CN109023223A - A kind of metal surface using low temperature plasma is turned blue method - Google Patents
A kind of metal surface using low temperature plasma is turned blue method Download PDFInfo
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- CN109023223A CN109023223A CN201811018958.8A CN201811018958A CN109023223A CN 109023223 A CN109023223 A CN 109023223A CN 201811018958 A CN201811018958 A CN 201811018958A CN 109023223 A CN109023223 A CN 109023223A
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- steel
- blue
- steel part
- pickling
- temperature plasma
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
- C23C8/38—Treatment of ferrous surfaces
-
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/80—After-treatment
Abstract
It is an object of the invention to overcome the defect for technique of turning blue in the prior art, a kind of metal surface using low temperature plasma is provided and is turned blue method, technical field of metal material surface treatment is belonged to.This method applies electric field under certain air pressure using vacuum equipped, makes inert gas and H2Glow discharge and ionization occur for O molecule, form low temperature plasma, generate the O with activation2+Ion.O2+Ion is attracted by the negative potential being applied on steel or steel part, bombards workpiece surface.Active O2+Oil blackeite reaction occurs for ion and steel workpiece surface iron chemical combination.The oxidation film that turns blue of preparation is fine and close, beautiful, at low cost, easy to operate, is conducive to industrialized production, pollution-free.Preparation method of the invention realizes low temperature plasma and turns blue processing, has wide range of applications.
Description
Technical field
The invention belongs to technical field of metal material surface treatment, in particular to a kind of metal using low temperature plasma
Surface is turned blue method.
Background technique
Steel or steel part are heated to proper temperature in air+vapor or chemicals makes its surface form one layer of tool
The technique of the blue or black oxide film that have protective effect, which is called, turns blue, and also referred to as blacks.The technics comparing of current use of turning blue is multiple
It is miscellaneous, because the chemicals environmental pollution that chemical method uses is larger, it is unfavorable for environmental protection and long-time industrialized production；And lead to
It is more to enter the parameter that the method that oxygen turns blue needs to control, it has not been convenient to operate.Lead to steel or steel piece surface turns blue effect not
Good, the oxidation film of formation is not beautiful enough or oxidation film is defective, influences anti-corrosion effect.
Summary of the invention
It is an object of the invention to overcome the defect for technique of turning blue in the prior art, provide a kind of using low temperature plasma
Metal surface turn blue method.This method applies electric field under certain air pressure using vacuum equipped, makes inert gas and H2O molecule
Glow discharge and ionization occurs, forms low temperature plasma, generates the O with activation2+Ion.O2+Ion is applied to
Negative potential on steel or steel part attracts, and bombards workpiece surface.Active O2+Oil blackeite occurs for ion and steel workpiece surface iron chemical combination anti-
It answers.
A kind of metal surface using low temperature plasma is turned blue method, is included the following steps:
(1) degreasing: by steel or steel part through ungrease treatment, surface oil stain is removed；
Preferably, the method for the ungrease treatment be steel or steel part are boiled in the degreasant solution of boiling wash 20~
30min, then rinsed in the deionized water of flowing, remove steel or steel piece surface degreasant solution；
The formula of the degreasant solution are as follows: NaOH:50~60g, Na2CO3: 70~80g, H2O:1L；
(2) pickling: by after degreasing steel or steel part through pickling processes, remove steel or steel piece surface rusty stain, oxide skin
Activating surface simultaneously；
Preferably, the method for the pickling processes is, by steel or steel part mass concentration 20~35% technical hydrochloric acid
Middle pickling, time > 30s, pickling to cleaning, but must not be corroded；After pickling, steel or steel part are first rinsed through deionized water, then
It is put into the Na of mass concentration 3~5%2CO3Residual acid is neutralized in solution, steel or steel piece surface through pickling are silver gray；
It further, is also the urea of hydrochloric acid quality 0.2~0.5% added with quality in the technical hydrochloric acid；
(3) turn blue: detailed process is as follows:
(3.1) steel after degreasing, pickling or steel part are put into low-temperature plasma generator cavity；
(3.2) it is vacuumized in cavity and reaches 3 × 10-3Pa or less；
(3.3) to heating up in cavity, steel or steel part are dried；
(3.4) be passed through Ar gas into cavity, size is 150~250sccm, opens substrate bias power supply, make Ar pneumoelectric from
Steel or steel piece surface are bombarded, the purpose of cleaning and activation steel or steel piece surface is realized, in low -100~-120V of bias state
10~15min of lower bombardment bombards 20~30min under high -280~-300V of bias state；
(3.5) H is passed through into cavity2O steam, size are 150~250sccm；
(3.6) open filament turn-on current, adjusting heater current be (4.5~5) A*4, control cavity air pressure be 0.3~
0.5Pa turns blue under operating air pressure, and the time of turning blue is 45~60min；
(4) it is saponified: by the steel after turning blue or steel part through saponification process, steel or steel part being made to turn blue the iron oxide film of generation
Micropore in iron be converted to ferric stearate, be in passive state, to improve resistance to corrosion；
Preferably, the method for saponification process is, by the steel after turning blue or steel part be immersed in the mass concentration 2 of boiling~
3~5min in 3% suds, is then dried；
(5) oil immersion: by after saponification steel or steel part do oil immersion processing, make surface formed oil film；
Preferably, the method for oil immersion processing is that will stop 1 in the steel or steel part 105~115 DEG C of hot oils of immersion after saponification
~3min goes moisture removal to form oil film.
