CN111637801A - PMMA-based graphene burst pressure test sensor and manufacturing method thereof - Google Patents
PMMA-based graphene burst pressure test sensor and manufacturing method thereof Download PDFInfo
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F42—AMMUNITION; BLASTING
- F42B—EXPLOSIVE CHARGES, e.g. FOR BLASTING, FIREWORKS, AMMUNITION
- F42B35/00—Testing or checking of ammunition
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- 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
- G01L9/08—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 piezoelectric devices, i.e. electric circuits therefor
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0035—Multiple processes, e.g. applying a further resist layer on an already in a previously step, processed pattern or textured surface
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Abstract
A PMMA-based graphene burst pressure test sensor comprises a substrate, wherein first boron nitride is arranged on the substrate through a transfer process, graphene is arranged on the first boron nitride through the transfer process, electrodes are sputtered at two ends of the graphene through an MEMS (micro-electro-mechanical system) process, second boron nitride is arranged on the graphene through the transfer process, and a packaging layer is arranged on the second boron nitride; the invention realizes the miniaturization of the boron nitride/graphene/boron nitride heterojunction sensitive element through the MEMS technology, so that the boron nitride/graphene/boron nitride heterojunction sensitive element is suitable for measuring the micro-scale explosive-filling detonation pressure; through the back exposure and development process of the substrate, the imaging of the electrode on the PMMA substrate is realized, and the damage to the substrate is avoided; different target substrates are utilized for fishing, so that transfer of graphene and boron nitride is realized, and the manufacturing process of the sensor is simplified; the sensor has the characteristics of small sensitive element size, quick response, high sensitivity, large measuring range, high precision and the like, and can be suitable for measuring the detonation pressure of micro-scale explosive filling.
Description
Technical Field
The invention belongs to the technical field of ultrahigh pressure sensors, and particularly relates to a PMMA-based graphene burst pressure test sensor and a manufacturing method thereof.
Background
MEMS initiating explosive devices are key technologies for supporting the development of new-generation miniaturized weapons and intelligent ammunitions, and have become the leading-edge field of high attention of military scientific research institutions of various countries. The micro-scale charging is used as a core component of the MEMS initiating explosive device, has great influence on the safety, reliability and operational efficiency of weapons and ammunition, and the output detonation pressure test of the micro-scale charging becomes the premise of the basic theoretical research and engineering application of the MEMS initiating explosive device. At present, the system is basically formed in the aspects of basic theory, integrated manufacturing, performance evaluation, test application and the like of the MEMS initiating explosive devices in the United states, and although key breakthroughs are made in the aspects of basic theory, integrated manufacturing and the like of the MEMS initiating explosive devices in China, the research on the output performance evaluation of the MEMS initiating explosive devices is weak, so that the research on the development of the quantitative characterization problem of the output detonation pressure of the micro-scale explosive charge has important scientific significance and engineering practical value.
The micro-scale charging is cylindrical charging with the charging diameter of 0.5-2 mm, and is constrained by a shell; the output detonation pressure of the micro-scale charge refers to the pressure at the center of the detonation wave front. The detonation of micro-scale explosive loading has three characteristics: (1) the diameter of the charge is millimeter or submillimeter; (2) the detonation wave belongs to constant two-dimensional axial symmetric flow; (3) the detonation pressure can reach GPa grade. The above detonation characteristics put some requirements on the sensor design: firstly, the size of a sensitive element is matched with the diameter of a charge; secondly, the transverse stretching effect of the micro-scale explosive charging detonation wave must be considered; and thirdly, the sensitive element can measure the pressure in the GPa grade. However, in the existing burst pressure test methods, most of the burst pressure test methods are used for measuring large-size explosive columns; a few detonation pressure testing methods aiming at micro-scale explosive charge ignore the transverse stretching effect of detonation waves and the impedance matching problem of a sensor measuring end.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the PMMA-based graphene detonation pressure testing sensor and the manufacturing method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the utility model provides a PMMA base graphite alkene detonation pressure test sensor, includes basement 1, is equipped with first boron nitride 2 through the transfer technology on the basement 1, is equipped with graphite alkene 3 through the transfer technology on the first boron nitride 2, and it has electrode 5 to go up both ends through MEMS technology sputtering on the graphite alkene 3, is equipped with second boron nitride 4 through the transfer technology on the graphite alkene 3, is equipped with packaging layer 6 on the second boron nitride 4.
