CN109518177A - A kind of alkali metal gas chamber production method promoting the anti-Relaxivity of coating based on Plasma hydroxylating - Google Patents
A kind of alkali metal gas chamber production method promoting the anti-Relaxivity of coating based on Plasma hydroxylating Download PDFInfo
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- CN109518177A CN109518177A CN201811452033.4A CN201811452033A CN109518177A CN 109518177 A CN109518177 A CN 109518177A CN 201811452033 A CN201811452033 A CN 201811452033A CN 109518177 A CN109518177 A CN 109518177A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
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Abstract
The present invention relates to a kind of alkali metal gas chamber production methods that the anti-Relaxivity of coating is promoted based on Plasma hydroxylating.This method using plasma cleaning machine carries out hydroxylating to gas chamber inner face, since alkali metal gas chamber tail pipe is thinner, eliminate the operation for needing to use glass capillary to extract out sticky cleaning solution after traditional hydroxylacion method cleaning, it avoids poking gas chamber during extraction cleaning solution, improve time-consuming in current gas chamber manufacturing process, effort, consistency and the undesirable problem of anti-relaxation effect, simultaneously, it may make glass surface that there are more hydroxyls, without removing cleaning solution and subsequent drying, shorten hydroxyl and extraneous time of contact, reduce hydroxyl contamination, it can maintain more hydroxyl quantity, during being reacted with organochlorosilane, realize the covering surface of more even uniform, increase the surface coverage to paramagnetic impurities, enhance the anti-Relaxivity of coating.In addition, multiple gas chambers can be handled simultaneously, the consistency and repeatability of enhancing coating production.
Description
Technical field
The present invention relates to the technical fields of alkali metal gas chamber production, and in particular to one kind is promoted based on Plasma hydroxylating and applied
The alkali metal gas chamber production method of the anti-Relaxivity of layer, can be applied to atomic clock, in atom magnetometer alkali metal gas chamber production,
Further, it is also possible to be applied to Magneto-Optical Trap, quantum storage and slower rays experiment.
Background technique
By taking atom magnetometer as an example, the core Sensitive Apparatus of atom magnetometer is alkali metal gas chamber, and alkali metal is former in gas chamber
The polarization time of son influences the sensitivity of atom magnetometer, and the polarization time is longer, and sensitivity is higher, therefore, it is former to promote alkali metal
The polarization time of son has great significance.The collision of alkali metal atom and alkali metal air chamber wall, which will affect, shortens alkali metal atom
Polarization time, there are two types of the methods for inhibiting alkali metal atom and air chamber wall collision at present, first is that by being filled with buffer gas, such as
The gases such as Ne, He, Ar, but there is spin between buffer gas atoms and destroy collision, spin, which destroys collision, can also shorten alkali gold
Belong to the polarization time of atom；Simultaneously because buffer gas atoms limit the movement of alkali metal atom, so that movement average effect
Weaken, due to the presence of gradient magnetic, alkali metal atom has different Larmor precession frequencies in different positions, also can shadow
Ring the polarization time of alkali metal atom；Buffer gas also results in the increase of optics line width, and then reduces photon absorption cross sections product,
Buffer gas pressure is bigger, then the pump intensity needed is bigger, is unfavorable for reducing the power consumption of magnetometer.In addition to being filled with buffer gas
It is outer to reduce steep that wall collision, anti-relaxation coating, such as paraffin, organic oxosilane and alkene can also be coated in alkali metal gas chamber inner wall
Deng.Anti- relaxation coating can effectively reduce steep that wall collision；Simultaneously because alkali metal atom free movement in gas chamber, can be averaged
The influence of gradient magnetic, so that alkali metal atom Larmor precession frequency having the same；Due to there is no buffer gas, reach phase
The pumping optical power that same pumping rate needs reduces, and is conducive to atom magnetometer and reduces power consumption.In addition to the advantages described above, anti-relaxation
The application of Henan coating can also reduce the demand to pumping spot size and be conducive to the small of atom magnetometer without precisely expanding
Typeization design.
Anti- relaxation coating alkali metal gas chamber manufacturing technology mainly includes four steps: cleaning, plated film, and alkali metal is filled in solidification
Atom.Consistency using gas chamber obtained by current production method is poor, even with the gas chamber of a batch production, different gas chambers it
Between performance difference it is very big, very big reason is that the cleaning step in the anti-relaxation coating production of alkali metal gas chamber is complex,
The a large amount of manual operations of time-consuming and needs, time-consuming will cause the loss of hydroxyl quantity, cause coating covering surface uneven, bring anti-
The problem of relaxation effect difference, and manual operations can bring cleaning effect to differ greatly, the poor problem of anti-relaxation effect consistency.