Compared with prior art, the beneficial effects of the present invention are:
1, preparation method of the invention applies electric field under certain air pressure using vacuum equipped, makes inert gas and H2O points
Glow discharge and ionization occur for son, form low temperature plasma, generate the O with activation2+Ion.O2+Ion is applied
Negative potential on steel workpiece attracts, and bombards workpiece surface.Active O2+Oil blackeite occurs for ion and steel workpiece surface iron chemical combination anti-
It answers.The oxidation film that turns blue of preparation is fine and close, beautiful, at low cost, easy to operate, is conducive to industrialized production, pollution-free.
2, preparation method of the invention realizes low temperature plasma and turns blue processing, has wide range of applications.
Specific embodiment
Embodiment 1
A kind of metal surface using low temperature plasma is turned blue method, is included the following steps:
(1) degreasing: steel or steel part are boiled in the degreasant solution of boiling and wash 20min, then in the deionized water of flowing
It rinses, steel or steel piece surface degreasant solution is removed, to remove surface oil stain；
The formula of the degreasant solution are as follows: NaOH:50~60g, Na2CO3: 70~80g, H2O:1L；
(2) pickling: by steel or steel part added with the urea that quality is hydrochloric acid quality 0.2%, mass concentration 20%
Technical hydrochloric acid in pickling, time 60s；After pickling, steel or steel part are first rinsed through deionized water, place into mass concentration 3%
Na2CO3Residual acid is neutralized in solution, steel or steel piece surface through pickling are silver gray, to remove steel or steel piece surface rust
Mark, oxide skin while activating surface；
(3) turn blue: detailed process is as follows:
(3.1) steel after degreasing, pickling or steel part are put into low-temperature plasma generator cavity；
(3.2) it is evacuated to 1 × 10-3Pa；
(3.3) to heating up in cavity, steel or steel part are dried；
(3.4) it is passed through Ar gas, size 150sccm opens substrate bias power supply, makes Ar pneumoelectric from bombardment steel or steel part
Surface realizes the purpose of cleaning and activation steel or steel piece surface, bombards 10min under low bias -100V state, high partially
20min is bombarded under pressure -280V state；
(3.5) H is passed through into cavity2O steam, size 150sccm；
(3.6) open filament turn-on current, adjusting heater current are 4.5A*4, and cavity air pressure reaches 0.5Pa, in work gas
Pressure is turned blue, and the time of turning blue is 45min；
(4) it is saponified: the steel after turning blue or steel part being immersed in 5min in the suds of the mass concentration 2% of boiling, so
The iron dried in the micropore for the iron oxide film for making steel or steel part turn blue generation afterwards is converted to ferric stearate, is in passive state, from
And improve resistance to corrosion；
(5) oil immersion: will stop 1min in the steel or steel part 115 DEG C of hot oils of immersion after saponification, moisture removal gone to form oil film,
Surface is set to form oil film.
Through detecting, oxidation film is in navy blue, and uniformly beauty is without bad point；1.1 μm of average film thickness；Film component is Fe3O4；Corrosion
Depth 0.102mm/a.