The substrate 1 is made of organic glass (PMMA) blocks.
The number of layers of the first boron nitride 2 and the second boron nitride 4 is the same, and is controlled to be 1-3.
The graphene 3 is single-layer graphene.
The electrode 5 is made of Au and has the thickness of about 200 nm.
The packaging layer 6 is made of organic glass (PMMA) materials through a glue-homogenizing curing process, and the thickness is about 25 micrometers.
The manufacturing method of the PMMA-based graphene detonation pressure test sensor comprises the following steps:
step 1: growing single-layer graphene 3 on the first metal foil 7-1, spin-coating a first photoresist 8-1 on the surface of the graphene 3, and curing;
step 2: preparing an etching solution for the first metal foil 7-1, and placing the first photoresist 8-1/graphene 3/first metal foil 7-1 in the etching solution to etch the first metal foil 7-1;
and step 3: growing a first boron nitride 2 on the second metal foil 7-2, and fishing a first photoresist 8-1/graphene 3 by using a first boron nitride 2/second metal foil 7-2 target substrate after the first metal foil 7-1 is etched;
and 4, step 4: preparing an etching solution for the second metal foil 7-2, and placing the first photoresist 8-1/graphene 3/first boron nitride 2/second metal foil 7-2 in the etching solution to etch the second metal foil 7-2; after the second metal foil 7-2 is etched, fishing the first photoresist 8-1/graphene 3/first boron nitride 2 by using the target substrate of the substrate 1;
and 5: carrying out ultraviolet exposure on the first photoresist 8-1/graphene 3/first boron nitride 2/first photoresist 8-1 on the surface of the substrate 1, then developing by using a developing solution, rinsing by using deionized water, and finally drying;
step 6: spin-coating a second photoresist 8-2 on the surface of the graphene 3/first boron nitride 2/substrate 1, and exposing the electrode position through an exposure and development process; sputtering a layer of Au thin film 5-1 on the surface of the second photoresist 8-2/graphene 3/first boron nitride 2/substrate 1;
and 7: exposing the second photoresist 8-2 through the substrate 1 on the back of the Au thin film 5-1/the second photoresist 8-2/the graphene 3/the first boron nitride 2/the substrate 1, developing by using a developing solution, and stripping the Au thin film 5-1 to form a first electrode 5-2 and a second electrode 5-3;
and 8: growing second boron nitride 4 on the third metal foil 7-3, and spin-coating a layer of packaging layer 6 on the surface of the second boron nitride 4;
and step 9: preparing an etching solution for the third metal foil 7-3, and placing the packaging layer 6/the second boron nitride 4/the third metal foil 7-3 in the etching solution to etch the third metal foil 7-3; after the third metal foil 7-3 is etched, fishing the packaging layer 6/the second boron nitride 4 by using the graphene 3/the first boron nitride 2/the substrate 1 target substrate formed in the step 7;
step 10: and etching the packaging layer 6/the second boron nitride 4/the graphene 3/the first boron nitride 2 by using oxygen plasma to form a required sensitive element size, exposing the first electrode 5-2 and the second electrode 5-3, and finally finishing the manufacture of the PMMA-based graphene detonation pressure test sensor.
The first photoresist 8-1 and the second photoresist 8-2 adopt AZ4620 photoresist, and spin coating parameters are as follows: low speed 500rpm, time 9 s; high speed 1500rpm, time 30 s; the curing time was 20min, the temperature was 85 ℃.
The first photoresist 8-1 and the second photoresist 8-2 are removed through an exposure and development process, and the exposure time is 30 s; the developing solution is 5 per mill NaOH solution, and the developing time is 3 min.
