CN109338346A - A kind of steel normal temperature phosphating method - Google Patents
A kind of steel normal temperature phosphating method Download PDFInfo
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- CN109338346A CN109338346A CN201811245501.0A CN201811245501A CN109338346A CN 109338346 A CN109338346 A CN 109338346A CN 201811245501 A CN201811245501 A CN 201811245501A CN 109338346 A CN109338346 A CN 109338346A
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- steel
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- phosphatization
- normal temperature
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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
- C23C22/05—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 using aqueous solutions
- C23C22/06—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 using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/07—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 using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
- C23C22/08—Orthophosphates
- C23C22/18—Orthophosphates containing manganese cations
- C23C22/182—Orthophosphates containing manganese cations containing also zinc cations
-
- 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
- C23C22/73—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 characterised by the process
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The present invention relates to steel surface processing technology fields, are related to a kind of steel normal temperature phosphating method, and steel to be processed is first carried out surface polishing, acid pickling and rust removing, is then fully immersed in phosphating solution, and the phosphatization under ultrasonic wave effect.Present invention process is simple, without oil removing, table tune and passivation filling work procedure, improves production efficiency；Meanwhile parkerizing process of the present invention is without heating, under room temperature can phosphatization, the energy is greatly saved；Also, present invention phosphatization under ultrasonication, it is low to be formed by phosphorization membrane surface porosity factor, and even film layer is fine and close, has good corrosion resistance, is suitable for commercial introduction.The experiment of copper sulphate drop reaches 322s, and it is not in rust staining that 3% sodium chloride solution soak at room temperature, which is more than 12 hours,.
Description
Technical field
The present invention relates to steel surface processing technology field, specific field is a kind of phosphorization treatment process.
Background technique
Phosphatization is common metal pretreatment technology, belongs to chemical conversion film process, is mainly used in steel, aluminium, zinc part
Equal metal surface phosphatings.Phosphatization is the process of a kind of chemistry and electrochemical reaction formation phosphate chemical conversion film, is formed by
Phosphate conversion film is referred to as phosphating coat.Steel is the widest structural material of modern Application.In order to enhance the anti-corruption of steel substrate
Corrosion energy, prolongs the service life, and is usually surface-treated to steel material, protect metal not vulnerable to water in surface formation energy and
The film layer that other corrosive mediums influence, and further increase in subsequent coating process the binding force of matrix and coating.
Currently, about steel surface parkerizing method there are many kinds of, be largely related to pre-process degreasing process, phosphatization
Preceding table tune process, phosphatization post-passivation or filling work procedure, and degreasing, table reconciliation phosphatization post-passivation or filling can all make phosphatization before phosphatization
Technique becomes complicated, while these three processes can also generate a large amount of waste water, and certain pollution is caused to environment.Moreover, most of
Phosphating process temperature is higher, belongs to high temperature phosphatization.Therefore, a kind of simple process, cleaning, energy-efficient method for bonderizing are found, it is right
Improving production efficiency, protection environment and the porosity for improving phosphatization film surface all has important realistic price and promotional value.
A kind of steel-iron components oxidation phosphorous chemical industry process is disclosed in Chinese invention patent application CN103805980A, is used
FS-1 aqua degreaser carries out oil removing to steel-iron components, while the technique uses 10g/L~30g/L at 70-75 DEG C after phosphatization
Potassium bichromate (K2Cr2O7) phosphatization part is filled.Not only energy consumption is high for the technique, but also produces in oil removing and fill process
Raw a large amount of waste water, especially contain Cr VI in filling liquid, endanger environment and human body serious.Chinese invention patent application
CN101693993A discloses a kind of carbon steel surface phosphorization treatment fluid and nickel plating enclosure method, by it after carbon steel coupon polishing cleaning
It is immersed in surface in the surface adjustment liquid of 5g/L polyphosphoric acids titanium (IV) and adjusts 1~2min, carbon steel coupon is put into nickel plating after phosphatization
Nickel plating enclosure under constant current in liquid, used nickel-plating liquid group become NiSO4.6H2O 200~300g/L, NiCl2.6H20 10
~50g/L, H3BO310~50g/L, 0.4~0.8g/L of saccharin, Isosorbide-5-Nitrae -0.1~0.5g/L of butynediols, lauryl sodium sulfate
0.05~0.2g/L, the nickel-plating liquid also contain nickel ion, have environment to have certain pollution.
Chinese invention patent application CN103938201A discloses a kind of high corrosion-resistance black phosphating method, used phosphorus
Changing temperature is 60~75 DEG C, and operation temperature is higher, and energy consumption is larger.One is disclosed in Chinese invention patent application CN102817023A
Kind high temperature corrosion-resisting phosphating solution, there is also the same problems, and phosphatization heating temperature is 80~95 DEG C, and energy consumption is too big.
