CN112388889A - Wide-range high-toughness nano conductive rubber sensor and preparation and packaging methods thereof - Google Patents
Wide-range high-toughness nano conductive rubber sensor and preparation and packaging methods thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/22—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length
- B29C43/24—Calendering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
- B29C43/18—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles incorporating preformed parts or layers, e.g. compression moulding around inserts or for coating articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/22—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length
- B29C43/28—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length incorporating preformed parts or layers, e.g. compression moulding around inserts or for coating articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/22—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length
- B29C43/30—Making multilayered or multicoloured articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/36—Moulds for making articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/56—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using mechanical means or mechanical connections, e.g. form-fits
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- 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
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
- B29C43/18—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles incorporating preformed parts or layers, e.g. compression moulding around inserts or for coating articles
- B29C2043/181—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles incorporating preformed parts or layers, e.g. compression moulding around inserts or for coating articles encapsulated
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/752—Measuring equipment
Abstract
The invention relates to the technical field of pressure measurement, and provides a wide-range high-toughness nano conductive rubber sensor and a preparation and packaging method thereof. The invention adopts a high-temperature banburying method to improve the dispersibility of the conductive filler, and the sandwich structure is cured under the high-pressure condition, so that the rubber structure is more compact; the nano conductive rubber sensor prepared by the invention has wide measurement range and good sensitivity and stability. The nano conductive rubber sensor is packaged by the rubber substrate, the rubber substrate packaged with the sensor is sealed by the shell, the cover plate and the sealing cover, the packaging structure is ingenious, the sensor can be stressed in a balanced manner, the phenomenon of structural damage caused by stress concentration is avoided, and meanwhile, the sensor integrally has excellent high-temperature resistance, water resistance, fire resistance, ultraviolet resistance, acid and alkali corrosion resistance and the like due to the packaging of the rubber substrate, so that the nano conductive rubber sensor has better aging resistance stability and longer service life and safety under the high-load condition.
Description
Technical Field
The invention relates to the technical field of pressure measurement, in particular to a wide-range high-toughness nano conductive rubber sensor and a preparation and packaging method thereof.
Background
The nanometer conductive rubber is a composite material with conductive performance obtained by doping nanometer conductive filler into an insulating polymer matrix, has good piezoresistive property, durability and flexibility, and has wide application in the pressure sensing field.
In the existing preparation process of the nanometer conductive rubber, the conductive filler is difficult to be uniformly dispersed in the rubber polymer, so that the seepage threshold can be reached only by adding a large amount of conductive filler, and the increase of the conductive filler can cause the deterioration of the strength, resilience and the like of the rubber, thereby further influencing the measurement range, sensitivity and the like of the sensor; and the pressure resistance, stability and the like of the nano conductive rubber prepared by the traditional method are also to be improved.
The traditional nanometer conductive rubber sensor has poor pressure resistance, so the test range is narrow, and the pressure test range is mostly distributed between 0-2 MPa. Aiming at few parts of large-range conductive rubber sensors, the problems of packaging structure design can not effectively offset the internal stress of the sensors, so that the local stress is concentrated, the structure of the sensors is easy to damage, and the service stability and the service life of the sensors are greatly influenced. The problems severely limit the application of the nano conductive rubber sensor in the aspects of building engineering, bridge engineering, internet of things, intelligent wearing, medical health and the like.
Disclosure of Invention
In view of the above, the invention provides a wide-range high-toughness nano conductive rubber sensor and preparation and packaging methods thereof. The nano conductive rubber sensor prepared by the invention has the advantages of good toughness, good sensitivity and stability and large test range, and the packaging method provided by the invention has a skillful packaging structure, can enable the whole stress of the sensor to be more balanced, and improves the service life and fatigue stability of the sensor.
In order to achieve the above object, the present invention provides the following technical solutions:
a preparation method of a wide-range high-toughness nano conductive rubber sensor comprises the following steps:
mixing a rubber matrix material and a nano conductive filler for high-temperature banburying to obtain a mixture;
mixing the mixture and a vulcanizing agent for low-temperature banburying to obtain a nano conductive rubber material;
carrying out calendering and thin-passing treatment on the nano conductive rubber material to obtain a calendered sheet;
respectively spreading a layer of conductive film material on the upper surface and the lower surface of the rolled sheet as an electrode, and then performing rolling and thin-passing treatment to obtain a sandwich structure;
carrying out hot-pressing curing treatment on the sandwich structure to obtain a nano conductive rubber sensor;
wherein the temperature of high-temperature banburying is 80-120 ℃; the temperature of the low-temperature banburying is 25-60 ℃; the pressure of the hot-pressing curing treatment is 5-25 MPa.
Preferably, the high-temperature banburying comprises a first banburying step and a second banburying step, wherein the first banburying step is carried out at a rotating speed of 20-50 rpm for 5-30 min, and the second banburying step is carried out at a rotating speed of 25-30 rpm for 5-10 min;
the low-temperature banburying time is 5-20 min, and the rotating speed is 20-45 rpm;
the temperature of the hot-pressing curing treatment is 150-185 ℃, and the time is 5-10 min.
