two of epoxy resin, organic silicon resin or urea resin.
Preferably, the surfactant is one or a mixture of a nonionic surfactant and an amphoteric surfactant.
Preferably, the solvent is one or two of dichloromethane, isopropanol and dimethylformamide.
The invention also discloses a preparation method of the conductive material with excellent conductivity, flexibility and fatigue resistance.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a preparation method of a conductive material comprises the following steps:
and uniformly mixing the binder, the surfactant and the solvent under the stirring action, adding the modified graphene, and continuously stirring to obtain the conductive material.
Preferably, the stirring speed is 150-250 r/min, and the stirring time is 15-30 min.
The invention also discloses the application of the conductive material in the preparation of the temperature sensor.
The invention also discloses application of the modified graphene in improving the conductivity of a conductive material.
The invention also discloses application of the modified graphene in improving the fatigue resistance of the conductive material.
According to the invention, 3, 4-dimethoxyphenyl isocyanate is adopted to modify graphene oxide to prepare modified graphene, and the modified graphene is used as a component of a conductive material to further prepare the conductive material; therefore, the following beneficial effects are achieved: the modified graphene has excellent dispersibility and stability in a solvent, namely, the 3, 4-dimethoxyphenyl isocyanate modifies the graphene oxide, so that the interlayer spacing of the graphene can be increased, and the physical and chemical properties of the graphene are improved; the conductive material is used as a component of the conductive material to prepare the conductive material, has excellent conductivity, and is coated on the surface of a substrate material to ensure that the substrate material has excellent fatigue resistance so as to still have good conductivity after repeated bending deformation; therefore, the modified graphene with good dispersibility and stability is used as a component of a conductive material, so that the conductive material has excellent conductivity and flexibility, and the modified graphene is coated on the surface of a substrate material, so that the substrate material still has excellent conductivity after undergoing multiple-cycle bending deformation, namely excellent fatigue resistance.
Drawings
Fig. 1 is an infrared spectrum of graphene before and after modification in example 1;
fig. 2 is an SEM image of modified graphene in example 1;
FIG. 3 is a sheet resistance of a conductive material;
FIG. 4 is a graph of the increase in sheet resistance of a conductive material;
fig. 5 shows the sheet resistance of the conductive material after the bending-recovery cycle test.
Detailed Description
In some embodiments of the present invention, a method for preparing a conductive material comprises the steps of:
(1) preparation of modified graphene
Placing 1-5 parts by weight of graphite oxide in 180-220 parts by weight of DMF (dimethyl formamide) for ultrasonic dispersion to obtain a graphene oxide dispersion liquid, then adding 5-10 parts by weight of 3, 4-dimethoxyphenyl isocyanate into the dispersion liquid, introducing nitrogen for protection, reacting for 20-28 h at 70-80 ℃, adjusting the pH of the dispersion liquid to 8.5-9.5 by using ammonia water, then heating to 90-100 ℃, and adding 1-3 parts by weight of hydrazine hydrate for reduction for 2-4 h; and after the reaction is finished, carrying out centrifugal washing for 3-5 times by using DMF (dimethyl formamide), so as to obtain the modified graphene.
(2) Preparation of conductive materials
According to the weight parts, 5-15 parts of binder, 0.02-0.8 part of surfactant and 10-30 parts of solvent are uniformly mixed under the stirring action, wherein the stirring speed is 150-250 r/min, the stirring time is 15-30 min, then 1-8 parts of modified graphene is added, and the stirring is continued for 20-30 min, so that the conductive material is obtained.
In order to provide the conductive material with excellent flexibility, preferable measures to be taken further include:
adding 0.5-1.5 parts by weight of benzyl fumarate into a surfactant; the conductive material has excellent flexibility due to the addition of the benzyl fumarate; the reason may be that benzyl fumarate and various components of the surfactant play a synergistic effect, and then are compounded with the modified graphene, the binder and other components to prepare the conductive material, so that the conductive material has excellent flexibility.
