CN101864564B - High corrosion-resistance black phosphating process - Google Patents
High corrosion-resistance black phosphating process Download PDFInfo
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- CN101864564B CN101864564B CN2010102254485A CN201010225448A CN101864564B CN 101864564 B CN101864564 B CN 101864564B CN 2010102254485 A CN2010102254485 A CN 2010102254485A CN 201010225448 A CN201010225448 A CN 201010225448A CN 101864564 B CN101864564 B CN 101864564B
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Abstract
The invention relates to a phosphating process, in particular to a high corrosion-resistance black phosphating process for steel pieces, which is characterized by comprising the following steps that: oil removal with organic solvent, chemical oil removal or sand spraying, activation, phosphating, water washing and drying, wherein the phosphating: steel components to be treated after being washed is immediately arranged inside phosphating liquid with the temperature of 65 to 75 DEG C to be soaked for 15 to 30 minutes, free acidity of the phosphating liquid is controlled at 12 to 20 points, and the total acidity is controlled at 120 to 180 points. The phosphating process ensures that the phosphating film crystal of the steel piece is fine, the attachment is firm, the blackness is good, and the corrosion resistance is high, and is particularly applicable to the steel components of optical instruments.
Description
Technical field
The present invention relates to a kind of phosphating process, particularly, belong to field of metal surface treatment technology to a kind of high corrosion-resistance black phosphating process of steel part.
Background technology
Phosphatization is meant that chemical reaction, electrochemical reaction take place metal parts in aqueous phosphate solution, form the process of the phosphate film (phosphatize phosphate coat) of one deck indissoluble in the metallic surface.Phosphatize phosphate coat can improve the solidity to corrosion of metal, improves metallic surface and adhesive force of coatings and heat-resisting, wear resisting property, improves the work-ing life of coat of metal parts.
Present domestic phosphating process is mainly used in the steel part product line for painting and handles, and the main problem that exists has:
1) rete is thin, and solidity to corrosion is poor, is not suitable for the war products of high anti-corrosion requirement;
2) phosphatize phosphate coat appearance luster blackness is not enough, is not suitable for the requirement of optical system part delustring.
For addressing the above problem, common method is a surfaces coated layer protecting film after the employing phosphatization, and this layer protective membrane is organic coating mostly, and the electroconductibility that influences part has increased the thickness of part simultaneously, is not suitable for high precision and cooperates the part that requires.
Summary of the invention
The objective of the invention is in order to solve the problems of the technologies described above: a kind of high corrosion-resistance black phosphating process is provided, makes the phosphorization membrane adhere firmly of steel part, color and luster is black, uniformity.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of high corrosion-resistance black phosphating process is characterized in that: comprise the steps:
1), uses Solvent degreasing;
2), electrochemical deoiling or sandblast;
3), washing;
4), activation;
5), washing;
6), phosphatization, the pending steel components after be about to cleaning is put into temperature immediately and was soaked 15 ~ 30 minutes at 65 ℃ ~ 75 ℃ phosphatization liquid, the free acidity of phosphatization liquid is controlled at 12 ~ 20 points, total acidity is controlled at 120 ~ 180 points;
7), washing;
8), drying.
The component of described phosphatization liquid is by the zinc oxide ZnO of 25 ~ 35g/L, the phosphoric acid H of 120 ~ 135 g/L
3PO
4, 100 ~ 150g/L zinc nitrate Zn (NO
3)
26H
2The nitric acid HNO of O, 5 ~ 8 g/L
3, 3 ~ 5 g/L the tartrate, the nickelous nitrate of 5 ~ 10 g/L of Hydrocerol A, 0.5 ~ 1 g/L form.
The component of described phosphatization liquid is by the zinc oxide ZnO of 30g/L, the phosphoric acid H of 128g/L
3PO
4, 125g/L zinc nitrate Zn (NO
3)
26H
2The nitric acid HNO of O, 6 g/L
3, 4g/L the tartrate, the nickelous nitrate of 8g/L of Hydrocerol A, 0.7g/L form.
Described is steel components to be soaked 3 ~ 5 minutes with clean gasoline or other organic solvent 10 ℃ ~ 35 ℃ of temperature with Solvent degreasing.