Embodiment 2
A kind of metal surface using low temperature plasma is turned blue method, is included the following steps:
(1) degreasing: steel or steel part are boiled in the degreasant solution of boiling and wash 30min, then in the deionized water of flowing
It rinses, steel or steel piece surface degreasant solution is removed, to remove surface oil stain；
The formula of the degreasant solution are as follows: NaOH:50~60g, Na2CO3: 70~80g, H2O:1L；
(2) pickling: by steel or steel part added with the urea that quality is hydrochloric acid quality 0.5%, mass concentration 35%
Technical hydrochloric acid in pickling, time 35s；After pickling, steel or steel part are first rinsed through deionized water, place into mass concentration 5%
Na2CO3Residual acid is neutralized in solution, steel or steel piece surface through pickling are silver gray, to remove steel or steel piece surface rust
Mark, oxide skin while activating surface；
(3) turn blue: detailed process is as follows:
(3.1) steel after degreasing, pickling or steel part are put into low-temperature plasma generator cavity；
(3.2) it is evacuated to 1 × 10-3Pa；
(3.3) to heating up in cavity, steel or steel part are dried；
(3.4) it is passed through Ar gas, size 250sccm opens substrate bias power supply, makes Ar pneumoelectric from bombardment steel or steel part
Surface realizes the purpose of cleaning and activation steel or steel piece surface, bombards 15min under low bias -120V state, high partially
30min is bombarded under pressure -300V state；
(3.5) H is passed through into cavity2O steam, size 250sccm；
(3.6) open filament turn-on current adjusts electric current, and heater current 5A*4, cavity air pressure reaches 0.3Pa, in work
Make to turn blue under air pressure, the time of turning blue is 1h；
(4) it is saponified: the steel after turning blue or steel part being immersed in 3min in the suds of the mass concentration 3% of boiling, so
The iron dried in the micropore for the iron oxide film for making steel or steel part turn blue generation afterwards is converted to ferric stearate, is in passive state, from
And improve resistance to corrosion；
(5) oil immersion: by after saponification steel or steel part immerse 105 DEG C, 3min is stopped in hot oil, moisture removal is gone to form oil
Film makes surface form oil film.
Through detecting, oxidation film is in navy blue, and uniformly beauty is without bad point；1.5 μm of average film thickness；Film component is Fe3O4；Corrosion
Depth 0.091mm/a.
Embodiment 3
A kind of metal surface using low temperature plasma is turned blue method, is included the following steps:
(1) degreasing: steel or steel part are boiled in the degreasant solution of boiling and wash 25min, then in the deionized water of flowing
It rinses, steel or steel piece surface degreasant solution is removed, to remove surface oil stain；
The formula of the degreasant solution are as follows: NaOH:50~60g, Na2CO3: 70~80g, H2O:1L；
(2) pickling: by steel or steel part added with the urea that quality is hydrochloric acid quality 0.3%, mass concentration 27%
Technical hydrochloric acid in pickling, time 50s；After pickling, steel or steel part are first rinsed through deionized water, place into mass concentration 4%
Na2CO3Residual acid is neutralized in solution, steel or steel piece surface through pickling are silver gray, to remove steel or steel piece surface rust
Mark, oxide skin while activating surface；
(3) turn blue: detailed process is as follows:
(3.1) steel after degreasing, pickling or steel part are put into low-temperature plasma generator cavity；
(3.2) it vacuumizes and reaches 1 × 10-3Pa；
(3.3) to heating up in cavity, steel or steel part are dried；
(3.4) it is passed through Ar gas, size 200sccm opens substrate bias power supply, makes Ar pneumoelectric from bombardment steel or steel part
Surface realizes the purpose of cleaning and activation steel or steel piece surface, bombards 13min under low bias -110V state, high partially
25min is bombarded under pressure -290V state；
(3.5) H is passed through into cavity2O steam, size 200sccm；；
(3.6) open filament turn-on current adjusts electric current, and heater current 4.8A*4, cavity air pressure 0.4Pa are working
It turns blue under air pressure, the time of turning blue is 52min；
(4) it is saponified: the steel after turning blue or steel part is immersed in 4min in the suds of the mass concentration 2.5% of boiling,
Then the iron dried in the micropore for the iron oxide film for making steel or steel part turn blue generation is converted to ferric stearate, is in passive state,
To improve resistance to corrosion；
(5) oil immersion: will stop 2min in the steel or steel part 110 DEG C of hot oils of immersion after saponification, moisture removal gone to form oil film,
Surface is set to form oil film.
Through detecting, oxidation film is in navy blue, and uniformly beauty is without bad point；1.3 μm of average film thickness；Film component is Fe3O4；Corrosion
Depth 0.096mm/a.
