CN111535023B - Preparation method of conductive nanofiber membrane - Google Patents
Preparation method of conductive nanofiber membrane Download PDFInfo
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- CN111535023B CN111535023B CN202010300850.9A CN202010300850A CN111535023B CN 111535023 B CN111535023 B CN 111535023B CN 202010300850 A CN202010300850 A CN 202010300850A CN 111535023 B CN111535023 B CN 111535023B
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- 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
- D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/02—Detecting, measuring or recording pulse, heart rate, blood pressure or blood flow; Combined pulse/heart-rate/blood pressure determination; Evaluating a cardiovascular condition not otherwise provided for, e.g. using combinations of techniques provided for in this group with electrocardiography or electroauscultation; Heart catheters for measuring blood pressure
- A61B5/0205—Simultaneously evaluating both cardiovascular conditions and different types of body conditions, e.g. heart and respiratory condition
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/103—Detecting, measuring or recording devices for testing the shape, pattern, colour, size or movement of the body or parts thereof, for diagnostic purposes
- A61B5/11—Measuring movement of the entire body or parts thereof, e.g. head or hand tremor, mobility of a limb
- A61B5/1118—Determining activity level
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/68—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient
- A61B5/6801—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be attached to or worn on the body surface
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/68—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient
- A61B5/6801—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be attached to or worn on the body surface
- A61B5/6843—Monitoring or controlling sensor contact pressure
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- 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
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/22—Polymers or copolymers of halogenated mono-olefins
Abstract
The invention discloses a preparation method of a conductive nanofiber membrane, which specifically comprises the following steps: step 1: preparing a gold seed solution; step 2: preparing a PVDF nanofiber membrane; and 3, step 3: cutting the nanofiber membrane prepared in the step 2 into sheets, soaking in anhydrous methanol, taking out, cleaning with deionized water, and storing in deionized water; and 4, step 4: performing primary gold plating in the gold seed solution prepared in the step 1; and 5: and preparing a solution A, and putting the nanofiber membrane plated with gold for the first time into the solution A for plating gold for the second time to obtain the conductive nanofiber membrane. The sensor using the conductive nanofiber membrane prepared by the invention as a sensing element has higher sensitivity and wider response range.
Description
Technical Field
The invention belongs to the technical field of sensing elements of flexible pressure sensors, and particularly relates to a preparation method of a conductive nanofiber membrane.
Background
In recent years, wearable electronic sensors that can be used for human health detection have attracted much attention. The key part in the flexible pressure sensor is a sensing element, and the magnitude of applied pressure is tested by the change of an output current signal generated by the deformation of the sensing element, so that the real-time detection of the actions and the states of a human body, such as joint bending, muscle movement, pulse, sounding and the like, is realized. Conventional sensing elements are generally composed of a non-conductive elastic polymer substrate with a microstructure design and a conductive layer, and therefore, the sensing element has low sensitivity to stress and a narrow sensing range, which limits the development of flexible pressure sensors.
Disclosure of Invention
The invention aims to provide a preparation method of a conductive nanofiber membrane, which solves the problems that a sensing element is low in stress sensitivity and narrow in sensing range and is used as a key component of a flexible pressure sensor at present.
The technical scheme adopted by the invention is that,
a preparation method of a conductive nanofiber membrane specifically comprises the following steps:
step 1: adding 15-25mM sodium citrate 120-;
step 2: preparing a PVDF nanofiber membrane;
and step 3: cutting the nanofiber membrane prepared in the step 2 into sheets, soaking in anhydrous methanol, taking out, cleaning with deionized water, and storing in deionized water;
and 4, step 4: soaking the nanofiber membrane obtained in the step 3 in the gold seed solution prepared in the step 1 for 15-30 minutes, and then taking out;
and 5: adding 1000 mu L of 5-8% polyvinylpyrrolidone solution 650-.
The present invention is also characterized in that,
in the step 2, the preparation of the PVDF nano-fiber membrane specifically comprises the following steps: and (2) preparing a spinning solution by taking DMF as a solvent, and then adding the spinning solution into an injector for electrostatic spinning to obtain the PVDF nanofiber membrane.
In step 3, the absolute methanol can be replaced by absolute ethanol.
In step 3, the sodium borohydride can be replaced by hydrazine hydrate, ascorbic acid or ammonia water.
In the step 3, the soaking time of the nanofiber membrane in the anhydrous methanol is controlled to be 15-25 minutes.
And 5, cleaning the nanofiber membrane by using deionized water.
The invention has the beneficial effects that:
according to the preparation method of the conductive nanofiber membrane, the gold layer is plated on the flexible nanofiber membrane prepared by the electrostatic spinning technology through a chemical plating method to serve as the conductive layer, and the conductive layer is uniformly plated and is not easy to fall off. The conductive nanofiber membrane has a microstructure with distinct fibers and staggered layers, and is used as a sensing element of the flexible pressure sensor, so that the sensing element of the pressure sensor has high sensitivity and a wide response range.
