CN113262105B - Wound dressing based on piezoelectric effect and preparation method thereof - Google Patents

Wound dressing based on piezoelectric effect and preparation method thereof Download PDF

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CN113262105B
CN113262105B CN202110499780.9A CN202110499780A CN113262105B CN 113262105 B CN113262105 B CN 113262105B CN 202110499780 A CN202110499780 A CN 202110499780A CN 113262105 B CN113262105 B CN 113262105B
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wound dressing
piezoelectric material
spin
electrode
substrate
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CN113262105A (en
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汪尧进
蔡园园
聂长文
宋树
潘韩
李娣洁
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61FFILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00Bandages or dressings; Absorbent pads
    • A61F13/02Adhesive bandages or dressings
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61FFILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00Bandages or dressings; Absorbent pads
    • A61F2013/00361Plasters
    • A61F2013/00902Plasters containing means
    • A61F2013/00919Plasters containing means for physical therapy, e.g. cold or magnetic

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  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Heart & Thoracic Surgery (AREA)
  • Vascular Medicine (AREA)
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Abstract

The invention discloses a wound dressing based on a piezoelectric effect and a preparation method thereof. The wound dressing based on the piezoelectric effect utilizes the interdigital electrode to polarize the piezoelectric material, so that the quantity of heterogeneous charges generated on the surface of the wound dressing is increased; the piezoelectric material generates pulse type current along with the motion of a human body, so that real-time electric stimulation is realized. The wound dressing prepared by the invention has simple preparation process, does not need to be disassembled and charged in the wound healing process, can reduce the bacterial breeding, reduce the infection rate and shorten the treatment time.

Description

Wound dressing based on piezoelectric effect and preparation method thereof
Technical Field
The invention relates to the field of piezoelectric material application, in particular to a wound dressing based on a piezoelectric effect and a preparation method thereof.
Background
In daily life activities, human beings inevitably leave wounds on the body surface due to accidental injuries or surgical operations.
Wound healing is considered to be a complex biological process associated with cell proliferation, differentiation and migration around the wound. It can be divided into three classical stages: inflammation, new tissue formation and remodeling. These three phases have no distinct boundaries and overlap each other. Many factors can interrupt the wound healing process, including chronic disease, vascular insufficiency, diabetes, malnutrition, infection, persistent inflammation, advanced age, mechanical stress, neuropathy, and the like. This also results in a higher incidence of chronic wounds with concomitant higher economic and social costs.
The process of wound healing can be accelerated by the use of wound dressings, and bandages and gauze are widely used as external protective barriers in conventional wound therapy, but they merely serve an anti-inflammatory effect on the wound and do not effectively promote wound healing. Especially for diabetes patients, the long-term control of blood sugar is poor, the tissue fluid has high sugar content, and the problems of arteriole, venule, even capillary vessel lesion and the like exist, and the healing speed of the wound is far slower than that of the common people. And therefore fatal infections during the healing process are likely to result in patient distress. To this end, researchers have undertaken a great deal of work in accelerating the healing of chronic wounds, such as debridement, physiotherapy, and functional dressings. However, most of these therapies are passively involved in the healing process and rarely in the control of the behavior of the relevant cells. The wound dressings on the market at present only focus on reducing infection to the maximum extent and increasing tissue fluid of wound parts, play roles in sterilizing, diminishing inflammation and reducing infection, so that the process of passive healing of wounds is accelerated, and related cells are not actively stimulated to fundamentally promote wound healing. Therefore, there is a need for a new therapeutic method capable of promoting skin cell regeneration activity and actively participating in skin regeneration.