Described is steel components to be soaked 4 minutes with clean gasoline or other organic solvent 20 ℃ of temperature with Solvent degreasing.
Described electrochemical deoiling is steel components to be put into chemical solvents when temperature is 70 ℃ ~ 85 ℃, soaked 3 ~ 10 minutes; Said chemical solvents component is by the technical pure sodium hydroxide NaOH of 30 ~ 40g/L, the technical pure yellow soda ash Na of 20 ~ 30g/L
2CO
3, 50 ~ 70g/L technical pure sodium phosphate Na
3PO
4Form.
Described electrochemical deoiling is steel components to be put into chemical solvents when temperature is 80 ℃, soaked 6 minutes; Said chemical solvents component is by the technical pure sodium hydroxide NaOH of 35g/L, the technical pure yellow soda ash Na of 25g/L
2CO
3, 60g/L technical pure sodium phosphate Na
3PO
4Form.
The temperature of described phosphatization is 70 ℃, and phosphating time is 22 minutes, and the free acidity of phosphatization liquid is controlled at 16 points, and total acidity is controlled at 150 points.
The advantage of a kind of high corrosion-resistance black phosphating process of the present invention is: owing to adopted a kind of high corrosion-resistance black phosphating process of the present invention, make the phosphatize phosphate coat crystallization of steel part fine and smooth, and adhere firmly, blackness is good, and solidity to corrosion is high; The steel components that is particularly suitable for opticinstrument uses.
Embodiment
Below in conjunction with embodiment the present invention is done further explain, but not as to qualification of the present invention.
Embodiment 1
1, preparation phosphatization liquid: press the zinc oxide ZnO of 30g/L, the phosphoric acid H of 128g/L
3PO
4, 125g/L zinc nitrate Zn (NO
3)
26H
2The nitric acid HNO of O, 6 g/L
3, 4g/L the liquor capacity amount of nickelous nitrate of tartrate, 8g/L of Hydrocerol A, 0.7g/L, calculate zinc oxide, phosphoric acid, zinc nitrate, nitric acid, Hydrocerol A, tartrate, the nickelous nitrate of requirement; In groove, add 1/3rd zero(ppm) water, phosphoric acid, nitric acid, Hydrocerol A, tartrate, nickelous nitrate are added successively and stir, again zinc oxide is added in the groove after with less water furnishing pasty state; Treat to dissolve fully the last zinc nitrate that adds metering in back, adding distil water stirs to the volume of regulation, can use after the adjustment acidity.
2, the chemical solvents in the preparation electrochemical deoiling: press the technical pure sodium hydroxide NaOH of 35g/L, the technical pure yellow soda ash Na of 25g/L
2CO
3, 60g/L technical pure sodium phosphate Na
3PO
4Calculate sodium hydroxide, yellow soda ash, the sodium phosphate of requirement according to required liquor capacity amount, in groove, add 1/3rd zero(ppm) water, add dissolution of sodium hydroxide earlier after; Add yellow soda ash, sodium phosphate after dissolving successively; Add the volume of tap water, stir, can use to regulation.
3, high corrosion-resistance black phosphating process:
With steel components in order through 1), use Solvent degreasing: it is with clean gasoline 20 ℃ of temperature; Also can be that other organic solvent soaks steel components 4 minutes; Can brush away greasy dirt with fine, soft fur for the bigger screw thread of other greasy dirt or the part of stria shape, oil removing relief titanium alloy component seasoning or dry up with pressurized air; 2), electrochemical deoiling: steel components is put into the above-mentioned chemical solvents for preparing when temperature is 80 ℃, soaked 6 minutes, except that electrochemical deoiling, also adopting can the sandblast mode; 3), washing: wash with mobile water; 4), activation; 5), washing: wash with mobile water; 6) phosphatization, the pending steel components after being about to clean are put into temperature immediately and were soaked 22 minutes at 70 ℃ of above-mentioned phosphatization liquid that prepare, and the free acidity of this phosphatization liquid is controlled at 16 points, and total acidity is controlled at 150 points; 7), washing: wash with mobile water; 8), drying.