Preferably, the rubber base material comprises polydimethylsiloxane, gas-phase silica gel, liquid silica gel, nitrile rubber, ethylene propylene diene monomer or polyurethane elastomer; the vulcanizing agents comprise a bis-25 vulcanizing agent and/or a bis-24 vulcanizing agent; the nano conductive filler comprises one or more of superconducting carbon black, conductive carbon nano tubes and conductive graphene;
the rubber matrix material, the nano conductive filler and the vulcanizing agent are 100% by total mass, the nano conductive filler is 6-7.5% by mass, and the vulcanizing agent is 1-1.2% by mass.
Preferably, the conductive film material further comprises, before being laid flat: and carrying out coupling agent wetting treatment on the conductive film material.
Preferably, the thickness of the rolled sheet is 0.5-2 mm; the thickness of the conductive film material is 0.02-0.05 mm, and the thickness of the sandwich structure is 0.2-2.5 mm.
The invention also discloses a wide-range high-toughness nano conductive rubber sensor prepared by the preparation method in the scheme, which comprises nano conductive rubber and electrodes respectively arranged on the upper surface and the lower surface of the nano conductive rubber.
The invention also provides a packaging method of the wide-range high-toughness nano conductive rubber sensor, which comprises the following steps of:
(1) providing a shell, wherein the shell is a hollow cylinder with an open top, a circle of threads are arranged at the top of the outer side of the shell, and a through hole is formed in the side wall of the shell;
providing a hot-pressing forming die, wherein the hot-pressing forming die is of a three-layer cylinder structure, the centers of three layers of cylinders in the three-layer cylinder structure are the same and are mutually connected, the diameters of the three layers of cylinders are sequentially reduced from top to bottom, and the diameter of the cylinder at the lowest layer is smaller than the inner diameter of the shell;
mixing a rubber base material and a vulcanizing agent, putting the mixture into a shell, pressurizing the mixture in the shell by using a hot-pressing forming die to perform hot-pressing curing treatment, and then removing the hot-pressing forming die to form a rubber concave cavity in the shell;
(2) respectively connecting electrodes on the upper surface and the lower surface of the nano conductive rubber sensor of claim 6 with leads, then placing the electrodes into the rubber cavity, leading the other end of the lead out of the through hole on the side wall of the shell, filling the shell with a mixture of a rubber base material and a vulcanizing agent, and then carrying out hot-pressing vulcanization packaging to obtain a packaging piece;
(3) providing a cover plate, wherein the longitudinal section of the cover plate is in a convex shape, and the bottom size of the cover plate is matched with the inner diameter of the shell;
providing a sealing cover, wherein the bottom of the sealing cover is open, the top of the sealing cover is provided with an open tubular structure, and the inner side wall of the sealing cover is provided with threads; the size of the opening at the top is matched with the size of the upper part of the cover plate; the size of the sealing cover is matched with that of the shell;
the cover plate is placed on the top of the package, the top opening of the sealing cover is penetrated through the upper part of the cover plate, and the sealing cover and the shell are fastened by screw threads.
Preferably, the temperature of the hot-pressing curing treatment in the step (1) is 150-185 ℃, the pressure is 5-25 MPa, and the time is 15 min.
Preferably, the temperature of the hot-pressing vulcanization packaging is 90-280 ℃, and the pressure is 2-25 MPa.
Preferably, a buffer pad is further disposed at a contact portion between the sealing cover and the cover plate.
The invention provides a preparation method of a wide-range high-toughness nano conductive rubber sensor, which comprises the steps of mixing a rubber matrix material and a nano conductive filler for high-temperature banburying, mixing the obtained mixture with a vulcanizing agent for low-temperature banburying to obtain a nano conductive rubber material; and carrying out calendering and thin-passing treatment on the nano conductive rubber material, then respectively paving a layer of conductive film material on the upper surface and the lower surface of the calendered sheet to be used as an electrode, then carrying out calendering and thin-passing treatment to obtain a sandwich structure, and finally carrying out hot-pressing curing treatment on the sandwich structure to obtain the nano conductive rubber sensor. According to the invention, the rubber matrix material and the nano conductive filler are mixed by a high-temperature banburying method, the rubber matrix material keeps higher fluidity at high temperature and can be fully contacted with the nano conductive filler, so that the dispersion degree of the nano conductive filler is higher, when the mass fraction of the nano conductive filler is 6.2%, the percolation threshold can be reached, and the conductivity of the nano conductive rubber is obviously increased; the method provided by the invention can increase the dispersion degree of the conductive filler, so that the using amount of the conductive filler is reduced, the content of the conductive filler is less, the permanent deformation of the obtained nano conductive rubber is minimum, the mechanical strength and the resilience performance are better, the obtained nano conductive rubber sensor can keep a wider pressure test range, and meanwhile, the nano conductive rubber sensor has better linearity, sensitivity and stability.