In the eighteenth century, galvani found that the sciatic nerve of an injured frog was able to stimulate contraction of the thigh muscle on the other side, raising the animal's electricity. Later, researchers discovered that a similar phenomenon also exists in human skin, where the ion concentration of the wound surface is different due to the breakdown of trans-epithelial potential (TEP), resulting in the generation of an endogenous electric field. The electric field will remain present and maintained until the skin rejuvenation process is complete. In the wound healing process, on one hand, the electric field has an antibacterial effect and can promote the movement of immunoreactive cells such as neutrophils, lymphocytes, macrophages, monocytes and the like. On the other hand, the endogenous electric field actively participates in the healing of skin wounds by regulating the behavior of skin cells and promoting the regenerative activity of the skin cells, mainly stimulates the proliferation and division of fibroblasts, increases the receptor level of transforming growth factor beta, promotes the generation of collagen and synthetic protein, the differentiation of myofibroblasts, the migration of keratinocytes and the generation of blood vessels. The importance of endogenous electric fields for wound healing is further verified by means of controlling genes involved in wound healing in the literature "Electrical signals control and healing wound phosphor-3-OH kinase-gamma and PTEN", min Zhao, et al, nature, volume 442, issue 7101, 2006.
Based on the discovery of endogenous electric fields at the wound, medical practitioners propose the use of electrical stimulation devices to treat the wound. The electric stimulation therapy simulates and enhances the effect of an endogenous electric field of a wound by applying an external electric field to the wound part, thereby accelerating the directional migration, proliferation and differentiation of cells related to repair and inflammation diminishing to the center of the wound and accelerating the healing speed of the wound surface. However, its use is severely limited in clinical practice. Early medical workers attempted to tie patients to large electrical devices, but the operation was complicated, the electrical stimulation duration was very limited, and the experience of patients was poor. Meanwhile, dc stimulation was used in the early days. The direct current stimulation has great side effect on the wound, and the direct current stimulation used for a long time can induce electrochemical reaction at the wound, change the PH value of the wound and influence the wound healing speed. Therefore, the related scholars propose the biological enzyme battery dressing, and free charges generated by chemical reactions are utilized to stimulate cell proliferation at the wound, so that the problems of heavy weight and difficulty in carrying of the electrical stimulation equipment are solved. However, the bio-enzyme battery provides the electric stimulation for 12 hours at most, and the patient needs to change the dressing continuously to prolong the time of the electric stimulation, so that the risk of inflammatory infection of the wound is increased. Therefore, there is an urgent need to invent a wearable self-powered flexible wound dressing, which can generate non-direct-current electrical stimulation at a wound site in real time to promote skin wound healing.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a wound dressing based on a piezoelectric effect and a preparation method thereof. The interdigital electrode is utilized to polarize the piezoelectric material, the prepared wound dressing can be attached to the surface of a wound of a patient without burden, charging is realized through natural activity of a human body, and the wound dressing does not need to be detached and charged in the whole process of wound healing; the wound dressing prepared by the invention can effectively kill harmful bacteria, avoid infection, promote the proliferation and differentiation of fibroblasts and accelerate the healing of wounds.
The technical scheme of the invention is as follows:
a wound dressing based on piezoelectric effect comprises an encapsulating material, an electrode, a piezoelectric material, a substrate and an adhesive.
The packaging material is obtained by spin coating and drying packaging raw materials, and the thickness of the packaging material is 1-2 mu m; the packaging raw material is one or more of PDMS and PMMA; the electrodes are interdigital electrodes.
The piezoelectric material is one or more of an inorganic piezoelectric material and an organic piezoelectric material.
The inorganic piezoelectric material is BaTiO 3 、GaN、ZnSnO 3 One or more of ZnO, lead zirconate titanate and lead magnesium niobate; the organic piezoelectric material is one or more of polyvinylidene fluoride and polyvinylidene fluoride.
The substrate is a flexible substrate; the substrate is a mica sheet which is purchased from Taiyuan fluorophlogopite Co., ltd, and the thickness of the single sheet is 10-20 μm.
The adhesive is one or more of medical adhesive tape and hydrogel.
