CN103866262B - A kind of preparation method of stainless steel surfaces silanization treatment film - Google Patents
A kind of preparation method of stainless steel surfaces silanization treatment film Download PDFInfo
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- CN103866262B CN103866262B CN201410116791.4A CN201410116791A CN103866262B CN 103866262 B CN103866262 B CN 103866262B CN 201410116791 A CN201410116791 A CN 201410116791A CN 103866262 B CN103866262 B CN 103866262B
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Abstract
The invention belongs to technical field of material surface treatment, the invention discloses the preparation method of a kind of stainless steel surfaces silanization treatment film, use silanization treating agent silicon tetrahydride and mix the mixed gas that agent hydrogenation phosphorus is formed, deposited by chemical gaseous phase, form one layer of unformed silicon at stainless steel surfaces and process film, in described mixed gas, the percent by volume of silicon tetrahydride is 95 99%, and the percent by volume of hydrogenation phosphorus is 0.1 5%.Relative to prior art, the invention have the benefit that stainless steel watch has good corrosion resistance after silanization treatment, gaseous sample containing acidic materials stores in stainless cylinder of steel and in transportation, concentration, without significant change, meets the requirement of atmospheric ambient gas sample collecting, analysis.
Description
Technical field
The present invention relates to technical field of material surface treatment, particularly relate at a kind of stainless steel surfaces silanization
The preparation method of reason film.
Background technology
Along with the accelerated development of process of industrialization, the continuous reinforcement of people's environmental consciousness, nuisance in air
The pollution of confrontation environment is increasingly paid close attention to by people, and a lot of harmful substances are all with penetrating odor, even
It is foul odour, these Odor stimulation organum olfactoriums, cause people unhappy and infringement living environment.Medical science is ground
Study carefully and show, the especially foul smell of the noxious odor in environment to human body respiration, digestion, cardiovascular, endocrine and
Nervous system can impact, and the stench of high concentration can also make contactee that pulmonary edema even death by suffocation occurs.
Prolonged and repeated stimulated by odorant, also can be caused olfactory fatigue, caused hyposmia, and penetrating odor
In some aromatics such as harmful substance such as benzene, toluene, styrene be also possible to make people produce distortion, canceration.
Generally harmful substance complicated component in atmospheric environment, concentration is low, needs by suitable environmental sample collection, divides
Analysis, provides reliable foundation for atmospheric environment preventing and treating.Stainless Steel Vacuum tank sampling system be current optimal greatly
One of gas environmental gas sample acquisition mode.For atmospheric ambient gas sample collecting Stainless Steel Vacuum tank also known as
For Soviet Union's agate tank, first the burr of stainless steel surfaces is tentatively gone by the most stainless cylinder of steel surface through electro-polish technology
Remove, smooth surface, reduce specific surface area, reduce reactivity, then stainless steel surfaces ferrum can be made through pickling processes
Atom generation passivation reaction, reduces atmospheric ambient gas sample and causes gas due to factors such as absorption in stainless cylinder of steel
The change of trace substance concentration in body sample.Soviet Union's agate tank first cleans and evacuation before atmospheric environment samples samples,
As long as Open valve completes environmental gas sample sampling during sampling, sampling process need not other sampling additional and set
Standby, gaseous sample can preserve for a long time, and volume is little, and sampling is convenient, and Soviet Union's agate tank is repeatable applicable, the longevity
Order at least two ten years, it is possible to achieve the fully sampled analysis of gas, divide the analysis of variance single sample through application of gas chromatorgraphy/mass method
Product VOCs, and can maximum can 1000 times of concentration of concentrated gas sample, improve accuracy of detection.But for containing
The gaseous sample of acidic corrosive material, during sample stores, acidic materials can be sent out with rustless steel tank skin surface
Raw reaction, causes concentration of narmful substance in gaseous sample to change, and stainless cylinder of steel surface still needs to be passivated further
Process, improve corrosion resistance.It is processed to improve stainless steel watch to stainless steel surfaces by Silicane Method
The corrosion resistance in face is paid close attention to by people, as Chinese patent CN103087569, CN103059625 divide
Do not report a kind of anticorrosion corrosion resistant plate surface silanization protective agent for surface treatment and preparation method thereof, but through silane
Rustless steel corrosion resistance after change processes has much room for improvement.