In addition, the sandwich structure is subjected to hot-pressing curing under a higher pressure condition (5-25 MPa), and the nano conductive rubber is vulcanized and formed under high pressure, so that the rubber structure is more compact, the high pressure resistance of the nano conductive rubber sensor is improved, the structural stability of the nano conductive rubber sensor is improved, and the service life of the nano conductive rubber sensor is prolonged.
Furthermore, the conductive film material is subjected to coupling agent wetting treatment before use, so that the bonding force between the conductive film material and rubber is enhanced, and the structural stability of the sensor is further ensured.
The invention also provides a wide-range high-toughness nano conductive rubber sensor prepared by the preparation method in the scheme, which comprises nano conductive rubber and electrodes arranged on the upper surface and the lower surface of the nano conductive rubber. The nano conductive rubber sensor provided by the invention has the advantages of wide measuring range, good toughness, and good linearity and sensitivity.
The invention also provides a packaging method of the wide-range high-toughness nano conductive rubber sensor, the packaging structure of the packaging method provided by the invention is ingenious, the sensor is packaged in the center of the rubber matrix, the rubber matrix can play a role of a buffer layer, so that the stress of the sensor is balanced, the phenomenon of structural damage caused by stress concentration is avoided, and meanwhile, the rubber matrix packaging enables the whole sensor to have excellent performances of high temperature resistance, water resistance, fire resistance, ultraviolet resistance, acid and alkali corrosion resistance and the like, so that the sensor has better aging resistance stability, and has longer service life and safety under a high load condition.
In addition, the packaging method provided by the invention also utilizes the shell, the cover plate and the sealing cover to seal the rubber matrix wrapped with the sensor, wherein the shell is wrapped on the outer side of the rubber matrix to play a role in protecting the rubber matrix; according to the invention, through the design of the shell, the cover plate and the sealing cover, the packaged sensor has stronger capacity of resisting external interference and corrosion, the stress of the conductive rubber is more balanced in a pressure cycle test, the conductive rubber has the capacity of recovering elastic compression deformation more quickly, the permanent deformation is reduced, the piezoelectric signal response frequency is higher, the baseline drift phenomenon cannot occur in the cycle test, and the sensor has longer service life and better fatigue stability.
The embodiment result shows that the measurement range of the nano conductive rubber sensor provided by the invention is 0-40 MPa, the current signal of the sensor is stable in multiple pressure cycle loading tests, the sensitivity is high, and the baseline drift phenomenon does not occur.
Drawings
FIG. 1 is a schematic structural view of a mold used in a process of thermocompression curing a sandwich structure according to an embodiment of the present invention;
FIG. 2 is a schematic structural view of a housing used in an embodiment of the present invention;
FIG. 3 is a schematic structural view of a hot press molding die used in an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of a cover plate used in an embodiment of the present invention;
FIG. 5 is a schematic view showing the structure of a sealing cap used in the embodiment of the present invention;
FIG. 6 is a schematic structural diagram of a packaged structure of a nano-conductive sensor according to the present invention; in fig. 6: 1-nanometer conductive rubber, 2-conductive film material, 3-lead, 4-shell, 5-rubber base, 6-top cover, 7-sealing cover and 8-buffer pad;
FIG. 7 is a schematic flow chart of the fabrication and packaging of a wide-range high-toughness nano conductive rubber sensor according to an embodiment of the present invention;
FIG. 8 is a graph showing the variation of the current signal with pressure of the sensor in embodiment 1 of the present invention;
FIG. 9 is a graph showing the change in current under cyclic loading pressure conditions of the sensor in example 1 of the present invention;
FIG. 10 is a graph showing the variation of the resistivity of the nano conductive rubber with the amount of the nano conductive filler added in example 3 of the present invention.
Detailed Description
The invention provides a preparation method of a wide-range high-toughness nano conductive rubber sensor, which comprises the following steps of:
mixing a rubber matrix material and a nano conductive filler for high-temperature banburying to obtain a mixture;
mixing the mixture and a vulcanizing agent for low-temperature banburying to obtain a nano conductive rubber material;
carrying out calendering and thin-passing treatment on the nano conductive rubber material to obtain a calendered sheet;
respectively spreading a layer of conductive film material on the upper surface and the lower surface of the rolled sheet as an electrode, and then performing rolling and thin-passing treatment to obtain a sandwich structure;
and carrying out hot-pressing curing treatment on the sandwich structure to obtain the nano conductive rubber sensor.
The invention mixes the rubber matrix material and the nanometer conductive filler for high-temperature banburying to obtain the mixture. In the present invention, the rubber base material preferably includes Polydimethylsiloxane (PDMS), fumed silica, Liquid Silica (LSR), nitrile rubber (NBR), Ethylene Propylene Diene Monomer (EPDM), or polyurethane elastomer (TPU), and in the specific embodiment of the present invention, the fumed silica is preferably GS-1050u in type; the rubber matrix materials selected by the invention are high-toughness rubber with higher mechanical property, bubbles are not easy to appear in the rubber matrix materials in the preparation process, and the conductive filler is easier to disperse uniformly.