A preparation method of a wound dressing based on piezoelectric effect comprises the following steps:
(1) Preparing piezoelectric material gel by using a sol-gel method;
(2) Placing a substrate in a spin coater, opening the spin coater, spin-coating the piezoelectric material gel prepared in the step (1) on the surface of the substrate, performing heat treatment on the substrate on which the piezoelectric material gel is spin-coated, and then placing the substrate in a muffle furnace for high-temperature annealing to obtain a first layer of piezoelectric material;
(3) Placing the first layer of piezoelectric material prepared in the step (2) in a spin coater, opening the spin coater, and repeating the spin coating, heat treatment and high-temperature annealing process in the step (2) until the thickness of the material is 800-1200 nm;
(4) Fixing one surface of the material prepared in the step (3), which is not coated with the piezoelectric material, on an upper target disc of a magnetic control coating system, fixing an electrode mask on the surface of the piezoelectric material, fixing a target material on a lower target disc of the magnetic control coating system, setting the power of the magnetic control coating system to be 35-45W, introducing argon, opening the magnetic control coating system, and sputtering the surface of the piezoelectric material to form an electrode according to the shape of the mask to obtain the wound dressing with the electrode;
(5) After the wound dressing with the electrode prepared in the step (4) is sputtered with the surface of the electrode in a spin coating manner, drying to obtain a packaged wound dressing;
(6) Taking the packaged wound dressing prepared in the step (5), removing the packaging materials on the fingertips at the two ends of the electrode, and respectively connecting a lead to the fingertips at the two ends of the electrode by silver paste to obtain the unpolarized wound dressing; connecting the other ends of the two leads with the positive electrode and the negative electrode of a high-voltage power supply respectively, and turning on the high-voltage power supply to perform high-voltage polarization on the piezoelectric material of the wound dressing to obtain a polarized/unpolarized wound dressing;
(7) And (4) cutting off two leads on the polarized/unpolarized wound dressing prepared in the step (6), dripping a packaging material on fingertips at two ends of the cut-off leads until the surfaces of the fingertips are flush, drying to obtain a completely packaged wound dressing, and attaching one side of the completely packaged wound dressing with the substrate to an adhesive to obtain the wound dressing based on the piezoelectric effect.
Further, in the step (2), the spin coating conditions are as follows: spin-coating at a speed of 600-700 r/min for 5-10 s, and then spin-coating at a speed of 3000-400 r/min for 30-40 s; the heat treatment is carried out in a glue baking machine, the heat treatment temperature is 200-300 ℃, and the time is 10-20 min; the annealing temperature is 650-750 deg.C, and the time is 10-20 min.
Further, in the step (4), the electrode mask is purchased from Ke Bao original technologies ltd, and is an interdigital electrode mask; the target material is one or more of platinum, gold and silver; the fixation is adhesive tape fixation; the flow rate of the argon is 30-35 sccm; the sputtering time is 1-5 min; the sputtering pressure is 0.5 to 1Pa; the thickness of the electrode is as follows: 80-100 nm, the electrode finger spacing is 100-200 μm, the finger width is 100-200 μm, the effective finger length is 4-5 mm, and the number of fingers is 20-24.
Further, in the step (5), the spin coating conditions are as follows: spin-coating at a speed of 600-700 r/min for 5-10 s, and then spin-coating at a speed of 3000-4000 r/min for 30-40 s; the drying temperature is 100-120 ℃, and the drying time is 3-6 h; further, in the step (6), the voltage of the high-voltage power supply is 0.5-5 KV; the polarization time is 10-20 min; further, in the step (7), the drying temperature is 100-120 ℃, and the drying time is 3-6 h.
The beneficial technical effects of the invention are as follows:
(1) The wound dressing containing the piezoelectric material is attached to a wound, the piezoelectric material moves along with a human body, charges generated on the surface of the piezoelectric material act on a skin wound to generate electric stimulation, the effect of an endogenous electric field of the wound is enhanced, proliferation and division of fibroblasts are stimulated, the level of a receptor of a transforming growth factor beta is improved, generation of collagen and synthetic protein is promoted, differentiation of myofibroblasts, migration of keratinocyte cells, generation of blood vessels, sterilization and inflammation diminishing, and infection is reduced.
