CN114843006A - Three-dimensional flexible sensor material and preparation method and application thereof - Google Patents
Three-dimensional flexible sensor material and preparation method and application thereof Download PDFInfo
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- CN114843006A CN114843006A CN202210591962.3A CN202210591962A CN114843006A CN 114843006 A CN114843006 A CN 114843006A CN 202210591962 A CN202210591962 A CN 202210591962A CN 114843006 A CN114843006 A CN 114843006A
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- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
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- A61B5/1071—Measuring physical dimensions, e.g. size of the entire body or parts thereof measuring angles, e.g. using goniometers
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- 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
- A61B5/1121—Determining geometric values, e.g. centre of rotation or angular range of movement
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- A61B5/45—For evaluating or diagnosing the musculoskeletal system or teeth
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- A—HUMAN NECESSITIES
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- A61B5/45—For evaluating or diagnosing the musculoskeletal system or teeth
- A61B5/4538—Evaluating a particular part of the muscoloskeletal system or a particular medical condition
- A61B5/4585—Evaluating the knee
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
- B29C64/112—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using individual droplets, e.g. from jetting heads
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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
The invention provides a three-dimensional flexible sensor material and a preparation method and application thereof, wherein the preparation method of the sensor material comprises the following steps: adding a conductive agent, a binder and a reinforcing agent into water, and uniformly dispersing to obtain printing ink; manufacturing the printing ink into a device in a 3D printing mode, and then soaking the device into a cross-linking agent solution for soaking; and drying the device containing the cross-linking agent in a freeze drying mode to obtain the device. The flexible sensor can effectively solve the problems of high hardness and poor fitting degree of the existing sensor.
Description
Technical Field
The invention belongs to the technical field of sensors, and particularly relates to a three-dimensional flexible sensor material, and a preparation method and application thereof.
Background
A sensor is a device that converts a non-electrical signal into an electrical signal, and is a "sensory organ" in modern life. The coating is widely applied to various fields in life, and plays an important role in the aspects of automobiles, household appliances, environmental protection, entertainment facilities and the like.
Bones are important parts of the human body and play a role in protection, support, hematopoiesis, exercise and the like in the human body. Among all the skeletal joints of the human body, the knee joint is a large and complex flexion joint of the human body, bears great force, has stable and flexible structure, completes the load transmission of the human body, and plays an important role in the motion of the human body. When the knee joint of a human body is injured, not only treatment but also postoperative rehabilitation are important. The degree of postoperative recovery requires a judgment criterion for evaluation. At present, a patient can only go to a hospital for rehabilitation and can be rehabilitated under the guidance of a doctor. In the process, due to the shortage of medical resources, the problems of difficulty in seeing a doctor, difficulty in registering and time consumption exist when a patient is rehabilitated, and a flexible rehabilitation mode is needed to solve the problems.
At present, a sensor capable of helping a patient to perform self-service rehabilitation is needed to monitor the recovery condition of the patient, so that the patient can be not limited in a hospital when performing rehabilitation, and then the effect of performing self-service rehabilitation outdoors at home is achieved, in addition, the traditional rehabilitation device is mostly a metal/semiconductor device with large hardness, and the degree of fitting and the comfort degree of the injured part do not reach an ideal state.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a three-dimensional flexible sensor material, and a preparation method and application thereof, and the sensor can effectively solve the problems of high hardness and poor fitting degree of the existing sensor.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of a three-dimensional flexible sensor material comprises the following steps:
(1) adding a conductive agent, a binder and a reinforcing agent into water, and uniformly dispersing to obtain printing ink;
(2) manufacturing the printing ink into a device in a 3D printing mode, and then soaking the device into a cross-linking agent solution for soaking;
(3) and drying the device containing the cross-linking agent in a freeze drying mode to obtain the device.
Further, the dosage ratio of the conductive agent, the binder and the reinforcing agent in the step (1) is 1:0.2-2:0.1-0.5, and the solid content in the printing ink is 10-15%.
Further, the conductive agent in step (1) includes one of carbon nanotubes, graphene, conductive carbon black and carbon fibers.
Further, the binder in the step (1) comprises one of cellulose, chitosan, polyethylene glycol, sodium alginate, water-soluble silicon dioxide, polyacrylamide, sodium alginate, casein, sodium polyacrylate and polyoxyethylene.