Summary of the invention
The purpose of the present invention is to provide a kind of steel normal temperature phosphating methods.The ultrasonic phosphatization under room temperature (20~40 DEG C),
The energy is saved, and the phosphorization membrane of even compact can be formed, further increases steel test piece corrosion resisting property.Pretreatment is reduced simultaneously
Table reconciliation phosphatization post-passivation filling work procedure, simplifies phosphating process, to improve production efficiency, subtracts simultaneously before degreasing, phosphatization
Few discharge of wastewater, protects environment, is conducive to industrialization promotion.
To achieve the above object, the invention provides the following technical scheme:
A kind of steel normal temperature phosphating method, comprising the following steps:
(1) steel test piece to be processed is subjected to surface polishing, washing；
(2) steel test piece is put into hydrochloric acid solution and derusts and descales, take out washing；
(3) it will be put into the phosphating solution for regulating pH value by pretreated steel test piece, under ultrasonication at phosphatization
Reason；
(4) steel test piece after phosphorating treatment is taken out, washing, hair dryer drying.
In the step (1), steel test piece surface is polished using No. 240, No. 360, No. 600, No. 1200 water millings
Sanding and polishing, the washing rinse 1min using flowing running water to paper step by step.
Hydrochloric acid solution is the aqueous solution that concentration is 18% in the step (2), and the temperature used that derusts and descale is 60
DEG C, the time used is 10min；The washing first rinses 1min using flowing running water, then washes 1min with deionized water.
In the step (3), phosphating solution composition are as follows: zinc oxide 12-18g/L, 85% phosphatase 24 0-52ml/L, 50%
Manganese nitrate solution 2-6g/L, citric acid 1-3g/L, hydroxyl sulfate 10-14g/L, surplus are water.
The preparation method of the phosphating solution the following steps are included:
A, the distilled water of total amount one third needed for being added into the beaker equipped with zinc oxide, mechanical stirring is at paste；
B, it is slowly added to the desired amount of phosphoric acid in batches into the resulting solution of step a, it is stirring while adding, keep zinc oxide abundant
Dissolution；
C, load weighted hydroxyl sulfate, citric acid, manganese nitrate are sequentially added in the resulting solution of step b, side edged stirs
It mixes, is stirred evenly to solution, add distilled water constant volume.
In the step (3), the pH of phosphating solution is that the hydroxide of 5mol/L is added dropwise in the case where magnetic stirrer
It is 2.5-2.8 that sodium, which is adjusted to pH value,.
Ultrasonic phosphating plant is ultrasonic cleaning equipment in the step (3), and supersonic frequency 40KHz, what phosphatization used surpasses
Acoustical power is 190~210W；Phosphatization temperature is room temperature, i.e., 20~40 DEG C, 20~35min of phosphating time.
In the step (4), the phosphatization test piece of taking-up washes 2min using flowing running water, then 1min is washed with deionized water.
The control of hair dryer hot blast temperature is dried up at 65-70 DEG C.
Compared with prior art, the beneficial effects of the present invention are:
1) simple process fills three process, operation side without table reconciliation phosphatization post-passivation before pre-processing degreasing, phosphatization
Just, processing cost is low；
2) energy saving, phosphorating treatment can be realized under room temperature；
3) clean manufacturing, entire phosphating process avoid the discharge of wastewater of degreasing, table reconciliation passivation filling work procedure, reduce
The murder by poisoning problem of environment and human body；
4) it works well, using ultrasonic phosphatization, is formed by that phosphorization membrane surface porosity factor is low, and even film layer is fine and close, tool
There is good corrosion resistance, is suitable for commercial introduction.
Detailed description of the invention
Fig. 1 is the process flow diagram of method for bonderizing in the prior art；
Fig. 2 is process flow diagram of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
A kind of steel normal temperature phosphating method, comprising the following steps:
(1) it is polished step by step steel test piece using No. 240, No. 360, No. 600, No. 1200 silicon carbide papers, throws steel surface
Then light rinses 1min using flowing running water.
(2) steel test piece of step (1) is put in 18% hydrochloric acid solution, at 60 DEG C, acid pickling and rust removing descales
Then 10min first rinses 1min using flowing running water, then washes 1min with deionized water.
(3) steel test piece of step (2) is put into phosphating solution and carries out phosphorating treatment, phosphating solution composition are as follows: zinc oxide
15g/L, 85% phosphatase 24 1ml/L, 50% manganese nitrate solution 6g/L, citric acid 1g/L, hydroxyl sulfate 10g/L, surplus is water.