(2) The utility model discloses an use interdigital electrode and piezoelectric material to combine, interdigital electrode can be better with the material surface receive the heterogeneous electric charge collection output that produces when external force is used to the wound to the disease wound, in addition, utilize interdigital electrode to polarize piezoelectric material, make the inside electric dipole of piezoelectric material arrange along same direction, receive external force when using, the heterogeneous electric charge that produces on the wound dressing surface after the polarization is more, make the output of free radical bigger, can act on the harmful bacterium of wound more effectively, make cell membrane lipid peroxide, strengthen the permeability of cell membrane, finally lead to the leakage of intracellular protein and the irreversible damage to the bacterium, reduce the possibility that the wound infects the inflammation, reduce healing time.
(3) The wound dressing accessible piezoelectric material that this application prepared produces pulsed current along with human motion, and the pulse current through self-power production realizes real-time electro photoluminescence, and equipment is simple, and no burden is pasted and is filled with the wound surface with patient's wound, and whole wound healing process need not to dismantle, and reducible bacterial growing reduces the infection rate, shortens treatment time, and therapeutic effect is superior to ordinary dressing.
Drawings
Fig. 1 is a schematic view of a wound dressing according to the present application.
In the figure: 1 is packaging material; 2 is an electrode; 3 is a piezoelectric material; 4 is a substrate; 5 is a binder.
Fig. 2 is a schematic view of a wound dressing of the present application for treating a wound.
In the figure: 1 is piezoelectric wound dressing; 2 is a skin layer; 3 is dermis layer; 4 is a wound; 5 is endogenous electric field; and 6 is current.
Fig. 3 is a biotoxicity test chart of the wound dressing prepared in example 1.
Fig. 4 is a piezoelectric performance test chart of the wound dressing prepared in example 1.
Fig. 5 is a reactive free radical test of the wound dressing prepared in example 1.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
The following are examples of wound dressing preparations based on the piezoelectric effect, but the examples do not limit the invention.
Example 1
A wound dressing based on piezoelectric effect is prepared by the following steps:
(1) Preparing lead zirconate titanate (PZT) piezoelectric material gel by using a sol-gel method;
(2) And (2) opening a spin coater, placing a mica sheet with the thickness of 10 mu m in the spin coater, wherein the mica sheet is purchased from Thailand fluorophlogopite GmbH, taking the piezoelectric material gel prepared in the step (1) to spin-coat the surface of the mica sheet, and setting the spin-coating parameters to be 600r/min 7s and 3000r/min 30s. Then placing the mica sheet coated with PZT piezoelectric material gel in a glue baking machine for heat treatment at 300 ℃ for 10min, placing the mica sheet in a muffle furnace for high-temperature annealing at 700 ℃ for 10min to obtain a first layer of piezoelectric material;
(3) Placing the first layer of piezoelectric material prepared in the step (2) in a spin coater, and repeating the spin coating, heat treatment and high-temperature annealing process in the step (2) until the thickness of the material is 800nm;
(4) Fixing one surface, which is not coated with the piezoelectric material, of the material prepared in the step (3) on an upper target disc of a magnetic control coating system, fixing an electrode mask on the surface of the piezoelectric material, wherein the electrode mask is an interdigital electrode mask which is purchased from Ke Bao original technology limited, and the target is platinum; the target material is fixed on a lower target plate of the magnetic control coating system by using an adhesive tape, the power of the magnetic control coating system is set to be 35W, and the flow rate of argon is set to be 30sccm; the sputtering time is 2min; the sputtering pressure is 1Pa; the thickness of the electrode obtained after sputtering was 80nm, the electrode finger pitch was 200 μm, the finger width was 100 μm, the effective finger length was 4.6mm, and the number of fingers was 24.
(5) And (3) placing the wound dressing with the electrode prepared in the step (4) on a spin coater, packaging the material by using PDMS (polydimethylsiloxane) under the spin coating parameters of 600r/min 7s and 3000r/min 30s, and drying in an oven at 100 ℃ for 6h to obtain a packaging material with the thickness of 1 mu m.
