CN105738038B - A kind of molecular flow referance leak and preparation method thereof - Google Patents
A kind of molecular flow referance leak and preparation method thereof Download PDFInfo
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- CN105738038B CN105738038B CN201610074144.0A CN201610074144A CN105738038B CN 105738038 B CN105738038 B CN 105738038B CN 201610074144 A CN201610074144 A CN 201610074144A CN 105738038 B CN105738038 B CN 105738038B
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- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
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- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
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Abstract
The present invention relates to a kind of molecular flow referance leaks and preparation method thereof.The purpose of the present invention is to solve referance leaks in the prior art can not ensure in the range of atmospheric pressure in molecular flow condition, leak rate size poor controllability, it is difficult to the problems such as obtaining predetermined leak rate size and complex manufacturing process.Referance leak provided by the present invention, structure include the first substrate, the first sealing material, the second substrate, the second sealing material, porous material；And the effective coverage that formation preliminary dimension and gas can pass through on the porous material, the effective coverage size are controllable.The leak rate Q of referance leak can pass through formulaC=A σ Cs, Q=C × (p1‑p2) calculate determine.Therefore, which has many advantages, such as in the range of atmospheric pressure in molecular flow condition, leak rate size is controllable, can obtain predetermined leak rate size and manufacturing process is simple.The present invention also provides the production methods of above-mentioned standard leakage hole.
Description
Technical field
The present invention relates to a kind of molecular flow referance leak and preparation method thereof, especially a kind of channel-style referance leak and its
Production method.
Background technology
So-called referance leak, be manufactured exclusively for vacuum leak hunting and calibration, can be under certain condition to vacuum
Internal system provides the element of known gas flow.The specification of referance leak is exactly provided gas flow (i.e. leak rate), and one
As to indicate corresponding gaseous species, temperature, pressure condition.If do not specialized, refer to temperature as 23 DEG C ± 7 DEG C, enter
Mouth pressure is 100kPa ± 5%, and outlet pressure is less than the leak rate of the dry air (its dew-point temperature is less than -25 DEG C) of 1kPa.It
It is a kind of common essential metering outfit in vacuum science technology and its application field, with referance leak manufacturing technology
Development, application field is also increasingly wider.Such as all must in aerospace field, spacecraft, suit etc. before heaven
Stringent leak detection need be passed through, the size of leak rate is by the normal use for directly affecting spacecraft and the life security of astronaut.
And the leakage detecting instrument used at present can not all directly give the leak rate size of detected pieces, it is necessary to rely on referance leak in identical item
It compares under part, can just draw the leak rate value of detected pieces.Therefore, the leak rate size of referance leak and controllability will directly affect inspection
The accuracy of drain junction fruit.
The core of referance leak is to generate the leakage hole element of constant leak rate, by the gas leakage mechanism of leakage hole element, can be divided into and ooze
Saturating type referance leak and channel-style referance leak.Referring to Liu Xiu woodss in document《Aviation measures technology》Vol.21, No.5,43-45
(2001) " referance leak and its calibration " one text, currently used referance leak include the non-matching referance leak of platinum filament-glass and
Metal flattening type referance leak.The non-matching referance leak of platinum filament-glass, be it is a kind of by diameter 0.1-0.15mm platinum filament with
11#After hard glass does unmatched sealing, the leakage hole obtained from two kinds of material expand coefficient differences；Metal flattening type standard
Leakage hole is a kind of by the oxygen-free copper pipe of certain diameter or can to cut down the standard for generating leak after effective hydraulic press flattens and being formed and leak
Hole.The leak rate scope of both referance leaks is generally 10-6~10-8Hold in the palm liter/second, leak rate narrow range, it is difficult to realize more small
The metering of leak rate；And the size of referance leak is difficult to accurately control in the production process, can not ensure in atmospheric pressure model
In molecular flow condition in enclosing, cause leak rate size poor controllability, it is difficult to obtain predetermined leak rate size, leak rate must be by it
Its equipment is demarcated (reference can be made to ten thousand clear will, leaf Sheng et al. is in document《Vacuum electronics technology》" mark in No.2,39-41 (2002)
Some problem and its solution in a quasi- Leak calibration " text).
Therefore, be badly in need of design one kind in the range of atmospheric pressure in molecular flow condition, leak rate size is controllable, can obtain
Predetermined leak rate size and the simple referance leak of manufacturing process.
The content of the invention
It can not ensure to be in the range of atmospheric pressure the purpose of the present invention is to solve referance leak in the prior art
Molecular flow condition, leak rate size poor controllability, it is difficult to the problems such as obtaining predetermined leak rate size and complex manufacturing process, and provide
A kind of molecular flow referance leak and preparation method thereof solves the above problems.
