CN112964339A - Hydrogel film modified quartz crystal microbalance sensor and preparation method and application thereof - Google Patents
Hydrogel film modified quartz crystal microbalance sensor and preparation method and application thereof Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01G—WEIGHING
- G01G3/00—Weighing apparatus characterised by the use of elastically-deformable members, e.g. spring balances
- G01G3/12—Weighing apparatus characterised by the use of elastically-deformable members, e.g. spring balances wherein the weighing element is in the form of a solid body stressed by pressure or tension during weighing
- G01G3/16—Weighing apparatus characterised by the use of elastically-deformable members, e.g. spring balances wherein the weighing element is in the form of a solid body stressed by pressure or tension during weighing measuring variations of frequency of oscillations of the body
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/02—Analysing fluids
- G01N29/022—Fluid sensors based on microsensors, e.g. quartz crystal-microbalance [QCM], surface acoustic wave [SAW] devices, tuning forks, cantilevers, flexural plate wave [FPW] devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
- G01N5/025—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content for determining moisture content
Abstract
The invention relates to a hydrogel film modified quartz crystal microbalance sensor and a preparation method and application thereof. The chitosan molecular structure contains abundant amino groups, and the oxidized graphene has a large number of oxygen-containing groups on the surface and the edge, so that the hydrogel can be used as a hydrophilic material.
Description
Technical Field
The invention belongs to the field of humidity sensing, and particularly relates to a quartz crystal microbalance sensor modified by a hydrogel film, and a preparation method and application thereof.
Background
The application of the conventional hydrogel as a novel intelligent material is limited due to the defects of poor mechanical property, slow response rate and the like. The micro-scale structure and properties of the nano material enable the nano material to show huge potential in the fields of electricity, optics, mechanics, biomedicine and the like. The inorganic nano material is added into the hydrogel by a simple preparation method, so that the mechanical property of the hydrogel is improved, and new properties such as environmental responsiveness, conductivity and the like can be endowed to the hydrogel. Researches show that the intelligent response characteristic of the graphene can be widely applied to the fields of brakes, sensors and the like through the modification of polymers and small molecular compounds which are stimulated to respond.
Graphene oxide/chitosan nanocomposites have been reported to be synthesized using a simple method (Graphene oxide/chitosan nanocomposite coated quartz crystal sensor for the detection of amine catalysts [ J ]. Sensors activators B: Chemical, 2017, 243: 721-730.) and used as a sensing material for quartz crystal microbalance Sensors to detect ammonia gas. A rGO/poly diallylmethylammonium chloride nanocomposite film sensor having high performance Humidity characteristics has also been reported (Humidity-sensing properties of chemically reduced graphene oxide/polymer nanocomposite film sensor based on layer-by-layer nano self-assembly [ J ]. Sensors Actuators B: Chemical, 2014, 197: 66-72.) and its mechanism of action, i.e. Humidity response, is related to GO p-type semiconductor behavior and Humidity-induced interlayer swelling effect of PDDA/RGO films.
However, the long-term stability and good repeatability of the quartz crystal microbalance sensor depend on the mechanical strength and structural functional groups of the sensitive film, and the polyacrylamide/chitosan/graphene oxide composite hydrogel has the excellent characteristics of the sensitive film, but the research on exploring humidity detection by using the composite hydrogel film as a quartz crystal microbalance sensing coating is not reported.
Disclosure of Invention
The invention aims to solve the technical problem of providing a hydrogel film modified quartz crystal microbalance sensor and a preparation method and application thereof.
The invention provides a hydrogel film modified quartz crystal microbalance sensor which is obtained by carrying out polymerization and crosslinking reaction on a quartz wafer containing a polyacrylamide/chitosan/graphene oxide hydrogel precursor solution.
The acrylamide/chitosan/graphene oxide hydrogel precursor solution is obtained by mixing acrylamide as a monomer, chitosan and graphene oxide as functional components and N, N' -methylene bisacrylamide as a cross-linking agent.
The deacetylation degree of the chitosan is more than or equal to 95%, and the viscosity is 100-200 MPa · s.