4, solidity to corrosion is measured:
Press WJ464-95 chemistry tectum opticinstrument with ferrous metal phosphatization method for normalizing mensuration, cupric sulphate dropping test variable color time >=3 of phosphatize phosphate coat minute reach as high as 11 minutes.
Embodiment 2
1, preparation phosphatization liquid: press the zinc oxide ZnO of 25g/L, the phosphoric acid H of 120g/L
3PO
4, 100g/L zinc nitrate Zn (NO
3)
26H
2The nitric acid HNO of O, 5 g/L
3, 3g/L the liquor capacity amount of nickelous nitrate of tartrate, 5g/L of Hydrocerol A, 0.5g/L, calculate zinc oxide, phosphoric acid, zinc nitrate, nitric acid, Hydrocerol A, tartrate, the nickelous nitrate of requirement; In groove, add 1/3rd zero(ppm) water, phosphoric acid, nitric acid, Hydrocerol A, tartrate, nickelous nitrate are added successively and stir, again zinc oxide is added in the groove after with less water furnishing pasty state; Treat to dissolve fully the last zinc nitrate that adds metering in back, adding distil water stirs to the volume of regulation, can use after the adjustment acidity.
2, the chemical solvents in the preparation electrochemical deoiling: press the technical pure sodium hydroxide NaOH of 30g/L, the technical pure yellow soda ash Na of 20g/L
2CO
3, 50g/L technical pure sodium phosphate Na
3PO
4Calculate sodium hydroxide, yellow soda ash, the sodium phosphate of requirement according to required liquor capacity amount, in groove, add 1/3rd zero(ppm) water, add dissolution of sodium hydroxide earlier after; Add yellow soda ash, sodium phosphate after dissolving successively; Add the volume of tap water, stir, can use to regulation.
3, high corrosion-resistance black phosphating process:
With steel components in order through 1), use Solvent degreasing: it is with clean gasoline 10 ℃ of temperature; Also can be that other organic solvent soaks steel components 3 minutes; Can brush away greasy dirt with fine, soft fur for the bigger screw thread of other greasy dirt or the part of stria shape, oil removing relief titanium alloy component seasoning or dry up with pressurized air; 2), electrochemical deoiling: steel components is put into the above-mentioned chemical solvents for preparing when temperature is 70 ℃, soaked 3 minutes, except that electrochemical deoiling, also adopting can the sandblast mode; 3), washing: wash with mobile water; 4), activation; 5), washing: wash with mobile water; 6) phosphatization, the pending steel components after being about to clean are put into temperature immediately and were soaked 15 minutes at 65 ℃ of above-mentioned phosphatization liquid that prepare, and the free acidity of this phosphatization liquid is controlled at 12 points, and total acidity is controlled at 120 points; 7), washing: wash with mobile water; 8), drying.
4, solidity to corrosion is measured:
Press WJ464-95 chemistry tectum opticinstrument with ferrous metal phosphatization method for normalizing mensuration, cupric sulphate dropping test variable color time >=3 of phosphatize phosphate coat minute reach as high as 11 minutes.
Embodiment 3
1, preparation phosphatization liquid: press the zinc oxide ZnO of 35g/L, the phosphoric acid H of 135g/L
3PO
4, 150g/L zinc nitrate Zn (NO
3)
26H
2The nitric acid HNO of O, 8 g/L
3, 5g/L the liquor capacity amount of nickelous nitrate of tartrate, 10g/L of Hydrocerol A, 1g/L, calculate zinc oxide, phosphoric acid, zinc nitrate, nitric acid, Hydrocerol A, tartrate, the nickelous nitrate of requirement; In groove, add 1/3rd zero(ppm) water, phosphoric acid, nitric acid, Hydrocerol A, tartrate, nickelous nitrate are added successively and stir, again zinc oxide is added in the groove after with less water furnishing pasty state; Treat to dissolve fully the last zinc nitrate that adds metering in back, adding distil water stirs to the volume of regulation, can use after the adjustment acidity.