Summary of the invention
For solving the problem that above-mentioned prior art exists, the present invention proposes a kind of stainless steel surfaces silanization
Process the preparation method of film, be by silylating reagent silicon tetrahydride (95.0-99.0%) and to mix agent hydrogenation phosphorus
PH3(5.0-0.1%) mixed gas, by vapour deposition, forms unformed silicon thin film in stainless steel surfaces,
After surface treated, rustless steel has good corrosion resistance.
The present invention adopts the technical scheme that:
The preparation method of the stainless steel surfaces silanization treatment film of the present invention, uses silanization treating agent tetrahydrochysene
SiClx and the mixed gas mixing agent hydrogenation phosphorus formation, deposited by chemical gaseous phase, form one at stainless steel surfaces
The unformed silicon of layer processes film, and in described mixed gas, the percent by volume of silicon tetrahydride is 95-99.9%,
The percent by volume of hydrogenation phosphorus is 0.1-5%.
In described mixed gas, the preferably percent by volume of silicon tetrahydride is 99.5%, the body of hydrogenation phosphorus
Long-pending percentage ratio is 0.5%.
In described mixed gas, the preferably percent by volume of silicon tetrahydride is 96%, the volume of hydrogenation phosphorus
Percentage ratio is 4%.
Specifically comprising the following steps that needs of the preparation method of the stainless steel surfaces silanization treatment film of the present invention
CVD chamber put into by the stainless cylinder of steel that surface processes, and removes stainless steel surfaces steam, chemical gaseous phase is sunk
Long-pending room is evacuated to vacuum, then is passed through with hydrogenation phosphorus mixed gas by silicon tetrahydride, and vapour deposition air pressure span of control exists
4 400Pa, control vapour deposition temperature, at 320-500 DEG C, carries out chemical gaseous phase deposition, sedimentation time 0.5-12
Hour, after having deposited, it is passed through nitrogen, is down to room temperature.
Preferably: vapour deposition air pressure 4Pa, depositing temperature 320 DEG C, vapor deposition times 2 hours.
Preferably: vapour deposition air pressure 100Pa, depositing temperature 410 DEG C, vapor deposition times 4.5 hours.
Preferably: vapour deposition air pressure 25Pa, depositing temperature 450 DEG C, vapor deposition times 6.8 hours.
Preferably: vapour deposition air pressure 400Pa, depositing temperature 500 DEG C, vapor deposition times 10 hours.
Corrosion resisting property detects:
Being put in salt fog machine by rustless steel sample and test, test condition is: 5% sodium chloride solution, temperature
Spend 35 DEG C, spray continuously, test period 120h.Carry out decay resistance evaluation.
1 grade: surface-brightening is clean, do not have corrosion pit.
2 grades: mattness, have a small amount of corrosion pit.
3 grades: corrosion pit is less than 30%.
4 grades: corrosion pit is more than 30%.
The positive effect of the present invention is as follows:
Stainless steel watch decay resistance after silanization treatment reaches 1 grade, has good corrosion resistance,
Gaseous sample containing acidic materials stores in stainless cylinder of steel and in transportation, concentration, without significant change, meets
Atmospheric ambient gas sample collecting, the requirement of analysis.
Detailed description of the invention
The following examples are that the present invention is described in further detail.