(6) Taking the packaged wound dressing prepared in the step (5), removing the packaging materials on the finger tips at the two ends of the interdigital electrode, and respectively connecting a lead to the finger tips at the two ends of the electrode by using silver paste to obtain the unpolarized wound dressing; connecting the other ends of the two leads with the positive and negative electrodes of a high-voltage power supply, and applying high voltage of 800V to polarize the piezoelectric material of the wound dressing for 10min to obtain a polarized/unpolarized wound dressing;
(7) And (3) cutting off two leads on the polarized/unpolarized wound dressing prepared in the step (6), dripping a packaging material on fingertips at two ends of the cut-off leads until the surfaces of the fingertips are flush, drying for 6h in an oven at 100 ℃ to obtain a completely packaged wound dressing, and attaching one side of the completely packaged wound dressing with a mica sheet to a medical adhesive tape to obtain the wound dressing based on the piezoelectric effect.
Example 2
A wound dressing based on piezoelectric effect is prepared by the following steps:
(1) The barium titanate (BaTiO) is prepared by a sol-gel method 3 ) A piezoelectric material gel;
(2) And (2) opening a spin coater, placing a mica sheet with the thickness of 15 mu m in the spin coater, wherein the mica sheet is purchased from Thai Yuan Flugjin mica Co., ltd, taking the piezoelectric material gel prepared in the step (1) to spin-coat on the surface of the mica sheet, and setting spin-coating parameters of 700r/min 10s and 4000r/min 40s. Then spin-coated with BaTiO 3 Placing the mica sheet of the piezoelectric material gel in a glue baking machine for heat treatment at 200 ℃, placing the mica sheet in a muffle furnace after heat treatment for 20min, and annealing at 750 ℃ for 20min to obtain a first layer of piezoelectric material;
(3) Placing the first layer of piezoelectric material prepared in the step (2) in a spin coater, and repeating the spin coating, heat treatment and high-temperature annealing process in the step (2) until the thickness of the material is 1000nm;
(4) Fixing one surface, which is not coated with the piezoelectric material, of the material prepared in the step (3) on an upper target disc of a magnetic control coating system, and fixing an electrode mask on the surface of the piezoelectric material, wherein the electrode mask is an interdigital electrode mask which is purchased from Ke Bao original technology limited, and the target is gold; the target material is fixed on a lower target disc of a magnetic control coating system by using an adhesive tape, the power of the magnetic control coating system is set to be 45W, and the flow rate of argon is set to be 35sccm; the sputtering time is 5min; the sputtering pressure is 0.5Pa; the thickness of the electrode obtained after sputtering was 100nm, the electrode finger pitch was 150 μm, the finger width was 200 μm, the effective finger length was 4mm, and the number of fingers was 20.
(5) And (3) placing the wound dressing with the electrode prepared in the step (4) on a spin coater, packaging the material by using PMMA (polymethyl methacrylate) at spin coating parameters of 700r/min 10s and 4000r/min 40s, and drying in an oven at 110 ℃ for 4 hours to obtain a packaging material with the thickness of 2 mu m.
(6) Taking the packaged wound dressing prepared in the step (5), removing the packaging materials on the finger tips at the two ends of the interdigital electrode, and respectively connecting a lead to the finger tips at the two ends of the electrode by using silver paste to obtain the unpolarized wound dressing; connecting the other ends of the two leads with the positive and negative electrodes of a high-voltage power supply, and applying high voltage of 0.5KV to polarize the piezoelectric material of the wound dressing for 20min to obtain a polarized/unpolarized wound dressing;
(7) And (3) cutting off two leads on the polarized/unpolarized wound dressing prepared in the step (6), dripping a packaging material on fingertips at two ends of the cut-off leads until the surfaces of the fingertips are flush, drying the fingertips in an oven for 4 hours at 110 ℃ to obtain a completely packaged wound dressing, and attaching one side of the completely packaged wound dressing with a mica sheet to hydrogel to obtain the wound dressing based on the piezoelectric effect.