A kind of molecular flow referance leak includes the first substrate, the first sealing material, the second substrate, the second sealing material, more
Porous materials；And the effective coverage that formation preliminary dimension and gas can pass through on the porous material；
First substrate is connected with the second substrate by the first sealing material；Second substrate passes through with porous material
Second sealing material is connected；Effective coverage size is controllable；The leak rate Q of referance leak can be determined by calculation.
The material of first substrate is oxygen-free copper, and the material of the second substrate is silicon<100>.
First sealing material is Agilent vacuum AB fluid sealants (Torr seal).
Second sealing material is a kind of high vacuum leakproof seal agent (VacSeal).
The porous material be bilateral porous anodic aluminium oxide, specification AAO-DP-12, aperture 70nm, pitch of holes
110nm, 50-70 μm of hole depth.
Effective coverage is formed by magnetron sputtering technology on the porous material, plates one on the porous material
The Al films of layer 150-300nm thickness cover other parts of the porous material surface in addition to effective coverage, therefore can be porous
The square effective coverage that the length of side is 70-300 μm is formed at material surface center, due to not covered by Al films, gas can be suitable
Profit passes through the nano-porous structure in effective coverage.
The leak rate Q of the referance leak can be determined by procedure below：
First, the conductance C of single nano-poresIt can be represented by the formula：
Wherein R is the gas constant of experimental gas, and T is environment temperature, and μ is the molal weight of gas, and d is on porous material
The diameter of nano-pore, l are the depth of nano-pore on porous material；
2nd, the conductance C of referance leak can be represented by following formula：
C=A σ Cs (2)
Wherein A is the area of effective coverage, and σ is the number of nano-pore in unit area；
3rd, the leak rate Q of referance leak can be represented by following formula：
Q=C × (p1-p2) (3)
Wherein p1It is that referance leak gas inflow side pressure is strong, p2It is referance leak gas outflow end pressure.
A kind of production method of molecular flow referance leak, comprises the following steps：
A, the through hole of preliminary dimension is formed in the first substrate and the second substrate；
B, the first substrate processed and the second substrate are placed on through over cleaning in 130 DEG C of baking oven and heat 30min, so
Oxygen gas plasma processing is carried out to it afterwards；Then diluted second sealing material of solvent is passed through in one layer of spin coating in the second substrate
Material；
C, porous material is placed in the second substrate for coating the second sealing material, slowly firmly compress, make its with
Second substrate is in close contact, and 30min is then heated in 250 DEG C of thermal station cures the second sealing material；
D, form the effective coverage that preliminary dimension and gas can pass through in porous material surface, ensure effective coverage with
Through hole alignment in first substrate and the second substrate；
E, the first substrate with installing the second substrate of porous material is connected, completes the making of this referance leak.
Through hole in the step a in the second substrate is processed to be formed by laser drilling, aperture
The vacuum degree of the step b plasmas processing is 25Pa, power 60w, bombardment time 5min；Second
The spin coating thickness of sealing material is 400-500nm, and retarder thinner is toluene.
Compared with the prior art, a kind of molecular flow referance leak provided by the present invention and preparation method thereof, because porous
The parameters such as aperture, the hole depth of material it is known that and effective coverage area it is controllable；Then, formula is passed through：(formula
In, R is the gas constant of experimental gas, and T is environment temperature, and μ is the molal weight of gas, and d is nano-pore on porous material
Diameter, l are the depth of nano-pore on porous material), C=A σ Cs(in formula, A is the area of effective coverage, and σ is in unit area
The number of nano-pore), Q=C × (p1-p2) (in formula, p1It is that referance leak gas inflow side pressure is strong, p2It is referance leak gas stream
Outlet pressure) the leak rate Q of referance leak can be calculated.Therefore, which has is in molecule in the range of atmospheric pressure
Stream mode, leak rate size are controllable, can obtain the advantages that predetermined leak rate size and manufacturing process are simple.
Description of the drawings
Fig. 1 is the first substrate of the related embodiment of the present invention and the schematic diagram of the second substrate.
Fig. 2 is the schematic diagram of the second sealing material of spin coating in the second substrate shown in Fig. 1.
Fig. 3 is to install the schematic diagram of porous material shown in Fig. 2 in the second substrate.
Fig. 4 is a kind of diagrammatic cross-section of molecular flow referance leak of the related present invention.
Wherein, the first substrates of 1-, the first sealing materials of 2-, the second substrates of 3-, the second sealing materials of 4-, 5- porous materials,
6- effective coverages.
Specific embodiment
The embodiment of the present invention will be described in further detail below in conjunction with the accompanying drawings.