Further, the reinforcing agent in the step (1) comprises graphene oxide.
Further, the preparation method of the printing ink in the step (1) is as follows: firstly, adding a binder into water, and dispersing for 8-12min by adopting ultrasonic; adding the reinforcing agent, and dispersing for 20-40min by using a high-speed dispersion instrument at the rotation speed of 5000-; and finally, adding the conductive agent into the solution, and continuously dispersing for 50-70min by using a high-speed dispersion instrument at the rotation speed of 1000-30000 rad/min.
Further, the specific printing manner is as follows: the printing ink is placed in a needle cylinder, a glass plate is used as a receiver and placed on a lower three-axis platform, the printing pressure is set to be 10-30 psi, the diameter of a printing needle head is 0.34-1.0 mm, and the moving speed of the three-axis platform is set to be 5-20 mm/min.
Further, the number of sample layers is 1-4, and the strand silk pitch in each layer is consistent with the diameter of the printing needle.
Further, in the step (2), the cross-linking agent is high-valence metal ions, the high-valence metal ions are divalent and trivalent, and the cross-linking agent comprises one of copper ions, iron ions, aluminum ions and calcium ions.
Further, the concentration of the cross-linking agent in the step (2) is 0.1-2M.
Further, the high-valence metal ions are derived from at least one of a chloride salt, a sulfate salt, and a nitrate salt thereof.
Further, the freeze-drying operation is as follows: and placing the printed device in liquid nitrogen for freezing, transferring the device into a freeze dryer, and performing vacuum drying for 24 hours to obtain the finished product.
A three-dimensional flexible sensor comprises the material prepared by the method.
The three-dimensional flexible sensor is used for medical detection and joint detection.
The beneficial effects produced by the invention are as follows:
1. the conductive agent and the binder adopted in the invention have the characteristic of high length-diameter ratio, the conductive agent and the binder are mutually entangled to form a substrate with certain mechanical property, and the conductive agent forms a conductive network in the substrate.
2. The binder, the conductive agent and the reinforcing agent adopted by the invention have rich polar functional groups, can be complexed with high-valence metal ions to realize the reinforcing effect of a three-dimensional network, and the pore structure endowed by the three-dimensional structure is combined with a freeze drying technology to realize the structure of a multi-level pore, so that the stress can be rapidly released when the porous structure is extruded from the outside, thereby ensuring better flexibility.
3. The three-dimensional flexible sensing device prepared by the invention has obvious resistance change and high sensitivity and accuracy in the states of compression and the like, and can be used as a piezoresistive sensing device.
4. The 3D printing technology adopted by the invention can easily realize customized device preparation, meets the requirements of users with differences, and has wide application prospect in the medical field of knee joint movement detection and the like.
Drawings
FIG. 1 is a characterization of the shear-thinning behavior of the 3D printing ink of example 1;
FIG. 2 is a characterization of the storage modulus/loss modulus performance of the 3D printed ink of example 1;
fig. 3 is a physical diagram of a fork structure for monitoring knee joint movement prepared by a 3D printing technique in example 1;
fig. 4 is a physical diagram showing the sensing device for monitoring knee joint movement prepared by the 3D printing technology in example 1 under the condition that the knee is extended and bent;
FIG. 5 is an internal Scanning Electron Microscope (SEM) image of a sensor material prepared by 3D printing techniques in example 1;
fig. 6 is a signal curve for knee joint movement monitoring prepared by the 3D printing technique in example 1.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are included to explain the invention and not to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
A three-dimensional flexible sensor is prepared by the following steps:
(1) firstly, 1g of cellulose is added into 10mL of water, and ultrasonic dispersion is adopted for 10 min; then 0.1g of graphene oxide is added, and a high-speed disperser is adopted for dispersing for 30min, wherein the rotating speed is 20000 rad/min; finally, adding 1g of carbon tubes into the solution, and continuously dispersing for 1h by using a high-speed disperser at the rotating speed of 30000rad/min to form printing ink;
(2) placing the printing ink obtained in the step (1) in a 30CC syringe, adopting a glass plate as a receiver, placing the glass plate on a lower three-axis platform, setting the printing pressure to be 30psi, the diameter of a printing needle head to be 0.84mm, setting the moving speed of the three-axis platform to be 15mm/min, and printing according to a preset program to obtain a forked sample, wherein the number of printing layers is 2;
(3) and (3) placing the printing sample obtained in the step (2) in a 0.5M copper chloride solution, crosslinking for 30 minutes, and then transferring to a freeze dryer for freeze drying to obtain the ink.