2, the chemical solvents in the preparation electrochemical deoiling: press the technical pure sodium hydroxide NaOH of 40g/L, the technical pure yellow soda ash Na of 30g/L
2CO
3, 70g/L technical pure sodium phosphate Na
3PO
4Calculate sodium hydroxide, yellow soda ash, the sodium phosphate of requirement according to required liquor capacity amount, in groove, add 1/3rd zero(ppm) water, add dissolution of sodium hydroxide earlier after; Add yellow soda ash, sodium phosphate after dissolving successively; Add the volume of tap water, stir, can use to regulation.
3, high corrosion-resistance black phosphating process:
With steel components in order through 1), use Solvent degreasing: it is with clean gasoline 35 ℃ of temperature; Also can be that other organic solvent soaks steel components 5 minutes; Can brush away greasy dirt with fine, soft fur for the bigger screw thread of other greasy dirt or the part of stria shape, oil removing relief titanium alloy component seasoning or dry up with pressurized air; 2), electrochemical deoiling: steel components is put into the above-mentioned chemical solvents for preparing when temperature is 85 ℃, soaked 10 minutes, except that electrochemical deoiling, also adopting can the sandblast mode; 3), washing: wash with mobile water; 4), activation; 5), washing: wash with mobile water; 6) phosphatization, the pending steel components after being about to clean are put into temperature immediately and were soaked 30 minutes at 75 ℃ of above-mentioned phosphatization liquid that prepare, and the free acidity of this phosphatization liquid is controlled at 20 points, and total acidity is controlled at 180 points; 7), washing: wash with mobile water; 8), drying.
4, solidity to corrosion is measured:
Press WJ464-95 chemistry tectum opticinstrument with ferrous metal phosphatization method for normalizing mensuration, cupric sulphate dropping test variable color time >=3 of phosphatize phosphate coat minute reach as high as 11 minutes.
Because the foregoing description has adopted a kind of high corrosion-resistance black phosphating process of the present invention, make the phosphatize phosphate coat crystallization of steel part fine and smooth, adhere firmly, blackness is good, and solidity to corrosion is high; The steel components that is particularly suitable for opticinstrument uses.
Claims (7)
1. a high corrosion-resistance black phosphating process is characterized in that: comprise the steps:
1), uses Solvent degreasing; 2), electrochemical deoiling or sandblast; 3), washing; 4), activation; 5), washing; 6), phosphatization, the pending steel components after be about to cleaning is put into temperature immediately and was soaked 15 ~ 30 minutes at 65 ℃ ~ 75 ℃ phosphatization liquid, the free acidity of phosphatization liquid is controlled at 12 ~ 20 points, total acidity is controlled at 120 ~ 180 points; 7), washing; 8), drying; The component of described phosphatization liquid is by the zinc oxide ZnO of 25 ~ 35g/L, the phosphoric acid H of 120 ~ 135 g/L
3PO
4, 100 ~ 150g/L zinc nitrate Zn (NO
3)
26H
2The nitric acid HNO of O, 5 ~ 8 g/L
3, 3 ~ 5 g/L the tartrate, the nickelous nitrate of 5 ~ 10 g/L of Hydrocerol A, 0.5 ~ 1 g/L form.
2. a kind of high corrosion-resistance black phosphating process according to claim 1 is characterized in that: the component of described phosphatization liquid is by the zinc oxide ZnO of 30g/L, the phosphoric acid H of 128g/L
3PO
4, 125g/L zinc nitrate Zn (NO
3)
26H
2The nitric acid HNO of O, 6 g/L
3, 4g/L the tartrate, the nickelous nitrate of 8g/L of Hydrocerol A, 0.7g/L form.
3. a kind of high corrosion-resistance black phosphating process according to claim 1 is characterized in that: described is steel components to be soaked 3 ~ 5 minutes with clean gasoline or other organic solvent 10 ℃ ~ 35 ℃ of temperature with Solvent degreasing.
4. a kind of high corrosion-resistance black phosphating process according to claim 1 is characterized in that: described is steel components to be soaked 4 minutes with clean gasoline or other organic solvent 20 ℃ of temperature with Solvent degreasing.
