CN106433310B - Ink, sensitive layer, biosensor and preparation method thereof - Google Patents
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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Abstract
The invention discloses ink, a sensitive layer, a biosensor and a preparation method thereof. The preparation method of the ink for ink-jet printing of the sensitive layer of the biosensor comprises the following steps: s1, preparing a certain mass of water-soluble polymer with the average molecular weight less than 20000, mesoporous material dispersion liquid, a water-soluble organic solvent, a surfactant and water; s2, mixing and stirring the water-soluble polymer, the water-soluble organic solvent and water uniformly to fully dissolve the water-soluble polymer; s3, adding the surfactant and the mesoporous material dispersion liquid into a mixed solution; s4, filtering to obtain filtrate, and preparing ink; wherein the mass of each substance in step S1 is such that the mass fraction of the components in the ink is: 1-6% of water-soluble polymer, 1-10% of mesoporous material dispersion liquid, 10-20% of water-soluble organic solvent, 0.1-2% of surfactant and the balance of water. The ink is suitable for preparing the biosensor by ink-jet printing, and the prepared biosensor has higher sensitivity.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to preparation of a biosensor, in particular to preparation of ink-jet ink for ink-jet printing of a sensitive layer of the biosensor and the biosensor.
[ background of the invention ]
With the continuous development of sensor technology, the sensor technology is applied more and more in the fields of biology, medical treatment, environment, health and the like. For biosensor systems for detecting substances, such as electronic nose, electronic tongue, etc., it is usually necessary to modify a specific sensitive layer material on a substrate to achieve the detection of a target substance. Different biosensors have different requirements on modification means and accuracy. The ink-jet printing technology is a convenient, efficient and standard image forming technology, is mature, is widely applied, and has the advantages of high printing speed, high positioning precision, simplicity in operation and the like. When the sensitive layer of the biosensor is printed by adopting an ink-jet printing mode, a biochemical sensitive material is generally prepared into ink, a commercial ink-jet printer is modified to print the prepared ink on the surface of a substrate, and the ink is sprayed on the optical waveguide substrate to form a film.
The ink needs to meet the printing requirements, such as viscosity, surface tension, conductivity and pH value, so as to ensure that the ink is qualified and cannot block or damage the nozzle. Based on the printing requirement, the selectivity of the ink material for printing the sensitive layer of the biosensor is low, and the biosensor prepared after printing also has the problem of low sensitivity.
[ summary of the invention ]
The technical problem to be solved by the invention is as follows: the ink, the sensitive layer, the biosensor and the preparation method thereof are provided, the ink is suitable for preparing the biosensor by ink-jet printing, and the prepared biosensor has high sensitivity.
The technical problem of the invention is solved by the following technical scheme:
a method for preparing ink for ink-jet printing of a sensitive layer of a biosensor, comprising the steps of: s1, preparing a certain mass of water-soluble polymer with the average molecular weight less than 20000, mesoporous material dispersion liquid, a water-soluble organic solvent, a surfactant and water; s2, mixing and stirring the water-soluble polymer, the water-soluble organic solvent and water uniformly to fully dissolve the water-soluble polymer; s3, adding the surfactant and the mesoporous material dispersion liquid into the mixed solution obtained in the step S2; s4, filtering to obtain filtrate, and obtaining the ink; wherein the mass of each substance in step S1 is such that the mass fraction of the components in the ink is: 1-6% of water-soluble polymer, 1-10% of mesoporous material dispersion liquid, 10-20% of water-soluble organic solvent, 0.1-2% of surfactant and the balance of water.
The technical problem of the invention is solved by the following further technical scheme:
an ink for ink-jet printing of a sensitive layer of a biosensor comprises the following components in percentage by mass: 1-6% of water-soluble polymer with the average molecular weight less than 20000, 1-10% of mesoporous material dispersion liquid, 10-20% of water-soluble organic solvent, 0.1-2% of surfactant and the balance of water.