Wherein, phosphating solution preparation method the following steps are included:
A, the distilled water of total amount one third needed for being added into the beaker equipped with zinc oxide, mechanical stirring is at paste；
B, it is slowly added to the desired amount of phosphoric acid in batches into the resulting solution of step a, it is stirring while adding, keep zinc oxide abundant
Dissolution；
C, load weighted hydroxyl sulfate, citric acid, manganese nitrate are sequentially added in the resulting solution of step b, side edged stirs
It mixes, is stirred evenly to solution, add distilled water constant volume.
(4) using the phosphating solution of the sodium hydroxide solution adjusting preparation of 5mol/L to pH value to 2.5-2.8.
(5) ultrasonic cleaning machine is set to supersonic frequency is 40KHz, ultrasonic power 200W, is room temperature in phosphatization temperature
Phosphatization 25min at 20 DEG C.
(6) the phosphatization test piece taken out washes 2min using flowing running water, then 1min is washed with deionized water.Hair dryer hot wind temperature
Degree control is dried up at 65-70 DEG C.
The phosphatization film outward appearance grey black that the present embodiment is prepared, even compact, the experiment of copper sulphate drop reach 151s,
It is not in rust staining that 3% sodium chloride solution soak at room temperature, which is more than 6 hours,.
Embodiment 2
A kind of steel normal temperature phosphating method, comprising the following steps:
(1) it is polished step by step steel test piece using No. 240, No. 360, No. 600, No. 1200 silicon carbide papers, throws steel surface
Then light rinses 1min using flowing running water.
(2) steel test piece of step (1) is put in 18% hydrochloric acid solution, at 60 DEG C, acid pickling and rust removing descales
Then 10min first rinses 1min using flowing running water, then washes 1min with deionized water.
(3) steel test piece of step (2) is put into phosphating solution and carries out phosphorating treatment, phosphating solution composition are as follows: zinc oxide
12g/L, 85% phosphatase 24 7ml/L, 50% manganese nitrate solution 4g/L, citric acid 2g/L, hydroxyl sulfate 12g/L, surplus is water.
Wherein, phosphating solution preparation method the following steps are included:
A, the distilled water of total amount one third needed for being added into the beaker equipped with zinc oxide, mechanical stirring is at paste；
B, it is slowly added to the desired amount of phosphoric acid in batches into the resulting solution of step a, it is stirring while adding, keep zinc oxide abundant
Dissolution；
C, load weighted hydroxyl sulfate, citric acid, manganese nitrate are sequentially added in the resulting solution of step b, side edged stirs
It mixes, is stirred evenly to solution, add distilled water constant volume.
(4) using the phosphating solution of the sodium hydroxide solution adjusting preparation of 5mol/L to pH value to 2.5-2.8.
(5) ultrasonic cleaning machine is set to supersonic frequency is 40KHz, ultrasonic power 210W, is room temperature in phosphatization temperature
Phosphatization 30min at 25 DEG C.
(6) the phosphatization test piece taken out washes 2min using flowing running water, then 1min is washed with deionized water.Hair dryer hot wind temperature
Degree control is dried up at 65-70 DEG C.
The phosphatization film outward appearance grey black that the present embodiment is prepared, even compact, the experiment of copper sulphate drop reach 169s.
It is not in rust staining that 3% sodium chloride solution soak at room temperature, which is more than 6 hours,.
Embodiment 3
A kind of steel normal temperature phosphating method, comprising the following steps:
(1) it is polished step by step steel test piece using No. 240, No. 360, No. 600, No. 1200 silicon carbide papers, throws steel surface
Then light rinses 1min using flowing running water.
(2) steel test piece of step (1) is put in 18% hydrochloric acid solution, at 60 DEG C, acid pickling and rust removing descales
Then 10min first rinses 1min using flowing running water, then washes 1min with deionized water.
(3) steel test piece of step (2) is put into phosphating solution and carries out phosphorating treatment, phosphating solution composition are as follows: zinc oxide
15g/L, 85% phosphoric acid 51ml/L, 50% manganese nitrate solution 5g/L, citric acid 3g/L, hydroxyl sulfate 10g/L, surplus is water.
Wherein, phosphating solution preparation method the following steps are included:
A, the distilled water of total amount one third needed for being added into the beaker equipped with zinc oxide, mechanical stirring is at paste；
B, it is slowly added to the desired amount of phosphoric acid in batches into the resulting solution of step a, it is stirring while adding, keep zinc oxide abundant
Dissolution；
C, load weighted hydroxyl sulfate, citric acid, manganese nitrate are sequentially added in the resulting solution of step b, side edged stirs
It mixes, is stirred evenly to solution, add distilled water constant volume.
(4) using the phosphating solution of the sodium hydroxide solution adjusting preparation of 5mol/L to pH value to 2.5-2.8.