In the invention, the nano conductive filler preferably comprises one or more of superconducting carbon black, conductive carbon nano tubes and conductive graphene; the temperature of the high-temperature banburying is 80-120 ℃, and preferably 90-110 ℃; the high-temperature banburying preferably comprises a first banburying step and a second banburying step, wherein the rotation speed of the first banburying step is preferably 20-50 rpm, more preferably 40rpm, the time is preferably 5-30 min, more preferably 10min, the rotation speed of the second banburying step is preferably 25-30 rpm, more preferably 26-28 rpm, the time is preferably 5-10 min, more preferably 6-8 min, and the temperature of the first banburying step and the temperature of the second banburying step are preferably the same; the invention reduces the banburying time and improves the dispersion uniformity of the nano conductive filler by banburying step by step.
After the mixture is obtained, the mixture and a vulcanizing agent are mixed and subjected to low-temperature banburying to obtain the nano conductive rubber material. In the present invention, the vulcanizing agents preferably include bis-25 vulcanizing agents and/or bis-24 vulcanizing agents; the rubber matrix material, the nano conductive filler and the vulcanizing agent are 100% by total mass, the mass percentage of the nano conductive filler is preferably 6-7.5%, more preferably 6.5-7%, and the mass percentage of the vulcanizing agent is preferably 1-1.2%, more preferably 1.1%. In the invention, the temperature of the low-temperature banburying is preferably 25-60 ℃, more preferably 40 ℃, the rotating speed of the low-temperature banburying is preferably 10rpm, and the time is preferably 5 min.
After the nano conductive rubber material is obtained, the invention carries out first calendering and thin passing treatment on the nano conductive rubber material to obtain a calendered sheet. In the invention, the thickness of the rolled sheet is preferably 0.5-2 mm, and more preferably 1-1.5 mm; the invention has no special requirements on the specific conditions of the calendering and thinning treatment, and can obtain the calendered sheet with the required thickness. The shape and area of the rolled sheet are not particularly required, and the rolled sheet can be arranged according to the shape and area of a target sensor.
After obtaining the rolled sheet, the invention respectively and flatly lays a layer of conductive film material on the upper surface and the lower surface of the rolled sheet to be used as electrodes, and then carries out rolling and thin passing treatment to obtain the sandwich structure. In the invention, the conductive film material is preferably copper foil, zinc foil, aluminum foil, copper mesh or conductive fabric; the conductive fabric is preferably silver-plated fiber fabric; the thickness of the conductive film material is preferably 0.02 mm-0.05 mm, and more preferably 0.03-0.04 mm; before the conductive film material is laid flatly, the method also comprises the step of carrying out coupling agent wetting treatment on the conductive film material; the coupling agent used for the wetting treatment of the coupling agent is preferably one or more of KH560, KH550 and KH 570; the invention has no special requirements on the specific method of the coupling agent wetting treatment, and the surface of the conductive film material can be wetted by using the coupling agent; the invention can improve the binding force between the conductive film material and the rubber through the wetting treatment of the coupling agent.
In the invention, the thickness of the sandwich structure is preferably 0.2-2.5 mm, and more preferably 0.5-2 mm; the invention has no special requirements on the specific conditions of the calendering and thin passing treatment, and can obtain a sandwich structure with required thickness.
After the sandwich structure is obtained, the invention carries out hot-pressing solidification treatment on the sandwich structure to obtain the nano conductive rubber sensor. In the invention, the pressure of the hot-pressing curing treatment is 5-25 MPa, preferably 10-20 MPa, the temperature of the hot-pressing curing is preferably 150-185 ℃, more preferably 155-180 ℃, and the time is preferably 15 min; in a specific embodiment of the present invention, a schematic structural diagram of the mold for performing the hot press curing of the sandwich structure is shown in fig. 1, and units of each dimension in fig. 1 are mm. In the hot-press curing process, the rubber matrix is vulcanized and molded to form a compact rubber structure, and the hot-press curing is carried out under the high-pressure condition, so that the obtained rubber has a more compact structure, better pressure resistance and structural stability and longer service life.
The invention also provides a wide-range high-toughness nano conductive rubber sensor prepared by the preparation method in the scheme, which comprises nano conductive rubber and electrodes respectively arranged on the upper surface and the lower surface of the nano conductive rubber; the nano conductive rubber sensor is wide in measuring range (0-40 MPa), good in toughness (the elongation at break is 500% and the tensile strength is 13MPa), and good in linearity and sensitivity.