Example 3
A wound dressing based on piezoelectric effect is prepared by the following steps:
(1) Preparing polyvinylidene fluoride (PVDF) piezoelectric material gel by using a sol-gel method;
(2) And (2) opening a spin coater, placing a mica sheet with the thickness of 20 mu m in the spin coater, wherein the mica sheet is purchased from Thailand fluorophlogopite GmbH, taking the piezoelectric material gel prepared in the step (1) to spin-coat on the surface of the mica sheet, and setting spin-coating parameters of 650r/min 5s and 3500r/min 35s. Then placing the mica sheet coated with PVDF piezoelectric material gel in a glue baking machine for heat treatment at 250 ℃, placing the mica sheet in a muffle furnace after heat treatment for 15min, and annealing at 650 ℃ for 15min to obtain a first layer of piezoelectric material;
(3) Placing the first layer of piezoelectric material prepared in the step (2) in a spin coater, and repeating the spin coating, heat treatment and high-temperature annealing process in the step (2) until the thickness of the material is 1200nm;
(4) Fixing one surface, which is not coated with the piezoelectric material, of the material prepared in the step (3) on an upper target disc of a magnetic control coating system, and fixing an electrode mask on the surface of the piezoelectric material, wherein the electrode mask is an interdigital electrode mask which is purchased from Ke Bao original technology limited, and the target is silver; the target material is fixed on a lower target plate of the magnetic control coating system by using an adhesive tape, the power of the magnetic control coating system is set to be 40W, and the flow rate of argon is set to be 33sccm; the sputtering time is 1min; the sputtering pressure is 0.7Pa; the thickness of the electrode obtained after sputtering was 90nm, the electrode finger pitch was 100 μm, the finger width was 150 μm, the effective finger length was 5mm, and the number of fingers was 22.
(5) And (4) placing the wound dressing with the electrode prepared in the step (4) on a spin coater, encapsulating the material by using PDMS (polydimethylsiloxane) at the spin coating parameters of 650r/min 5s and 3500r/min 35s, and drying in an oven at 120 ℃ for 3h to obtain the encapsulating material with the thickness of 1.5 mu m.
(6) Taking the packaged wound dressing prepared in the step (5), removing the packaging materials on the finger tips at the two ends of the interdigital electrode, and respectively connecting a lead to the finger tips at the two ends of the electrode by using silver paste to obtain the unpolarized wound dressing; connecting the other ends of the two leads with the positive and negative electrodes of a high-voltage power supply, and applying high voltage of 5KV to polarize the piezoelectric material of the wound dressing for 15min to obtain a polarized/unpolarized wound dressing;
(7) And (3) cutting off two leads on the polarized/unpolarized wound dressing prepared in the step (6), dripping a packaging material on fingertips at two ends of the cut-off leads until the surfaces of the fingertips are flush, drying in an oven at 120 ℃ for 3h to obtain a completely packaged wound dressing, and attaching one side of the completely packaged wound dressing with a mica sheet to a medical adhesive tape to obtain the wound dressing based on the piezoelectric effect.
Test example:
the wound dressing based on piezoelectric effect prepared in example 1 of the present application was subjected to bactericidal performance test:
the wound dressing based on the piezoelectric effect prepared in the embodiment 1 of the application is polarized under high pressure, leads wires are respectively led to be communicated with high-voltage equipment through fingertips at two ends of an interdigital electrode, and is polarized for 10min under the high pressure of 800V, so that electric dipoles in the piezoelectric material are arranged along the same direction, and the piezoelectric performance is enhanced. The method comprises the steps of simulating a vibration environment by using an ultrasonic, placing the prepared dressing in deionized water for ultrasonic treatment, performing primary sampling by using a capillary after the ultrasonic treatment is performed for 3min, placing the sampling on an EPR (electron paramagnetic resonance spectrometer) for testing, and performing sampling after the ultrasonic treatment is performed for 5min for testing, as shown in figure 5, the wound dressing based on the piezoelectric effect prepared in the embodiment 1 of the application generates a large amount of active free radicals, and the yield of the active free radicals is gradually increased along with the prolonging of the vibration time, which shows that the wound dressing can efficiently and quickly remove bacteria at a wound by generating the active free radicals in the wound healing process, so that infection is avoided, and the performance of a polarized sample is better.