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
example 1
A preparation method of a conductive material comprises the following steps:
(1) the preparation method of the modified graphene comprises the following steps:
placing 2.5 parts by weight of graphite oxide into 195 parts by weight of DMF (dimethyl formamide) for ultrasonic dispersion to obtain graphene oxide dispersion liquid, then adding 6 parts by weight of 3, 4-dimethoxyphenyl isocyanate into the dispersion liquid, introducing nitrogen for protection, reacting for 26 hours at 75 ℃, adjusting the pH of the dispersion liquid to 9.2 by using ammonia water, then heating to 95 ℃, and then adding 2 parts by weight of hydrazine hydrate for reduction for 3 hours; after the reaction is finished, carrying out centrifugal washing for 5 times by using DMF (dimethyl formamide) to obtain modified graphene;
(2) preparation of conductive materials
According to the weight portion, 8 portions of urea-formaldehyde resin, 0.25 portion of nicotinyl alcohol tartrate and 15 portions of dimethylformamide are uniformly mixed under the stirring action, wherein the stirring speed is 200r/min, the stirring time is 15min, then 6 portions of the modified graphene are added, and the stirring is continued for 25min, so that the conductive material is obtained.
Example 2
A preparation method of a conductive material comprises the following steps:
(1) the preparation method of the modified graphene comprises the following steps:
placing 4 parts by weight of graphite oxide in 200 parts by weight of DMF (dimethyl formamide) for ultrasonic dispersion to obtain graphene oxide dispersion liquid, then adding 8.5 parts by weight of 3, 4-dimethoxyphenyl isocyanate into the dispersion liquid, introducing nitrogen for protection, reacting for 28 hours at 70 ℃, adjusting the pH of the dispersion liquid to 9.5 by using ammonia water, then heating to 90 ℃, and then adding 1.5 parts by weight of hydrazine hydrate for reduction for 2 hours; after the reaction is finished, carrying out centrifugal washing for 5 times by using DMF (dimethyl formamide) to obtain modified graphene;
(2) preparation of conductive materials
According to the weight portion, 10 portions of epoxy resin, 0.5 portion of 2-phenylthiazolidine-4-carboxylic acid and 12 portions of dimethylformamide are uniformly mixed under the stirring action, wherein the stirring speed is 180r/min, the stirring time is 20min, then 4 portions of the modified graphene are added, and the stirring is continued for 25min, so that the conductive material is obtained.
Example 3
A preparation method of a conductive material comprises the following steps:
(1) the preparation method of the modified graphene comprises the following steps:
placing 5 parts by weight of graphite oxide in 220 parts by weight of DMF (dimethyl formamide) for ultrasonic dispersion to obtain graphene oxide dispersion liquid, then adding 10 parts by weight of 3, 4-dimethoxyphenyl isocyanate into the dispersion liquid, introducing nitrogen for protection, reacting for 24 hours at 80 ℃, adjusting the pH of the dispersion liquid to 8.7 by using ammonia water, then heating to 100 ℃, and then adding 3 parts by weight of hydrazine hydrate for reduction for 4 hours; after the reaction is finished, carrying out centrifugal washing for 5 times by using DMF (dimethyl formamide) to obtain modified graphene;
the other steps were the same as in example 1.
Example 4
A preparation method of a conductive material comprises the following steps:
step (1) same as example 1;
(2) preparation of conductive materials
According to the weight portion, 12 portions of urea-formaldehyde resin, 0.05 portion of nicotinyl tartrate and 30 portions of dimethylformamide are uniformly mixed under the stirring action, wherein the stirring speed is 250r/min, the stirring time is 15min, then 2 portions of the modified graphene by weight are added, and the stirring is continued for 30min, so that the conductive material is obtained.
Example 5
A preparation method of a conductive material comprises the following steps:
step (1) same as example 1;
(2) preparation of conductive materials
According to the weight portion, 8 portions of urea-formaldehyde resin, 0.25 portion of nicotinyl alcohol tartrate, 15 portions of dimethylformamide and 1 portion of benzyl fumarate are uniformly mixed under the stirring action, wherein the stirring speed is 200r/min, the stirring time is 15min, then 6 portions of the modified graphene are added, and the stirring is continued for 25min, so that the conductive material is obtained.
Example 6
A preparation method of a conductive material comprises the following steps:
step (1) same as example 1;
(2) preparation of conductive materials
According to the weight portion, 8 portions of urea-formaldehyde resin, 0.25 portion of nicotinyl alcohol tartrate, 15 portions of dimethylformamide and 1.5 portions of benzyl fumarate are uniformly mixed under the stirring action, wherein the stirring speed is 200r/min, the stirring time is 15min, then 6 portions of the modified graphene are added, and the stirring is continued for 25min, so that the conductive material is obtained.
Comparative example 1
A preparation method of a conductive material comprises the following steps:
according to the weight portion, 8 portions of urea-formaldehyde resin, 0.25 portion of nicotinyl alcohol tartrate, 15 portions of dimethylformamide and 1 portion of benzyl fumarate are uniformly mixed under the stirring action, wherein the stirring speed is 200r/min, the stirring time is 15min, then 6 portions of graphene oxide by weight are added, and the stirring is continued for 25min, so that the conductive material is obtained.