5. a kind of high corrosion-resistance black phosphating process according to claim 1 is characterized in that: described electrochemical deoiling is put into chemical solvents with steel components and when temperature is 70 ℃ ~ 85 ℃, was soaked 3 ~ 10 minutes; Said chemical solvents component is by the technical pure sodium hydroxide NaOH of 30 ~ 40g/L, the technical pure yellow soda ash Na of 20 ~ 30g/L
2CO
3, 50 ~ 70g/L technical pure sodium phosphate Na
3PO
4Form.
6. a kind of high corrosion-resistance black phosphating process according to claim 1 is characterized in that: described electrochemical deoiling is steel components to be put into chemical solvents when temperature is 80 ℃, soaked 6 minutes; Chemical solvents is by the technical pure sodium hydroxide NaOH of 35g/L, the technical pure yellow soda ash Na of 25g/L
2CO
3, 60g/L technical pure sodium phosphate Na
3PO
4Form.
7. a kind of high corrosion-resistance black phosphating process according to claim 1 is characterized in that: the temperature of described phosphatization is 70 ℃, and phosphating time is 22 minutes, and the free acidity of phosphatization liquid is controlled at 16 points, and total acidity is controlled at 150 points.
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| CN2010102254485A CN101864564B (en) | 2010-07-14 | 2010-07-14 | High corrosion-resistance black phosphating process |
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| CN101864564B true CN101864564B (en) | 2012-06-06 |
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Families Citing this family (9)
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|---|---|---|---|---|
| CN102212816A (en) * | 2011-06-02 | 2011-10-12 | 江西昌远机械制造有限公司 | Process for chemically converting phosphate into film by using chemical and electrochemical reaction |
| CN102501181A (en) * | 2011-11-16 | 2012-06-20 | 安徽奥丰汽车配件有限公司 | Metal piece surface deoiling and derusting technology |
| CN102424963B (en) * | 2011-12-23 | 2013-09-18 | 无锡鸿海龙船机有限公司 | Phosphate treatment technology for deformation-free scuffing-resistant inner sleeve |
| CN102978598B (en) * | 2012-12-06 | 2015-07-22 | 三达奥克化学股份有限公司 | General phosphate agent for cast iron, hot steel, hot-rolled plate, pickling board and cold-rolled plate and preparation method thereof |
| CN105112903A (en) * | 2015-09-23 | 2015-12-02 | 尚成荣 | Method for phosphating treatment of clamp for wear-resistant hopper processing |
| CN106757280B (en) * | 2016-12-13 | 2018-09-11 | 河南恒星钢缆股份有限公司 | A kind of low temperature On-line electrolytic dissolution phosphating solution |
| CN108330480B (en) * | 2018-02-26 | 2020-05-15 | 安徽启明表面技术有限公司 | Single-component nickel-free medium-temperature black phosphating solution |
| CN108677174A (en) * | 2018-04-28 | 2018-10-19 | 江苏恒加机械工程有限公司 | A kind of bolt phosphating process |
| CN109097764A (en) * | 2018-07-18 | 2018-12-28 | 苏州瑞沁精密机械有限公司 | A kind of bolt treatment process |
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| CN1210904A (en) * | 1998-07-06 | 1999-03-17 | 王梅 | Zinc-calcium series phosphorization liquid for metal plastic working |
| CN1769522A (en) * | 2005-11-10 | 2006-05-10 | 贵州群建齿轮有限公司 | Formula of phosphatizing liquid for metal surface anti-rusting and phosphatizing process |
| CN101328583A (en) * | 2007-06-22 | 2008-12-24 | 宝山钢铁股份有限公司 | Manganese phosphating liquor, preparation and use thereof |
| CN101713070B (en) * | 2009-11-12 | 2011-08-17 | 浙江金泽恩标准件有限公司 | Process for surface coating of ferrous metal |
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Application publication date: 20101020 Assignee: Xi'an Xiguang Surface Finishing Co., Ltd. Assignor: North Electro-Optics Group Co.,Ltd. Contract record no.: 2013610000015 Denomination of invention: High corrosion-resistance black phosphating process Granted publication date: 20120606 License type: Exclusive License Record date: 20130412 |
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