CN101082129A - Method for carbon steel surface blackening - Google Patents
Method for carbon steel surface blackening Download PDFInfo
- Publication number
- CN101082129A CN101082129A CN 200710069984 CN200710069984A CN101082129A CN 101082129 A CN101082129 A CN 101082129A CN 200710069984 CN200710069984 CN 200710069984 CN 200710069984 A CN200710069984 A CN 200710069984A CN 101082129 A CN101082129 A CN 101082129A
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- CN
- China
- Prior art keywords
- carbon steel
- coating
- superloy
- steel surface
- surface blackening
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910000975 Carbon steel Inorganic materials 0.000 title claims abstract description 23
- 239000010962 carbon steel Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 19
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 15
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 13
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 33
- 238000000576 coating method Methods 0.000 claims description 24
- 239000011248 coating agent Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 229910000831 Steel Inorganic materials 0.000 claims description 18
- 239000010959 steel Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 229910000627 Superloy Inorganic materials 0.000 claims description 7
- 238000000280 densification Methods 0.000 claims description 7
- 239000011790 ferrous sulphate Substances 0.000 claims description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 6
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 abstract description 10
- 230000001590 oxidative effect Effects 0.000 abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 6
- 235000010288 sodium nitrite Nutrition 0.000 abstract description 5
- 230000000711 cancerogenic effect Effects 0.000 abstract description 3
- 231100000315 carcinogenic Toxicity 0.000 abstract description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract 2
- 239000011259 mixed solution Substances 0.000 abstract 1
- 231100000331 toxic Toxicity 0.000 abstract 1
- 230000002588 toxic effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 28
- 238000005516 engineering process Methods 0.000 description 12
- 229910052742 iron Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910001374 Invar Inorganic materials 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 229940001516 sodium nitrate Drugs 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
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- Chemical Treatment Of Metals (AREA)
Abstract
The present invention discloses process of blackening carbon steel surface. Through the hydrothermal reaction of carbon steel substrate and the mixed solution of ferrous salt, strong base and hydrazine hydrate at the temperature of 100-250 deg.c, one black compact protecting layer comprising superfine Fe3O4 in the thickness of 1-10 microns and fusing mutually to the carbon steel substrate is formed. The process is superior to traditional high temperature alkaline oxidizing process and has no use of sodium nitrite and other carcinogenic toxic matter. The present invention is suitable for carbon steel surface blackening treatment.
Description
Technical field
The present invention relates to the processing of ferrous metal, especially relate to the method for superloy surface blackening.
Background technology
According to statistics, the whole world reaches more than 100,000,000 tons because of the iron and steel loss that corrosion causes every year, the direct economic loss that caused of U.S.'s invar iron rot in 1975 only up to more than 700 hundred million dollars, accounts for the U.S.'s 4.2% (above all do not contain indirect financial loss) of gross national product then.The data of China's Statistical department shows, the annual invar iron rot of China, and the direct economic loss that is caused accounts for 4% of gross national product.One class iron and steel of the carbon steel amount of being to use maximum, but with respect to stainless steel and cast iron, the antiseptic power of carbon steel is relatively poor.For economizing on resources, the protection environment reduces financial loss, and exploitation is the key that solves the steel corrosion problem with using effective carbon steel aseptic technic.
At present, steel anti-corrosive technology commonly used adopts at steel surface and forms fine and close protective layer, i.e. steel surface coating technology.At present the common coatings technology mainly comprises and sprays paint, electroplates and turn black etc., wherein the surface blackening technology is low because of cost, efficient is high, one of the technology the most frequently used in the steel surface processing that becomes simple to operate, mainly comprises room temperature blackening technology and high-temperature alkaline oxidizing process two big classes.Though the alkaline oxygenated technology cost of room temperature blackening technology relatively-high temperature is lower, to operate simplyr, the quality that the high-temperature alkaline oxidizing process is handled is significantly better than room temperature blackening technology.Therefore, also be widely adopted up to high-temperature alkaline oxidizing process nowadays.The high-temperature alkaline oxidizing process mainly is that raw materials such as sodium hydroxide, SODIUMNITRATE, Sodium Nitrite and some other additive are combined in proportion, and wiring solution-forming immerses surface treatment in the solution with iron and steel under the temperature about 140 ℃ then, obtains Fe
3O
4Black coating.But unfortunately, the Sodium Nitrite of high-temperature alkaline oxidizing process employing is a kind of carcinogenic highly toxic substance.Therefore, the development of new black-emitting technology that do not have a Sodium Nitrite has become the direction of black-emitting technology development from now on.