Comparative example 2
A preparation method of a conductive material comprises the following steps:
according to the weight portion, 8 portions of urea-formaldehyde resin, 0.25 portion of nicotinyl alcohol tartrate and 15 portions of dimethylformamide are uniformly mixed under the stirring action, wherein the stirring speed is 200r/min, the stirring time is 15min, then 6 portions of graphene oxide by weight are added, and the stirring is continued for 25min, so that the conductive material is obtained.
Test example 1
1. Determination of infrared spectrum of modified graphene
In the test, a Bruker Optics VERTEX-70/70v Fourier external spectrometer is adopted to characterize a sample, the sample and KBr are ground, and the tabletting measurement range is 4000--1。
Fig. 1 is an infrared spectrum of graphene before and after modification in example 1. As can be seen from FIG. 1, the modified graphene is 3412cm in comparison with graphene oxide-1The characteristic absorption peak in the vicinity becomes strong due to the amide group; at 3097cm-1A strong characteristic absorption peak appears nearby, which is the stretching vibration of a benzene ring in the 3, 4-dimethoxyphenyl isocyanate; at 2936cm-1The specific absorption peak appearing nearby is the stretching vibration of methyl; at 1679cm-1The characteristic absorption peak appearing nearby is the stretching vibration of an amide group; at 1235cm-1The characteristic absorption peak appearing nearby is the stretching vibration of the bond between the aromatic ring and oxygen; therefore, the modified graphene is prepared by modifying the graphene oxide with 3, 4-dimethoxyphenyl isocyanate.
2. Determination of surface morphology of modified graphene
In the test, a Japanese Hitachi S4800 field emission type scanning electron microscope is adopted to detect the micro-morphology of the sample.
Fig. 2 is an SEM image of modified graphene in example 1. As can be seen from fig. 2, the modified graphite has a lamellar structure, a smooth surface, and a certain interlayer distance.
3. Determination of dispersibility of modified graphene
In the experiment, graphene samples before and after modification are dissolved in DMF, standing is carried out for 3 months, the dispersion condition of the graphene samples in the DMF is observed, and unmodified graphene is used as a control group.
As can be seen from table 1, the non-modified graphene shows delamination and coagulation at 2 months, while examples 1 to 3 show no delamination and coagulation, which indicates that the modified graphene prepared by using 3, 4-dimethoxyphenyl isocyanate modified graphene oxide has excellent dispersibility and stability in a solvent; the reason may be that the 3, 4-dimethoxyphenyl isocyanate modifies the graphene oxide to enable the graphene oxide to be inserted into graphene sheets, so that van der waals force between the graphene sheets is weakened, namely, the molecular structure of the graphene is changed, and further, the physical and chemical properties of the graphene are improved, so that the graphene has better dispersibility and stability in a solvent.
Test example 2
The properties of the conductive material were measured by uniformly coating the conductive material on the surface of a base material (PET) according to the conventional art.
1. Determination of the conductivity of conductive materials
The test adopts an SX1934 type digital four-probe measuring instrument to measure the surface resistance of the material.
Fig. 3 is a sheet resistance of a conductive material. As can be seen from fig. 3, the sheet resistance of the examples 1 to 4 is lower than 122 Ω/, the sheet resistance of the comparative examples 1 and 2 is lower than that of the comparative example 2, and the sheet resistance of the example 1 is lower than that of the comparative example 2, which indicates that the modified graphene prepared by modifying the graphene oxide with 3, 4-dimethoxyphenyl isocyanate is used as a component of the conductive material, so that the conductivity of the conductive material is improved; comparing example 1 with example 5, comparative example 1 with comparative example 2, the sheet resistance of example 5 is not significantly different from example 1, and the sheet resistance of comparative example 2 is not significantly different from comparative example 1, which shows that the addition of benzyl fumarate to the conductive material has almost no effect on the conductivity of the conductive material.
2. Measurement of flexibility of conductive Material
The test is to test the bending sheet resistance of the conductive material with the curvature radius of 5 mm; the bending test step is to test the sheet resistance R of the unbent conductive material0After the material was bent 3 times at a given radius of curvature, the sheet resistance of the material was tested again to be R1According to the increase of the sheet resistance (R)1-R0) The bending resistance of the material, i.e. the flexibility of the material, was determined.