Drawings
FIG. 1 is an electron microscope image of a PVDF nanofiber membrane obtained in example 1 in the preparation method of a conductive nanofiber membrane of the present invention;
fig. 2 is an electron microscope image of the conductive nanofiber film prepared in example 5 of the method for preparing the conductive nanofiber film according to the present invention.
Detailed Description
The following describes a method for preparing a conductive nanofiber membrane in detail with reference to the accompanying drawings and specific embodiments.
The invention provides a preparation method of a conductive nanofiber membrane, which specifically comprises the following steps:
step 1: preparing a gold seed solution;
adding 15-25mM sodium citrate 120-;
step 2: preparing a PVDF nanofiber membrane;
preparing 10mL of spinning solution by using DMF as a solvent, wherein the concentration of PVDF is 10-12wt%, heating and stirring the solution in water bath for 6 hours at 50 ℃, then adding the solution into a 10mL syringe for spinning, wherein the distance between a needle head and a receiving roller is 15cm, the feeding speed of the solution is 0.5mL/h, the spinning voltage is +16KV, -4KV, the rotating speed of the receiving roller is 100rpm, and spinning is carried out for 6 hours to obtain the PVDF nano-fiber membrane.
And step 3: cutting PVDF nanofiber membrane into 1.0 multiplied by 1.0cm2Soaking the small pieces in anhydrous methanol for 10-20 minutes, taking out, washing redundant methanol with deionized water, and storing in deionized water for later use;
and 4, step 4: plating gold on the nanofiber membrane;
the first time of gold plating is carried out,
soaking the nanofiber membrane obtained in the step 3 in the gold seed solution prepared in the step 1 for 15-30 minutes, and then taking out;
and 5: the second time of gold plating is carried out,
adding 5-8% of polyvinylpyrrolidone solution 650-.
The method for preparing the conductive nanofiber membrane of the present invention is described in detail by the following specific examples.
Example 1
The invention provides a preparation method of a conductive nanofiber membrane, which specifically comprises the following steps:
step 1: preparing a gold seed solution;
adding 120 mu L of 15mM sodium citrate and 100 mu L of 15mM chloroauric acid solution into 8mL deionized water, stirring, adding 300 mu L of 80mM sodium borohydride solution, and reacting for 2 minutes to obtain a gold seed solution;
step 2: preparing a PVDF nanofiber membrane;
preparing 10mL of spinning solution by using DMF as a solvent, wherein the concentration of PVDF is 10%, heating and stirring the solution in water bath for 6 hours at 50 ℃, then adding the solution into a 10mL injector for spinning, wherein the distance between a needle head and a receiving roller is 15cm, the feeding speed of the solution is 0.5mL/h, the spinning voltage is +16KV, -4KV, the rotating speed of the receiving roller is 100rpm, and the PVDF nanofiber membrane is obtained after 6 hours of spinning, wherein an electron microscope image of the PVDF nanofiber membrane is shown in figure 1.
And step 3: cutting PVDF nanofiber membrane into 1.0 multiplied by 1.0cm2Soaking the small pieces in anhydrous methanol for 10 minutes, taking out the small pieces, washing redundant methanol with deionized water, and storing the washed redundant methanol in the deionized water for later use;
and 4, step 4: plating gold on the nanofiber membrane;
the first time of gold plating is carried out,
soaking the nanofiber membrane obtained in the step 3 in the gold seed solution prepared in the step 1 for 15 minutes, and then taking out the nanofiber membrane;
and 5: the second time of gold plating is carried out,
adding 650 mu L of 5% polyvinylpyrrolidone solution, 250 mu L of 20mM chloroauric acid solution and 300 mu L of 20mM potassium iodide solution into 5mL of deionized water, stirring to obtain solution A, placing the nanofiber membrane after primary gold plating into the solution A, adding 400 mu L of 10mM ascorbic acid solution, stirring again, taking out the nanofiber membrane, cleaning the nanofiber membrane and drying at 45 ℃ to obtain the conductive nanofiber membrane.
Example 2
The invention provides a preparation method of a conductive nanofiber membrane, which specifically comprises the following steps:
step 1: preparing a gold seed solution;
adding 230 mu L of 25mM sodium citrate and 200 mu L of 25mM chloroauric acid solution into 12mL deionized water, stirring, adding 500 mu L of 150mM sodium borohydride solution, and reacting for 4 minutes to obtain a gold seed solution;
step 2: preparing a PVDF nanofiber membrane;
preparing 10mL of spinning solution by using DMF as a solvent, wherein the concentration of PVDF is 12%, heating and stirring the solution in water bath for 6 hours at 50 ℃, then adding the solution into a 10mL injector for spinning, wherein the distance between a needle head and a receiving roller is 15cm, the feeding speed of the solution is 0.5mL/h, the spinning voltage is +16KV, -4KV, the rotating speed of the receiving roller is 100rpm, and spinning is carried out for 6 hours to obtain the PVDF nano-fiber membrane.