The wound dressing based on the piezoelectric effect and prepared in example 1 is placed in a culture dish containing gram-negative bacteria and gram-positive bacteria, after ultrasonic vibration is carried out for 2 hours, death of a large number of bacteria is observed, and the result is consistent with an EPR (ethylene propylene rubber) test result, and the wound dressing based on the piezoelectric effect and prepared in the application has good sterilization performance.
The wound healing effect test was performed on the wound dressing based on the piezoelectric effect prepared in example 1 of the present application:
the wound dressing based on the piezoelectric effect prepared in example 1 of the application is placed in a culture dish containing NIH-3T3 cells, the culture dish of a control group only contains the NIH-3T3 cells and does not contain the wound dressing, the two culture dishes are respectively subjected to ultrasonic treatment for one hour and then are placed in an incubator at 37 ℃ for 24 hours, and then migration, proliferation and differentiation conditions of fibroblasts of an experimental group containing the wound dressing and a control group without the wound dressing are observed under a microscope. Experiments show that the fibroblasts in the experimental group containing the wound dressing have migrated, proliferated and differentiated, which indicates that PZT can promote wound healing by inducing cell behavior.
The wound dressing based on the piezoelectric effect prepared in the embodiment 1 of the application is subjected to a biotoxicity test and a piezoelectric performance test:
and (3) biological toxicity test: the wound dressing based on piezoelectric effect prepared in example 1 of the present application and the mica sheet used in example 1 of the present application were placed in a culture dish containing fibroblasts, and cultured together with a control group containing only fibroblasts for 3 days, and the activity of the cells was observed by a confocal microscope every day. As shown in fig. 3, the cells have very good activity when cultured on mica sheets or the wound dressing based on piezoelectric effect prepared in the present application, which indicates that the wound dressing based on piezoelectric effect prepared in the present application has no biological toxicity.
And (3) testing the piezoelectric performance: the prepared wound dressing based on the piezoelectric effect is fixed on an excitation table, and the open-circuit voltage and the short-circuit current of the wound dressing based on the piezoelectric effect, which is prepared in embodiment 1 of the application, under different bending degrees are tested by setting different curvature radiuses. As shown in FIG. 4, under a bending condition having a curvature radius of 2cm, the open-circuit voltage may reach 100V and the short-circuit current may reach 0.3 μ A. This shows that the wound dressing based on piezoelectric effect prepared by the application has better piezoelectric performance.
The wound dressing based on the piezoelectric effect provided by the invention promotes the development of flexible wearable self-powered medical equipment, provides a more humanized treatment mode for chronic wound patients, promotes the healing speed of the wounds of the patients through real-time electrical stimulation, and reduces the infection risk.
The above description of embodiments should be taken as illustrative, and it will be readily understood that many variations and combinations of the features set forth above may be made without departing from the spirit and scope of the invention as set forth in the claims, and that such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such variations are intended to be included within the scope of the following claims.