The spin coating parameters of the packaging layer 6 are as follows: low speed 500rpm, time 5 s; high speed 2000rpm, time 20 s; curing time 30min, temperature 60 ℃.
The invention has the beneficial effects that:
according to the PMMA-based graphene detonation pressure test sensor, the second boron nitride 4/graphene 3/first boron nitride 2 heterojunction is in a pressure range of 0-5 GPa, and the in-plane current of the graphene 3 is 10℃ along with the increase of pressure6pA is reduced to 103pA, so that the sensor has higher measuring range and sensitivity; the in-plane current change of the second boron nitride 4/graphene 3/first boron nitride 2 heterojunction under the action of an external force is caused by the interaction between atoms, so that the response time of the sensor is prolonged; the substrate 1 and the packaging layer 6 are made of PMMA materials, so that the PMMA materials are approximately matched with the impedance of common condensed explosive, the reflection of shock waves at an interface is reduced, and the measurement precision is improved. In addition, in the manufacturing method, the miniaturization of the second boron nitride 4/graphene 3/first boron nitride 2 heterojunction sensitive element is realized through the MEMS technology, so that the micro-scale charge detonation pressure sensor is suitable for measuring the micro-scale charge detonation pressure; through the back exposure and development process of the substrate 1, the imaging of the electrode on the PMMA substrate is realized, and the damage of the substrate 1 caused by the traditional acetone stripping process is avoided; and different target substrates are utilized for fishing, so that the transfer of the graphene 3, the first boron nitride 2 and the second boron nitride 4 is realized, and the manufacturing process of the sensor is simplified.
The PMMA-based graphene detonation pressure test sensor has the characteristics of small sensitive element size, quick response, high sensitivity, large measuring range, high precision and the like, can be suitable for measuring the micro-scale explosive detonation pressure, and can also be expanded to measure the pressure of other micro-scale axisymmetric dynamic high-pressure flow fields.
Drawings
Fig. 1 is a schematic structural diagram of a PMMA-based graphene detonation pressure test sensor according to the present invention.
Fig. 2 is a flow chart of a manufacturing method of the PMMA-based graphene detonation pressure test sensor of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
Referring to fig. 1, the PMMA-based graphene detonation pressure test sensor includes a substrate 1, on which a first boron nitride 2 is disposed by a transfer process; graphene 3 is arranged on the first boron nitride 2 through a transfer process; electrodes 5 are sputtered at two ends of the graphene 3 through an MEMS (micro-electromechanical systems) process; the graphene 3 is provided with second boron nitride 4 through a transfer process; a packaging layer 6 is arranged on the second boron nitride 4; the miniaturization of a second boron nitride 4/graphene 3/first boron nitride 2 heterojunction sensitive element is realized through an MEMS (micro-electromechanical systems) technology, so that the micro-scale charge detonation pressure sensor is suitable for measuring micro-scale charge detonation pressure; the back of the substrate 1 realizes the imaging of the electrode on the substrate 1 through exposure and development processes, and avoids the damage of the substrate 1 caused by the traditional acetone stripping process; and different target substrates are utilized for fishing, so that the transfer of the graphene 3, the first boron nitride 2 and the second boron nitride 4 is realized, and the manufacturing process of the sensor is simplified.
The working principle of the PMMA-based graphene detonation pressure test sensor is as follows:
c in graphene 3 due to atomic interaction between graphene 3 and first and second boron nitrides 2 and 41Negative induced charge appears near the type carbon atom, and C of graphene 32Positive induced charges appear near the type carbon atoms, and the induced charges destroy the symmetry of the carbon atoms in the graphene 3 to form a dipole; when external pressure acts on the first boron nitride 2/graphene 3/second boron nitride 4 heterojunction, the interlayer distance between the graphene 3 and the first boron nitride 2 and the second boron nitride 4 is reduced, dipole polarization is enhanced, the symmetry of carbon atoms in the graphene 3 is further destroyed, and an energy gap is increased, and the change of the energy gap can cause the change of current in the first boron nitride 2/graphene 3/second boron nitride 4 heterojunction; the current value flowing in the 3 planes of the graphene is collected and input into a signal detection moduleThe block can obtain an external pressure value.