Referring to Fig. 4, a kind of molecular flow referance leak that first embodiment of the invention is provided, including the first substrate 1, first
Sealing material 2, the second substrate 3, the second sealing material 4, porous material 5；And preliminary dimension and gas are formed on the porous material
The effective coverage 6 that can be passed through；
First substrate 1 is connected with the second substrate 3 by the first sealing material 2；Second substrate 3 and porous material
5 are connected by the second sealing material 4；6 size of effective coverage is controllable；The leak rate Q of referance leak can be determined by calculation.This reality
There is provided referance leak is applied available for the measurement of minipump pumping speed, the Registration of helium mass spectrometer leak detector, gas-solid interface
In scientific research, the fields such as the gas of tiny flow quantity are provided.
Wherein, the material of the first substrate 1 be oxygen-free copper, the model of mounting flange when specific size is detected by referance leak
It determines；The material of second substrate 3 can be silicon, it is preferred that be silicon<100>.First sealing material 2 is Agilent vacuum AB fluid sealants
(Torr seal).Second sealing material 4 is a kind of high vacuum leakproof seal agent (VacSeal).Porous material 5 is porous for bilateral
Anodised aluminium, specification AAO-DP-12, aperture 70nm, pitch of holes 110nm, 50-70 μm of hole depth.Effective district on porous material 5
The formation in domain 6 and the specific method of size Control include：Effective coverage 6 is to pass through magnetron sputtering technology on porous material 5
It is formed, the Al films of one layer of 150-300nm thickness is plated on porous material 5, by 5 surface of porous material in addition to effective coverage 6
Other parts cover, therefore the square effective coverage that the length of side is 70-300 μm can be formed at 5 centre of surface of porous material
6, due to not covered by Al films, gas can pass through the nano-porous structure in effective coverage 6.
The calculating for the referance leak leak rate that the present embodiment is provided will be described in detail below.Such as pressure is atmospheric pressure
Helium, under conditions of 20 DEG C, mean free path λ=189nm, due toTherefore the standard that the present embodiment is provided
For leakage hole in molecular flow condition in the range of atmospheric pressure, conductance, which can use, gram exerts once (Knusen) formula calculating.The present embodiment
A diameter of d of nano-pore, length l, and l >=20d on middle porous material, the leak rate Q of referance leak can be true by procedure below
It is fixed：
First, the conductance C of single nano-poresIt can be represented by the formula：
R is the gas constant of experimental gas in the present embodiment：8.315J/ (Kmol), T are environment temperatures：T=293K, μ
It is the molal weight of gas:μ=4 × 10-3Kg/mol, d are the diameters of nano-pore on porous material 5:D=7 × 10-8M, l are more
The depth of nano-pore on Porous materials 5:Take l=7 × 10-5m；
2nd, the conductance C of referance leak can be represented by following formula：
C=A σ Cs (2)
A is the area of effective coverage in the present embodiment：Take A=70 × 70=4.9 × 103μm2, σ is nanometer in unit area
The number in hole：σ=95.42/μm2；
C=A σ Cs=4.9 × 103×95.42×3.26×10-14=1.52 × 10-8L/s
3rd, the leak rate Q of referance leak can be represented by following formula：
Q=C × (p1-p2) (3)
P in the present embodiment1It is that referance leak gas inflow side pressure is strong：Take p1=760Torr, p2It is referance leak gas stream
Outlet pressure：p2=0；
Q=C × (p1-p2)=1.52 × 10-8× 760=1.16 × 10-5Torr·L/s
Work as p1During=1Torr, referance leak provided by the present invention can realize 1.52 × 10-8The leak rate of TorrL/s, and
By controlling the area of effective coverage 6, the accurate control of leak rate size can be realized.
Referring to Fig. 1~Fig. 4, a kind of making side for molecular flow referance leak that above-described embodiment is provided is described below
Method comprises the following steps：
A, the through hole of preliminary dimension is formed in the first substrate 1 and the second substrate 3.Wherein, the through hole in the first substrate 1 is
It is process by drilling machine, aperture isAnd the through hole in the second substrate 3 is to process to be formed by laser drilling
, apertureWhen the aperture is smaller, can be also process by deep reaction ion etching technology.
B, the first substrate 1 processed and the second substrate 3 are placed in 130 DEG C of baking oven through over cleaning and heat 30min,
Cleaning process includes：By the first substrate 1 and the second substrate 3 ultrasound 5min in acetone, surface organic dirt is removed；Through deionization
It is dried up after water washing with nitrogen.Then oxygen gas plasma processing is carried out to it, increases surface energy, increases the first substrate and second
The surface adhesion force of substrate, the vacuum degree of corona treatment is 25Pa, power 60w, bombardment time 5min.Then
Spin coating a layer thickness is 400-500nm by diluted second sealing material 4 of toluene solvant, experiment proof toluene in two substrates 3
The polarity of the second sealing material 4 can be changed, it is made more uniformly to be distributed in the surface of the second substrate 3.