The invention also provides a packaging method of the wide-range high-toughness nano conductive rubber sensor, which comprises the following steps of:
(1) providing a shell, wherein the shell is a hollow cylinder with an open top, a circle of threads are arranged at the top of the outer side of the shell, and a through hole is formed in the side wall of the shell;
providing a hot-pressing forming die, wherein the hot-pressing forming die is of a three-layer cylinder structure, the centers of three layers of cylinders in the three-layer cylinder structure are the same and are mutually connected, the diameters of the three layers of cylinders are sequentially reduced from top to bottom, and the diameter of the cylinder at the lowest layer is smaller than the inner diameter of the shell;
mixing a rubber base material and a vulcanizing agent, putting the mixture into a shell, pressurizing the mixture in the shell by using a hot-pressing forming die to perform hot-pressing curing treatment, and then removing the hot-pressing forming die to form a rubber concave cavity in the shell;
(2) connecting electrodes on the upper surface and the lower surface of the nano conductive rubber sensor in the scheme with a lead, then placing the lead into the rubber cavity, leading the other end of the lead out of a through hole on the side wall of the shell, filling the shell with a mixture of a rubber base material and a vulcanizing agent, and then carrying out hot-pressing vulcanization packaging to obtain a packaging piece;
(3) providing a cover plate, wherein the longitudinal section of the cover plate is in a convex shape, and the bottom size of the cover plate is matched with the inner diameter of the shell;
providing a sealing cover, wherein the bottom of the sealing cover is open, the top of the sealing cover is provided with an open tubular structure, and the inner side wall of the sealing cover is provided with threads; the size of the opening at the top is matched with the size of the upper part of the cover plate; the size of the sealing cover is matched with that of the shell;
the cover plate is placed on the top of the package, the top opening of the sealing cover is penetrated through the upper part of the cover plate, and the sealing cover and the shell are fastened by screw threads.
The invention firstly provides a shell and a hot-press forming die. In the invention, the shell is a hollow cylinder with an open top, the top of the outer side of the shell is provided with a circle of threads, and the side wall of the shell is provided with a through hole; the thickness of the shell is preferably 2 mm; the invention has no special requirements on the size and the position of the through hole, and the lead can be led out.
In the invention, the hot-press forming die is of a three-layer cylinder structure, the centers of three layers of cylinders in the three-layer cylinder structure are the same and are connected with each other, the diameters of the three layers of cylinders are sequentially reduced from top to bottom, and the diameter of the cylinder at the lowest layer is smaller than the inner diameter of the shell; the invention has no special requirement on the height of the three-layer cylinder and can be arranged according to the shape of the rubber concave cavity; in the present invention, the hot press molding die is preferably a solid structure.
In the present invention, the housing and the hot press molding die are preferably made of stainless steel.
The invention has no special requirements on the specific sizes of the shell and the hot-press forming die, and the specific sizes are set according to the size of the sensor to be packaged; in a specific embodiment of the present invention, a schematic structural diagram of the housing is shown in fig. 2, wherein an outer diameter of the housing is 20mm, an inner diameter is 16mm, a height is 12mm, a thickness of the housing is 2mm, a diameter of a hole on a side wall is 1.5mm, a thread specification is M20 × 1.5, and a thread depth is 6.4 mm; the structural schematic diagram of the hot-press forming die is shown in fig. 3, wherein the diameter of the topmost cylinder is 25mm, the diameter of the middle cylinder is 15.92mm, and the diameter of the bottommost cylinder is 14 mm.
After the shell and the die are provided, the rubber matrix material and the vulcanizing agent are mixed and then are placed into the shell, the hot-press forming die is used for pressurizing the mixture in the shell for hot-press curing, and then the hot-press forming die is removed, so that a rubber concave cavity is formed in the shell. In the invention, the type of the rubber base material is preferably consistent with the rubber base material used for preparing the nano conductive rubber sensor in the scheme; the mechanical properties of the same rubber base material are similar, the rubber base and the nano conductive rubber sensor have synchronous stress contraction ratios after being packaged, the structural damage caused by unbalanced stress in the sensor is avoided, and the sensitivity and the consistency of the sensor can be improved; the addition amount of the vulcanizing agent is 0.8-1.2% of the mass of the rubber base material; the optional types of the vulcanizing agents are consistent with the scheme, and are not described again; the mixing method of the rubber matrix material and the vulcanizing agent has no special requirement, and the rubber matrix material and the vulcanizing agent can be uniformly mixed by using a mixing method well known by the technical personnel in the field.
In the invention, the temperature of the hot-pressing curing treatment is preferably 150-185 ℃, more preferably 155-180 ℃, the pressure is preferably 5-25 MPa, more preferably 10-20 MPa, and the time is preferably 15 min.
In the invention, the size of the rubber concave cavity is matched with the nano conductive rubber sensor, so that the nano conductive rubber sensor can be placed in the concave cavity conveniently.
After the rubber concave cavity is formed, the electrodes on the upper surface and the lower surface of the nano conductive rubber sensor are connected with the conducting wire, then the conducting wire is placed into the rubber concave cavity, the other end of the conducting wire is led out from the hole in the side wall of the shell, the shell is filled with a mixture of a rubber base material and a vulcanizing agent, and then hot-pressing vulcanization packaging is carried out to obtain the packaging piece. In the invention, the types of the rubber matrix material and the vulcanizing agent are consistent with those in the step (1), and the description is omitted; the temperature of the hot-pressing vulcanization packaging is preferably 90-280 ℃, more preferably 110-260 ℃, the pressure is preferably 2-25 MPa, more preferably 4-22 MPa, and the time is preferably 7-15 min; in the invention, the hot-press vulcanization packaging method is particularly preferably flat-plate hot-press vulcanization; after the hot-pressing vulcanization packaging is finished, the rubber base material in the shell is vulcanized and molded, the nano conductive rubber sensor is completely packaged in the rubber base, and the rubber base plays a role of a buffer layer; in the invention, the thickness of the rubber matrix is preferably 4-6 mm; the position of the nano conductive rubber sensor is preferably the center of the rubber substrate.