The number of layers of the first boron nitride 2 and the second boron nitride 4 is the same and is controlled to be 1-3; the graphene 3 is single-layer graphene; the second boron nitride 4/graphene 3/first boron nitride 2 heterojunction has high sensitivity in the range of 0-5 GPa, and has quick response time to external pressure, so that the sensor has the characteristics of high measuring range, high sensitivity, quick response and the like.
The electrode 5 is made of Au material and is formed by a sputtering process, and the thickness is about 200 nm.
The substrate 1 is made of an organic glass (PMMA) block material; the packaging layer 6 is made of organic glass (PMMA) material through a glue-homogenizing curing process, and the thickness is about 25 micrometers; because the impact resistance of the organic glass (PMMA) is close to that of explosive detonation products, the organic glass (PMMA) used as the substrate 1 and the packaging layer 6 of the sensor can enable the shock waves to approximately reach impedance matching in the transmission process, and errors caused by impedance mismatching are reduced.
The manufacturing method of the PMMA-based graphene detonation pressure test sensor comprises the following steps:
step 1: referring to fig. 2 (a), high-quality single-layer graphene 3 is grown on a first metal foil 7-1 (e.g., Cu, Ni) using a Chemical Vapor Deposition (CVD) method; placing the graphene 3/first metal foil 7-1 between two smooth and flat carriers (such as silicon wafers) and flattening; spin-coating a first photoresist 8-1 (such as AZ4620) on the surface of the graphene 3, and curing on a hot plate to enable the first photoresist 8-1 to support the graphene 3 in a transfer process;
step 2: preparing an etching solution (such as FeCl) for the first metal foil 7-13Solution), the first photoresist 8-1/graphene 3/first metal foil 7-1 is placed in an etching solution by tweezers to etch the first metal foil 7-1, and the first metal foil 7-1 is etched away, as shown in fig. 2 (b);
under the buoyancy action of the first photoresist 8-1, the first metal foil 7-1 is ensured to be in good contact with the etching liquid;
and step 3: referring to fig. 2(c), high-quality first boron nitride 2 is grown on the second metal foil 7-2 (e.g., Cu, Ni) by CVD; after the first metal foil 7-1 is etched, the first photoresist 8-1/graphene 3 floats on the surface of etching liquid, and at the moment, the first photoresist 8-1/graphene 3 is taken out of the etching liquid by using a first boron nitride 2/second metal foil 7-2 target substrate, so that the graphene 3 is ensured to be in contact with the first boron nitride 2; then releasing the first photoresist 8-1/graphene 3 into deionized water for rinsing so as to remove various impurities, metal ions and other pollutants on the surface of the graphene 3; after rinsing, placing the first photoresist 8-1/graphene 3/first boron nitride 2/second metal foil 7-2 on a flat experiment table, and drying by using a small airflow of a nitrogen gun, so as to ensure that the graphene 3 is tightly attached to the first boron nitride 2 by using the airflow force, reduce wrinkles and cracks of the graphene 3, and remove surface moisture; then, placing the first photoresist 8-1/graphene 3/first boron nitride 2/second metal foil 7-2 on a hot plate for drying, removing all water, and increasing Van der Waals force between the graphene 3 and the first boron nitride 2;
and 4, step 4: referring to (d) of FIG. 2, an etching solution (e.g., FeCl) for the second metal foil 7-2 is prepared3Solution), placing the first photoresist 8-1/graphene 3/first boron nitride 2/second metal foil 7-2 in an etching solution to etch the second metal foil 7-2; after the second metal foil 7-2 is etched, fishing out the first photoresist 8-1/graphene 3/first boron nitride 2 by using the target substrate of the substrate 1, and then rinsing by using deionized water, drying by using nitrogen and drying by using a hot plate;