Claims (6)

1. A wound dressing based on the piezoelectric effect, characterized in that the wound dressing comprises an encapsulating material, electrodes, a piezoelectric material, a substrate and an adhesive;
the piezoelectric material is one or more of an inorganic piezoelectric material and an organic piezoelectric material;
the inorganic piezoelectric material is BaTiO 3 、GaN、ZnSnO 3 One or more of ZnO, lead zirconate titanate and lead magnesium niobate; the organic piezoelectric material is one or more of polyvinylidene fluoride and polyvinylidene fluoride;
the preparation method of the wound dressing comprises the following steps:
(1) Preparing piezoelectric material gel by using a sol-gel method;
(2) Placing the substrate in a spin coater, opening the spin coater, spin-coating the piezoelectric material gel prepared in the step (1) on the surface of the substrate, performing heat treatment on the substrate spin-coated with the piezoelectric material gel, and then placing the substrate in a muffle furnace for high-temperature annealing to obtain a substrate containing a first layer of piezoelectric material;
(3) Placing the substrate containing the first layer of piezoelectric material prepared in the step (2) in a spin coater, opening the spin coater, and repeating the spin coating, heat treatment and high-temperature annealing process in the step (2) until the total thickness of the piezoelectric material spin-coated on the substrate is 800-1200 nm;
(4) Fixing one surface, which is not coated with the piezoelectric material, of the material prepared in the step (3) on an upper target disc of a magnetic control coating system, fixing an electrode mask on the surface of the piezoelectric material, fixing a target material on a lower target disc of the magnetic control coating system, setting the power of the magnetic control coating system to be 35-45W, introducing argon, opening the magnetic control coating system, and sputtering the surface of the piezoelectric material to form an electrode according to the shape of the mask to obtain the wound dressing with the electrode;
(5) After the wound dressing with the electrode prepared in the step (4) is sputtered with the surface of the electrode in a spin coating manner, drying to obtain a packaged wound dressing;
(6) Taking the packaged wound dressing prepared in the step (5), removing the packaging materials on the fingertips at the two ends of the electrode, and respectively connecting a lead to the fingertips at the two ends of the electrode by silver paste to obtain the unpolarized wound dressing; connecting the other ends of the two leads with the positive electrode and the negative electrode of a high-voltage power supply respectively, and opening the high-voltage power supply to carry out high-voltage polarization on the piezoelectric material of the wound dressing to obtain a polarized/unpolarized wound dressing;
(7) Cutting off two leads on the polarized/unpolarized wound dressing prepared in the step (6), dripping packaging materials on fingertips at two ends of the cut-off leads until the surfaces of the fingertips are flush, drying to obtain a completely packaged wound dressing, and bonding one side of the completely packaged wound dressing, which is provided with a substrate, with a bonding agent to obtain the wound dressing based on the piezoelectric effect; the thickness of the electrode is as follows: 80 to 100nm, the electrode finger spacing is 100 to 200 mu m, the finger width is 100 to 200 mu m, the effective finger length is 4 to 5mm, and the number of fingers is 20 to 24;
the packaging material is obtained by spin coating and drying a packaging raw material, and the thickness of the packaging material is 1~2 mu m; the packaging raw material is one or more of PDMS and PMMA; the electrodes are interdigital electrodes.
2. The wound dressing of claim 1, wherein the substrate is a flexible substrate; the substrate is a mica sheet, and the thickness of a single chip is 10 to 20 mu m.
3. The wound dressing of claim 1, wherein the adhesive is one or more of a medical tape, a hydrogel.
4. The wound dressing of claim 1, wherein in step (2), the spin coating conditions are: spin-coating at a speed of 600-700r/min for 5-10s, and then spin-coating at a speed of 3000-4000r/min for 30-40s; the heat treatment is carried out in a glue baking machine, the heat treatment temperature is 200 to 300 ℃, and the time is 10 to 20min; the annealing temperature is 650 to 750 ℃, and the annealing time is 10 to 20min.
5. The wound dressing of claim 1, wherein in step (4), the electrode mask is an interdigitated electrode mask; the target material is one or more of platinum, gold and silver; the fixation is adhesive tape fixation; the flow rate of the argon is 30 to 35sccm; the sputtering time is 1 to 5min; the pressure of sputtering is 0.5 to 1Pa.
6. The wound dressing of claim 1, wherein in step (5), the spin coating conditions are: spin-coating at a speed of 600-700r/min for 5-10s, and then spin-coating at a speed of 3000-4000r/min for 30-40s; the drying temperature is 100 to 120 ℃, and the drying time is 3 to 6h; in the step (6), the voltage of the high-voltage power supply is 0.5 to 5KV; the polarization time is 10 to 20min; in the step (7), the drying temperature is 100 to 120 ℃, and the drying time is 3 to 6 hours.
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CN113786282A (en) * 2021-09-15 2021-12-14 电子科技大学 Heat-activation-electricity cooperative dressing for accelerating wound healing and preparation method thereof
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