Fig. 4 shows the increase in sheet resistance of the conductive material. As can be seen from fig. 4, the sheet resistance increase of examples 1 to 3 is less than 1.3 Ω/, the sheet resistance increase of examples 1 and 2 is much less than that of comparative example 2, which shows that the sheet resistance increase of example 1 to example 1 is much less than that of comparative example 2, and that the modified graphene prepared by modifying graphene oxide with 3, 4-dimethoxyphenyl isocyanate is used as a component of the conductive material, so that the conductive material has a small sheet resistance change amount and still has excellent conductivity after being subjected to bending change, that is, the bending resistance of the conductive material is improved, and the conductive material has good flexibility; the variance of the sheet resistance of the conductive material in the examples 5 and 6 is less than 0.65 Ω/, the sheet resistance of the conductive material in the examples 1 and 5 and the sheet resistance of the conductive material in the comparative examples 1 and 2 are compared, the increase of the sheet resistance of the conductive material in the examples 5 is less than that in the examples 1 and the increase of the sheet resistance of the conductive material in the comparative examples 1 and 1 is less than that in the comparative examples 2, which shows that the conductive material added with benzyl fumarate is coated on a substrate material, so that the bending resistance of the conductive material is improved, and the conductive material has more excellent flexibility.
3. Determination of fatigue resistance of conductive material
In the test, the bending condition was set to 5mm in radius of curvature, and the bending-recovery cycle test was carried out 10000 times using an anti-fatigue tester to measure the sheet resistance change rate of each sample.
Fig. 5 shows the sheet resistance of the conductive material after the bending-recovery cycle test. As can be seen from fig. 5, the sheet resistance change rate of examples 1 to 4 is not higher than 1.85%, the sheet resistance change rate of comparative examples 1 and 2, example 5 and comparative example 1, the sheet resistance change rate of example 1 is much lower than that of comparative example 1, and the sheet resistance change rate of example 5 is much lower than that of comparative example 1, which indicates that the modified graphene prepared by modifying graphene oxide with 3, 4-dimethoxyphenyl isocyanate is used as a component of a conductive material, and the modified graphene is coated on a base material, so that the conductive material has excellent fatigue resistance; comparing example 1 with example 5 and comparing example 1 with comparative example 2, the sheet resistance change rate of example 5 is not obviously different from example 1, and the sheet resistance change rate of comparative example 1 is also not obviously different from comparative example 2, which shows that the addition of benzyl fumarate in the conductive material has no obvious influence on the fatigue resistance of the conductive material.
Conventional operations in the operation steps of the present invention are well known to those skilled in the art and will not be described herein.
The above embodiments are merely illustrative, and not restrictive, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention, and the protection scope of the present invention should be defined by the claims.
Claims (6)
1. A preparation method of a conductive material comprises the following steps:
uniformly mixing the binder, the surfactant and the solvent under the stirring action, adding the modified graphene, and continuously stirring to obtain a conductive material;
the modified graphene is prepared from 3, 4-dimethoxyphenyl isocyanate modified graphene oxide;
the modified graphene comprises, by weight, 1-8 parts of modified graphene, 5-15 parts of a binder, 0.02-0.8 part of a surfactant and 10-30 parts of a solvent;
0.5 to 1.5 parts by weight of benzyl fumarate is added to the surfactant.
2. The method of claim 1, wherein the step of forming the conductive material comprises: the stirring speed is 150-250 r/min, and the stirring time is 15-30 min.
3. The method for preparing a conductive material according to claim 1, wherein: the binder is one or a mixture of two of epoxy resin, organic silicon resin or urea resin.
4. The method for preparing a conductive material according to claim 1, wherein: the preparation method of the modified graphene comprises the following steps: placing 1-5 parts by weight of graphite oxide in 180-220 parts by weight of DMF (dimethyl formamide) for ultrasonic dispersion to obtain a graphene oxide dispersion liquid, then adding 5-10 parts by weight of 3, 4-dimethoxyphenyl isocyanate into the dispersion liquid, introducing nitrogen for protection, reacting for 20-28 h at 70-80 ℃, adjusting the pH of the dispersion liquid to 8.5-9.5 by using ammonia water, then heating to 90-100 ℃, and adding 1-3 parts by weight of hydrazine hydrate for reduction for 2-4 h; and after the reaction is finished, carrying out centrifugal washing for 3-5 times by using DMF (dimethyl formamide), so as to obtain the modified graphene.
5. The method for preparing a conductive material according to claim 1, wherein: the solvent is one or two of dichloromethane, isopropanol and dimethylformamide.
6. Use of the conductive material as claimed in claim 1 for the preparation of a temperature sensor.
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