Embodiment 1
The stainless cylinder of steel needing surface to process is put into CVD chamber, removes stainless steel surfaces water
Vapour, is evacuated to CVD chamber vacuum, then silicon tetrahydride (99.9%) and hydrogenation phosphorus (0.1%) is mixed
Conjunction gas is passed through, vapour deposition air pressure span of control 4Pa, and depositing temperature 320 DEG C, vapor deposition times 2 is little
Time, carry out chemical gaseous phase deposition, after having deposited, be passed through nitrogen, be down to room temperature.Stainless steel surfaces gas phase is sunk
Long-pending unformed silicon film thickness 180 angstroms, stainless steel watch decay resistance after silanization treatment reaches 1 grade, has
Good corrosion resistance, the air containing corrosive substance gathers sample and stores 72 little up-to-date styles in stainless cylinder of steel
Product concentration is unchanged, reaches atmospheric ambient gas sample collecting, analyzes requirement.
Embodiment 2
The stainless cylinder of steel needing surface to process is put into CVD chamber, removes stainless steel surfaces water
Vapour, is evacuated to CVD chamber vacuum, then silicon tetrahydride (99.5%) and hydrogenation phosphorus (0.5%) is mixed
Conjunction gas is passed through, vapour deposition air pressure span of control 100Pa, depositing temperature 410 DEG C, vapor deposition times 4.5
Hour, carry out chemical gaseous phase deposition, after having deposited, be passed through nitrogen, be down to room temperature.Stainless steel surfaces gas phase
Depositing unformed silicon film thickness 380 angstroms, stainless steel watch decay resistance after silanization treatment reaches 1 grade, tool
Having good corrosion resistance, the air containing corrosive substance gathers sample and stores 72 hours in stainless cylinder of steel
Sample concentration is unchanged, reaches atmospheric ambient gas sample collecting, analyzes requirement.
Embodiment 3
The stainless cylinder of steel needing surface to process is put into CVD chamber, removes stainless steel surfaces water
Vapour, is evacuated to vacuum by CVD chamber, then by silicon tetrahydride (98.0%) and hydrogenation phosphorus (2.0) mixing
Gas is passed through, vapour deposition air pressure span of control 25Pa, and depositing temperature 450 DEG C, vapor deposition times 6.8 is little
Time, carry out chemical gaseous phase deposition, after having deposited, be passed through nitrogen, be down to room temperature.Stainless steel surfaces gas phase is sunk
Long-pending unformed silicon film thickness 650 angstroms, stainless steel watch decay resistance after silanization treatment reaches 1 grade, has
Good corrosion resistance, the air containing corrosive substance gathers sample and stores 72 little up-to-date styles in stainless cylinder of steel
Product concentration is unchanged, reaches atmospheric ambient gas sample collecting, analyzes requirement.
Embodiment 4
The stainless cylinder of steel needing surface to process is put into CVD chamber, removes stainless steel surfaces water
Vapour, is evacuated to CVD chamber vacuum, then silicon tetrahydride (96.0%) and hydrogenation phosphorus (4.0%) is mixed
Conjunction gas is passed through, vapour deposition air pressure span of control 400Pa, depositing temperature 500 DEG C, vapor deposition times 10
Hour, carry out chemical gaseous phase deposition, after having deposited, be passed through nitrogen, be down to room temperature.Stainless steel surfaces gas phase
Depositing unformed silicon film thickness 920 angstroms, stainless steel watch decay resistance after silanization treatment reaches 1 grade, tool
Having good corrosion resistance, the air containing corrosive substance gathers sample and stores 72 hours in stainless cylinder of steel
Sample concentration is unchanged, reaches atmospheric ambient gas sample collecting, analyzes requirement.
The above, the only detailed description of the invention of the present invention, but protection scope of the present invention is not limited to
In this, the present invention is applied not only to stainless cylinder of steel surface reason it can also be used to other rustless steel device surface processes,
Any change expected without creative work or replacement, all should contain within protection scope of the present invention.
Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims are limited.