Claims (6)
- A kind of method 1. metal surface using low temperature plasma is turned blue, which comprises the steps of:(1) degreasing: by steel or steel part through ungrease treatment, surface oil stain is removed；(2) pickling: by after degreasing steel or steel part through pickling processes, remove steel or steel piece surface rusty stain, oxide skin simultaneously Activating surface；(3) turn blue: detailed process is as follows:(3.1) steel after degreasing, pickling or steel part are put into low-temperature plasma generator cavity；(3.2) it is vacuumized in cavity and reaches 3 × 10-3Pa or less；(3.3) to heating up in cavity, steel or steel part are dried；(3.4) Ar gas is passed through into cavity, size is 150~250sccm, opens substrate bias power supply, makes Ar pneumoelectric from bombardment Steel or steel piece surface bombard 10~15min, in high -280~-300V of bias state under low -100~-120V of bias state 20~30min of lower bombardment；(3.5) H is passed through into cavity2O steam, size are 150~250sccm；(3.6) open filament turn-on current, adjusting heater current are (4.5~5) A*4, and control cavity air pressure is 0.3~0.5Pa, It turns blue under operating air pressure, the time of turning blue is 45~60min；(4) be saponified: by the steel after turning blue or steel part through saponification process, make steel or steel part turn blue generation iron oxide film it is micro- Iron in hole is converted to ferric stearate；(5) oil immersion: by after saponification steel or steel part do oil immersion processing, make surface formed oil film.
- The method 2. metal surface according to claim 1 is turned blue, which is characterized in that ungrease treatment described in step (1) Method is to boil steel or steel part in the degreasant solution of boiling and wash 20~30min, then rinse in the deionized water of flowing, Remove steel or steel piece surface degreasant solution；The formula of the degreasant solution are as follows: NaOH:50~60g, Na2CO3: 70~80g, H2O:1L.
- The method 3. metal surface according to claim 1 is turned blue, which is characterized in that pickling processes described in step (2) Method is the pickling in the technical hydrochloric acid of mass concentration 20~35% by steel or steel part, time > 30s, pickling to cleaning, but It must not be corroded；After pickling, steel or steel part are first rinsed through deionized water, place into the Na of mass concentration 3~5%2CO3Solution Neutralize residual acid.
- The method 4. metal surface according to claim 3 is turned blue, which is characterized in that matter is also added in the technical hydrochloric acid Amount is the urea of hydrochloric acid quality 0.2~0.5%.
- The method 5. metal surface according to claim 1 is turned blue, which is characterized in that saponification process in the step (4) Method is then 3~5min in the suds for the mass concentration 2~3% that the steel after turning blue or steel part are immersed boiling is done It is dry.
- The method 6. metal surface according to claim 1 is turned blue, which is characterized in that the processing of oil immersion described in step (5) Method is that will stop 1~3min in the steel or steel part 105~115 DEG C of hot oils of immersion after saponification, moisture removal is gone to form oil film.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811018958.8A CN109023223B (en) | 2018-09-03 | 2018-09-03 | Metal surface bluing method using low-temperature plasma |
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| CN201811018958.8A CN109023223B (en) | 2018-09-03 | 2018-09-03 | Metal surface bluing method using low-temperature plasma |
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| CN109023223B CN109023223B (en) | 2020-07-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111036047A (en) * | 2019-12-31 | 2020-04-21 | 深圳粤鹏环保技术股份有限公司 | Method for improving plasma electric field processing efficiency |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105369199A (en) * | 2015-10-15 | 2016-03-02 | 南京理工大学 | Method for preparing frictional wear resisting and corrosion resisting carbon-based film |
| CN105734549A (en) * | 2014-12-09 | 2016-07-06 | 重庆渝南科技股份有限公司 | Surface bluing technique for steel piece |
| CN105951035A (en) * | 2016-05-28 | 2016-09-21 | 上海大学 | Method of spring steel for bluing under low-temperature plasma |
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2018
- 2018-09-03 CN CN201811018958.8A patent/CN109023223B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105734549A (en) * | 2014-12-09 | 2016-07-06 | 重庆渝南科技股份有限公司 | Surface bluing technique for steel piece |
| CN105369199A (en) * | 2015-10-15 | 2016-03-02 | 南京理工大学 | Method for preparing frictional wear resisting and corrosion resisting carbon-based film |
| CN105951035A (en) * | 2016-05-28 | 2016-09-21 | 上海大学 | Method of spring steel for bluing under low-temperature plasma |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111036047A (en) * | 2019-12-31 | 2020-04-21 | 深圳粤鹏环保技术股份有限公司 | Method for improving plasma electric field processing efficiency |
| CN111036047B (en) * | 2019-12-31 | 2023-10-27 | 深圳粤鹏环保技术股份有限公司 | Method for improving plasma electric field treatment efficiency |
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