Hydrothermal method is meant in special closed reactor (autoclave), adopt the aqueous solution as reaction system, by reaction system being heated to critical temperature (or near critical temperature), in reaction system, produce hyperbaric environment and a kind of effective ways of carrying out inorganic synthetic and material preparation.At present, hydrothermal method become the synthesis of nano structured material the most frequently used one of preparation method, have simple to operate, reaction conditions is gentle, product tiny even, with low cost, easily realize advantages such as scale operation.Utilize the special reaction conditions of hydrothermal method, allow the nano particle that in hydrothermal solution, generates constantly grow on the substrate material, can realize the preparation of the fine and close ultra-fine film of high quality.
Summary of the invention
The object of the present invention is to provide the method for superloy surface blackening, make carbon steel in the mixing solutions of ferrous salt, highly basic and hydrazine hydrate through hydro-thermal reaction, form the Fe of black densification on its surface
3O
4Coating.
The technical solution used in the present invention step is as follows:
1) ferrous salt is soluble in water, control its volumetric molar concentration in 0.005~0.1 mol, stir; Adding mole number again is the highly basic of 0~50 times of ferrous salt and 1~10 times hydrazine hydrate, continues to stir; The solution that finally prepares is transferred in the autoclave, and keeping compactedness is 80~90%.
2) the carbon steel substrate is put into above-mentioned autoclave and sealing, in 100~250 ℃ of temperature ranges, handled 4~100 hours, can form the Fe of black densification at steel surface
3O
4Coating.
Described ferrous salt is ferrous sulfate or iron protochloride.
Described highly basic is sodium hydroxide or potassium hydroxide.
Described coating is by superfine Fe
3O
4Granulometric composition, Fe
3O
4Particle diameter is 200~800 nanometers, and thickness is 1~10 micron, and coating and steel surface merge mutually.
The beneficial effect that the present invention has is: adopt common chemical medicine (as ferrous salt, highly basic and hydrazine hydrate), utilize hydro-thermal reaction to generate fine and close Fe at steel surface
3O
4Supercoat.Compare with traditional high-temperature alkaline oxidizing process, present method need not to use carcinogenic highly toxic substances such as Sodium Nitrite, can realize high-quality blackout processing, coat-thickness can be controlled in 1~10 micrometer range, and the present invention can be used for the surface blackening of various carbon steels and handles.
Description of drawings
Fig. 1 is the photomacrograph of embodiment 1 gained blackout sample.
Fig. 2 is the XRD figure spectrum of embodiment 1 gained blackout sample and carbon steel substrate thereof: (a) carbon steel substrate, (b) blackout sample.
Fig. 3 is the field emission scanning electron microscope photo and the sectional view thereof on embodiment 1 gained sample coatings surface: (a) 10,000 times of following stereoscan photographs and sectional view, (b) 100,000 times of following stereoscan photographs.
Embodiment
Embodiment 1:
With 0.222 gram ferrous sulfate (FeSO
47H
2O) be dissolved in 160 ml deionized water, volumetric molar concentration 0.005 mol of ferrous sulfate stirs after 5 minutes; Add 0.128 gram sodium hydroxide again, the volumetric molar concentration of sodium hydroxide is 0.02 mol, stirs after 5 minutes; In above-mentioned solution, add 0.047 gram mass concentration again and be 85% hydrazine hydrate solution, the hydrazine hydrate volumetric molar concentration is 0.005 mol in the final solution, continue to stir after 10 minutes, the above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, keeping compactedness is 80%; Carbon steel side's sheet that will be of a size of 10 millimeters is at last put into above-mentioned solution, and this side's sheet polishes through abrasive paper for metallograph.Above-mentioned solution was handled 8 hours down at 150 ℃, can form the fine and close Fe of black at steel surface
3O
4Supercoat.Fig. 1 is the photomacrograph of present embodiment gained coating, and for clear coating and the substrate distinguished of energy, the right half part of sample removes coating through sand papering, and the steel surface after hydrothermal treatment consists forms the supercoat of black densification as seen from Figure 1.Fig. 2 a is a carbon steel substrate XRD figure spectrum, fits like a glove with the standard card JCPDS no.87-0721 of iron, and Fig. 2 b is the XRD figure spectrum of black coating sample, and except the XRD diffraction peak of iron, other all peak all and Fe among Fig. 2 b
3O
4Standard card JCPDS no.88-0866 fit like a glove.Can show that thus the black coating material is Fe
3O
4Fig. 3 is the field emission scanning electron microscope photo and the sectional view of present embodiment gained coatingsurface, and Fig. 3 shows that black coating is by ultra-fine Fe
3O
4Particle is formed, the about 500nm of particle diameter, and closely arrange between particle.Can find out that from its sectional view coat-thickness is 3 microns, and coating and carbon steel substrate merge mutually.