The invention also provides a preparation method of the hydrogel film modified quartz crystal microbalance sensor, which comprises the following steps:
(1) preparing a chitosan aqueous solution; adding a graphene oxide aqueous solution and a NaOH solution into a chitosan aqueous solution to obtain a chitosan/graphene oxide dispersion solution; adding N, N' -methylene bisacrylamide and acrylamide into the dispersion liquid, shaking uniformly, and adding a potassium persulfate solution into the dispersion liquid under stirring at the temperature of 0-4 ℃ to obtain an acrylamide/chitosan/graphene oxide hydrogel precursor solution;
(2) and spin-coating the acrylamide/chitosan/graphene oxide hydrogel precursor solution on a quartz wafer, and reacting at 60-80 ℃ for 6-12h to obtain the hydrogel film modified quartz crystal microbalance sensor.
The mass ratio of the acrylamide, the chitosan, the N, N' -methylene bisacrylamide and the potassium persulfate in the step (1) is 90-110:20-25:20-25: 1; the mass ratio of the graphene oxide to the acrylamide is 0.5-2.5%.
The concentration of the NaOH solution in the step (1) is 1-2M.
The spin coating in the step (2) is specifically as follows: spin coating at low speed for 30-40s and spin coating at high speed for 10-20 s.
The invention also provides an application of the hydrogel film modified quartz crystal microbalance sensor in humidity sensing.
Advantageous effects
(1) The invention prepares the polyacrylamide/chitosan/graphene oxide hydrogel by a free radical polymerization method, has the advantages of simple process compared with the traditional method with longer preparation route and more complex preparation method, and the chitosan material has low price and environment-friendly performance;
(2) according to the invention, the addition of the graphene oxide increases the crosslinking degree of the polyacrylamide/chitosan hydrogel, and due to the interaction of hydrogen bonds and static electricity between the graphene oxide nanosheets and the hydrogel, good interface combination between the graphene oxide and the hydrogel is formed, so that the breaking stress and the breaking elongation of the polyacrylamide/chitosan/graphene oxide hydrogel are effectively improved;
(3) according to the invention, the chitosan molecular structure contains abundant amino groups, and the graphene oxide has a large number of oxygen-containing groups on the surface and the edge, so that the hydrogel can be used as a hydrophilic material.
Drawings
FIG. 1 is a schematic diagram of the detection and preparation principle of the present invention.
FIG. 2 is a scanning electron microscope image of the 2.0 wt% PAM/CS/GO hydrogel obtained in example 3.
FIG. 3 is a stress-strain curve of the hydrogels obtained in examples 1-4 and comparative example 1.
FIG. 4 is a comparison of frequency response curves of PAM/CS/GO2.0 wt% hydrogel film modified sensor obtained in example 3 at different humidity (a) and the frequency response at adsorption equilibrium (b).
FIG. 5 shows the frequency response values of the PAM/CS hydrogel thin film modified sensor obtained in comparative example 1 at the frequency response adsorption equilibrium under different humidity.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) Preparation of polyacrylamide/chitosan/graphene oxide precursor solution
Weighing 2g of chitosan (the deacetylation degree is more than or equal to 95 percent, and the viscosity is 100-200 MPa & s), dissolving in 100mL of acetic acid solution (the volume fraction is 25 percent), and completely dissolving to prepare 2 percent chitosan aqueous solution. And weighing 250mg of graphene oxide to prepare a 25mg/mL aqueous solution, and performing ultrasonic treatment to form a stable aqueous dispersion. The graphene oxide aqueous solution (375 μ L) was aspirated by a pipette, an appropriate amount of the aqueous solution (1625 μ L) and 1mL of NaOH solution (concentration 1M) were added, respectively, and finally the mixture was poured into 5mL of chitosan aqueous solution for ultrasonic treatment to prepare a chitosan/graphene oxide dispersion. And controlling the mass ratio of the graphene oxide to the acrylamide to be 0.5%. After the ultrasound treatment is finished, 1mL of N, N' -methylene bisacrylamide and 2.132g of acrylamide are added into the chitosan/graphene oxide dispersion liquid, and the mixture is shaken uniformly. Then, adding 1mL of potassium persulfate solution (21mg/mL) at 0 ℃ under stirring to obtain a polyacrylamide/chitosan/graphene oxide precursor solution;
(2) preparation of polyacrylamide/chitosan/graphene oxide hydrogel film modified quartz crystal microbalance sensor
Sucking a quartz wafer on a spin coater, weighing 100 mu L of polyacrylamide/chitosan/graphene oxide precursor solution by using a pipette, dripping the solution on a gold electrode of the quartz wafer, and spin-coating to form a film (spin-coating at a low rotation speed (300r/min) for 30s and spin-coating at a high rotation speed (1000 r/min) for 20 s). And (3) reacting the gold-plated quartz wafer with the hydrogel precursor solution on the surface at the temperature of 60 ℃ for 6h to initiate polymerization and crosslinking reaction to form the polyacrylamide/chitosan/graphene oxide hydrogel film. Finally obtaining the quartz crystal microbalance sensor repaired by the hydrogel film. The hydrogel label of this example was PAM/CS/GO 0.5%.