A sensitive layer in a biosensor is obtained by drying after ink-jet printing of the ink.
A biosensor comprising a substrate and a sensitive layer on the substrate, the sensitive layer being as described above.
A method for preparing a biosensor, comprising the steps of: u1, preparing a substrate material for the biosensor; u2 ink jet printing an ink as described above onto the base material; u3, drying the ink on the substrate material in a vacuum environment to form a sensitive layer on the substrate material, and obtaining the biosensor.
Compared with the prior art, the invention has the advantages that:
the ink is prepared from a water-soluble polymer serving as a sensitive layer, a mesoporous material dispersion liquid, a water-soluble organic solvent and a surfactant according to a certain mass fraction ratio. On one hand, the water-soluble organic solvent and the surfactant added into the ink enable the polymer material to be effectively dissolved in water, and the overall printing performance, particularly the viscosity, of the prepared ink is ensured, so that the requirements of ink-jet printing are met. On the other hand, the arranged mesoporous material has a large specific surface area, so that the ink is printed to prepare the sensitive layer of the biosensor, the specific surface area of the sensitive layer can be finally improved, and the sensitivity of the biosensor is further improved. Proved by verification, the sensitivity of the biosensor is improved by more than 10 percent compared with the existing biosensor. In addition, the mesoporous material also has a developed and ordered pore structure, and is also beneficial to improving the structural strength and the physical and chemical properties of a printed sensitive layer. The ink disclosed by the invention is not only suitable for ink-jet printing, but also the biosensor prepared after ink-jet printing has better performance, and can be suitable for application scenes with higher requirements.
[ description of the drawings ]
FIG. 1 is a graph showing a sensitivity detection curve when acetone gas is detected by the biosensor manufactured in Experimental example 1 according to the embodiment of the present invention;
FIG. 2 is a graph showing a sensitivity detection curve when acetone gas is detected by the biosensor referred to in Experimental example 1 according to the embodiment of the present invention;
FIG. 3 is a graph showing a sensitivity detection curve when acetone gas is detected by the biosensor manufactured in Experimental example 2 according to the embodiment of the present invention;
fig. 4 is a sensitivity detection graph when the biosensor referred to in experimental example 2 of the present embodiment detects acetone gas.
[ detailed description ] embodiments
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings.
The conception of the invention is as follows: although the ink-jet printing technology has the advantages of high positioning precision and simple and convenient operation compared with the scheme of directly coating a substrate by a sensitive layer, such as coating, sputtering and the like, the ink-jet printing has printing requirements on ink, and the properties of the ink, such as viscosity, surface tension, PH and the like, need to be controlled to ensure that a spray head is not blocked and damaged. Based on this, the ink formula has less selectivity in material use, and is generally a single polymer material, and the manufactured sensitive layer is also a single polymer material, which also results in that the manufactured biosensor has generally lower properties of electric conductivity, thermal conductivity, sensitivity, structural strength and the like.
The invention improves the formula of the ink. The aperture of the mesoporous material is generally 2-50 nm, and the viscosity of the ink and the like cannot be greatly influenced when the mesoporous material is added into the polymer ink, so that the requirements of ink-jet printing are met. Meanwhile, the mesoporous material is a regular and ordered pore channel structure with extremely high specific surface area, and can realize physical adsorption of a large number of molecules. Some mesoporous materials can also play a catalytic role in some physicochemical reactions, and the mesoporous materials with specific properties are added into the sensitive layer, so that the electric conductivity and the heat conductivity of the sensitive layer can be greatly improved. It is therefore contemplated to add the mesoporous material to the polymer sensitive layer solution. When the mesoporous material is added for improvement, not only the printing properties of the ink but also the solubility and dispersibility of the added mesoporous material, the influence on the solubility of the polymer, and other factors need to be considered. Based on multiple considerations, the ink formula for ink-jet printing is finally provided, wherein the ink formula is prepared from a water-soluble polymer, a mesoporous material dispersion liquid, a water-soluble organic solvent and a surfactant according to a certain proportion. The ink formula is suitable for ink-jet printing on one hand, and can improve the performance of the finally prepared biosensor on the other hand.