Example 2
A three-dimensional flexible sensor is prepared by the following steps:
(1) firstly, adding 1g of chitosan into 12mL of water, and dispersing for 10min by adopting ultrasonic; adding 0.2g of graphene oxide, and dispersing for 30min by using a high-speed disperser at a rotating speed of 25000 rad/min; finally, adding 1g of graphene into the solution, and continuously dispersing for 1h by using a high-speed disperser at the rotating speed of 30000rad/min to form printing ink;
(2) placing the printing ink obtained in the step (1) in a 30CC syringe, placing a glass plate serving as a receiver on a lower three-axis platform, setting the printing pressure to be 20psi, the diameter of a printing needle head to be 0.5mm, setting the moving speed of the three-axis platform to be 15mm/min, and printing according to a preset program to obtain a forked sample, wherein the number of printing layers is 2;
(3) and (3) placing the printing sample obtained in the step (2) in a 0.5M copper nitrate solution, crosslinking for 30 minutes, and then transferring to a freeze dryer for freeze drying to obtain the ink.
Example 3
A three-dimensional flexible sensor is prepared by the following steps:
(1) firstly, adding 1g of sodium alginate into 10mL of water, and dispersing for 10min by adopting ultrasonic; then 0.2g of graphene oxide is added, and the mixture is dispersed for 60min by adopting a high-speed dispersion instrument, wherein the rotating speed is 20000 rad/min; finally, adding 1.5g of carbon fiber into the solution, and continuously dispersing for 2 hours by using a high-speed disperser at the rotating speed of 30000rad/min to form printing ink;
(2) placing the printing ink obtained in the step (1) in a 30CC syringe, placing a glass plate serving as a receiver on a lower three-axis platform, setting the printing pressure to be 20psi, setting the diameter of a printing needle head to be 1mm, setting the moving speed of the three-axis platform to be 10mm/min, and printing according to a preset program to obtain a forked sample, wherein the number of printing layers is 2;
(3) and (3) placing the printing sample obtained in the step (2) into a 1M ferric chloride solution, crosslinking for 30 minutes, and then transferring to a freeze dryer for freeze drying to obtain the ink.
Example 4
A three-dimensional flexible sensor is prepared by the following steps:
(1) firstly, 1g of cellulose is added into 10mL of water, and ultrasonic dispersion is adopted for 10 min; then 0.1g of graphene oxide is added, and a high-speed disperser is adopted for dispersing for 30min, wherein the rotating speed is 10000 rad/min; finally, adding 1.5g of carbon tubes into the solution, and continuously dispersing for 1h by using a high-speed disperser at the rotating speed of 30000rad/min to form printing ink;
(2) placing the printing ink obtained in the step (1) in a 30CC syringe, placing a glass plate serving as a receiver on a lower three-axis platform, setting the printing pressure to be 20psi, setting the diameter of a printing needle head to be 0.7mm, setting the moving speed of the three-axis platform to be 18mm/min, and printing according to a preset program to obtain a forked sample, wherein the number of printing layers is 2;
(3) and (3) placing the printing sample obtained in the step (2) in a 1M aluminum chloride solution, crosslinking for 30 minutes, and then transferring to a freeze dryer for freeze drying to obtain the ink.
Test examples
The devices prepared in examples 1 to 4 were packaged in VHB tapes, and attached to human knee joints to prepare sensors, both ends of the sensors were clamped by positive and negative electrode clamps of a digital display source meter, and the changes in resistance under the changes in the actions of different human knee joints were measured at constant voltage to determine the health conditions of specific parts of the human body.
