WO2021012297A1 - 一种基于带刺空心碳微球超灵敏度压力传感薄膜及其制备方法 - Google Patents
一种基于带刺空心碳微球超灵敏度压力传感薄膜及其制备方法 Download PDFInfo
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- WO2021012297A1 WO2021012297A1 PCT/CN2019/098277 CN2019098277W WO2021012297A1 WO 2021012297 A1 WO2021012297 A1 WO 2021012297A1 CN 2019098277 W CN2019098277 W CN 2019098277W WO 2021012297 A1 WO2021012297 A1 WO 2021012297A1
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- microspheres
- barbed
- sensing film
- pressure sensing
- hollow
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- 239000004005 microsphere Substances 0.000 title claims abstract description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
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Images
Classifications
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- 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
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- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- 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
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Definitions
- the invention belongs to an ultra-sensitive pressure sensing film based on barbed hollow carbon microspheres and a preparation method thereof, and belongs to the technical field of preparation of flexible electronic materials.
- Pressure sensing material refers to the change in the internal microstructure of the material after a certain pressure on the surface of the material, which leads to the change of the overall electrical properties of the material.
- the pressure sensing function can be realized by detecting the electrical signal change of the material.
- Sensing materials are at the core of this process.
- Pressure sensors are widely used in various industries and fields such as aerospace, aviation, navigation, petrochemical, power machinery, medical treatment, meteorology, geology and so on. In the industrial field, pressure sensors can be used to detect the real-time stress conditions of various instruments and equipment. For example, it is used to test the pressure of patient's breathing, oil and gas transportation pipelines, the deformation of the rails in use, whether foreign objects are encountered in the operation of the equipment, the dynamic distortion of the engine air intake and so on.
- resistive and capacitive flexible pressure sensors are the most commonly used for static force.
- the purpose of the present invention is to provide an ultra-sensitive pressure sensing film based on barbed hollow carbon microspheres and a preparation method thereof. While having ultra-high sensitivity, it also has the ability to respond with signals parallel to the pressure direction and not to feedback signals perpendicular to the pressure direction, laying the foundation for its application in ultra-high-density array sensing, and its theoretical detection density point It can reach more than 3.2 million per square centimeter.
- the system's sensing material has good environmental stability, it can work normally under water, and its stress detection ability is not affected by temperature changes. It also takes into account excellent fatigue resistance and has certain advantages in mass production. , Compatible with the mature spin coating and other thin film preparation processes, so it has good theoretical research and practical application value.
- the present invention proposes an ultra-sensitive pressure sensing film based on barbed hollow carbon microspheres.
- the pressure sensing film includes conductive barbed hollow carbon microspheres and a siloxane material with dielectric properties.
- the barbed hollow carbon microspheres The mass percentage of carbon microspheres and siloxane materials is 0.5%-20%.
- the film thickness of the pressure sensing film is 0.1 ⁇ m to 200 ⁇ m.
- the mass percentage of nitrogen and carbon is 0.2% to 15%; the mass percentage of oxygen and carbon is 2% to 35%.
- the present invention proposes a method for preparing a super-sensitive pressure sensing film based on barbed hollow carbon microspheres, and the specific steps are as follows:
- step (2) Put the prickly hollow organic nanospheres obtained in step (1) in an inert gas (Ar or N 2 ), heat to 330-360°C, hold for 50-70 minutes, and then heat up to 600-950°C, After holding for 1 to 2 hours, cool down with the furnace to obtain barbed hollow carbon microspheres;
- an inert gas Ar or N 2
- step (2) Take the barbed hollow carbon microspheres and siloxane materials obtained in step (2), and the mass percentage of the barbed hollow carbon microspheres and siloxane materials is 0.5%-20%. Under ice bath conditions, high speed Stir for 4.5-5.5 hours to obtain slurry for preparing pressure sensing film;
- the slurry of the pressure sensing film obtained in step (4) is formed on the substrate obtained in step (3) through a film forming process, and cured in an oven at 60-120°C for 15 to 180 minutes; Soak in a solvent that can dissolve the sacrificial layer for 2 hours to obtain a pressure sensing film with ultra-high sensitivity.