The invention provides a cover plate and a sealing cover. In the invention, the longitudinal section of the cover plate is in a convex shape, and the bottom size of the cover plate is matched with the inner diameter of the shell; the bottom of the cover plate is specifically the end with larger size, and the top of the cover plate is specifically the end with smaller size; the sealing cover is of a cylindrical structure with an opening at the bottom and an opening at the top, and threads are arranged on the inner side wall of the sealing cover; the size of the opening of the top part is matched with the size of the upper part of the cover plate, so that the upper part of the cover plate can pass through the opening; the size of the sealing cover is matched with that of the shell. In the present invention, the cover plate and the sealing cover are preferably made of stainless steel. The invention has no special requirement on the specific size of the cover plate and the sealing cover, and the cover plate and the sealing cover are arranged according to the size of the shell. In one embodiment of the present invention, the structure of the cover plate is schematically shown in fig. 4, wherein the diameter of the bottom of the cover plate is 15.94mm, the diameter of the top is 10mm, the thickness of the bottom is 2mm, and the thickness of the top is 4.5mm, and the structure of the sealing cover is schematically shown in fig. 5, wherein the diameter of the sealing cover is 24mm, the diameter of the opening is 10.1mm, the thickness of the sealing cover is 2mm, the length of the side wall is 6mm, the thread specification is M20 × 1.5, and the thread depth is 6 mm.
After the package is obtained, the invention places the cover plate on the top of the package, then the top opening of the sealing cover passes through the upper part of the cover plate, and the sealing cover and the shell are fastened by screw threads. In the invention, the top of the cover plate extends out of the opening of the sealing cover, when pressure test is carried out, the top of the cover plate is directly pressurized, the arrangement of the cover plate can enlarge the test range and reserve space for the compression deformation of the nano rubber sensor; the sealing cover can fix the cover plate to prevent bias. In the invention, the contact part of the sealing cover and the cover plate is preferably provided with a buffer pad; the invention does not require a special buffer pad, and the buffer pad known to those skilled in the art can be used.
The structure schematic diagram of the nano conductive sensor packaging structure obtained after packaging is shown in fig. 6, wherein 1-nano conductive rubber, 2-conductive film material, 3-lead, 4-shell, 5-rubber matrix, 6-top cover, 7-sealing cover and 8-cushion pad.
The schematic flow diagram of the preparation and packaging of the large-range high-toughness nano conductive rubber sensor in the embodiment of the invention is shown in fig. 7, wherein a rubber base material and a nano conductive filler are subjected to high-temperature banburying, then a vulcanizing agent is added for low-temperature banburying, then calendering and thin-passing are carried out to obtain a calendering sheet, a conductive film material is arranged on the upper surface and the lower surface of the calendering sheet, then calendering and thin-passing are carried out again to obtain a sandwich structure, and then the nano conductive rubber sensor is obtained through hot-pressing curing treatment; in the shell, a rubber cavity is formed by matching a rubber base material with a hot-press forming die, then a nano conductive rubber sensor, a connecting wire and a rubber base material are placed in the rubber cavity, the nano conductive sensor is packaged in the rubber base body through hot-press vulcanization, and finally the packaging part is sealed through a cover plate and a sealing cover.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
Preparing a nano conductive rubber sensor:
the rubber base material comprises 100 parts by mass of high-strength gas-phase silica gel GS-1050u, 7.8 parts by mass of nano conductive filler and 7.78 parts by mass of vulcanizing agent bis-250.6; the conductive film material is silver-plated fiber fabric, and the thickness is 0.02 mm;
mixing the rubber matrix material and the nano conductive filler for high-temperature banburying at 120 ℃, firstly banburying at 40rpm for 10min, and then banburying at 20rpm for 5min to obtain a mixture;
mixing the mixture and a vulcanizing agent for banburying at a low temperature of 40 ℃, at a rotating speed of 40rpm for 5min to obtain a nano conductive rubber material;
carrying out calendering and thin-passing treatment on the nano conductive rubber material to obtain a calendered sheet with the thickness of 1.5 mm;
respectively spreading a layer of conductive film material on the upper surface and the lower surface of the rolled sheet as electrodes, and then performing rolling and thin-passing treatment to obtain a sandwich structure with the thickness of 2.1 mm;
and (2) carrying out hot-pressing curing treatment on the sandwich structure in a mould shown in figure 1 at 175 ℃, under 15MPa for 15min to obtain the nano conductive rubber sensor, and testing to obtain the nano conductive rubber sensor with the breaking elongation of 500%, the tensile strength of 13MPa and the tearing strength of 30N/mm, which indicates that the obtained nano conductive rubber sensor has the characteristic of high toughness.