The specific embodiment provides ink for ink-jet printing of a sensitive layer of a biosensor, which comprises the following components in percentage by mass: 1-6% of water-soluble polymer with the average molecular weight less than 20000, 1-10% of mesoporous material dispersion liquid, 10-20% of water-soluble organic solvent, 0.1-2% of surfactant and the balance of water.
Wherein, the water-soluble polymer with the average molecular weight less than 20000 is selected to ensure that the printing nozzle is not jammed when the ink is printed. The polymer may be one of polyvinyl alcohol (PVA), polyethylene glycol (PEG), polyacrylic acid (PAA), polyvinylpyrrolidone (PVP) and polyquaternium. The polymer is a sensitive material, and the polymer plays a role of detecting substances in the sensitive layer subsequently, and can be selected according to the detection requirement of the prepared biosensor, for example, when the biosensor for detecting acetone gas is manufactured, polyvinyl alcohol or polyvinylpyrrolidone can be used as the polymer. The kind of the polymer is not limited to the above-exemplified case.
The mesoporous material dispersion liquid can be one or a mixture of more of single-walled carbon nanotube dispersion liquid, multi-walled carbon nanotube dispersion liquid, nano-silica dispersion liquid and nano-titania dispersion liquid. According to different types of the selected mesoporous materials, the performance of the sensitive layer prepared subsequently is improved differently. For example, nanosilica can improve heat resistance, light transmission, and catalytic performance. The nano titanium dioxide can improve the thermal stability and the catalytic performance. Generally, the mesoporous material dispersion liquid includes a mesoporous material, a dispersant, and a solvent. The dispersing agent can ensure that the nano-scale mesoporous material particles obtain enough acting force to be mutually dispersed, thereby avoiding agglomeration. The mesoporous material is added into the system in the form of mesoporous material dispersion liquid, so that the solubility and the dispersibility of the mesoporous material in the ink system can be ensured. The dispersant in the mesoporous material dispersion may be a surfactant or other organic solvent. Preferably a surfactant, which can be added in small amounts so as not to have a significant effect on the printed sensitive layer, while at the same time adjusting the surface tension of the solution. The solvent in the mesoporous material dispersion liquid is preferably water or ethanol, so that the ink property is not greatly influenced, and the printing is facilitated.
The water-soluble organic solvent is used as a cosolvent, so that the water-insoluble substance has a good dissolving effect, the solubility of the polymer material in water can be improved, and the polymer can be favorably prepared into ink.
The surfactant may aid in the dispersion of the polymer in the solution, reducing the surface tension of the solution, thereby helping the printed ink drops to bond well to the substrate of the sensor. The surfactant adjusts the surface tension of the whole ink, the surface tension is one of important properties of the water-based ink-jet ink, and the size of the surface tension directly influences the smoothness of the ink-jet ink during printing and the printing quality of the printing. The surface tension is too large, so that ink is not easy to wet the nozzle, and ink is not easy to drop; if the surface tension is too small, the ink is easy to directly drop, the ink drop is broken, and uniform and stable ink drops cannot be formed, or in the printing process, the ink drop is easy to have a trailing phenomenon, so that the printing fineness is reduced.
Preferably, the water-soluble organic solvent is propylene glycol, and the surfactant is a nonionic surfactant. The propylene glycol can improve the solubility of the polymer material, is a better cosolvent, is suitable for being matched with other solvents, and has an effect of improving the stability of the ink. The nonionic surfactant has good water solubility and good intersolubility with propylene glycol, and the two materials have little influence on the performance of the polymer material, so that the prepared ink is more suitable for ink-jet printing.