- the precursor of step (1) contains at least one of aniline, pyrrole, dopamine, melamine or amino acid.
- the hollow template nanospheres in step (1) comprise at least one of nano-polystyrene microspheres, nano-silica microspheres or nano-polymethyl methacrylate microspheres.
- the particle size of the barbed hollow carbon microspheres obtained in step (2) is 100 nm to 1000 nm.
- the film forming process described in step (5) includes any one of spin coating method, casting method, spray coating method, blade coating method, drop coating method or reverse mold method.
- the sacrificial layer material in step (3) contains at least one of polyvinyl alcohol, polymethyl methacrylate or dextran.
- the siloxane material in step (4) is polydimethylsiloxane.
- the sensing material has been reasonably optimized design, and its specific mass concentration makes it work under the condition of FN tunneling effect.
- the stress deformation reaction can be super-exponentially The signal changes to achieve ultra-high sensitivity sensing.
- the filling unit is thin-walled hollow carbon spheres, after being compounded with the polydimethylsiloxane matrix, the hollow structure can effectively absorb changes in the internal structure distribution caused by changes in external temperature, so that it can be A pressure sensing material that does not respond to temperature.
- the barbed hollow carbon nanosphere/polydimethylsiloxane composite film pressure sensing material prepared by the present invention has ultra-high sensitivity, high array density, transparency, low delay, and no temperature interference, and can be used for complex In the environment (such as submerged detection, high and low temperature conversion environment, complex surface, etc.), and the preparation method is simple, the process is mature, and it does not pollute the environment.
- Figure 1 is a scanning transmission electron microscope and transmission electron microscope photos of 600nm conductive barbed microspheres.
- Figure 2 is a physical image of the pressure sensing film.
- Figure 3 shows the light transmittance spectrum of the film.
- Figure 4 shows the resistance-pressure curve and sensitivity-pressure curve of the sensing film.
- Figure 5 shows the relaxation response curve of the sensing film.
- Figure 6 shows the fatigue response test curve of the sensing film.
- Figure 7 shows the resistance values of the sensing film at different pressures from 25°C to 160°C.
- Figure 8 is an implementation diagram of the sensing film used in PBS submerged test.
- Figure 9 shows the resistance-pressure curve and sensitivity-pressure curve of the sensing film tested in PBS.
- Figure 10 shows the sensor test demonstration of the sensor film applied to the 64 ⁇ 64 array electrode. Among them: (a) is the array electrode test chart, (b) is the real-time result display chart.
- Figure 11 shows the X-ray photoelectric spectroscopy analysis results of Example 1.
- Figure 12 shows the resistance of the sensing film of Example 2 under different pressure conditions, and calculates its specific sensitivity index.
- Figure 13 shows the X-ray photoelectric spectroscopy analysis results of Example 2.
- the present invention will be further described below in conjunction with specific embodiments and drawings, but the present invention is not limited to the following embodiments.
- the methods are conventional methods unless otherwise specified.
- the raw materials can be obtained from open commercial channels unless otherwise specified.
- Example 1 First, 0.5 g of polystyrene microspheres with a particle size of 600 nm were dispersed in 10 mL of deionized water at room temperature for 10 minutes ultrasonically, and then 0.5 g of aniline precursor was added, followed by magnetic stirring for 3 hours at 100 rpm. Then add 100 mL of 0.5M Fe(NO 3 ) 3 aqueous solution to the solution, and magnetically stir at room temperature for 24 hours at 300 rpm. The obtained solution was washed three times with deionized water and ethanol solution in a centrifuge at 5000 rpm, placed in a freeze dryer, and dried for 48 hours.
- Figure 1 is its scanning transmission electron microscope and transmission electron microscope microscopic pictures.
- Figure 3 shows the film's ability to transmit light at different wavelengths, and its transparency is close to that of a cover glass.
- Figure 4 shows the resistance of the sensing film under different pressure conditions, and calculates its specific sensitivity index.
- Figure 5 shows the response speed of the sensing film to pressure, with a pressure response time of 60ms and a pressure release response time of 30ms.
- Figure 6 shows the pressure response signal of the sensor film during 5000 times of load-release.
