CN115246989B - Porous hierarchical structure foam material and preparation method thereof - Google Patents
Porous hierarchical structure foam material and preparation method thereof Download PDFInfo
- Publication number
- CN115246989B CN115246989B CN202111365984.XA CN202111365984A CN115246989B CN 115246989 B CN115246989 B CN 115246989B CN 202111365984 A CN202111365984 A CN 202111365984A CN 115246989 B CN115246989 B CN 115246989B
- Authority
- CN
- China
- Prior art keywords
- conductive filler
- composite conductive
- foam material
- nano
- polydimethylsiloxane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
- G01L9/04—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning of resistance-strain gauges
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Silicon Polymers (AREA)
Abstract
The invention provides a porous hierarchical structure foam material and a preparation method thereof, and the steps are as follows: adding the nano-scale composite conductive filler into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension; adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent; mixing the nano-scale composite conductive filler suspension with polydimethylsiloxane diluent, and continuing to ultrasonically disperse to obtain a three-phase suspension; heating the three-phase suspension on a hot plate to quickly volatilize toluene; adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring; coating a glass sheet to form a film, standing to remove bubbles, heating until ammonium bicarbonate is completely decomposed, and performing normal pressure plasma discharge treatment to obtain the porous hierarchical structure foam material. The invention utilizes the nano-scale composite conductive filler to create a mesoporous structure, ammonium bicarbonate particles form a macroporous structure to generate a foam material with a porous hierarchical structure, and the sensitivity of the foam material can reach 0.168 kPa at most when the foam material is applied to a sensor ‑1 。
Description
Technical Field
The invention relates to the field of plastic materials, in particular to a porous hierarchical structure foam material and a preparation method thereof.
Background
With the development of modern material science, porous materials have received increasing attention due to their wide range of applications. The materials with micropores (aperture less than 2 nm), mesopores (aperture 2-50 nm) and macropores (aperture more than 50 nm) can be synthesized by taking amines, surfactants, segmented copolymer or polymer pellets and the like as templates. The porosification of the material endows the material with brand-new excellent performance, greatly expands the application of the material in the aspects of exchange, separation, electrochemical process, catalytic reaction engineering, bioengineering and the like, and is one of the pressure sensors. The pressure sensor is a device for converting pressure applied by an external environment into an electric signal, and the traditional pressure sensor mainly comprises a rigid sensitive material and an electrode and can only be applied to the test of a flat surface. The mechanism of the flexible pressure sensor is a piezoelectric effect, when the material is deformed under the action of external force, positive and negative charges in the material are separated, polarization phenomenon occurs, and positive and negative charges on the opposite sides of the material are accumulated to form an internal potential difference. The invention aims to provide a flexible porous foam material which is high in sensitivity when applied to the field of sensors.
Disclosure of Invention
The technical problems to be solved are as follows: aiming at the problem of poor sensitivity of the porous material used by the pressure sensor at present, the invention utilizes the nano-scale composite conductive filler to create a mesoporous structure, ammonium bicarbonate particles form a macroporous structure, and finally a porous hierarchical structure foam material is generated, and the sensitivity of the porous hierarchical structure foam material can reach 0.168 kPa at most when the porous hierarchical structure foam material is applied to the sensor -1 。
The technical scheme is as follows: a porous hierarchical structure foam material having both macropores having a pore diameter of 10-40 μm and mesopores of 10-30 nm; the porous hierarchical structure foam material is prepared from polydimethylsiloxane as a main raw material, a mesoporous structure is created by nano-scale composite conductive filler, and a macroporous structure is formed by ammonium bicarbonate particles, so that the porous hierarchical structure foam material is finally generated.
The preparation method of the porous hierarchical structure foam material comprises the following steps:
step 1: adding the nano-scale composite conductive filler into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: and carrying out normal pressure plasma discharge treatment on the foam material to obtain the porous hierarchical structure foam material.
Further, the preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding a silane coupling agent to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 60-80 ℃, and dropwise adding a hydrochloric acid mixed solution of 2-3wt% of tin tetrachloride and 2-3wt% of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 30-40min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: filtering, drying the filter cake, and calcining in a muffle furnace at 400-500 ℃ to obtain the nano-scale composite conductive filler.