Embodiment 2:
With 2.502 gram ferrous sulfate (FeSO
47H
2O) be dissolved in 180 ml deionized water, volumetric molar concentration 0.05 mol of ferrous sulfate stirs after 5 minutes; Add 9 gram sodium hydroxide again, the volumetric molar concentration of sodium hydroxide is 1.25 mol, stirs after 5 minutes; In above-mentioned solution, add 2.647 gram mass concentration again and be 85% hydrazine hydrate solution, the hydrazine hydrate volumetric molar concentration is 0.005 mol in the final solution, continue to stir after 10 minutes, the above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, keeping compactedness is 90%; Carbon steel side's sheet that will be of a size of 10 millimeters is at last put into above-mentioned solution, and this side's sheet polishes through abrasive paper for metallograph.Above-mentioned solution was handled 100 hours down at 100 ℃, can form the Fe of black densification at steel surface
3O
4Supercoat.This black coating is by ultra-fine Fe
3O
4Particle is formed, the about 600nm of particle diameter, and closely arrangement between particle, and coat-thickness is 3 microns, and coating and carbon steel substrate merge mutually.
Embodiment 3:
With 3.378 gram iron protochloride (FeCl
24H
2O) be dissolved in 170 ml deionized water, volumetric molar concentration 0.1 mol of iron protochloride stirs after 5 minutes; Add 10 gram mass concentration again and be 85% hydrazine hydrate solution, the hydrazine hydrate volumetric molar concentration is 1 mol in the final solution, continues to stir after 10 minutes, and the above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, and the maintenance compactedness is 85%; Carbon steel side's sheet that will be of a size of 10 millimeters is at last put into above-mentioned solution, and this side's sheet polishes through abrasive paper for metallograph.Above-mentioned solution was handled 4 hours down at 250 ℃, can form the Fe of black densification at steel surface
3O
4Supercoat.This black coating is by ultra-fine Fe
3O
4Particle is formed, the about 200nm of particle diameter, and closely arrangement between particle, and coat-thickness is 5 microns, and coating and carbon steel substrate merge mutually.
Embodiment 4:
With 0.318 gram iron protochloride (FeCl
24H
2O) be dissolved in 160 ml deionized water, volumetric molar concentration 0.01 mol of iron protochloride stirs after 5 minutes; Add 4.488 gram potassium hydroxide again, the volumetric molar concentration of potassium hydroxide is 0.5 mol, stirs after 5 minutes; In above-mentioned solution, add 0.941 gram mass concentration again and be 85% hydrazine hydrate solution, the hydrazine hydrate volumetric molar concentration is 0.1 mol in the final solution, continue to stir after 10 minutes, the above-mentioned solution for preparing is put in the polytetrafluoroethyllining lining of autoclave, keeping compactedness is 80%; Carbon steel side's sheet that will be of a size of 10 millimeters is at last put into above-mentioned solution, and this side's sheet polishes through abrasive paper for metallograph.Above-mentioned solution was handled 100 hours down at 250 ℃, can form the Fe of black densification at steel surface
3O
4Supercoat.This black coating is by ultra-fine Fe
3O
4Particle is formed, the about 800nm of particle diameter, and closely arrangement between particle, and coat-thickness is 10 microns, and coating and carbon steel substrate merge mutually.
Claims (4)
1, the method for superloy surface blackening is characterized in that the step of this method is as follows:
1) ferrous salt is soluble in water, control its volumetric molar concentration in 0.005~0.1 mol, stir; Adding mole number again is the highly basic of 0~50 times of ferrous salt and 1~10 times hydrazine hydrate, continues to stir.The solution that finally prepares is transferred in the autoclave, and keeping compactedness is 80~90%.