Comparative example 1
The other conditions and steps were the same as in example 1, except that graphene oxide was not added, and the obtained hydrogel was a polyacrylamide/chitosan hydrogel (labeled PAM/CS).
Example 2
(1) Preparation of polyacrylamide/chitosan/graphene oxide precursor solution
Weighing 2g of chitosan (the deacetylation degree is more than or equal to 95 percent, and the viscosity is 100-200 MPa & s), dissolving in 100mL of acetic acid solution (the volume fraction is 25 percent), and completely dissolving to prepare 2 percent chitosan aqueous solution. And weighing 250mg of graphene oxide to prepare a 25mg/mL aqueous solution, and performing ultrasonic treatment to form a stable aqueous dispersion. Absorbing the graphene oxide aqueous solution (750 mu L) by a pipette, respectively adding a proper amount of the aqueous solution (1250 mu L) and 1mL of NaOH solution (with the concentration of 1M) correspondingly, and finally pouring the mixed solution into 5mL of chitosan aqueous solution for ultrasonic treatment to prepare the chitosan/graphene oxide dispersion solution. And controlling the mass ratio of the graphene oxide to the acrylamide to be 1.0%. After the ultrasound treatment is finished, 1mL of N, N' -methylenebisacrylamide crosslinking agent and 2.132g of acrylamide monomer are added into the chitosan/graphene oxide dispersion liquid, and the mixture is uniformly shaken. Then, adding 1mL of potassium persulfate solution (21mg/mL) at 0 ℃ under stirring to obtain a polyacrylamide/chitosan/graphene oxide precursor solution;
(2) preparation of polyacrylamide/chitosan/graphene oxide hydrogel film modified quartz crystal microbalance sensor
Sucking a quartz wafer on a spin coater, weighing 100 mu L of polyacrylamide/chitosan/graphene oxide precursor solution by using a pipette, dripping the solution on a gold electrode of the quartz wafer, and spin-coating to form a film (spin-coating at a low rotation speed (300r/min) for 30s and spin-coating at a high rotation speed (1000 r/min) for 20 s). And (3) reacting the gold-plated quartz wafer with the hydrogel precursor solution on the surface at the temperature of 70 ℃ for 8h to initiate polymerization and crosslinking reaction to form the polyacrylamide/chitosan/graphene oxide hydrogel film. Finally obtaining the quartz crystal microbalance sensor repaired by the hydrogel film. The hydrogel label for this example was PAM/CS/GO 1.0%.
Example 3
(1) Preparation of polyacrylamide/chitosan/graphene oxide precursor solution
Weighing 2g of chitosan (the deacetylation degree is more than or equal to 95 percent, and the viscosity is 100-200 MPa & s), dissolving in 100mL of acetic acid solution (the volume fraction is 25 percent), and completely dissolving to prepare 2 percent chitosan aqueous solution. And weighing 250mg of graphene oxide to prepare a 25mg/mL aqueous solution, and performing ultrasonic treatment to form a stable aqueous dispersion. Absorbing the graphene oxide aqueous solution (1500 mu L) by a pipette, respectively adding a proper amount of aqueous solution (500 mu L) and 1mL of NaOH solution (concentration is 1M) correspondingly, and finally pouring the mixed solution into 5mL of chitosan aqueous solution for ultrasonic treatment to prepare the chitosan/graphene oxide dispersion solution. And controlling the mass ratio of the graphene oxide to the acrylamide to be 2.0%. After the ultrasound treatment is finished, 1mL of N, N' -methylenebisacrylamide crosslinking agent and 2.132g of acrylamide monomer are added into the chitosan/graphene oxide dispersion liquid, and the mixture is uniformly shaken. Then, adding 1mL of potassium persulfate solution (21mg/mL) at 0 ℃ under stirring to obtain a polyacrylamide/chitosan/graphene oxide precursor solution;
(2) preparation of polyacrylamide/chitosan/graphene oxide hydrogel film modified quartz crystal microbalance sensor
Sucking a quartz wafer on a spin coater, weighing 100 mu L of polyacrylamide/chitosan/graphene oxide precursor solution by using a pipette, dripping the solution on a gold electrode of the quartz wafer, and spin-coating to form a film (spin-coating at a low rotation speed (300r/min) for 30s and spin-coating at a high rotation speed (1000 r/min) for 20 s). And (3) reacting the gold-plated quartz wafer with the hydrogel precursor solution on the surface at the temperature of 75 ℃ for 10h to initiate polymerization and crosslinking reaction to form the polyacrylamide/chitosan/graphene oxide hydrogel film. Finally obtaining the quartz crystal microbalance sensor repaired by the hydrogel film. The hydrogel label of this example is PAM/CS/GO 2.0%.