Further, the particle size of the nano-scale composite conductive filler is 10-40nm.
Further, the porous hierarchical structure foam material has a thickness of 1-5mm.
Further, the mass of the nano-scale composite conductive filler is 7-9% of that of the polydimethylsiloxane, and the mass of the ammonium bicarbonate is 5-7% of that of the polydimethylsiloxane.
Further, in the step 5, the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1.
Further, the plasma temperature and the ion density in the normal pressure plasma discharge treatment are respectively 4 eV and 1010 cm -3 。
Further, the silane coupling agent is KH550, KH560, KH570 or KH792.
The application of the porous hierarchical structure foam material in the sensor field.
The beneficial effects are that:
1. the invention uses nano-scale composite conductive filler to create a mesoporous structure, uses ammonium bicarbonate particles to form a macroporous structure, and finally generates the porous hierarchical structure foam material.
2. The invention adopts serpentine to prepare the nano composite conductive material, the serpentine is a hydrous magnesium-rich silicate mineral, the crystal structure of the serpentine is in fibrous curling arrangement, and conductive ions can be greatly loaded, so that the loading rate of tin and antimony is improved, and the conductivity is improved.
3. The method adopts normal pressure plasma discharge treatment, so that the generated cells are more uniform.
4. The porous hierarchical foam material prepared by the method can be used for preparing a sensor, and the sensitivity of the porous hierarchical foam material can reach 0.168 kPa at most -1 。
5. The universal material testing machine is adopted for testing, when the stress interval is 0-160kPa, the number of times of pressure application/pressure (kPa) can reach 20000/160, and the better sensitivity can still be kept, and the descending amplitude is not more than 5%. The number of times of pressure application/pressure (kPa) of similar products can only reach 7000/50 or 10000/2.
Drawings
FIG. 1 is a graph of the rate of change of resistance for various embodiments;
fig. 2 is a scanning electron microscope image of example 12.
Detailed Description
Example 1
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 7% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 5% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH550 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 60 ℃, and dropwise adding a hydrochloric acid mixed solution of 2 weight percent of stannic chloride and 2 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 30min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 400 ℃ to obtain the nanoscale composite conductive filler.
Example 2
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 5% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH550 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 60 ℃, and dropwise adding a hydrochloric acid mixed solution of 2 weight percent of stannic chloride and 2 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 30min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 400 ℃ to obtain the nanoscale composite conductive filler.
Example 3
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 9% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 5% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH550 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 60 ℃, and dropwise adding a hydrochloric acid mixed solution of 2 weight percent of stannic chloride and 2 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 30min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 400 ℃ to obtain the nanoscale composite conductive filler.
Example 4
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 6% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH550 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 60 ℃, and dropwise adding a hydrochloric acid mixed solution of 2 weight percent of stannic chloride and 2 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 30min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 400 ℃ to obtain the nanoscale composite conductive filler.
Example 5
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 7% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH550 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 60 ℃, and dropwise adding a hydrochloric acid mixed solution of 2 weight percent of stannic chloride and 2 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 30min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 400 ℃ to obtain the nanoscale composite conductive filler.
Example 6
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 6% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH560 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 70 ℃, and dropwise adding hydrochloric acid mixed solution of 2 weight percent of stannic chloride and 2.5 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 35min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 400 ℃ to obtain the nanoscale composite conductive filler.
Example 7
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 6% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH570 for surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 80 ℃, and dropwise adding a hydrochloric acid mixed solution of 2wt% of tin tetrachloride and 3wt% of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 40min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 500 ℃ to obtain the nanoscale composite conductive filler.
Example 8
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 6% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH550 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 60 ℃, and dropwise adding a hydrochloric acid mixed solution of 2.5 weight percent of stannic chloride and 2 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 30min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 450 ℃ to obtain the nanoscale composite conductive filler.