Packaging of the sensor:
providing a shell, wherein the structure is shown in figure 2, the structure of the hot-press forming die is shown in figure 3, the structure of the cover plate is shown in figure 4, the structure of the sealing cover is shown in figure 5, and the shell, the hot-press forming die, the cover plate and the sealing cover are all made of stainless steel; the rubber base material for packaging is gas-phase silica gel GS-1050u, the vulcanizing agent is bis-25, and the addition amount of the vulcanizing agent is 1% of the mass of the gas-phase silica gel; the wire is a red copper enameled wire.
Mixing a rubber base material and a vulcanizing agent, putting the mixture into a shell, pressurizing the mixture in the shell by using a hot-press forming die to carry out hot-press curing treatment, wherein the temperature is 175 ℃, the pressure is 10MPa, and the time is 10min, and then removing the hot-press forming die to form a rubber concave cavity in the shell;
connecting electrodes on the upper surface and the lower surface of the nano conductive rubber sensor with a lead, then placing the lead into a rubber cavity, leading the other end of the lead out of a hole on the side wall of a shell, filling a mixture of a rubber base material and a vulcanizing agent in the shell, and then carrying out hot-pressing vulcanization packaging at 175 ℃, under 10MPa for 10min to obtain a packaging piece;
and placing a cover plate on the top of the packaging part, then enabling the top opening of the sealing cover to penetrate through the upper part of the cover plate, and fastening the sealing cover and the shell through threads to obtain the sensor packaging structure.
And (3) performance testing:
applying pressure to the sensor packaging structure at the top of the cover plate, connecting a lead with a paperless recorder, collecting current change inside the sensor under different pressure conditions, wherein the current signal of the sensor along with the change of the pressure is shown in fig. 8; fig. 8 shows the pressure applied to the sensor package on the left and the change in the electrical signal of the sensor under pressurized conditions on the right. As can be seen from fig. 8, the variation trend of the sensor electrical signal is the same as the variation trend of the pressurizing pressure, and the current intensity is relatively large, which indicates that the sensor provided by the present invention has high sensitivity and accurate test result.
A cyclic loading pressure of 40MPa is applied to the cover plate of the sensor package structure, the sensor wire is connected to a paperless recorder and the current change of the sensor is recorded, and the obtained result is shown in fig. 9. According to fig. 9, it can be seen that after pressure is applied, the sensor generates a strong current signal, the sensitivity is high, and in the process of circularly applying pressure, the stability of the sensor is good, and the baseline drift phenomenon is avoided.
Example 2
Preparing a nano conductive rubber sensor:
the other conditions are the same as the example 1, only the dosage of the gas-phase silica gel GS-1050u is changed to 70 parts, the dosage of the superconducting carbon black is changed to 5.0 parts, and the dosage of the vulcanizing agent is changed to 0.6 part; the conductive film material is changed into copper foil, and the thickness is 0.05 mm;
packaging of the sensor:
other conditions were the same as in example 1 except that the temperature for curing the package was changed to 180 ℃.
The resulting sensor package was subjected to performance testing in the same manner as in example 1, and the results were similar to those of example 1.
Example 3
The preparation process of the nano conductive rubber sensor is the same as that of the embodiment 2, and only the adding amounts of the superconducting carbon black are respectively controlled to be 4.0 parts, 4.5 parts, 4.6 parts, 4.7 parts, 4.85 parts, 5.0 parts, 5.5 parts and 6.0 parts.
The obtained nano conductive rubber was tested for resistivity, and the obtained results are shown in fig. 10. As can be seen from fig. 10, when the amount of the conductive filler added is 6.2%, the percolation threshold can be reached, which shows that the method of the present invention can highly disperse the conductive filler, and the percolation threshold can be reached at a low amount of the conductive filler added.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a wide-range high-toughness nano conductive rubber sensor is characterized by comprising the following steps:
mixing a rubber matrix material and a nano conductive filler for high-temperature banburying to obtain a mixture;
mixing the mixture and a vulcanizing agent for low-temperature banburying to obtain a nano conductive rubber material;
carrying out calendering and thin-passing treatment on the nano conductive rubber material to obtain a calendered sheet;
respectively spreading a layer of conductive film material on the upper surface and the lower surface of the rolled sheet as an electrode, and then performing rolling and thin-passing treatment to obtain a sandwich structure;
carrying out hot-pressing curing treatment on the sandwich structure to obtain a nano conductive rubber sensor;
wherein the temperature of high-temperature banburying is 80-120 ℃; the temperature of the low-temperature banburying is 25-60 ℃; the pressure of the hot-pressing curing treatment is 5-25 MPa.
2. The preparation method according to claim 1, wherein the high-temperature banburying comprises a first banburying step and a second banburying step, wherein the first banburying step is performed at a rotating speed of 20-50 rpm for 5-30 min, and the second banburying step is performed at a rotating speed of 25-30 rpm for 5-10 min;
the low-temperature banburying time is 5-20 min, and the rotating speed is 20-45 rpm;
the temperature of the hot-pressing curing treatment is 150-185 ℃, and the time is 5-10 min.