Example 4
(1) Preparation of polyacrylamide/chitosan/graphene oxide precursor solution
Weighing 2g of chitosan (the deacetylation degree is more than or equal to 95 percent, and the viscosity is 100-200 MPa & s), dissolving in 100mL of acetic acid solution (the volume fraction is 25 percent), and completely dissolving to prepare 2 percent chitosan aqueous solution. And weighing 250mg of graphene oxide to prepare a 25mg/mL aqueous solution, and performing ultrasonic treatment to form a stable aqueous dispersion. Absorbing the graphene oxide aqueous solution (2000 mu L) by a pipette, respectively adding a proper amount of aqueous solution (0 mu L) and 1mL of NaOH solution (with the concentration of 1M) correspondingly, and finally pouring the mixed solution into 5mL of chitosan aqueous solution for ultrasonic treatment to prepare the chitosan/graphene oxide dispersion solution. And controlling the mass ratio of the graphene oxide to the acrylamide to be 2.5%. After the ultrasound treatment is finished, 1mL of N, N' -methylenebisacrylamide crosslinking agent and 2.132g of acrylamide monomer are added into the chitosan/graphene oxide dispersion liquid, and the mixture is uniformly shaken. Then, adding 1mL of potassium persulfate solution (21mg/mL) at 0 ℃ under stirring to obtain a polyacrylamide/chitosan/graphene oxide precursor solution;
(2) preparation of polyacrylamide// chitosan graphene oxide hydrogel film modified quartz crystal microbalance sensor
Sucking a quartz wafer on a spin coater, weighing 100 mu L of polyacrylamide/chitosan/graphene oxide precursor solution by using a pipette, dripping the solution on a gold electrode of the quartz wafer, and spin-coating to form a film (spin-coating at a low rotation speed (300r/min) for 30s and spin-coating at a high rotation speed (1000 r/min) for 20 s). And (3) reacting the gold-plated quartz wafer with the hydrogel precursor solution on the surface at the temperature of 80 ℃ for 12h to initiate polymerization and crosslinking reaction to form the polyacrylamide/chitosan/graphene oxide hydrogel film. Finally obtaining the quartz crystal microbalance sensor repaired by the hydrogel film. The hydrogel label of this example is PAM/CS/GO 2.5%.
The quartz crystal microbalance sensor modified by the hydrogel thin film of the above example was placed in different humidity environments (by putting LiCl, MgCl2NaCl and KCl are respectively prepared into saturated salt solutions, and the experimental humidity is respectively controlled to be 11% RH, 33% RH, 75% RH and 85% RH). And (3) monitoring the curve of the resonance frequency of the quartz wafer along with the time change in real time by utilizing a quartz crystal microbalance technology, and obtaining a frequency change value during adsorption balance.
FIG. 1 is a schematic diagram of the detection and preparation principle of the present invention.
FIG. 2 is a scanning electron micrograph of PAM/CS/GO2.0 wt% hydrogel obtained in example 3, and the porous network structure is completely retained. But its wall thickness is increased and the fibrous structure of chitosan disappears and the pore size is about 55.7 μm, which is also advantageous for increasing the adsorption sites of water molecules. On the other hand, two-dimensional graphiteThe size and area of the alkene nano-sheet are small (about 0.04 mu m)2) The dispersion is good, and the polymer is also embedded into a cross-linked network structure, thereby being beneficial to improving the mechanical property of the network.