and 5: performing ultraviolet exposure on the first photoresist 8-1/graphene 3/first boron nitride 2/first photoresist 8-1 on the surface of the substrate 1, then developing by using a developing solution, then rinsing by using deionized water, and finally drying, as shown in (e) in fig. 2;
step 6: referring to (f) in fig. 2, spin-coating a second photoresist 8-2 on the surface of the graphene 3/first boron nitride 2/substrate 1, and exposing the electrode position through an exposure and development process; then sputtering an Au thin film 5-1 with the thickness of 200nm on the surface of the second photoresist 8-2/graphene 3/first boron nitride 2/substrate 1;
and 7: referring to (g) and (h) of fig. 2, since the substrate 1, the first boron nitride 2, and the graphene 3 have light-transmitting properties, the Au thin film 5-1 can be peeled off by exposing the second photoresist 8-2 through the back side of the substrate 1 and then developing it with a developing solution, thereby forming the first electrode 5-2 and the second electrode 5-3;
and 8: referring to (i) of fig. 2, high-quality second boron nitride 4 is grown on a third metal foil 7-3 (e.g., Cu, Ni) using CVD, and then a 25 μm thick encapsulation layer 6 is spin-coated on the surface of the second boron nitride 4 and cured on a hot plate;
and step 9: referring to (j) of FIG. 2, an etching solution (e.g., FeCl) for the third metal foil 7-3 is prepared3Solution), the packaging layer 6/the second boron nitride 4/the third metal foil 7-3 are placed in etching liquid to etch the third metal foil 7-3; after the third metal foil 7-3 is etched, the packaging layer 6/the second boron nitride 4 is fished out by the graphene 3/the first boron nitride 2/the substrate 1 target substrate formed in the step 7, and then deionized water rinsing, nitrogen blow drying and hot plate drying are carried out;
step 10: referring to (k) in fig. 2, etching the packaging layer 6/the second boron nitride 4/the graphene 3/the first boron nitride 2 by using oxygen plasma to form a required sensitive element size and expose the first electrode 5-2 and the second electrode 5-3, and finally completing the manufacture of the PMMA-based graphene detonation pressure test sensor.
The first photoresist 8-1 and the second photoresist 8-2 adopt AZ4620 photoresist, and spin coating parameters are as follows: low speed 500rpm, time 9 s; high speed 1500rpm, time 30 s; the curing time was 20min, the temperature was 85 ℃.
The first photoresist 8-1 and the second photoresist 8-2 are removed through an exposure and development process, and the exposure time is 30 s; the developing solution is 5 per mill NaOH solution, and the developing time is 3 min.
The spin coating parameters of the packaging layer 6 are as follows: low speed 500rpm, time 5 s; high speed 2000rpm, time 20 s; curing time 30min, temperature 60 ℃.
Claims (10)
1. The utility model provides a PMMA base graphite alkene detonation pressure test sensor, includes base (1), its characterized in that: the substrate (1) is provided with first boron nitride (2) through a transfer process, the first boron nitride (2) is provided with graphene (3) through the transfer process, electrodes (5) are sputtered on the graphene (3) at two ends through an MEMS (micro electro mechanical system) process, the graphene (3) is provided with second boron nitride (4) through the transfer process, and the second boron nitride (4) is provided with a packaging layer (6).
2. The PMMA-based graphene detonation pressure test sensor of claim 1, wherein: the substrate (1) is made of organic glass (PMMA) blocks.
3. The PMMA-based graphene detonation pressure test sensor of claim 1, wherein: the number of layers of the first boron nitride (2) and the second boron nitride (4) is the same and is controlled to be 1-3.
4. The PMMA-based graphene detonation pressure test sensor of claim 1, wherein: the graphene (3) adopts single-layer graphene.
5. The PMMA-based graphene detonation pressure test sensor of claim 1, wherein: the electrode (5) is made of Au material and has a thickness of about 200 nm.