Through the mutual cooperation and cooperation of the materials, the finally prepared ink is suitable for preparing the biosensor through ink-jet printing, and the specific surface area of the sensitive layer prepared after the ink is printed is also higher, so that the detection sensitivity of the biosensor is higher finally.
Preferably, the mesoporous material in the mesoporous material dispersion liquid is a carbon nanotube with a length of 0.5-3 μm. The carbon nanotubes of this length range belong to short carbon nanotubes, and have high modulus and high strength. The carbon nano tube and the polymer material form a polymer-based carbon nano tube material, and the polymer material is used as an effective component in subsequent detection and is distributed in the pore canal of the short carbon nano tube, so that the distribution area of the polymer is effectively increased, and the detection sensitivity of the formed sensitive layer is further improved. The method is particularly suitable for the polymer material which is sensitive to gas, and the sensitivity is remarkably improved. In addition, the mesoporous material adopts the carbon nano tube, and the electric conduction and heat conduction performance of the sensitive layer can be improved.
More preferably, the mass fraction of the mesoporous material dispersion is 5 to 10%. The mesoporous material is used as an effective component for improving the performance of the biosensor, and the added content is high, so that the performance improvement effect is good.
As follows, specific examples were set up to verify the performance of biosensors produced by ink printing of the present embodiment.
Experimental example 1:
this example uses formulated inks to print a sensitive layer of polyvinyl alcohol based carbon nanotubes on a quartz wafer (AT-cut, 1 inch, 5 MHz). The printed quartz wafer was mounted on a probe whose quartz crystal is a balance (SRS corporation, QCM-200) as a sensing element of a gas biosensor, and 200ppm of acetone gas was detected to test the response condition of the sensing layer to the acetone gas.
100g of polyvinyl alcohol (PVA) sensitive layer solution is prepared to be used as ink-jet printing ink, and the components and the mass percentage are as follows: 3g of polyvinyl alcohol, 10g of aqueous dispersion of short multi-walled carbon nanotubes (the length is 0.5-3 mu m) (wherein the mass fraction of the short multi-walled carbon nanotubes in the aqueous dispersion is 1 wt%), 15g of propylene glycol, 1.5g of nonionic surfactant (Surfynol 465 is selected), and the balance of deionized water.
The preparation process of the polyvinyl alcohol sensitive layer solution comprises the following steps:
a. filtering the short multi-walled carbon nanotube dispersion liquid by using a vacuum suction filter, and sealing and storing;
b. after the components are weighed, mixing polyvinyl alcohol, water and propylene glycol into a feed liquid, adding a magnetic stirrer into a feed liquid bottle, sealing, and standing for 20 minutes;
c. placing the feed liquid on a magnetic stirrer, and stirring for 3 hours at a constant temperature of 80 ℃ until the polymer is dissolved;
d. stirring the feed liquid, naturally cooling, adding the short multi-walled carbon nanotube dispersion liquid and Surfynol 465, and stirring for 30 minutes at normal temperature;
e. installing a vacuum suction filter, selecting nylon filter paper with a filter hole of 0.45 mu m, wetting the filter paper with water, flatly attaching the filter paper to a filter element of the filter, introducing the feed liquid into a funnel of the vacuum suction filter, covering a funnel cover, and starting a vacuum pump for filtering;
f. and after filtering, closing the vacuum pump, pouring the filtrate into a solution bottle, and sealing to obtain the finished ink product.
The viscosity of the prepared ink solution was measured at room temperature, and the viscosity was 4.23mpa · s, which was suitable for inkjet printing. The ink solution was loaded into a printer (Epson R330) cartridge and the quartz wafer was mounted on an inkjet printing tray. The ink is printed on the quartz wafer, and the phenomenon of nozzle blockage does not occur in the printing process. After printing, after a period of standing, drying for 1 hour by using a vacuum drying oven, and forming a sensitive layer on the quartz wafer. The prepared biological sensitive element is connected to a quartz crystal microbalance sensor, acetone gas is detected, and the frequency response value of the quartz crystal microbalance sensor to the concentration of the acetone gas is observed. The measurements were repeated 3 times and averaged to obtain a sensitivity (frequency response value) of about 80 Hz. Fig. 1 is a diagram showing the response of a sensor during a measurement.