FIG. 3 is a stress-strain curve of the hydrogels obtained in examples 1-4 and comparative example 1, in which the elongation at break and the stress at break of the hydrogel increased from 1107% and 74kPa to 2039% and 237kPa, respectively, as the content of graphene oxide increased from 0.5% to 2.5%. This is because during stretching, the graphene oxide nanoplatelets can rotate parallel to the strain axis in the polymer network, resulting in dissipation of the strain. Meanwhile, due to the interaction of hydrogen bonds and static electricity between the graphene oxide nanosheets and the hydrogel, good interface bonding between the graphene oxide and the hydrogel is formed, and the mechanical properties of the nanocomposite hydrogel can be improved by breaking the reversible cross-linking points during stretching.
FIG. 4 is a comparison of frequency response curves of PAM/CS/GO 2.0% hydrogel film modified sensor obtained in example 3 at different humidity (a) and at adsorption equilibrium (b). The frequency response of the sensor modified by the hydrogel film under different humidity environments (33% RH, 75% RH and 85% RH) is known to change, the frequency is also reduced, and finally, the adsorption balance is achieved. The maximum frequency change obtained when the adsorption equilibrium was reached under a humidity environment of 75% RH was 21.7Hz, and the maximum frequency change obtained when the adsorption equilibrium was reached under a humidity environment of 85% RH was 22.3 Hz. The maximum frequency changes of the sensor under different humidity conditions are compared, and along with the increase of the humidity, the frequency changes of the quartz crystal microbalance sensor coated with the hydrogel film are increased in sequence.
FIG. 5 shows the frequency response values of the PAM/CS hydrogel thin film modified sensor obtained in comparative example 1 at the frequency response adsorption equilibrium under different humidity. The maximum frequency change obtained when the adsorption equilibrium was reached under a humidity environment of 75% RH was 16.9Hz, and the maximum frequency change obtained when the adsorption equilibrium was reached under a humidity environment of 85% RH was 19.9 Hz. Compared with FIG. 4, the humidity sensing performance of the PAM/CS hydrogel film modified sensor obtained in comparative example 1 is weaker than that of the PAM/CS/GO 2.0% hydrogel film modified sensor obtained in example 3.
Therefore, the hydrogel thin film is coated on the quartz crystal microbalance sensor wafer, the sensitivity of the sensor is improved, physical adsorption is carried out between hydrogel and water molecules, and the used hydrogel modified sensor can be repeatedly used through heating, drying and desorption, so that the hydrogel modified sensor has great potential in the application field of humidity sensors.
Claims (8)
1. A hydrogel film modified quartz crystal microbalance sensor is characterized in that: the material is obtained by polymerizing and crosslinking a quartz wafer containing a polyacrylamide/chitosan/graphene oxide hydrogel precursor solution.
2. The sensor of claim 1, wherein: the acrylamide/chitosan/graphene oxide hydrogel precursor solution is obtained by mixing acrylamide as a monomer, chitosan and graphene oxide as functional components and N, N' -methylene bisacrylamide as a cross-linking agent.
3. The sensor of claim 1, wherein: the deacetylation degree of the chitosan is more than or equal to 95%, and the viscosity is 100-200 MPa · s.
4. A preparation method of a hydrogel film modified quartz crystal microbalance sensor comprises the following steps:
(1) preparing a chitosan aqueous solution; adding a graphene oxide aqueous solution and a NaOH solution into a chitosan aqueous solution to obtain a chitosan/graphene oxide dispersion solution; adding N, N' -methylene bisacrylamide and acrylamide into the dispersion liquid, shaking uniformly, and adding a potassium persulfate solution into the dispersion liquid under stirring at the temperature of 0-4 ℃ to obtain an acrylamide/chitosan/graphene oxide hydrogel precursor solution;
(2) and spin-coating the acrylamide/chitosan/graphene oxide hydrogel precursor solution on a quartz wafer, and reacting at 60-80 ℃ for 6-12h to obtain the hydrogel film modified quartz crystal microbalance sensor.
5. The method of claim 4, wherein: the mass ratio of the acrylamide, the chitosan, the N, N' -methylene bisacrylamide and the potassium persulfate in the step (1) is 90-110:20-25:20-25: 1; the mass ratio of the graphene oxide to the acrylamide is 0.5-2.5%.
6. The method of claim 4, wherein: the concentration of the NaOH solution in the step (1) is 1-2M.
7. The method of claim 4, wherein: the spin coating in the step (2) is specifically as follows: spin coating at low speed for 30-40s and spin coating at high speed for 10-20 s.
8. Use of the hydrogel thin film modified quartz crystal microbalance sensor of claim 1 for humidity sensing.
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Application publication date: 20210615 |