Claims (7)
1. the preparation method of a stainless steel surfaces silanization treatment film, it is characterised in that: use silanization treatment
Agent silicon tetrahydride and the mixed gas mixing agent hydrogenation phosphorus formation, deposited by chemical gaseous phase, at stainless steel surfaces
Forming one layer of unformed silicon and process film, in described mixed gas, the percent by volume of silicon tetrahydride is
95-99.9%, the percent by volume of hydrogenation phosphorus is 0.1-5%；
Chemical gaseous phase deposition put into by the stainless cylinder of steel needing surface to process by specifically comprising the following steps that of described method
Room, removes stainless steel surfaces steam, and CVD chamber is evacuated to vacuum, then by silicon tetrahydride and hydrogenation phosphorus
Mixed gas is passed through, and vapour deposition air pressure span of control, at 4 400Pa, controls vapour deposition temperature and exists
320-500 DEG C, carry out chemical gaseous phase deposition, sedimentation time 0.5-12 hour, after having deposited, be passed through nitrogen,
It is down to room temperature.
2. preparation method as claimed in claim 1, it is characterised in that: in described mixed gas, tetrahydro
The percent by volume of silicon is 99.5%, and the percent by volume of hydrogenation phosphorus is 0.5%.
3. preparation method as claimed in claim 1, it is characterised in that: in described mixed gas, tetrahydro
The percent by volume of silicon is 96%, and the percent by volume of hydrogenation phosphorus is 4%.
4. preparation method as claimed in claim 1, it is characterised in that: vapour deposition air pressure 4Pa, deposition temperature
Spend 320 DEG C, vapor deposition times 2 hours.
5. preparation method as claimed in claim 1, it is characterised in that: vapour deposition air pressure 100Pa, deposition
Temperature 410 DEG C, vapor deposition times 4.5 hours.
6. preparation method as claimed in claim 1, it is characterised in that: vapour deposition air pressure 25Pa, deposition temperature
Spend 450 DEG C, vapor deposition times 6.8 hours.
7. preparation method as claimed in claim 1, it is characterised in that: vapour deposition air pressure 400Pa, deposition
Temperature 500 DEG C, vapor deposition times 10 hours.
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| CN201410116791.4A CN103866262B (en) | 2014-03-26 | 2014-03-26 | A kind of preparation method of stainless steel surfaces silanization treatment film |
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| CN201410116791.4A CN103866262B (en) | 2014-03-26 | 2014-03-26 | A kind of preparation method of stainless steel surfaces silanization treatment film |
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| CN103866262B true CN103866262B (en) | 2016-08-17 |
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| CN105112886B (en) * | 2015-09-18 | 2018-04-17 | 杭州天净检测技术有限公司 | A kind of inactive surfaces treatment technology |
| CN214538795U (en) * | 2020-08-19 | 2021-10-29 | 赵永刚 | Sampling tank for collecting and storing ambient air samples |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059625A (en) * | 2012-12-18 | 2013-04-24 | 芜湖恒坤汽车部件有限公司 | Protective treating agent for silanizing surface of anti-corrosion stainless steel plate surface and preparation method thereof |
| CN103087569A (en) * | 2012-12-18 | 2013-05-08 | 芜湖恒坤汽车部件有限公司 | Surface silanization protection treatment agent for stainless steel plates and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20030017359A1 (en) * | 2001-07-17 | 2003-01-23 | American Air Liquide, Inc. | Increased stability low concentration gases, products comprising same, and methods of making same |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059625A (en) * | 2012-12-18 | 2013-04-24 | 芜湖恒坤汽车部件有限公司 | Protective treating agent for silanizing surface of anti-corrosion stainless steel plate surface and preparation method thereof |
| CN103087569A (en) * | 2012-12-18 | 2013-05-08 | 芜湖恒坤汽车部件有限公司 | Surface silanization protection treatment agent for stainless steel plates and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| CVD技术在制备含硅化合物膜层中的应用;刘立等;《材料科学与工程》;20010630;第19卷(第02期);128-131 * |
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Effective date of registration: 20170118 Address after: Beijing City, Haidian District Third Street No. 9 block C C1008 Patentee after: Beijing Youdeze Technology Co. Ltd. Address before: Beijing City, Haidian District Third Street No. 9 block C C1008 Patentee before: BCTTECHNOLOGY., LTD. |