Therefore high-performance is explored, the alkali metal coating of high consistency is coated with technology and has a very important significance.
Simplify cleaning step when anti-relaxation coating is coated with by using plasma cleaner, shorten gas chamber Production Time,
Greater number of hydroxyl is maintained, realizes more uniform covering surface, enhances the consistency and anti-relaxation effect of coating, is had huge
Prospect.
Summary of the invention
The technical problem to be solved by the present invention is overcoming the shortcomings of existing conventional method, propose a kind of based on Plasma hydroxyl
Baseization promotes the alkali metal gas chamber production method of the anti-Relaxivity of coating, has efficiently, and quickly, environmental protection, consistency is good, anti-relaxation
The good feature of effect.
The present invention solves the technical solution that above-mentioned technical problem uses are as follows: one kind is anti-based on Plasma hydroxylating promotion coating
The alkali metal gas chamber production method of Relaxivity, the specific steps of which are as follows:
(1) glass capillary for selecting 0.9-1.1mm is connect by polytetrafluoroethylene (PTFE) with glass syringe.
(2) by the alkali metal gas chamber, the glass syringe equipped with glass capillary, beaker, polytetrafluoroethyl-ne of high borosilicate material
Alkene magnetic stir bar, which is placed in supersonic wave cleaning machine, cleans after twenty minutes, is placed in electric drying oven with forced convection several times with ultrapure water rinsing
In dried, temperature set 105 DEG C slightly above water boiling points, dry 30 minutes.
(3) the alkali metal gas chamber of high borosilicate material is placed in plasma washing machine, setting plasma washing machine is clear
Time 5min is washed, vacuum degree is less than 0.2mbar, opens vacuum pump and is evacuated to plasma cleaner, and opening and oxygenerator
The gas circuit of connection, supplies oxygen plasma cleaner, meets sets requirement to vacuum degree, plasma is excited, to alkali metal
Gas chamber carries out hydroxylating processing.
(4) solvent according to volume configuration 1 part of chloroform and 4 parts of n-hexane mixed solution as OTS.By OTS
OTS solution is configured according to the concentration of 0.8ml/L.
(5) polytetrafluoroethylene (PTFE) magnetic stir bar is placed in configured coating reagent solution, it is stirred 60 seconds.It is described
Coating reagent is organochlorosilane class reagent, including but not limited to OTS (Octadecyltrichlorosilane), DTS
(dodecyltrichlorosilane) or BTS (Butyltrichlorosilane) reagent.
(6) the alkali metal gas chamber cleaned up is taken out, send to draught cupboard and carries out coating operation, takes out electric drying oven with forced convection
In glass capillary and glass syringe, draw coating reagent solution, will coating reagent solution inject alkali metal gas chamber in.It will
Alkali metal gas chamber equipped with coating reagent solution is placed under atmospheric environment is sucked out OTS solution using glass capillary after five minutes,
And alkali metal gas chamber is cleaned three times with chloroform.
(7) the alkali metal gas chamber for being coated with coating reagent is placed in vacuum oven, 200 DEG C of set temperature, is heated for 24 hours,
Alkali metal gas chamber coating is solidified.
(8) alkali metal gas chamber is connected to the glass branch road of gas chamber platform for making after, to pipeline vacuumize process, is used in combination
Heating tape is heated to 150 DEG C -200 DEG C, removes the impurity of glass piping, drives alkali metal atom to alkali metal with heat gun and steeps handle
It is interior, pay attention to noticing that heat gun should not be against alkali metal gas chamber coating, with tamper-proof alkali metal during driving alkali metal atom
Gas chamber coating then removes alkali metal gas chamber.
The principle of the invention lies in: hydroxylating processing is carried out using integrated plasma washing machine, in gas chamber
After wall carries out hydroxylating processing, it is not necessarily to vacuum drying, coating operation can be carried out, shorten the time of traditional hydroxylacion method,
The pollution that hydroxyl can be reduced reacts the hydroxyl of gas chamber inner wall preferably with coating reagent, and it is anti-to increase alkali metal gas chamber inner wall
The coverage rate of relaxation coating, improves the anti-Relaxivity of alkali metal gas chamber, while simplifying operating procedure, solves to a certain extent
The poor problem of consistency caused by artificial cleaning alkali metal gas chamber, it is convenient to have, fast, efficiently, the advantages of high quality.