The sensor in the embodiment 1 has the remarkable capacity of continuously changing the resistance under the conditions that the bending angles of the knee joint are 30 degrees, 90 degrees and 120 degrees, and the resistance change rates are 220%, 750% and 2200% respectively;
in the sensor in embodiment 2, the resistance change rate data of the sensing performance obtained under the conditions of the bending motion of the knee joint at the bending angle of 30 °, 90 ° and 120 ° are 170%, 640% and 1900%, respectively;
in the sensor in embodiment 3, the resistance change rate data of the sensing performance obtained under the conditions of the bending motion of the knee joint at the bending angle of 30 °, 90 ° and 120 ° are respectively 180%, 720% and 2000%;
the sensor in example 4 obtained resistance change rate data of the sensory performance of 165%, 600%, and 1780% respectively under the conditions of the bending motions of the knee joint at the bending angles of 30 °, 90 °, and 120 °.
The rheological property of the ink comprises shear thinning property and modulus condition, a rotational rheometer is used for performing rheological test on the dispersed ink, the viscosity change of the dispersed ink is tested at a certain shear rate, and when the ink shows shear thinning behavior, the ink has the characteristic of being easily extruded from a narrow needle under the action of air pressure. In addition, the higher storage modulus before the critical shear pressure ensures shape retention after printing, while the air pressure reaches the critical point, which indicates that the ink may assume a liquid form and may be squeezed out of the needle, as shown in fig. 1 and 2.
As can be seen from fig. 1, the viscosity of the ink gradually decreased with the increase of the shearing time, which proves that the ink is easily extruded from a narrow needle and is convenient for printing.
It can be seen from fig. 2 that the ink has a higher storage modulus before the critical pressure, which ensures that the shape of the sample is maintained after printing.
It can be known from fig. 4 that a large number of pore structures exist in the sensor material prepared in the application, so that the material has a loose characteristic, and when the knee joint is bent, the shape of the sensor material is changed, so that the resistance change of the sensor material is influenced, and the detection of the health condition of the human body is realized.
As can be seen from fig. 5, the resistance of the sensor changes significantly when the knee joint bending angle changes, so as to achieve the purpose of detection.
While the present invention has been described in detail with reference to the specific embodiments thereof, it should not be construed as limited by the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (10)
1. A preparation method of a three-dimensional flexible sensor material is characterized by comprising the following steps:
(1) adding a conductive agent, a binder and a reinforcing agent into water, and uniformly dispersing to obtain printing ink;
(2) manufacturing the printing ink into a device in a 3D printing mode, and then soaking the device into a cross-linking agent solution for soaking;
(3) and drying the device containing the cross-linking agent in a freeze drying mode to obtain the device.
2. The method for preparing a three-dimensional flexible sensor material according to claim 1, wherein the amount ratio of the conductive agent, the binder and the reinforcing agent in the step (1) is 1:0.2-2:0.1-0.5, and the solid content in the printing ink is 10-15%.
3. The method of claim 1, wherein the conductive agent in step (1) comprises one of carbon nanotubes, graphene, conductive carbon black, and carbon fibers.
4. The method of claim 1, wherein the binder in step (1) comprises one of cellulose, chitosan, polyethylene glycol, sodium alginate, water-soluble silica, polyacrylamide, sodium alginate, casein, sodium polyacrylate, and polyoxyethylene.
5. The method for preparing a three-dimensional flexible sensor material according to claim 1, wherein the reinforcing agent in step (1) comprises graphene oxide.
6. The method for preparing a three-dimensional flexible sensor material according to claim 1, wherein the printing ink in the step (1) is prepared by: firstly, adding a binder into water, and dispersing for 8-12min by adopting ultrasonic; adding the reinforcing agent, and dispersing for 20-40min by using a high-speed dispersion instrument at the rotation speed of 5000-; and finally, adding the conductive agent into the solution, and continuously dispersing for 50-70min by using a high-speed dispersion instrument at the rotation speed of 1000-30000 rad/min.
7. The method for preparing a three-dimensional flexible sensor material according to claim 1, wherein the cross-linking agent in step (2) is a high-valence metal ion, and the cross-linking agent comprises one of copper ion, iron ion, aluminum ion and calcium ion.
8. The method for preparing a three-dimensional flexible sensor material according to claim 1, wherein the concentration of the cross-linking agent in the step (2) is 0.1-2M.
9. A three-dimensional flexible sensor comprising a sensor material made by the method of any one of claims 1-8.
10. The three-dimensional flexible sensor of claim 9 is used in medical testing, joint testing.
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