CN113510988A - Standard leak based on graphene/PMMA (polymethyl methacrylate) composite film and preparation method - Google Patents

Standard leak based on graphene/PMMA (polymethyl methacrylate) composite film and preparation method Download PDF

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CN113510988A
CN113510988A CN202110864030.7A CN202110864030A CN113510988A CN 113510988 A CN113510988 A CN 113510988A CN 202110864030 A CN202110864030 A CN 202110864030A CN 113510988 A CN113510988 A CN 113510988A
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layer
graphene
pmma
metal
far away
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刘招贤
孟冬辉
闫荣鑫
孙立臣
任国华
韩琰
张骁
王莉娜
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Beijing Institute of Spacecraft Environment Engineering
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0079—Manufacture of membranes comprising organic and inorganic components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/021—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B9/045—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
    • G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
    • G01M3/202—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material using mass spectrometer detection systems
    • G01M3/205—Accessories or associated equipment; Pump constructions
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
    • G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
    • G01M3/207—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material calibration arrangements

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  • Chemical Kinetics & Catalysis (AREA)
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  • General Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The application provides a standard leak based on a graphene/PMMA composite film and a preparation method thereof, wherein the standard leak comprises a pressure side metal knife edge flange, a core infiltration assembly and a vacuum side metal knife edge flange; the core infiltration component comprises an infiltration part and a supporting part; the pressure side metal knife edge flange is connected to one side of the penetration part relatively far away from the supporting part in a sealing manner; the vacuum side metal knife edge flange is connected to one side of the supporting part relatively far away from the supporting part in a sealing manner; the permeation part comprises a first PMMA layer and a first graphene layer which are arranged in an attaching mode, and at least one second graphene layer which is arranged on one side, far away from the first PMMA layer, of the first graphene layer in an attaching mode; the supporting part is attached to one side of the permeation part, which is relatively far away from the first PMMA layer. This application had both had the advantage of graphite alkene film to gaseous extremely low leak rate, had solved the very easily damaged problem of graphite alkene film again, and in practical application, the accessible is adjusted the number of piles of second graphite alkene layer to the realization is to the control of leak rate size.

Description

Standard leak based on graphene/PMMA (polymethyl methacrylate) composite film and preparation method
Technical Field
The application relates to the technical field of ultrasensitive leak detection, in particular to a standard leak hole based on a graphene/PMMA composite film and a preparation method.
Background
In the existing leak rate detection technology, the helium mass spectrometry leak detection technology has the highest detection precision, and the leak detection limit of an ultra-sensitive leak detection system based on helium mass spectrometry can reach 10-15Pa·m3And s. The hypersensitive leak detection system mainly comprises a mass spectrometer and a standard leak hole, wherein the standard leak hole is equipment with known constant leak rate to leak-indicating gas under specific conditions, plays a role in leak rate calibration in leak detection, and generally requires that the deviation between the leak rate of the standard leak hole and the leak rate of a product to be detected does not exceed one order of magnitude. However, the limit of the current standard orifice is 10-12Pa·m3And/s is three orders of magnitude larger than the limit of the ultra-sensitive leak detection system, and the accuracy of the test result of the tested product with small leak rate is influenced.
Graphene is a two-dimensional material with a single atomic layer in which carbon atoms are regularly arranged, and the crystal lattice of the graphene has a compact electron cloud structure. Nano Lett.2008,8(8)2458-2462 reported that defect-free graphene is impermeable to any gas. The graphene prepared by a Chemical Vapor Deposition (CVD) method has molecular-scale intrinsic pores, and when gas passes through a CVD graphene film, only the gas with the molecular size smaller than the intrinsic pore size can be allowed to pass at an extremely low and stable rate due to the size discrimination effect, so that the gas leakage rate is controlled. However, the CVD graphene thin film with atomic-scale thickness has insufficient mechanical strength, and is liable to generate large pores, which have large leakage rate to gas, so that the leakage rate of the CVD graphene thin film is difficult to decrease, and the generation of the pores has randomness, so that the controllability of the leakage rate of the CVD graphene thin film is poor.
Disclosure of Invention
The application aims to solve the problems and provides a standard leak based on a graphene/PMMA composite film and a preparation method.