2) the carbon steel substrate is put into above-mentioned autoclave and sealing, in 100~250 ℃ of temperature ranges, handled 4~100 hours, can form the Fe of black densification at steel surface
3O
4Coating.
2, the method for superloy surface blackening according to claim 1,, it is characterized in that: described ferrous salt is ferrous sulfate or iron protochloride.
3, the method for superloy surface blackening according to claim 1,, it is characterized in that: described highly basic is sodium hydroxide or potassium hydroxide.
4, the method for superloy surface blackening according to claim 1,, it is characterized in that: described coating is by superfine Fe
3O
4Granulometric composition, Fe
3O
4Particle diameter is 200~800 nanometers, and thickness is 1~10 micron, and coating and steel surface merge mutually.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2007100699849A CN100526505C (en) | 2007-07-11 | 2007-07-11 | Method for carbon steel surface blackening |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2007100699849A CN100526505C (en) | 2007-07-11 | 2007-07-11 | Method for carbon steel surface blackening |
Publications (2)
Publication Number | Publication Date |
---|---|
CN101082129A true CN101082129A (en) | 2007-12-05 |
CN100526505C CN100526505C (en) | 2009-08-12 |
Family
ID=38911904
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Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2007100699849A Expired - Fee Related CN100526505C (en) | 2007-07-11 | 2007-07-11 | Method for carbon steel surface blackening |
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Country | Link |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102011110A (en) * | 2009-09-08 | 2011-04-13 | 日本帕卡濑精株式会社 | Iron group metal material after black surface treatment and manufacturing method thereof |
CN102011117A (en) * | 2010-12-02 | 2011-04-13 | 合肥华清金属表面处理有限责任公司 | Environmental-friendly room-temperature steel blackening agent and preparation method thereof |
CN103255406A (en) * | 2013-05-16 | 2013-08-21 | 浙江吉利汽车研究院有限公司杭州分公司 | Surface treatment method of round steel camshaft and round steel camshaft |
CN108300990A (en) * | 2018-01-31 | 2018-07-20 | 沈阳建筑大学 | A kind of environment-friendly type coloring process of stainless steel cloth |
CN111515578A (en) * | 2019-02-04 | 2020-08-11 | 林肯环球股份有限公司 | Coated welding wire |
CN114107976A (en) * | 2020-08-28 | 2022-03-01 | 湖北大学 | Method for preparing black super-hydrophobic stainless steel based on alkaline hydrothermal reaction |
-
2007
- 2007-07-11 CN CNB2007100699849A patent/CN100526505C/en not_active Expired - Fee Related
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102011110A (en) * | 2009-09-08 | 2011-04-13 | 日本帕卡濑精株式会社 | Iron group metal material after black surface treatment and manufacturing method thereof |
CN102011110B (en) * | 2009-09-08 | 2014-06-25 | 日本帕卡濑精株式会社 | Iron group metal material after black surface treatment and manufacturing method thereof |
CN102011117A (en) * | 2010-12-02 | 2011-04-13 | 合肥华清金属表面处理有限责任公司 | Environmental-friendly room-temperature steel blackening agent and preparation method thereof |
CN103255406A (en) * | 2013-05-16 | 2013-08-21 | 浙江吉利汽车研究院有限公司杭州分公司 | Surface treatment method of round steel camshaft and round steel camshaft |
CN103255406B (en) * | 2013-05-16 | 2016-03-02 | 浙江吉利汽车研究院有限公司杭州分公司 | The surface treatment method of round steel camshaft and round steel camshaft |
CN108300990A (en) * | 2018-01-31 | 2018-07-20 | 沈阳建筑大学 | A kind of environment-friendly type coloring process of stainless steel cloth |
CN108300990B (en) * | 2018-01-31 | 2020-09-22 | 杭州诺诗五金有限公司 | Environment-friendly coloring process for stainless steel wire mesh |
CN111515578A (en) * | 2019-02-04 | 2020-08-11 | 林肯环球股份有限公司 | Coated welding wire |
CN114107976A (en) * | 2020-08-28 | 2022-03-01 | 湖北大学 | Method for preparing black super-hydrophobic stainless steel based on alkaline hydrothermal reaction |
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Publication number | Publication date |
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CN100526505C (en) | 2009-08-12 |
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