3. The method of claim 1, wherein the rubber base material comprises polydimethylsiloxane, fumed silica, liquid silica, nitrile rubber, ethylene propylene diene monomer rubber, or polyurethane elastomer; the vulcanizing agents comprise a bis-25 vulcanizing agent and/or a bis-24 vulcanizing agent; the nano conductive filler comprises one or more of superconducting carbon black, conductive carbon nano tubes and conductive graphene;
the rubber matrix material, the nano conductive filler and the vulcanizing agent are 100% by total mass, the nano conductive filler is 6-7.5% by mass, and the vulcanizing agent is 1-1.2% by mass.
4. The method of claim 1, wherein the conductive film material further comprises, before the tiling: and carrying out coupling agent wetting treatment on the conductive film material.
5. The production method according to claim 1, wherein the thickness of the rolled sheet is 0.5 to 2 mm; the thickness of the conductive film material is 0.02-0.05 mm, and the thickness of the sandwich structure is 0.2-2.5 mm.
6. The wide-range high-toughness nano conductive rubber sensor prepared by the preparation method of any one of claims 1 to 5 comprises nano conductive rubber and electrodes respectively arranged on the upper surface and the lower surface of the nano conductive rubber.
7. A packaging method of a wide-range high-toughness nano conductive rubber sensor is characterized by comprising the following steps:
(1) providing a shell, wherein the shell is a hollow cylinder with an open top, a circle of threads are arranged at the top of the outer side of the shell, and a through hole is formed in the side wall of the shell;
providing a hot-pressing forming die, wherein the hot-pressing forming die is of a three-layer cylinder structure, the centers of three layers of cylinders in the three-layer cylinder structure are the same and are mutually connected, the diameters of the three layers of cylinders are sequentially reduced from top to bottom, and the diameter of the cylinder at the lowest layer is smaller than the inner diameter of the shell;
mixing a rubber base material and a vulcanizing agent, putting the mixture into a shell, pressurizing the mixture in the shell by using a hot-pressing forming die to perform hot-pressing curing treatment, and then removing the hot-pressing forming die to form a rubber concave cavity in the shell;
(2) respectively connecting electrodes on the upper surface and the lower surface of the nano conductive rubber sensor of claim 6 with leads, then placing the electrodes into the rubber cavity, leading the other end of the lead out of the through hole on the side wall of the shell, filling the shell with a mixture of a rubber base material and a vulcanizing agent, and then carrying out hot-pressing vulcanization packaging to obtain a packaging piece;
(3) providing a cover plate, wherein the longitudinal section of the cover plate is in a convex shape, and the bottom size of the cover plate is matched with the inner diameter of the shell;
providing a sealing cover, wherein the bottom of the sealing cover is open, the top of the sealing cover is provided with an open tubular structure, and the inner side wall of the sealing cover is provided with threads; the size of the opening at the top is matched with the size of the upper part of the cover plate; the size of the sealing cover is matched with that of the shell;
the cover plate is placed on the top of the package, the top opening of the sealing cover is penetrated through the upper part of the cover plate, and the sealing cover and the shell are fastened by screw threads.
8. The packaging method according to claim 7, wherein the temperature of the thermosetting treatment in step (1) is 150 to 185 ℃, the pressure is 5 to 25MPa, and the time is 15 min.
9. The packaging method according to claim 7, wherein the temperature of the hot-press vulcanization packaging is 90-280 ℃ and the pressure is 2-25 MPa.
10. The method of claim 7, wherein a cushion is further provided at a portion where the sealing cover contacts the cover plate.
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| CN202011143979.XA CN112388889B (en) | 2020-10-23 | 2020-10-23 | Wide-range high-toughness nano conductive rubber sensor and preparation and packaging methods thereof |
| PCT/CN2021/120847 WO2022083415A1 (en) | 2020-10-23 | 2021-09-27 | Wide-range high-toughness nano-conductive rubber sensor, and preparation and packaging methods therefor |
| ZA2022/10850A ZA202210850B (en) | 2020-10-23 | 2022-09-30 | Wide-range high-toughness nano-conductive rubber sensor, and preparation and packaging methods therefor |
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| CN202011143979.XA CN112388889B (en) | 2020-10-23 | 2020-10-23 | Wide-range high-toughness nano conductive rubber sensor and preparation and packaging methods thereof |
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| WO2022083415A1 (en) * | 2020-10-23 | 2022-04-28 | 深圳市市政设计研究院有限公司 | Wide-range high-toughness nano-conductive rubber sensor, and preparation and packaging methods therefor |
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| CN112388889B (en) * | 2020-10-23 | 2021-08-31 | 深圳市市政设计研究院有限公司 | Wide-range high-toughness nano conductive rubber sensor and preparation and packaging methods thereof |
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- 2020-10-23 CN CN202011143979.XA patent/CN112388889B/en active Active
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- 2021-09-27 WO PCT/CN2021/120847 patent/WO2022083415A1/en unknown
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| CN112388889B (en) | 2021-08-31 |
| ZA202210850B (en) | 2022-12-21 |
| WO2022083415A1 (en) | 2022-04-28 |
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