Example 9
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 6% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH570 for surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 60 ℃, and dropwise adding a hydrochloric acid mixed solution of 2.5 weight percent of tin tetrachloride and 2.5 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 35min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 450 ℃ to obtain the nanoscale composite conductive filler.
Example 10
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 6% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH792 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 60 ℃, and dropwise adding a hydrochloric acid mixed solution of 2.5 weight percent of stannic chloride and 3 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 35min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 500 ℃ to obtain the nanoscale composite conductive filler.
Example 11
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 6% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH792 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 80 ℃, and dropwise adding a hydrochloric acid mixed solution of 3wt% of tin tetrachloride and 2wt% of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 40min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 500 ℃ to obtain the nanoscale composite conductive filler.
Example 12
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 6% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH792 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 80 ℃, and dropwise adding a hydrochloric acid mixed solution of 3 weight percent of stannic chloride and 2.5 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 40min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 500 ℃ to obtain the nanoscale composite conductive filler.
Example 13
A method for preparing a porous hierarchical foam material, comprising the steps of:
step 1: adding the nano-scale composite conductive filler with the particle size of 10-40nm into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with the polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension, wherein the mass of the nano-scale composite conductive filler is 8% of that of the polydimethylsiloxane;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring, wherein the mass of the ammonium bicarbonate is 6% of that of the polydimethylsiloxane; the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: subjecting it to normal pressure plasma discharge treatment at ion temperature and density of 4 eV and 1010 cm respectively -3 I.e. a porous hierarchical structure foam.
The preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding KH792 to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 80 ℃, and dropwise adding a hydrochloric acid mixed solution of 3 weight percent of stannic chloride and 3 weight percent of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 40min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: and (3) filtering, drying the filter cake, and calcining the filter cake in a muffle furnace at 500 ℃ to obtain the nanoscale composite conductive filler.
The prepared material is cut into a cuboid with the length of 10 mm, the width of 5mm and the thickness of 3mm, and the cuboid is packaged in a polyimide film with two gold electrodes to prepare the sensor, and the sensor is tested in a stress area under the pressure of 0-160 kPa.
As can be seen from fig. 1, in comparative examples 1 to 3, the greater the content of the nano-scale composite conductive filler, the greater the rate of change of resistance, and in comparative examples 2, 4 and 5, the ammonium bicarbonate was found to affect the rate of change of resistance by more than 6%, and the improvement of the rate of change of resistance was less remarkable. As is clear from comparative examples 4 and examples 6 to 13, the effect was best when the mass ratio of tin tetrachloride to antimony trichloride was 1:1, and the effect of improving the rate of change of resistance was not significant when the contents of both exceeded 6%. While the rate of change of resistance increases the fastest at pressures of 20-100 kPa.
TABLE 1 sensitivity of different examples
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | Example 13 | |
| Sensitivity (kPa) -1 ） | 0.124 | 0.128 | 0.139 | 0.142 | 0.130 | 0.145 | 0.151 | 0.148 | 0.157 | 0.164 | 0.144 | 0.167 | 0.168 |
As can be seen from Table 1, the sensitivity (0-160 kPa) of the sensors for the different materials of example 12 and example 13 are optimal, and the data are relatively close, meaning that the effect is not obvious by continuously increasing the contents of tin tetrachloride and antimony trichloride.
TABLE 2 sensitivity after various pressing times for example 12
| 1 | 10 | 100 | 1000 | 2000 | 5000 | 10000 | 15000 | 20000 | |
| Sensitivity (kPa) -1 ） | 0.167 | 0.167 | 0.167 | 0.167 | 0.166 | 0.165 | 0.164 | 0.162 | 0.159 |
As shown in Table 2, the test by using the universal material tester shows that the number of times of pressure application/pressure (kPa) can reach 20000/160 when the stress is 160kPa, and the better sensitivity can still be maintained, and the reduction degree is not more than 5%. The number of times of pressure application/pressure (kPa) of similar products can only reach 7000/50 or 10000/2.