In order to compare the performance improvement of the sensitive layer prepared above, a reference example was set: a sensitive layer only comprising a polyvinyl alcohol sensitive material is manufactured by using a spin coating method, and then the manufactured biological sensitive element is connected to a quartz crystal microbalance sensor for testing. The quality of the sensitive layer controlled in spin coating during the experiment was the same as in the inkjet printing process described above. Acetone gas was probed and the gas concentration tested was also 200ppm acetone. The measurements were repeated 3 times and averaged to obtain a sensitivity (frequency response) of about 55 Hz. Fig. 2 is a graph showing the response of the sensor during one measurement.
Example 2:
this example uses formulated inks to print a polyvinylpyrrolidone-based carbon nanotube-sensitive layer on a quartz wafer (AT-cut, 1 inch, 5 MHz). The printed quartz wafer was mounted on a probe whose quartz crystal is a balance (SRS corporation, QCM-200) as a sensing element of a gas biosensor, and 200ppm of acetone gas was detected to test the response condition of the sensing layer to the acetone gas.
100g of polyvinylpyrrolidone (PVP) sensitive layer solution is prepared to be used as ink-jet printing ink, and the ink-jet printing ink comprises the following components in percentage by mass: 4g of polyvinylpyrrolidone (PVP), 10g of dispersion liquid of short single-walled carbon nanotubes (the length is 0.5-3 mu m) (wherein the mass fraction of the short single-walled carbon nanotubes in the dispersion liquid is 1 wt%), 15g of propylene glycol, 1.5g of nonionic surfactant (Surfynol 465 is selected), and the balance of deionized water.
The preparation process of the polyvinylpyrrolidone sensitive layer solution is as follows:
a. filtering the short single-walled carbon nanotube dispersion liquid by using a vacuum suction filter, and sealing and storing;
b. after all the components are weighed, mixing polyvinylpyrrolidone, water and propylene glycol into a feed liquid, adding a magnetic stirrer into a feed liquid bottle, sealing, and standing for 20 minutes;
c. placing the feed liquid on a magnetic stirrer, and stirring for 3 hours at a constant temperature of 80 ℃ until the polymer is dissolved;
d. stirring the feed liquid, naturally cooling, adding Surfynol 465 and the short single-walled carbon nanotube dispersion liquid, and stirring for 30 minutes at normal temperature;
e. installing a vacuum suction filter, selecting nylon filter paper with a filter hole of 0.45 mu m, wetting the filter paper with water, flatly attaching the filter paper to a filter element of the filter, introducing the feed liquid into a funnel of the vacuum suction filter, covering a funnel cover, and starting a vacuum pump for filtering;
f. and after filtering, closing the vacuum pump, pouring the filtrate into a solution bottle, and sealing to obtain the finished ink product.
The viscosity of the prepared ink solution was measured at room temperature, and the viscosity was 2.66mpa · s, which was suitable for inkjet printing. The ink solution was loaded into a printer (Epson R330) cartridge and the quartz wafer was mounted on an inkjet printing tray. The ink is printed on the quartz wafer, and the phenomenon of nozzle blockage does not occur in the printing process. After printing, after a period of standing, drying for 1 hour by using a vacuum drying oven, and forming a sensitive layer on the quartz wafer. The prepared biological sensitive element is connected to a quartz crystal microbalance sensor, acetone gas is detected, and the frequency response value of the quartz crystal microbalance sensor to the concentration of the acetone gas is observed. The measurements were repeated 3 times and averaged to obtain a sensitivity (frequency response) of about 245 Hz. Fig. 3 is a graph showing the response of the sensor during one measurement.