The advantages of the present invention over the prior art are that:
With " Piranha " solution pair by hydrogenperoxide steam generator and the concentrated sulfuric acid according to 3:7 proportional arrangement is widely used at present
Glass surface carries out method for hydroxylation difference, and this method using plasma cleaning machine carries out hydroxylating to glass surface, by
It is thinner in alkali metal gas chamber tail pipe, it needs to use sticky " Piranha " solution after eliminating traditional hydroxylacion method cleaning
The operation of glass capillary extraction has prevented the generation for extracting the phenomenon that poking alkali metal gas chamber in " Piranha " solution processes out.
Meanwhile this method can make glass surface wash out more hydroxyls, without removing cleaning solution and subsequent drying, shorten
Hydroxyl guarantees that hydroxyl is not contaminated, further maintains more hydroxyl quantity in the extraneous time, subsequent with organochlorine silicon
During alkane reacts, the covering surface of more even uniform may be implemented, increase the surface coverage to paramagnetic impurities, enhancing applies
The anti-Relaxivity of layer.In addition, carrying out hydroxylating processing to multiple alkali metal gas chambers simultaneously, current alkali is solved to a certain extent
The problem of the anti-relaxation effect difference of metal air chamber coating plating method and manual operation bring repeatability difference.It avoids using biography
The volatile malicious chemical reagent of easy system, there is nontoxic, quick, safe, anti-relaxation effect to increase needed for " Piranha " solution allocation of uniting
Strong advantage.
Detailed description of the invention
Fig. 1 is the glass syringe figure for being connected to capillary of the invention, wherein 1 is glass capillary, and 2 be syringe, 3
For polyfluortetraethylene pipe；
Fig. 2 is a kind of alkali metal gas chamber production method that the anti-Relaxivity of coating is promoted based on Plasma hydroxylating of the present invention
Flow chart；
Specific embodiment
With reference to the accompanying drawing and specific embodiment further illustrates the present invention.
As shown in Figure 1, it is connected to the glass syringe of glass capillary, including glass capillary 1, and syringe 2, polytetrafluoroethyl-ne
Alkene pipe 3；Has the function of general syringe, simultaneously because all coating can be effectively reduced and be coated with process using glass material
In, the introducing of impurity.
As shown in Fig. 2, a kind of alkali metal gas chamber system for promoting the anti-Relaxivity of coating based on Plasma hydroxylating of the present invention
It is accomplished by as method
(1) glass capillary for selecting 0.9-1.1mm is connect by polytetrafluoroethylene (PTFE) with glass syringe.
(2) by the alkali metal gas chamber, the glass syringe equipped with glass capillary, beaker, polytetrafluoroethyl-ne of high borosilicate material
Alkene magnetic stir bar, which is placed in supersonic wave cleaning machine, cleans after twenty minutes, is placed in electric drying oven with forced convection several times with ultrapure water rinsing
In dried, temperature set 105 DEG C slightly above water boiling points, dry 30 minutes.
(3) the alkali metal gas chamber of high borosilicate material is placed in plasma washing machine, setting plasma washing machine is clear
Time 5min is washed, vacuum degree is less than 0.2mbar, opens vacuum pump and is evacuated to plasma cleaner, and opening and oxygenerator
The gas circuit of connection, supplies oxygen plasma cleaner, meets sets requirement to vacuum degree, plasma is excited, to alkali metal
Gas chamber carries out hydroxylating processing.
(4) solvent according to volume configuration 1 part of chloroform and 4 parts of n-hexane mixed solution as coating reagent.
OTS is configured into coating reagent solution according to the concentration of 0.8ml/L.
(5) polytetrafluoroethylene (PTFE) magnetic stir bar is placed in configured coating reagent solution, it is stirred 60 seconds, it is described
Coating reagent is organochlorosilane class reagent, including OTS (Octadecyltrichlorosilane), BTS
(Butyltrichlorosilane) or DTS (dodecyltrichlorosilane) reagent.
(6) the alkali metal gas chamber cleaned up is taken out, send to draught cupboard and carries out coating operation, takes out electric drying oven with forced convection
In glass capillary and glass syringe, draw coating reagent solution, will coating reagent solution inject alkali metal gas chamber in.It will
Alkali metal gas chamber equipped with coating reagent solution is placed under atmospheric environment is sucked out coating reagent using glass capillary after five minutes
Solution, and alkali metal gas chamber is cleaned three times with chloroform.
(7) the alkali metal gas chamber for being coated with coating reagent is placed in vacuum oven, 200 DEG C of set temperature, is heated for 24 hours,
Alkali metal gas chamber coating is solidified.