In a first aspect, the application provides a standard leak based on a graphene/PMMA composite film, which comprises a pressure side metal edge flange, a core infiltration assembly and a vacuum side metal edge flange; wherein the core infiltration assembly comprises an infiltration section and a support section; the pressure side metal knife edge flange is connected to one side of the penetration part, which is relatively far away from the supporting part in a sealing manner; the vacuum side metal knife edge flange is connected to one side of the supporting part, which is relatively far away from the supporting part in a sealing manner;
the permeation part comprises a first PMMA layer and a first graphene layer which are arranged in an attaching mode, and at least one second graphene layer which is arranged on one side, far away from the first PMMA layer, of the first graphene layer in an attaching mode; the supporting part is attached to one side, relatively far away from the first PMMA layer, of the penetrating part; the support portion has a penetration through hole.
According to the technical scheme provided by some embodiments of the application, the supporting part comprises a metal cushion layer and a coating layer which are tightly attached; one side of the film coating layer, which is relatively far away from the metal cushion layer, is hermetically connected with the pressure side metal knife edge flange; and one side of the coating layer, which is relatively far away from the metal cushion layer, is hermetically connected with the vacuum side metal knife edge flange.
According to the technical scheme provided by some embodiments of the application, the coating layer comprises a titanium film layer and a platinum film layer; the thickness of the titanium film layer is 5 nm; the thickness of the platinum film layer is 200 nm.
According to the technical scheme provided by certain embodiments of the application, the diameter of the permeation through hole is 5 μm.
In a second aspect, the application provides a method for preparing a standard leak based on a graphene/PMMA composite film, the method comprising the following steps:
preparing a permeable part of the core permeable component; the permeation part comprises a first PMMA layer and a first graphene layer which are arranged in an attaching mode, and at least one second graphene layer which is arranged on one side, far away from the first PMMA layer, of the first graphene layer in an attaching mode;
preparing a supporting part of the core infiltration component; the supporting part is provided with a penetration through hole;
transferring the permeate onto the support to obtain a core permeate assembly;
one side of the permeation part of the core permeation assembly is hermetically connected with a pressure side metal knife edge flange, and one side of the supporting part is hermetically connected with a vacuum side metal knife edge flange.
According to the technical scheme provided by certain embodiments of the application, the specific steps for preparing the permeable part of the core permeable component comprise:
selecting a first metal foil with graphene growing on two sides, spin-coating PMMA on the surface of one side of the first metal foil, and heating and curing to form a first PMMA layer;
removing graphene on one side, relatively far away from the first PMMA layer, of the first metal foil by using oxygen plasma;
etching the metal foil layer of the first metal foil by using ferric chloride etching solution, wherein the remaining graphene attached to the first PMMA layer is the first graphene layer;
washing the attached first PMMA layer and the first graphene layer by using deionized water to obtain a single-layer graphene/PMMA composite film;
transferring the single-layer graphene/PMMA composite film onto a second metal foil, and attaching the first graphene layer to the graphene layer on one side of the second metal foil; and etching the metal foil layer of the second metal foil and the graphene layer relatively far away from the first graphene layer to obtain the double-layer graphene/PMMA composite film.
According to the technical scheme provided by certain embodiments of the application, the specific steps of preparing the supporting part of the core infiltration component comprise:
selecting a metal gasket with two polished surfaces as a metal cushion layer;
thinning the center of one side of the metal gasket;
punching the thinned area of the metal gasket to obtain the permeation through hole;
and coating a film on one side of the metal gasket relatively far away from the thinning area to obtain a film coating layer.
According to the technical scheme provided by some embodiments of the application, the penetration through hole is obtained by adopting a laser etching method; the diameter of the permeation through hole is 5 μm.
According to the technical scheme provided by some embodiments of the application, the plating on the side of the metal gasket relatively far away from the thinning area to obtain the plated film layer specifically comprises:
plating titanium with the thickness of 5nm on one side of the metal gasket, which is relatively far away from the thinning area, so as to obtain a titanium film layer;
and plating platinum with the thickness of 200nm on the surface of one side of the titanium film layer relatively far away from the metal gasket to obtain a platinum film layer.
According to the technical solution provided by some embodiments of the present application, the step of transferring the permeable section to the support section to obtain the core permeable module further comprises:
and spin-coating PMMA on the surface of one side of the permeation part relatively far away from the support part, and heating and drying to obtain a second PMMA layer.
Compared with the prior art, the beneficial effect of this application: the permeation part of the core permeation component based on the standard leak hole of the graphene/PMMA composite film comprises a single-layer graphene/PMMA composite film consisting of a first PMMA layer and a first graphene layer and at least one second graphene layer which is attached to one side, far away from the first PMMA layer, of the first graphene layer, and the standard leak hole has the advantage that the leakage rate of the graphene film to gas is extremely low due to the arrangement of the first graphene layer and the second graphene layer; the supporting part is arranged, so that a good supporting effect on the permeation part can be achieved; through setting up pressure side metal edge of a knife flange and vacuum side metal edge of a knife flange, when using, pressure side metal edge of a knife flange is linked together with the air supply room for standard leak hunting hole provides the leakage indicating gas, vacuum side metal edge of a knife flange and leak hunting system's real empty room is sealed to be communicated, is favorable to providing the leakage indicating gas of stable leak hunting for leak hunting system, thereby carries out the leak hunting test.
Drawings
Fig. 1 is a schematic structural diagram of a standard leak based on a graphene/PMMA composite film provided in an embodiment of the present application;
FIG. 2 is a process flow diagram for preparing a permeate portion of a core permeate module;
FIG. 3 is a process flow diagram for preparing a support portion of a core infiltration module.
The text labels in the figures are represented as:
1. a pressure side metal knife edge flange; 2. a core infiltration module; 201. a first PMMA layer; 202. a first graphene layer; 203. a second graphene layer; 204. a second PMMA layer; 205. a metal pad layer; 206. coating a film layer; 207. penetrating through the through hole; 3. a vacuum side metal knife edge flange; 4. a pressure side gas source interface; 5. a vacuum chamber interface flange.
Detailed Description
The following detailed description of the present application is given for the purpose of enabling those skilled in the art to better understand the technical solutions of the present application, and the description in this section is only exemplary and explanatory, and should not be taken as limiting the scope of the present application in any way.
As shown in fig. 1, the embodiment provides a standard leak based on a graphene/PMMA composite film, which includes a pressure side metal edge flange 1, a core permeation component 2, and a vacuum side metal edge flange 3; wherein the core infiltration module 2 comprises an infiltration part and a support part; the pressure side metal knife edge flange 1 is connected to one side of the penetration part, which is relatively far away from the supporting part in a sealing manner; the vacuum side metal knife edge flange 3 is connected to one side of the supporting part, which is relatively far away from the supporting part in a sealing manner; the permeation part comprises a first PMMA layer 201 and a first graphene layer 202 which are arranged in an attaching mode, and at least one second graphene layer 203 which is arranged on one side, far away from the first PMMA layer 201, of the first graphene layer 202 in an attaching mode, in the embodiment, one second graphene layer 203 is arranged, in other embodiments of the application, the number of layers of the second graphene layer 203 can be adjusted according to actual needs, and therefore control over the leakage rate is achieved; the supporting part is attached to one side, far away from the first PMMA layer 201 relatively, of the penetration part, plays a role in fixed support for the penetration part, is provided with a penetration through hole 207 through which leakage gas can pass, and the diameter of the penetration through hole 207 can be adjusted according to actual leakage rate requirements during preparation.
Further, the support part comprises a metal cushion layer 205 and a coating layer 206 which are tightly attached; one side of the coating layer 206 relatively far away from the metal cushion layer 205 is hermetically connected with the pressure side metal edge flange 1; the side of the coating layer 206 relatively far away from the metal cushion layer 205 is hermetically connected with the vacuum side metal edge flange 3. Preferably, the metal gasket is an oxygen-free copper gasket.
Further, the coating layer 206 includes a titanium film layer and a platinum film layer; the thickness of the titanium film layer is 5 nm; the thickness of the platinum film layer is 200 nm. The coating layer 206 can prevent the etching liquid remained on the penetration part from partially etching the metal pad layer 205, so as to prevent the bonding effect of the penetration part and the supporting part from being affected and prevent the leakage from the contact surface of the penetration part and the supporting part.
Further, the diameter of the penetration through hole 207 is 5 μm.
Further, the area of the penetration part is smaller than that of the support part, and a second PMMA layer 204 is arranged on one side of the penetration part relatively far from the second graphene layer 203 and on one surface of the support part relatively close to the penetration part and is not covered by the penetration part; the second PMMA layer 204 is a protective layer, the penetrating part is sealed in a space surrounded by the second PMMA layer 204 and the supporting part, and the second PMMA layer 204 is arranged to be beneficial to enhancing the close fitting performance and the sealing performance of the pressure side metal knife edge flange 1 and the core penetrating component 2.
The preparation method of the standard leak based on the graphene/PMMA composite film comprises the following steps:
s1, preparing a permeable part of the core permeable component, wherein the process flow diagram is shown in figure 2, and the process flow diagram specifically comprises the following steps:
s11, selecting a first metal foil with the thickness of 25 mu m and the two sides growing CVD graphene, cutting the size of the first metal foil to 10mm multiplied by 10mm, randomly dividing the two sides of the first metal foil into a pressure side and a vacuum side, spin-coating PMMA on the pressure side surface of the first metal foil, setting the rotation speed to 3000rpm and continuing for 60S, and then placing the first metal foil on a hot plate at 170 ℃ for 3min to solidify the PMMA to form a first PMMA layer 201;
s12, removing the graphene on the vacuum side of the first metal foil by using oxygen plasma, and setting the etching power to be 100W and the etching time to be 60S;
s13, suspending the first metal foil with the vacuum-side graphene etched away on the liquid level of the ferric chloride etching solution, and making one side of the metal foil layer of the first metal foil, which is relatively far away from the first PMMA layer 201, contact with the ferric chloride etching solution, and after the metal foil layer of the first metal foil is completely etched, the remaining graphene attached to the first PMMA layer 201 is the first graphene layer 202; wherein, the proportion of the ferric chloride etching liquid is anhydrous ferric chloride: water: concentrated hydrochloric acid 16 g: 50 ml: 50 ml;
s14, fishing out the first PMMA layer 201 and the first graphene layer 202 which are attached to each other by using a glass slide, suspending the first PMMA layer 201 and the first graphene layer 202 on the surface of deionized water by using the tension of the water, standing and cleaning for 30min, and repeatedly cleaning at least three times to complete the preparation of the single-layer graphene/PMMA composite film, wherein the single-layer graphene/PMMA composite film is the first PMMA layer 201 and the first graphene layer 202 which are attached to each other;
s15, selecting a second metal foil with the thickness of 25 mu m and the two sides growing with CVD graphene, cutting the size of the second metal foil to 15mm multiplied by 15mm, transferring the single-layer graphene/PMMA composite film prepared in the step S14 to graphene on any side of the second metal foil to obtain a first intermediate assembly, and placing the first intermediate assembly in a drying box for standing for 48 hours; a graphene layer adjacent to the single-layer graphene/PMMA composite film on the second metal foil is marked as a second graphene layer 203, and the single-layer graphene/PMMA composite film is required to be ensured to be positioned at the center of the second metal foil during transfer;
s16, placing the first intermediate assembly on a hot plate at 120 ℃ for 10min, wherein the first graphene layer 202 and the second graphene layer 203 of the single-layer graphene/PMMA composite film are tightly attached, and no redundant impurities exist in the middle;
s17, etching the second metal foil in the first intermediate assembly away from the graphene layer of the single-layer graphene/PMMA composite film, and etching the metal foil layer of the second metal foil in the first intermediate assembly to obtain a double-layer graphene/PMMA composite film; the etching manner in this step is similar to that in steps S12 and S13, and therefore, the description thereof is omitted here.
It should be noted that the permeable part of the core permeable module prepared in this embodiment is a double-layer graphene/PMMA composite film, that is, the core permeable module includes a first graphene layer 202 and a second graphene layer; in other embodiments of the present application, the permeable portion of the core permeable component may be a multi-layer graphene/PMMA composite film, i.e., comprising one first graphene layer and at least two second graphene layers; the preparation process of the multilayer graphene/PMMA composite film is that the double-layer graphene/PMMA composite film is tightly attached to graphene on one side of a new metal foil with CVD graphene growing on two sides, and then the other time of graphene and the metal foil layer of the new metal foil are etched, so that the number of second graphene layers is the number of new metal foils.
S2, preparing a supporting part of the core infiltration component, wherein the process flow diagram is shown in figure 3, and the process flow diagram specifically comprises the following steps:
s21, selecting a double-sided polished oxygen-free copper gasket as the metal cushion layer 205, wherein the diameter of the gasket is 21.4mm, the thickness of the gasket is 2mm, and milling a conical table with the bottom surface diameter of 8mm, the top surface diameter of 1mm and the shaft height of 1.5mm by using CNC in the central area of one side of the oxygen-free copper gasket to ensure that the residual thickness of the central area of the copper gasket is 0.5 mm; then, punching holes in the central area of the gasket by utilizing laser etching to obtain a penetration through hole 2007, wherein the diameter of a pore of the penetration through hole 207 is 5 microns;
s22, ultrasonically cleaning the oxygen-free copper gasket by using dilute hydrochloric acid, acetone and ethanol, drying the oxygen-free copper gasket by using nitrogen, and then respectively carrying out physical weather deposition of titanium/platinum on one side of the oxygen-free copper gasket, which is relatively far away from the conical table, by using a magnetron sputtering coating instrument to form a coating layer 206, wherein the titanium coating layer is firstly coated and then coated with platinum, and the thickness of the titanium coating layer is 5 nm; the thickness of the platinum film layer is 200nm, and the preparation of the core permeation component supporting part is completed.
S3, transferring the penetration part onto the supporting part to obtain a core penetration assembly, which specifically comprises:
s31, transferring the double-layer graphene/PMMA composite film prepared in the step S17 to the center of the oxygen-free copper gasket substrate prepared in the step S22, and enabling the second graphene layer 203 of the double-layer graphene/PMMA composite film to be tightly attached to the surface, provided with the titanium platinum coating, of the oxygen-free copper gasket;
s32, placing the penetration part and the support part which are tightly attached in the step S31 into a drying box to stand still for 48 hours for drying;
s33, spin-coating PMMA on the surface of the side, away from the conical table, of the closely-adhered penetration part and the support part dried in the step S32, setting the rotation speed to be 1500rpm and continuing for 60S, then placing the support part on a hot plate at 170 ℃ for 3min to cure the PMMA to form a second PMMA layer 204, wherein the second PMMA layer 204 is a protective layer, and thus, the preparation of the core penetration assembly is completed.
S4, hermetically connecting a pressure side metal knife edge flange 1 on one side of a permeation part of the core permeation assembly, and hermetically connecting a vacuum side metal knife edge flange 3 on one side of a supporting part, so as to finish the preparation of the standard leak hole based on the graphene/PMMA composite film.
The pressure side metal knife edge flange 1 is communicated with the gas source chamber through a pressure side gas source interface 4 and is used for providing leakage-showing gas for the standard leakage hole; vacuum side metal edge flange 3 passes through vacuum chamber interface flange 5 and the sealed intercommunication of vacuum chamber of leak hunting system, and when using, the indoor leakage-indicating gas of air supply reaches the infiltration portion of core infiltration subassembly through pressure side air supply interface to pass the infiltration through-hole 207 on the supporting part and get into the vacuum side, provide the leakage-indicating gas of stable leak rate for the leak hunting system.
Optionally, the first metal foil is a copper foil or a nickel foil; the second metal foil is copper foil or nickel foil; in this embodiment, the first metal foil and the second metal foil are both copper foils.
The graphene/PMMA composite film-based standard leak prepared by the preparation method has the following advantages:
(1) the mechanical strength of the graphene/PMMA composite film is obviously superior to that of the graphene film, the graphene/PMMA composite film can bear the air pressure of more than 200kPa on a substrate with pores with micron-sized, the leakage rate stability of the composite film is good, and the graphene/PMMA composite film can be produced in batches;
(2) due to the nanometer-scale thickness of the graphene/PMMA composite film, the response speed of the standard leak hole manufactured by the method to the change of the pressure side air pressure is less than 2s, and is superior to the response speed of the current common quartz-type standard leak hole for hours.
(3) The standard leak hole of the double-layer graphene/PMMA composite film manufactured by the invention is 10-15Pa·m3The/s order is superior to the prior common quartz type standard leak hole 10-11Pa·m3The leakage rate of the order of/s can be used for an ultra-sensitive leakage detection system, and the reliability of ultra-sensitive leakage detection is improved.
The principles and embodiments of the present application are explained herein using specific examples, which are provided only to help understand the method and the core idea of the present application. The foregoing is only a preferred embodiment of the present application, and it should be noted that there are no specific structures which are objectively limitless due to the limited character expressions, and it will be apparent to those skilled in the art that a plurality of modifications, decorations or changes can be made without departing from the principle of the present invention, and the technical features mentioned above can be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention in other instances, which may or may not be practiced, are intended to be within the scope of the present application.

Claims (10)

1. The standard leak based on the graphene/PMMA composite film is characterized by comprising a pressure side metal knife edge flange (1), a core infiltration assembly (2) and a vacuum side metal knife edge flange (3); wherein the core infiltration assembly (2) comprises an infiltration section and a support section; the pressure side metal knife edge flange (1) is connected to one side of the penetration part, which is relatively far away from the supporting part in a sealing manner; the vacuum side metal knife edge flange (3) is connected to one side of the supporting part, which is relatively far away from the supporting part in a sealing manner;
the permeation part comprises a first PMMA layer (201) and a first graphene layer (202) which are arranged in an attaching mode, and at least one second graphene layer (203) which is arranged on one side, far away from the first PMMA layer (201), of the first graphene layer (202) in an attaching mode; the supporting part is attached to one side of the permeation part, which is relatively far away from the first PMMA layer (201); the support portion has a penetration through hole (207).
2. The graphene/PMMA based composite film standard leak of claim 1, wherein the support part comprises a metal cushion layer (205) and a coating layer (206) which are closely attached; one side of the film coating layer (206) relatively far away from the metal cushion layer (205) is hermetically connected with the pressure side metal edge flange (1); one side of the film coating layer (206) relatively far away from the metal cushion layer (205) is hermetically connected with the vacuum side metal edge flange (3).
3. The graphene/PMMA based composite thin film standard leak according to claim 2, characterized in that the coating layer (206) comprises a titanium film layer and a platinum film layer; the thickness of the titanium film layer is 5 nm; the thickness of the platinum film layer is 200 nm.
4. The graphene/PMMA composite film based standard leak according to claim 1, characterized in that the diameter of the permeation through hole (207) is 5 μm.
5. A preparation method of a standard leak hole based on a graphene/PMMA composite film is characterized by comprising the following steps:
preparing a permeable part of the core permeable component; the permeation part comprises a first PMMA layer and a first graphene layer which are arranged in an attaching mode, and at least one second graphene layer which is arranged on one side, far away from the first PMMA layer, of the first graphene layer in an attaching mode;
preparing a supporting part of the core infiltration component; the supporting part is provided with a penetration through hole;
transferring the permeate onto the support to obtain a core permeate assembly;
one side of the permeation part of the core permeation assembly is hermetically connected with a pressure side metal knife edge flange, and one side of the supporting part is hermetically connected with a vacuum side metal knife edge flange.
6. The graphene/PMMA composite film based standard leak preparation method according to claim 5, wherein the specific step of preparing the penetration part of the core penetration assembly comprises:
selecting a first metal foil with graphene growing on two sides, spin-coating PMMA on the surface of one side of the first metal foil, and heating and curing to form a first PMMA layer;
removing graphene on one side, relatively far away from the first PMMA layer, of the first metal foil by using oxygen plasma;
etching the metal foil layer of the first metal foil by using ferric chloride etching solution, wherein the remaining graphene attached to the first PMMA layer is the first graphene layer;
washing the attached first PMMA layer and the first graphene layer by using deionized water to obtain a single-layer graphene/PMMA composite film;
transferring the single-layer graphene/PMMA composite film onto a second metal foil, and attaching the first graphene layer to the graphene layer on one side of the second metal foil; and etching the metal foil layer of the second metal foil and the graphene layer relatively far away from the first graphene layer to obtain the double-layer graphene/PMMA composite film.
7. The graphene/PMMA composite film based standard leak preparation method according to claim 5, wherein the specific step of preparing the support part of the core infiltration assembly comprises:
selecting a metal gasket with two polished surfaces as a metal cushion layer;
thinning the center of one side of the metal gasket;
punching the thinned area of the metal gasket to obtain the permeation through hole;
and coating a film on one side of the metal gasket relatively far away from the thinning area to obtain a film coating layer.
8. The graphene/PMMA composite film based standard leak preparation method according to claim 7, characterized in that the penetration through hole is obtained by a laser etching method; the diameter of the permeation through hole is 5 μm.
9. The graphene/PMMA composite film-based standard leak hole preparation method of claim 7, wherein a coating layer is obtained by coating on a side of the metal gasket relatively far away from the thinning area, and the method specifically comprises the following steps:
plating titanium with the thickness of 5nm on one side of the metal gasket, which is relatively far away from the thinning area, so as to obtain a titanium film layer;
and plating platinum with the thickness of 200nm on the surface of one side of the titanium film layer relatively far away from the metal gasket to obtain a platinum film layer.
10. The graphene/PMMA composite film based standard leak hole preparation method according to claim 5, wherein the step of transferring the penetration part to the support part to obtain the core penetration assembly further comprises the following steps:
and spin-coating PMMA on the surface of one side of the permeation part relatively far away from the support part, and heating and drying to obtain a second PMMA layer.
CN202110864030.7A 2021-07-29 2021-07-29 Standard leak based on graphene/PMMA (polymethyl methacrylate) composite film and preparation method Pending CN113510988A (en)

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Application publication date: 20211019