Claims (7)
1. A porous hierarchical foam material characterized by having both macropores having a pore diameter of 10-40 μm and mesopores having a pore diameter of 10-30 nm; the porous hierarchical structure foam material is prepared by using polydimethylsiloxane as a main raw material and a nanoscale composite conductive filler to create a mesoporous structure, forming a macroporous structure by using ammonium bicarbonate particles, and finally generating the porous hierarchical structure foam material;
the preparation method of the porous hierarchical structure foam material comprises the following steps:
step 1: adding the nano-scale composite conductive filler into toluene for ultrasonic dispersion to obtain nano-scale composite conductive filler suspension;
step 2: adding polydimethylsiloxane into toluene and stirring to obtain polydimethylsiloxane diluent;
step 3: mixing the nano-scale composite conductive filler suspension with polydimethylsiloxane diluent, and continuing to ultrasonically disperse for 10 h to obtain a three-phase suspension;
step 4: heating the three-phase suspension on a hot plate to quickly volatilize toluene;
step 5: adding ammonium bicarbonate and methyl tetrahydrophthalic anhydride, and fully stirring;
step 6: coating a glass sheet to form a film, standing for 1 h, removing bubbles, and heating at 100 ℃ until ammonium bicarbonate is completely decomposed;
step 7: carrying out normal pressure plasma discharge treatment on the foam material to obtain a porous hierarchical structure foam material;
the preparation method of the nanoscale composite conductive filler comprises the following steps:
the first step: taking serpentine, crushing and grinding to obtain serpentine powder, and adding a silane coupling agent to perform surface activation treatment;
and a second step of: adding distilled water after drying, regulating the suspension to 4 by using dilute hydrochloric acid, continuously stirring at the temperature of 60-80 ℃, and dropwise adding a hydrochloric acid mixed solution of 2-3wt% of tin tetrachloride and 2-3wt% of antimony trichloride;
and a third step of: after the mixed liquid drops are finished, curing is continued for 30-40min;
fourth step: filtering, washing with distilled water until the filtrate is free of Cl - ；
Fifth step: filtering, drying the filter cake, and calcining in a muffle furnace at 400-500 ℃ to obtain the nano-scale composite conductive filler.
2. A cellular hierarchical structure foam material according to claim 1, characterized in that: the particle size of the nano-scale composite conductive filler is 10-40nm.
3. A cellular hierarchical structure foam material according to claim 1, characterized in that: the mass of the nano-scale composite conductive filler is 7-9% of that of the polydimethylsiloxane, and the mass of the ammonium bicarbonate is 5-7% of that of the polydimethylsiloxane.
4. A cellular hierarchical structure foam material according to claim 1, characterized in that: in the step 5, the mass ratio of the ammonium bicarbonate to the methyltetrahydrophthalic anhydride is 10:1.
5. A cellular hierarchical structure foam material according to claim 1, characterized in that: the plasma temperature and density in the normal pressure plasma discharge treatment are respectively 4 eV and 1010 cm -3 。
6. A cellular hierarchical structure foam material according to claim 1, characterized in that: the silane coupling agent is KH550, KH560, KH570 or KH792.