- Figure 7 shows the resistance signal of the sensing film under different pressure conditions at 25°C to 160°C.
- Figure 8 shows the response test of the sensor film to pressure after simulating the human body fluid environment for 20 cm in PBS solution.
- Figure 9 shows the ability of the sensing film to detect pressure signals in the PBS solution.
- Figure 10 shows the mass resolution capability of the sensing film for two slight objects on a detection electrode array with a size of 3.2 ⁇ 3.2cm with 64 ⁇ 64
- Figure 11 shows the X-ray photoelectric spectroscopy analysis results of Example 1.
- the stirred slurry was spin-coated on a petri dish coated with a PVA sacrificial layer by a spin coating method, and the spin coating procedure was: 600 rpm, 9 s, 5000 rpm, 35 s.
- Figure 12 shows the resistance of the sensing film of Example 2 under different pressure conditions, and calculates its specific sensitivity index.
- Figure 13 shows the X-ray photoelectric spectroscopy analysis results of Example 2.
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Abstract
Description
Claims (10)
- 一种基于带刺空心碳微球超灵敏度压力传感薄膜,其特征在于,所述压力传感薄膜包括可导电的带刺空心碳微球与具有介电性能的硅氧烷类材料,所述带刺空心碳微球与硅氧烷类材料的质量百分比为0.5%~20%。
- 根据权利要求1所述的压力传感薄膜,其特征在于,所述压力传感薄膜的膜厚为0.1μm~200μm。
- 根据权利要求1所述的压力传感薄膜,其特征在于,带刺空心碳微球中,氮元素与碳元素的质量百分比为0.2%~15%;氧元素与碳元素的质量百分比为2%~35%。
- 一种如权利要求1所述的基于带刺空心碳微球超灵敏度压力传感薄膜的制备方法,其特征在于,具体步骤如下:(1)、10~30℃下,量取10mL去离子水,加入空心模板纳米微球0.1~1g,和前驱体0.1~0.5g,超声分散8-12分钟后,密封搅拌溶胀1-8小时,然后加入与前驱体对应聚合引发剂,搅拌18-28小时后,离心,冷冻干燥,得到带刺空心有机纳米微球;(2)、将步骤(1)得到的带刺空心有机纳米微球置于惰性气体(Ar或N 2)中,加热至330-360℃,保温50-70分钟,再升温至600~950℃,保温1~2小时后随炉冷却,即可获得带刺空心碳微球;(3)、取制备薄膜的载体基板,在其上涂布一层牺牲层,得到基材,备用;(4)、取步骤(2)所得带刺空心碳微球与硅氧烷类材料,带刺空心碳微球与硅氧烷类材料的质量百分比为0.5%~20%,在冰浴条件下,高速搅拌4.5-5.5小时,即可获得用于制备压力传感薄膜的浆料;(5)、将步骤(4)所得压力传感薄膜的浆料通过成膜工艺成型于步骤(3)所得基材上,于60-120℃烘箱中,固化15~180分钟;取出后置于可溶解牺牲层的溶剂中浸泡2小时,即可获得一种具备超高灵敏度的压力传感薄膜。
- 根据权利要求4所述的制备方法,其特征在于,步骤(1)所述前驱体包含苯胺、吡咯、多巴胺、三聚氰胺或氨基酸中的至少一种。
- 根据权利要求4所述的制备方法,其特征在于,步骤(1)中空心模板纳米微球包含纳米聚苯乙烯微球、纳米二氧化硅微球或纳米聚甲基丙烯酸甲酯微球中的至少一种。
- 根据权利要求4所述的制备方法,其特征在于,步骤(2)所得带刺空心碳微球的粒径为100nm~1000nm。
- 根据权利要求4所述的制备方法,其特征在于,步骤(5)所述的成膜工艺包含旋涂法、流延法、喷涂法、刮涂法、滴涂法或倒模法中的任一种。
- 根据权利要求4所述的制备方法,其特征在于,步骤(3)中所述牺牲层材料包含聚乙烯醇、聚甲基丙烯酸甲酯或葡聚糖中的至少一种。
- 根据权利要求4所述的制备方法,其特征在于,步骤(4)中硅氧烷类材料为聚二甲基硅氧烷。
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