6. The PMMA-based graphene detonation pressure test sensor of claim 1, wherein: the packaging layer (6) is made of organic glass (PMMA) through a glue-homogenizing curing process, and the thickness of the packaging layer is about 25 micrometers.
7. The manufacturing method of the PMMA-based graphene detonation pressure test sensor according to claim 1, characterized by comprising the following steps:
step 1: growing single-layer graphene (3) on a first metal foil (7-1), spin-coating a first photoresist (8-1) on the surface of the graphene (3), and curing;
step 2: preparing an etching solution for the first metal foil (7-1), and placing the first photoresist (8-1)/graphene (3)/first metal foil (7-1) in the etching solution to etch the first metal foil (7-1);
and step 3: growing first boron nitride (2) on the second metal foil (7-2), and fishing out the first photoresist (8-1)/graphene (3) by using a first boron nitride (2)/second metal foil (7-2) target substrate after the first metal foil (7-1) is etched;
and 4, step 4: preparing etching liquid of the second metal foil (7-2), and placing the first photoresist (8-1)/graphene (3)/first boron nitride (2)/second metal foil (7-2) in the etching liquid to etch the second metal foil (7-2); after the second metal foil (7-2) is etched, fishing the first photoresist (8-1)/graphene (3)/first boron nitride (2) by using the target substrate of the substrate (1);
and 5: carrying out ultraviolet exposure on the first photoresist (8-1) on the surface of the first photoresist (8-1)/graphene (3)/first boron nitride (2)/substrate (1), developing by using a developing solution, rinsing by using deionized water, and finally drying;
step 6: spin-coating a second photoresist (8-2) on the surface of the graphene (3)/first boron nitride (2/) substrate (1), and exposing the electrode position through an exposure and development process; sputtering a layer of Au thin film (5-1) on the surface of the second photoresist (8-2)/graphene (3)/first boron nitride (2)/substrate 1;
and 7: exposing the second photoresist (8-2) through the substrate (1) on the back of the Au thin film (5-1)/the second photoresist (8-2)/the graphene (3)/the first boron nitride (2)/the substrate (1), developing by using a developing solution, and stripping the Au thin film (5-1) to form a first electrode (5-2) and a second electrode (5-3);
and 8: growing second boron nitride (4) on the third metal foil (7-3), and spin-coating an encapsulation layer (6) on the surface of the second boron nitride (4);
and step 9: preparing etching liquid of the third metal foil (7-3), and placing the packaging layer (6)/the second boron nitride (4)/the third metal foil (7-3) in the etching liquid to etch the third metal foil (7-3); after the third metal foil (7-3) is etched, the target substrate of the graphene (3)/the first boron nitride (2)/the base (1) formed in the step (7) is used for fishing the packaging layer (6)/the second boron nitride (4);
step 10: and etching the packaging layer (6)/the second boron nitride (4)/the graphene (3)/the first boron nitride (2) by using oxygen plasma to form a required sensitive element size, exposing the first electrode (5-2) and the second electrode (5-3), and finally finishing the manufacture of the PMMA-based graphene detonation pressure test sensor.
8. The manufacturing method of the PMMA-based graphene detonation pressure test sensor according to claim 7, is characterized in that: the first photoresist (8-1) and the second photoresist (8-2) adopt AZ4620 photoresist, and spin coating parameters are as follows: low speed 500rpm, time 9 s; high speed 1500rpm, time 30 s; the curing time was 20min, the temperature was 85 ℃.
9. The manufacturing method of the PMMA-based graphene detonation pressure test sensor according to claim 7, is characterized in that: the first photoresist (8-1) and the second photoresist (8-2) are removed through an exposure and development process, and the exposure time is 30 s; the developing solution is 5 per mill NaOH solution, and the developing time is 3 min.
10. The manufacturing method of the PMMA-based graphene bursting pressure test sensor according to claim 7, wherein the spin coating parameters of the packaging layer (6) are as follows: low speed 500rpm, time 5 s; high speed 2000rpm, time 20 s; curing time 30min, temperature 60 ℃.
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