(8) alkali metal gas chamber is connected to the glass branch road of gas chamber platform for making after, to pipeline vacuumize process, is used in combination
Heating tape is heated to 150 DEG C -200 DEG C, removes the impurity of glass piping, drives alkali metal atom to alkali metal with heat gun and steeps handle
It is interior, pay attention to noticing that heat gun should not be against alkali metal gas chamber coating, with tamper-proof alkali metal during driving alkali metal atom
Gas chamber coating then removes alkali metal gas chamber.
The content not being described in detail in description of the invention belongs to the prior art well known to professional and technical personnel in the field.
Claims (2)
1. a kind of alkali metal gas chamber production method for promoting the anti-Relaxivity of coating based on Plasma hydroxylating, it is characterised in that:
It comprises the following steps that
(1) glass capillary for selecting 0.9-1.1mm is connect by polytetrafluoroethylene (PTFE) with glass syringe；
(2) by the alkali metal gas chamber of high borosilicate material, the glass syringe equipped with glass capillary, beaker, polytetrafluoroethylene (PTFE) magnetic
Power stirrer be placed in supersonic wave cleaning machine cleans after twenty minutes, with ultrapure water rinsing be placed in electric drying oven with forced convection several times into
Row drying, temperature set 105 DEG C of boiling points for being slightly above water, dry 30 minutes；
(3) the alkali metal gas chamber of high borosilicate material is placed in plasma washing machine, when setting plasma washing machine cleans
Between 5min, vacuum degree be less than 0.2mbar, open vacuum pump plasma cleaner is evacuated, and open connect with oxygenerator
Gas circuit, plasma cleaner is supplied oxygen, meets sets requirement to vacuum degree, plasma is excited, to alkali metal gas chamber
Carry out hydroxylating processing；
(4) solvent according to volume configuration 1 part of chloroform and 4 parts of n-hexane mixed solution as coating reagent, will apply
Layer reagent configures coating reagent solution according to the concentration of 0.8ml/L；
(5) polytetrafluoroethylene (PTFE) magnetic stir bar is placed in configured coating reagent solution, it is stirred 60 seconds；
(6) the alkali metal gas chamber cleaned up is taken out, send to draught cupboard and carries out coating operation, is taken out in electric drying oven with forced convection
Glass capillary and glass syringe draw coating reagent solution, and coating reagent solution is injected in alkali metal gas chamber, will be equipped with
The alkali metal gas chamber of coating reagent solution is placed molten using glass capillary suction coating reagent after five minutes under atmospheric environment
Liquid, and alkali metal gas chamber is cleaned with chloroform；
(7) the alkali metal gas chamber for being coated with coating reagent is placed in vacuum oven, 200 DEG C of set temperature, is heated for 24 hours, to alkali
Metal air chamber coating is solidified；
(8) alkali metal gas chamber is connected to the glass branch road of gas chamber platform for making, to pipeline vacuumize process, and with heating after
Band is heated to 150 DEG C -200 DEG C, removes the impurity of glass piping, is driven in alkali metal atom to alkali metal bubble handle with heat gun,
Pay attention to noticing that heat gun should not be against alkali metal gas chamber coating, with tamper-proof alkali metal gas chamber during driving alkali metal atom
Coating then removes alkali metal gas chamber.
2. a kind of alkali metal gas chamber system for promoting the anti-Relaxivity of coating based on Plasma hydroxylating according to claim 1
Make method, it is characterised in that: the coating reagent is organochlorosilane class reagent, including Octadecyltrichlorosilane
(OTS), DTS (dodecyltrichlorosilane) or BTS (Butyltrichlorosilane) reagent.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110319854A (en) * | 2019-05-17 | 2019-10-11 | 北京航空航天大学 | A kind of alkali metal air chamber structure convenient for making anti-relaxation coating |
| CN110357451A (en) * | 2019-05-31 | 2019-10-22 | 北京航空航天大学 | A kind of anti-relaxation coating and alkali metal gas chamber and method |
| CN110981212A (en) * | 2019-12-18 | 2020-04-10 | 北京航空航天大学 | Method for manufacturing single-layer TCTS anti-relaxation coating in alkali metal gas chamber |
| CN111024123A (en) * | 2019-12-18 | 2020-04-17 | 北京航空航天大学 | Method for manufacturing multi-layer OTS coating in alkali metal air chamber |
| CN114950923A (en) * | 2022-06-28 | 2022-08-30 | 北京科技大学广州新材料研究院 | Preparation method of glass capillary tube for thermometer |
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| CN114950923A (en) * | 2022-06-28 | 2022-08-30 | 北京科技大学广州新材料研究院 | Preparation method of glass capillary tube for thermometer |
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