C, porous material 5 is placed in the second substrate 3 for coating the second sealing material 4, firmly compressing slowly makes it
It is in close contact with the second substrate, 30min is then heated in 250 DEG C of thermal station cures the second sealing material 4.
D, in the effective coverage 6 that 5 surface of porous material forms preliminary dimension and gas can pass through, effective coverage is ensured
6 align with the through hole in the first substrate 1 and the second substrate 3；The tool of the formation of effective coverage 6 and size Control on porous material 5
Body method includes：Effective coverage 6 is formed by magnetron sputtering technology on porous material 5, and one is plated on porous material 5
The Al films of layer 150-300nm thickness cover other parts of 5 surface of porous material in addition to effective coverage 6, therefore can be more
The square effective coverage 6 that the length of side is 70-300 μm, due to not covered by Al films, gas energy are formed at 5 centre of surface of Porous materials
Enough pass through the nano-porous structure in effective coverage 6.
E, the first substrate 1 with installing the second substrate 3 of porous material by the first sealing material 2 is connected, completes this
The making of referance leak.First sealing material 2 selects Agilent vacuum AB fluid sealants (Torr seal), and most of materials are connect
It is excellent to touch property, such as metal, ceramics and glass bonding are all very perfect, can check leakage feelings at sealing-in immediately after solidification
Condition, it is quick and convenient.In use, the first sealing material 2 is heated 10min in baking oven first, temperature setting is 100 DEG C, then
A glue and B glue are mixed and stirred for uniformly rapidly, it is possible to for sealing-in.After sealing-in, under room ambient conditions, 1 can be hard when small
Change, at the same 24 it is small when eliminate leakage scenarios；It at 60 DEG C, can be hardened in 30 minutes, leakage scenarios can be eliminated in 90 minutes.
In addition, those skilled in the art can also do other variations in spirit of the invention.As porous material 5 uses other materials
The designs such as material, the area that effective coverage 6 is controlled using other methods.Certainly, these variations done according to present invention spirit, all
It should include within scope of the present invention.
Claims (3)
1. a kind of production method of molecular flow referance leak, it is characterised in that comprise the following steps：
A, the through hole of preliminary dimension is formed in the first substrate (1) and the second substrate (3)；
B, the first substrate (1) processed and the second substrate (3) are placed in 130 DEG C of baking oven through over cleaning and heat 30min,
Then oxygen gas plasma processing is carried out to it；Then one layer of spin coating is close by solvent diluted second in the second substrate (3)
Closure material (4)；
C, porous material (5) is placed in the second substrate (3) for coating the second sealing material (4), firmly compressing slowly makes
It is in close contact with the second substrate (3), and 30min is then heated in 250 DEG C of thermal station cures the second sealing material (4)；
D, in the effective coverage (6) that porous material surface forms preliminary dimension and gas can pass through, ensure effective coverage (6)
It aligns with the through hole in the first substrate (1) and the second substrate (3)；The porous material be bilateral porous anodic aluminium oxide, specification
For AAO-DP-12, aperture 70nm, pitch of holes 110nm, 50-70 μm of hole depth；
E, the first substrate (1) with installing the second substrate (3) of porous material by the first sealing material (2) is connected, made
The porous material completes the making of this referance leak between the first substrate (1) and the second substrate (3).
2. the production method of a kind of molecular flow referance leak according to claim 1, it is characterised in that in the step a
Through hole in second substrate (3) is processed to be formed by laser drilling, aperture
3. the production method of a kind of molecular flow referance leak according to claim 1, it is characterised in that in the step b
The vacuum degree of corona treatment is 25Pa, power 60w, bombardment time 5min；The spin coating thickness of second sealing material (4)
For 400-500nm, retarder thinner is toluene.
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| CN106981432B (en) * | 2017-04-11 | 2019-04-23 | 合肥工业大学 | A kind of method of copper copper bonding production channel-style referance leak |
| CN108507719A (en) * | 2018-03-26 | 2018-09-07 | 合肥工业大学 | A method of referance leak is made based on graphene self-defect |
| US11187609B2 (en) * | 2018-05-31 | 2021-11-30 | Goertek Inc. | Test device and calibrating method |
| US20210223134A1 (en) * | 2018-05-31 | 2021-07-22 | Goertek Inc. | Test device and calibrating method |
| CN109186864B (en) * | 2018-08-15 | 2020-05-26 | 北京卫星环境工程研究所 | Vacuum standard leak with minimum leak rate |
| CN109115425A (en) * | 2018-09-26 | 2019-01-01 | 长春微控机械制造有限公司 | A kind of gas leakage marking apparatus |
| CN109485012B (en) * | 2018-12-07 | 2021-03-09 | 合肥工业大学 | Standard leak sealing method based on glass slurry |
| 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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