And step 3: cutting PVDF nanofiber membrane into 1.0 multiplied by 1.0cm2Soaking the small pieces in anhydrous methanol for 20 minutes, taking out, washing redundant methanol with deionized water, and storing in the deionized water for later use;
and 4, step 4: plating gold on the nanofiber membrane;
the first time of gold plating is carried out,
soaking the nanofiber membrane obtained in the step 3 in the gold seed solution prepared in the step 1 for 30 minutes, and then taking out the nanofiber membrane;
and 5: the second time of gold plating is carried out,
adding 1000 mu L of 8% polyvinylpyrrolidone solution, 500 mu L of 25mM chloroauric acid solution and 600 mu L of 25mM potassium iodide solution into 10mL of deionized water, stirring to obtain solution A, placing the nanofiber membrane plated with gold for the first time into the solution A, adding 600 mu L of 20mM ascorbic acid solution, stirring again, taking out the nanofiber membrane, cleaning the nanofiber membrane, and drying at 50 ℃ to obtain the conductive nanofiber membrane.
Example 3
The invention provides a preparation method of a conductive nanofiber membrane, which specifically comprises the following steps:
step 1: preparing a gold seed solution;
adding 230 mu L of 25mM sodium citrate and 200 mu L of 25mM chloroauric acid solution into 10mL deionized water, stirring, adding 500 mu L of 150mM sodium borohydride solution, and reacting for 4 minutes to obtain a gold seed solution;
step 2: preparing a PVDF nanofiber membrane;
preparing 10mL of spinning solution by using DMF as a solvent, wherein the concentration of PVDF is 12%, heating and stirring the solution in water bath for 6 hours at 50 ℃, then adding the solution into a 10mL injector for spinning, wherein the distance between a needle head and a receiving roller is 15cm, the feeding speed of the solution is 0.5mL/h, the spinning voltage is +16KV, -4KV, the rotating speed of the receiving roller is 100rpm, and spinning is carried out for 6 hours to obtain the PVDF nano-fiber membrane.
And 3, step 3: mixing PVDF sodiumCutting rice fiber film into 1.0 × 1.0cm2Soaking the small pieces in anhydrous methanol for 20 minutes, taking out, washing redundant methanol with deionized water, and storing in the deionized water for later use;
and 4, step 4: plating gold on the nanofiber membrane;
the first time of gold plating is carried out,
soaking the nanofiber membrane obtained in the step 3 in the gold seed solution prepared in the step 1 for 25 minutes, and then taking out;
and 5: the second time of gold plating is carried out,
adding 1000 mu L of 8% polyvinylpyrrolidone solution, 500 mu L of 25mM chloroauric acid solution and 600 mu L of 25mM potassium iodide solution into 7mL of deionized water, stirring to obtain solution A, placing the nanofiber membrane plated with gold for the first time into the solution A, adding 600 mu L of 20mM ascorbic acid solution, stirring again, taking out the nanofiber membrane, cleaning the nanofiber membrane, and drying at 50 ℃ to obtain the conductive nanofiber membrane.
Example 4
The invention provides a preparation method of a conductive nanofiber membrane, which specifically comprises the following steps:
step 1: preparing a gold seed solution;
adding 200 mu L of 25mM sodium citrate and 200 mu L of 22mM chloroauric acid solution into 11mL deionized water, stirring, adding 500 mu L of 120mM sodium borohydride solution, and reacting for 4 minutes to obtain a gold seed solution;
step 2: preparing a PVDF nanofiber membrane;
preparing 10mL of spinning solution by using DMF as a solvent, wherein the concentration of PVDF is 12%, heating and stirring the solution in water bath for 6 hours at 50 ℃, then adding the solution into a 10mL injector for spinning, wherein the distance between a needle head and a receiving roller is 15cm, the feeding speed of the solution is 0.5mL/h, the spinning voltage is +16KV, -4KV, the rotating speed of the receiving roller is 100rpm, and spinning is carried out for 6 hours to obtain the PVDF nano-fiber membrane.