7. Use of a porous hierarchical foam material according to any of claims 1-6 in the field of sensors.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111365984.XA CN115246989B (en) | 2021-11-18 | 2021-11-18 | Porous hierarchical structure foam material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111365984.XA CN115246989B (en) | 2021-11-18 | 2021-11-18 | Porous hierarchical structure foam material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115246989A CN115246989A (en) | 2022-10-28 |
| CN115246989B true CN115246989B (en) | 2023-07-18 |
Family
ID=83699050
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111365984.XA Active CN115246989B (en) | 2021-11-18 | 2021-11-18 | Porous hierarchical structure foam material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115246989B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999025761A1 (en) * | 1997-11-15 | 1999-05-27 | Ge Bayer Silicones Gmbh & Co. Kg | Silicon foams with closed pores, method for the production and use thereof |
| CN102074279A (en) * | 2010-12-30 | 2011-05-25 | 北京工业大学 | Preparation method of multihole-structure-characterized conducting diatomaceous earth |
| CN106928723A (en) * | 2017-03-21 | 2017-07-07 | 电子科技大学 | CaCu 3 Ti 4 O/dimethyl silicone polymer composite and flexible foam and its preparation method and application |
| CN110101904A (en) * | 2019-06-20 | 2019-08-09 | 北京幸福益生再生医学科技有限公司 | A kind of regenerated degradable regenerative medical material of promotion tissue in situ and preparation method thereof |
-
2021
- 2021-11-18 CN CN202111365984.XA patent/CN115246989B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999025761A1 (en) * | 1997-11-15 | 1999-05-27 | Ge Bayer Silicones Gmbh & Co. Kg | Silicon foams with closed pores, method for the production and use thereof |
| CN102074279A (en) * | 2010-12-30 | 2011-05-25 | 北京工业大学 | Preparation method of multihole-structure-characterized conducting diatomaceous earth |
| CN106928723A (en) * | 2017-03-21 | 2017-07-07 | 电子科技大学 | CaCu 3 Ti 4 O/dimethyl silicone polymer composite and flexible foam and its preparation method and application |
| CN110101904A (en) * | 2019-06-20 | 2019-08-09 | 北京幸福益生再生医学科技有限公司 | A kind of regenerated degradable regenerative medical material of promotion tissue in situ and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115246989A (en) | 2022-10-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xiao et al. | Graphene/nanofiber aerogels: performance regulation towards multiple applications in dye adsorption and oil/water separation | |
| Zu et al. | Superhydrophobic ultraflexible triple-network graphene/polyorganosiloxane aerogels for a high-performance multifunctional temperature/strain/pressure sensing array | |
| Makhado et al. | Microwave assisted synthesis of xanthan gum-cl-poly (acrylic acid) based-reduced graphene oxide hydrogel composite for adsorption of methylene blue and methyl violet from aqueous solution | |
| Guan et al. | Silane bonded graphene aerogels with tunable functionality and reversible compressibility | |
| Zheng et al. | Macroporous graphene oxide–polymer composite prepared through Pickering high internal phase emulsions | |
| Bourgeat-Lami et al. | Latex routes to graphene-based nanocomposites | |
| Tian et al. | High performance dielectric composites by latex compounding of graphene oxide-encapsulated carbon nanosphere hybrids with XNBR | |
| Guimont et al. | Viscoelasticity of graphite oxide-based suspensions in PDMS | |
| KR101856214B1 (en) | Conducting film and manufacturing method of the same | |
| CN105542228A (en) | Preparation method of functionalized nano-silica based on graphene | |
| CN112452299A (en) | MXene-based three-dimensional porous flexible self-supporting film, preparation method thereof and application thereof in electrochemical adsorption of dye | |
| Zheng et al. | Flexible, strong, multifunctional graphene oxide/silica-based composite aerogels via a double-cross-linked network approach | |
| CN109705527B (en) | Graphene dispersion paste, preparation method and use method thereof | |
| CN111218090A (en) | Preparation method of anisotropic modified graphene epoxy resin composite material | |
| RU2662484C2 (en) | Method of producing an electrically conductive hydrophilic aerogel based on composite of graphene and carbon nanotubes | |
| CN110357083A (en) | The preparation method of polymolecularity graphene powder | |
| Xu et al. | Enhancing mechanical performances of polystyrene composites via constructing carbon nanotube/graphene oxide aerogel and hot pressing | |
| CN109499497B (en) | Preparation method of graphene/carbon microsphere composite aerogel | |
| CN107032329A (en) | A kind of three-dimensional grapheme of nano-micrometre classification pore passage structure and preparation method thereof | |
| Xu et al. | Surface modification of Sb2O3 nanoparticles with dioctylphthalate | |
| CN108192137B (en) | Preparation method of high-dispersion carbon nano tube used as rubber filler | |
| CN115246989B (en) | Porous hierarchical structure foam material and preparation method thereof | |
| CN109294283B (en) | Preparation method of multiphase nanoscale composite carbon material | |
| CN104843677B (en) | porous graphene and preparation method thereof | |
| Dutta et al. | Laser induced incorporation of CNTs in graphene electrodes improves flexibility and conductivity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |