CN108507719A - A method of referance leak is made based on graphene self-defect - Google Patents
A method of referance leak is made based on graphene self-defect Download PDFInfo
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- CN108507719A CN108507719A CN201810253643.5A CN201810253643A CN108507719A CN 108507719 A CN108507719 A CN 108507719A CN 201810253643 A CN201810253643 A CN 201810253643A CN 108507719 A CN108507719 A CN 108507719A
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- graphene
- polymethyl methacrylate
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- 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
- G01M3/007—Leak detector calibration, standard leaks
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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Abstract
The invention discloses a kind of methods of the referance leak based on graphene self-defect, single-layer graphene is made on copper foil first, a strata methyl methacrylate is applied on graphene, copper foil is removed using copper corrosion liquid, then graphene is put on the silicon chip having had openning hole, silicon chip is finally placed on KF40 sealing flanges by the transfer for completing graphene in dry about 1 hour, it is evenly coated in the surrounding of silicon chip using Torr Seal glue, stands 12 hours obtained single-layer graphene referance leaks cured above.The present invention proposes a kind of novel method for making referance leak, the size of the number of plies control channel of control graphene can be passed through, the referance leak of leak rate required for obtaining, therefore, referance leak leak rate size controllability is good, leak rate range is wide for this, small leakage rate measurement can be achieved, it is ensured that gas is in molecular flow condition in channel.
Description
Technical field
The present invention relates to a kind of referance leak and preparation method thereof, especially a kind of standard based on graphene self-defect
Leakage hole and preparation method thereof.
Background technology
In recent years, since there is graphene good mechanical property, permeance property and chemical stability to cause extensively
Concern.Graphene is by carbon atom by carbon simple substance made of hexagonal lattice proper alignment, and the connection between each carbon atom is non-
Often flexible, when applying external force, carbon atom face will produce flexural deformation, and carbon atom need not be rearranged to adapt to external force, maintain
The stabilization of structure.Currently, carrying out infiltration and the Separation Research of gas using graphene or graphene oxide, there are mainly two types of sides
To first is the defect using graphene or graphene oxide itself in the production process；Another kind is by extraneous means, example
Such as focused ion beam bombardment, high-temperature oxydation, beam bombardment, ultraviolet light irradiation utilize monomer chemistries synthetic method in stone
Manufacturing defect on black alkene or graphene oxide.Finally, referance leak is made using these of graphene or graphene oxide defect.
Referance leak is one kind having constant leak rate device in rated condition, is generally divided into channel-style referance leak and infiltration
Type referance leak.Osmosis type leakage hole is the leakage generated using the osmosis of gas；Channel-style leakage hole, which is utilization, to be limited
The leakage that the channel of gas flowing generates.The referance leak often said in vacuum leak hunting, effect be under given conditions to
The inside for the vacuum system studied provides known gas flow, and referance leak has very important in technical field of vacuum
Effect.
Currently used referance leak mainly has metal flattening type referance leak and glass-platinum filament type referance leak.This two
The size of kind referance leak is difficult to accurately control, leak rate size poor controllability, and leak rate range is relatively narrow, it is difficult to realize small leakage
The measurement of rate.Therefore, it is necessary to provide a kind of referance leak, leak rate size has certain controllability, leak rate range it is wide, it can be achieved that
Small leakage rate measurement, it is ensured that gas is in the features such as molecular flow condition always in channel.
Invention content
The present invention provides a kind of method of the referance leak based on graphene self-defect to solve the above problems.It will
Polymethyl methacrylate is coated with the copper foil of chemical vapor deposition graphene, after being put into corrosive liquid removal copper foil,
It cleans in deionized water；It transfers graphene to again on the silicon chip having had openning hole, the graphene after transfer is placed on evaporation
In ware, dry 60min；Acetone is poured into later and removes polymethyl methacrylate in evaporating dish, re-dry completes graphene
Transfer.Finally the silicon chip for the adhering to graphene back of the body is placed on KF40 flanges, is then sealed using Torr-Seal vacuum compounds
Silicon chip and flange, then stand about 12 hours obtained referance leaks.
The present invention solves technical problem and adopts the following technical scheme that：
A kind of method of the referance leak based on graphene self-defect of the present invention, coats poly- first in graphene copper foil first
Base methyl acrylate is subsequently placed into the corrosive liquid removal copper foil prepared, puts and clean in deionized water；Graphene is gone to again
On the silicon chip having had openning hole, the graphene after transfer is placed in evaporating dish, acetone is poured into evaporation by dry 60min later
Polymethyl methacrylate is removed in ware, re-dry completes the transfer of graphene, cures and referance leak is made.
As the preferred embodiment of the above method, the method operates as follows：
A, it takes a copper foil to be put into vacuum tube furnace, controls the concentration of hydrogen and methane, carry out the growth of graphene, finally wait for
Fast cooling is carried out after growth, and after temperature cooling, the graphene for obtaining single layer is deposited in copper foil surface；
B, on the graphene prepared polymethyl methacrylate is controlled with uniform spin coating polymethyl methacrylate
Thickness, first 800r/s continues 5s to sol evenning machine at a slow speed, then quick 3000r/s continues 10s；
C, a silicon chip is taken, is spiled on silicon chip using laser, acetone is used respectively on ultrasonic machine later, alcohol and goes
Ionized water cleans, the substrate as graphene；
D, it clamps the copper foil with graphene obtained in step b with tweezers to be put into etchant solution, the proportioning of corrosive liquid
For copper sulphate：Hydrochloric acid：Water=1:5:5, copper is eroded completely, graphene/polymethyl methacrylate of acquisition is placed on
It is cleaned in ionized water, obtains polymethyl methacrylate/graphene film；
E, after transferring graphene on the silicon chip that step c is obtained, it is put into evaporating dish dry 60min, completes single layer
The transfer of graphene obtains single-layer graphene/polymethyl methacrylate structure.If wanting to obtain multi-layer graphene/poly- methyl-prop
E pioic acid methyl ester structure after obtaining single-layer graphene/polymethyl methacrylate structure, removes polymethyl methacrylate, then do
After dry, then a layer graphene polymethyl methacrylate is shifted on it, bilayer graphene/poly- methyl-prop has just been obtained after drying
The structure of e pioic acid methyl ester repeats the step and can be obtained multi-layer graphene/polymethyl methacrylate structure；
F, the silicon chip of graphene-containing is placed on KF40 sealing flanges, by the aperture on silicon chip and the macropore phase on flange
It is corresponding, then using Torr-Seal vacuum compounds sealing silicon chip and flange, then stand about 12 hours obtained referance leaks.
As the preferred embodiment of the above method, in step a, copper foil, which is put into vacuum tube furnace, is evacuated to the left sides 10Pa
The right side, then half an hour be warming up to 1020 DEG C, then insulation annealing 60min.
As the preferred embodiment of the above method, in step b on the graphene prepared the poly- methyl-prop of uniform spin coating
E pioic acid methyl ester, thickness are controlled substantially in 300-500nm.
As the preferred embodiment of the above method, a diameter of 300-800um for being punched on silicon chip in step c.
As the preferred embodiment of the above method, it is put into copper corrosion liquid and impregnates 3 hours in step d.
It is third to remove the substance that polymethyl methacrylate uses as the preferred embodiment of the above method, in step e
Ketone.
Compared with the prior art, advantageous effects of the invention are embodied in：
1, the present invention makes referance leak using the defect of graphene, it is proposed that a kind of novel making ultrahigh vacuum standard
The processing method of leakage hole, this method are not only simple, it is easy to accomplish, the production method comparative maturity of graphene, compared to biography
The production method of system referance leak, the equipment that the present invention uses is few, and cost is relatively low, and success rate is high, can produce in batches.
2, since there is graphene very strong thermal stability, the referance leak that the present invention makes can be applied to complicated work
Condition condition.
3, the present invention can obtain required referance leak by the size of the number of plies control channel of control graphene.
Therefore, which has many advantages, such as that leak rate size controllability is good, leak rate range is wide, small leakage rate measurement can be achieved.
Description of the drawings
Fig. 1 is to make single-layer graphene/polymethyl methacrylate laminated film standard leakage based on graphene self-defect
Hole flow chart.
Fig. 2 is to make multi-layer graphene/polymethyl methacrylate laminated film standard leakage based on graphene self-defect
Hole flow chart.
Fig. 3 is a kind of molecular flow single-layer graphene/polymethyl methacrylate laminated film standard leakage of the related present invention
The diagrammatic cross-section in hole.
Figure label：1- single-layer graphenes, 2- copper foils, 3- polymethyl methacrylates, 4- copper corrosions liquid, 5- deionizations
Water, 6- silicon chips, 7-Torr-Seal vacuum compounds, 8-KF40 flanges.
Specific implementation mode
Embodiment 1：
It is operated as follows using the method that graphene self-defect makes referance leak in this example：
1, it takes a copper foil 2 to be put into vacuum tube furnace, the pipeline in vacuum tube furnace is carried out first with methane and hydrogen clear
Wash, be evacuated to 10Pa or so, then half an hour be warming up to 1020 DEG C, insulation annealing 60min, control containing for hydrogen and methane
Amount, carries out the growth of graphene, and fast cooling is carried out after finally to be grown, after temperature cooling, is deposited in copper foil surface
Obtain single-layer graphene 1；
2, the uniform spin coating polymethyl methacrylate 3 on the graphene prepared, first 800r/s continues sol evenning machine at a slow speed
5s, then quick 3000r/s continue 10s, and the thickness for measuring polymethyl methacrylate is 355nm.
3, a silicon chip is taken, a diameter of 500 microns of aperture is beaten on silicon chip using laser, makes respectively on ultrasonic machine later
With acetone, alcohol and deionized water 5 are cleaned, the substrate as graphene；
4, it clamps the copper foil with graphene obtained in step b with tweezers to be put into etchant solution, impregnate 3 hours, copper
The proportioning of corrosive liquid 4 is copper sulphate：Hydrochloric acid：Water=10g:50ml:50ml erodes copper completely, by the graphene of acquisition/poly-
Methyl methacrylate is put to be cleaned in deionized water, obtains polymethyl methacrylate/graphene film.
5, after transferring graphene on the silicon chip 6 that step 3 obtains, it is put into evaporating dish dry 60min, completes single layer
The transfer of graphene obtains single-layer graphene/polymethyl methacrylate structure.
6, the silicon chip of graphene-containing is placed on KF40 sealing flanges, by the aperture on silicon chip and the macropore phase on flange
It is corresponding, then using Torr-Seal vacuum compounds sealing silicon chip and flange, then stand about 12 hours obtained referance leaks.
Single-layer graphene manufactured in the present embodiment/polymethyl methacrylate laminated film leakage hole, test pressure range from
1000Pa to 7000Pa, leak rate minimum have basically reached the requirement of ultrahigh vacuum leakage hole in minus nine order of magnitude.
Embodiment 2：
This example and 1 operating process of example are essentially identical, and different places is after completing step 5, then shifts one on it
Layer graphene/polymethyl methacrylate has just obtained the structure of bilayer graphene/polymethyl methacrylate after drying.With
Single layer found after comparing, double-deck flow-rate ratio single layer it is about order of magnitude greater, test pressure range from 1000Pa to
7000Pa, leak rate minimum is in minus eight order of magnitude.
Embodiment 3：
This example and 1 operating process of example are essentially identical, and different places are after completing step 5, then by second graphite
It is spread after alkene cleaning on the first layer, dries 20min or so, then remove polymethyl methacrylate, then steps be repeated alternatively until
It is paved with five layers.Notice that the polymethyl methacrylate on layer 5 does not remove, drying.With bilayer graphene/poly- methyl-prop
The structure of e pioic acid methyl ester finds after being compared, about big two orders of magnitude of five layers of flow-rate ratio bilayer, test pressure range from
1000Pa to 7000Pa, leak rate minimum is in minus six order of magnitude.
Claims (7)
1. a kind of method making referance leak based on graphite itself alkene defect, it is characterized in that being coated first in graphene copper foil poly-
Methyl methacrylate is subsequently placed into the corrosive liquid removal copper foil prepared, puts and clean in deionized water；Graphene is turned again
Onto the silicon chip having had openning hole, the graphene after transfer is placed in evaporating dish, acetone is poured into steaming by dry 60min later
Polymethyl methacrylate is removed in hair ware, re-dry completes the transfer of graphene, cures and referance leak is made.
2. the method for making referance leak based on graphene self-defect according to 1, it is characterized in that operating as follows：
A, it takes a copper foil to be put into vacuum tube furnace, controls the concentration of hydrogen and methane, carry out the growth of graphene, it is last to be grown
After carry out fast cooling, after temperature cooling after, copper foil surface deposit obtain single layer graphene；
B, the uniform spin coating polymethyl methacrylate on the graphene prepared, controls the thickness of polymethyl methacrylate
Degree, first 800r/s continues 5s to sol evenning machine at a slow speed, then quick 3000r/s continues 10s；
C, a silicon chip is taken, is spiled on silicon chip using laser, uses acetone, alcohol and deionization respectively on ultrasonic machine later
Water cleans, the substrate as graphene；
D, it clamps the copper foil with graphene obtained in step b with tweezers to be put into etchant solution, the proportioning of corrosive liquid is sulphur
Sour copper：Hydrochloric acid：Water=1:5:5, copper is eroded completely, graphene/polymethyl methacrylate of acquisition is placed on deionization
It is cleaned in water, obtains polymethyl methacrylate/graphene film；
E, after transferring graphene on the silicon chip that step c is obtained, it is put into evaporating dish dry 60min, completes mono-layer graphite
The transfer of alkene obtains single-layer graphene/polymethyl methacrylate structure, if wanting to obtain multi-layer graphene/polymethylacrylic acid
Methyl esters structure after obtaining single-layer graphene/polymethyl methacrylate structure, removes polymethyl methacrylate, after re-dry,
It shifts a layer graphene polymethyl methacrylate on it again, bilayer graphene/polymethylacrylic acid has just been obtained after drying
The structure of methyl esters repeats the step and can be obtained multi-layer graphene/polymethyl methacrylate structure；
F, the silicon chip of graphene-containing is placed on KF40 sealing flanges, the aperture on silicon chip is opposite with the macropore on flange
It answers, then using Torr-Seal vacuum compounds sealing silicon chip and flange, then stands about 12 hours obtained referance leaks.
3. according to the method described in claim 2, it is characterized in that copper foil is put into vacuum tube furnace and is evacuated to 10Pa in step a
Left and right, then half an hour be warming up to 1020 DEG C, then insulation annealing 60min.
4. according to the method described in claim 2, it is characterized in that in step b on the graphene prepared the poly- methyl of uniform spin coating
Methyl acrylate, thickness are controlled substantially in 300-500nm.
5. according to the method described in claim 2, it is characterized in that a diameter of 300-800um punched on silicon chip in step c.
6. according to the method described in claim 2, being impregnated 3 hours it is characterized in that being put into step d in copper corrosion liquid.
7. according to the method described in claim 2, it is characterized in that remove polymethyl methacrylate in step e is using substance
Acetone.
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| CN112284634A (en) * | 2020-10-27 | 2021-01-29 | 北京卫星环境工程研究所 | Standard leak based on graphene and preparation method |
| CN113510988A (en) * | 2021-07-29 | 2021-10-19 | 北京卫星环境工程研究所 | Standard leak based on graphene/PMMA (polymethyl methacrylate) composite film and preparation method |
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| CN113510988A (en) * | 2021-07-29 | 2021-10-19 | 北京卫星环境工程研究所 | Standard leak based on graphene/PMMA (polymethyl methacrylate) composite film and preparation method |
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Application publication date: 20180907 |