And step 3: cutting PVDF nanofiber membrane into 1.0 multiplied by 1.0cm2Soaking the small pieces in anhydrous methanol for 20 minutes, taking out, washing redundant methanol with deionized water, and storing in the deionized water for later use;
and 4, step 4: plating gold on the nanofiber membrane;
the first time of gold plating is carried out,
soaking the nanofiber membrane obtained in the step 3 in the gold seed solution prepared in the step 1 for 28 minutes, and then taking out;
and 5: the second time of gold plating is carried out,
adding 900 mu L of 5% polyvinylpyrrolidone solution, 500 mu L of 25mM chloroauric acid solution and 600 mu L of 25mM potassium iodide solution into 6mL of deionized water, stirring to obtain solution A, placing the nanofiber membrane plated with gold for the first time into the solution A, adding 500 mu L of 20mM ascorbic acid solution, stirring again, taking out the nanofiber membrane, washing the nanofiber membrane, and drying at 53 ℃ to obtain the conductive nanofiber membrane.
Example 5
The invention provides a preparation method of a conductive nanofiber membrane, which specifically comprises the following steps:
step 1: preparing a gold seed solution;
adding 180 mu L of 18mM sodium citrate and 180 mu L of 22mM chloroauric acid solution into 9mL deionized water, stirring, adding 350 mu L of 95mM sodium borohydride solution, and reacting for 3 minutes to obtain a gold seed solution;
and 2, step: preparing a PVDF nanofiber membrane;
preparing 10mL of spinning solution by using DMF as a solvent, wherein the concentration of PVDF is 10%, heating and stirring the solution in water bath for 6 hours at 50 ℃, then adding the solution into a 10mL injector for spinning, wherein the distance between a needle head and a receiving roller is 15cm, the feeding speed of the solution is 0.5mL/h, the spinning voltage is +16KV, -4KV, the rotating speed of the receiving roller is 100rpm, and spinning is carried out for 6 hours to obtain the PVDF nano-fiber membrane.
And step 3: cutting PVDF nanofiber membrane into 1.0 multiplied by 1.0cm2Soaking the small pieces in anhydrous methanol for 13 minutes, taking out the small pieces, washing redundant methanol with deionized water, and storing the methanol in the deionized water for later use;
and 4, step 4: plating gold on the nanofiber membrane;
the first time of gold plating is carried out,
soaking the nanofiber membrane obtained in the step 3 in the gold seed solution prepared in the step 1 for 17 minutes, and then taking out;
and 5: the second time of gold plating is carried out,
adding 800 mu L of 5% polyvinylpyrrolidone solution, 300 mu L of 22mM chloroauric acid solution and 400 mu L of 22mM potassium iodide solution into 6mL of deionized water, stirring to obtain solution A, placing the nanofiber membrane plated with gold for the first time into the solution A, adding 550 mu L of 12mM ascorbic acid solution, stirring again, taking out the nanofiber membrane, cleaning the nanofiber membrane, and drying at 48 ℃ to obtain the conductive nanofiber membrane.
According to the preparation method of the conductive nanofiber membrane, the gold layer is plated on the flexible nanofiber membrane prepared by the electrostatic spinning technology through a chemical plating method to serve as the conductive layer, and the conductive layer is uniformly plated and is not easy to fall off. The conductive nanofiber membrane has a microstructure with distinct fibers and staggered layers and is used as a sensing element of the pressure sensor, so that the pressure sensor has high sensitivity and a wide response range.
Claims (6)
1. The preparation method of the conductive nanofiber membrane is characterized by comprising the following steps:
step 1: adding 15-25mM sodium citrate 120-;
step 2: preparing a PVDF nanofiber membrane;
and step 3: cutting the nanofiber membrane prepared in the step 2 into sheets, soaking the sheets in anhydrous methanol for 10-20 minutes, taking out the sheets, washing the sheets with deionized water, and storing the sheets in the deionized water;
and 4, step 4: soaking the nanofiber membrane obtained in the step 3 in the gold seed solution prepared in the step 1 for 15-30 minutes, and then taking out;
and 5: adding 1000 mu L of 5-8% polyvinylpyrrolidone solution 650-.
2. The method for preparing a conductive nanofiber membrane as claimed in claim 1, wherein in the step 2, the preparation of the PVDF nanofiber membrane specifically comprises: and (2) preparing a spinning solution by taking DMF as a solvent, and then adding the spinning solution into an injector for electrostatic spinning to obtain the PVDF nano-fiber membrane.
3. The method for preparing a conductive nanofiber membrane as claimed in claim 1, wherein in step 3, the absolute methanol is replaced by absolute ethanol.
4. The method for preparing a conductive nanofiber membrane as claimed in claim 1, wherein in step 3, the sodium borohydride can be replaced by hydrazine hydrate, ascorbic acid or ammonia water.
5. The method for preparing a conductive nanofiber membrane as claimed in claim 1, wherein in step 3, the soaking time of the nanofiber membrane in anhydrous methanol is controlled to be 15-25 minutes.
6. The method for preparing a conductive nanofiber membrane as claimed in claim 1, wherein in step 5, the nanofiber membrane is washed with deionized water.
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