In order to compare the performance improvement of the sensitive layer prepared above, a reference example was set: a sensitive layer only comprising a polyvinylpyrrolidone sensitive material is manufactured by using a spin coating method, and then the manufactured biological sensitive element is connected to a quartz crystal microbalance sensor for testing. The quality of the sensitive layer controlled in spin coating during the experiment was the same as in the inkjet printing process described above. Acetone gas was probed and the gas concentration tested was also 200ppm acetone. The measurements were repeated 3 times and averaged to obtain a sensitivity (frequency response value) of about 215 Hz. Fig. 4 is a graph showing the response of the sensor during one measurement.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several alternatives or obvious modifications can be made without departing from the spirit of the invention, and all equivalents in performance or use should be deemed to fall within the scope of the invention.
Claims (7)
1. A preparation method of ink for ink-jet printing of a sensitive layer of a biosensor is characterized by comprising the following steps: the method comprises the following steps: s1, preparing a certain mass of water-soluble polymer with the average molecular weight less than 20000, mesoporous material dispersion liquid, a water-soluble organic solvent, a surfactant and water; the mesoporous material dispersion liquid is one or a mixture of nano silicon dioxide dispersion liquid and nano titanium dioxide dispersion liquid; s2, mixing and stirring the water-soluble polymer, the water-soluble organic solvent and water uniformly to form a feed liquid, adding a magnetic stirrer into a feed liquid bottle, sealing, and standing; placing the feed liquid on a magnetic stirrer, and stirring at a constant temperature until the water-soluble polymer is fully dissolved; s3, stirring the feed liquid, naturally cooling, and adding the surfactant and the mesoporous material dispersion liquid into the mixed solution obtained in the step S2; s4, installing a vacuum suction filter, selecting nylon filter paper with a filter hole of 0.45 mu m, wetting the filter paper with water, flatly attaching the filter paper to a filter element of the filter, introducing the feed liquid into a funnel of the vacuum suction filter, covering a funnel cover, starting a vacuum pump, and filtering to obtain filtrate, thereby preparing the ink; wherein the mass of each substance in step S1 is such that the mass fraction of the components in the ink is: 1-6% of water-soluble polymer, 1-10% of mesoporous material dispersion liquid, 10-20% of water-soluble organic solvent, 0.1-2% of surfactant and the balance of water; the dispersing agent in the mesoporous material dispersion liquid is a surfactant or an organic solvent, and the solvent in the mesoporous material dispersion liquid is water or ethanol.
2. An ink for ink-jet printing of a sensitive layer of a biosensor, comprising: the preparation method of the compound preparation comprises the following components in percentage by mass: 1-6% of water-soluble polymer with the average molecular weight less than 20000, 1-10% of mesoporous material dispersion liquid, 10-20% of water-soluble organic solvent, 0.1-2% of surfactant and the balance of water; the dispersing agent in the mesoporous material dispersion liquid is a surfactant or an organic solvent, and the solvent in the mesoporous material dispersion liquid is water or ethanol.
3. The ink of claim 2, wherein: the water-soluble organic solvent is propylene glycol, and the surfactant is a nonionic surfactant.
4. The ink of claim 2, wherein: the mass fraction of the mesoporous material dispersion liquid is 5-10%.
5. A sensitive layer in a biosensor, comprising: the sensitive layer is obtained by drying the ink of any one of claims 2 to 4 after ink-jet printing.
6. A biosensor comprising a substrate and a sensitive layer on the substrate, characterized in that: the sensitive layer is the sensitive layer as claimed in claim 5.
7. A method for preparing a biosensor, comprising: the method comprises the following steps: u1, preparing a substrate material for the biosensor; u2 ink jet printing the ink of any one of claims 2 to 4 onto the substrate material; u3, drying the ink on the substrate material in a vacuum environment to form a sensitive layer on the substrate material, and obtaining the biosensor.
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