(5) ultrasonic cleaning machine is set to supersonic frequency is 40KHz, ultrasonic power 190W, is room temperature in phosphatization temperature
Phosphatization 35min at 35 DEG C.
(6) the phosphatization test piece taken out washes 2min using flowing running water, then 1min is washed with deionized water.Hair dryer hot wind temperature
Degree control is dried up at 65-70 DEG C.
The phosphatization film outward appearance grey black that the present embodiment is prepared, even compact, the experiment of copper sulphate drop reach 322s.
It is not in rust staining that 3% sodium chloride solution soak at room temperature, which is more than 12 hours,.
Comparative example
Phosphating coat corrosion resistance obtained by existing method for bonderizing and method for bonderizing of the present invention is compared.
Wherein, Fig. 1 be application No. is the existing method for bonderizing of CN108034938A, institute in the bright book of technological parameter
The embodiment 3 of column is consistent；Fig. 2 is method for bonderizing of the present invention, and technological parameter and the embodiment of the present invention 3 are consistent.
The phosphating coat anti-corrosion time obtained by two kinds of method for bonderizing is measured using copper sulphate drop experimental method, is shown from Fig. 1 and Fig. 2
The copper sulphate drop time shown is it is found that can obtain the high phosphating coat of corrosion resistance, phosphorus of the present invention using method for bonderizing of the invention
Drop time of the phosphating coat drop time made from change method much larger than phosphating coat obtained by existing method for bonderizing.Illustrate province of the present invention
Go that pretreatment degreasing, table pacing is rapid before phosphatization and phosphatization can significantly improve phosphating coat corrosion resistance under room temperature ultrasonication, simultaneously
Not only reduce discharge of wastewater, but also save the energy.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of steel normal temperature phosphating method, which comprises the following steps:
(1) steel test piece to be processed is subjected to surface polishing, washing；
(2) steel test piece is put into hydrochloric acid solution and derusts and descales, take out washing；
(3) it will be put into the phosphating solution for regulating pH value by pretreated steel test piece, the phosphorating treatment under ultrasonication；
(4) steel test piece after phosphorating treatment is taken out, washing, hair dryer drying.
2. steel normal temperature phosphating method according to claim 1, it is characterised in that: in the step (1), steel test piece table
Face polishing is using No. 240, No. 360, No. 600, No. 1200 silicon carbide papers sanding and polishing step by step, and the washing is using flowing oneself
Water rinses 1min.
3. steel normal temperature phosphating method according to claim 1, it is characterised in that: hydrochloric acid solution is in the step (2)
The aqueous solution that concentration is 18%, the temperature used that derusts and descale is 60 DEG C, and the time used is 10min；The washing is first adopted
1min is rinsed with flowing running water, then washes 1min with deionized water.
4. steel normal temperature phosphating method according to claim 1, it is characterised in that: in the step (3), phosphating solution is matched
Side is zinc oxide 12-18g/L, 85% phosphatase 24 0-52ml/L, 50% manganese nitrate solution 2-6g/L, citric acid 1-3g/L, sulphur
Sour azanol 10-14g/L, surplus are water.
5. steel normal temperature phosphating method according to claim 4, it is characterised in that: the preparation method of the phosphating solution includes
Following steps:
(1) distilled water of total amount one third needed for being added into the beaker equipped with zinc oxide, mechanical stirring is at paste；
(2) it is slowly added to the desired amount of phosphoric acid in batches into step (1) resulting solution, it is stirring while adding, keep zinc oxide abundant
Dissolution；
(3) load weighted hydroxyl sulfate, citric acid, manganese nitrate are sequentially added in step (2) resulting solution, side edged stirs
It mixes, is stirred evenly to solution, add distilled water constant volume.
6. steel normal temperature phosphating method according to claim 1, it is characterised in that: in the step (3), the pH of phosphating solution
For value in the case where magnetic stirrer, it is 2.5-2.8 that the sodium hydroxide that 5mol/L is added dropwise, which is adjusted to pH value,.
7. steel normal temperature phosphating method according to claim 1, it is characterised in that: in the step (3), the ultrasound phosphorus
Change uses device for ultrasonic cleaning equipment, supersonic frequency 40KHz, and phosphatization ultrasonic power is 190~210W；Ultrasonic phosphatization temperature
For room temperature, i.e., 20~40 DEG C, ultrasonic 20~35min of phosphating time.
8. steel normal temperature phosphating method according to claim 1, it is characterised in that: in the step (4), the phosphatization of taking-up
Test piece washes 2min using flowing running water, then 1min is washed with deionized water, and is then blown with hair dryer control temperature at 65-70 DEG C
It is dry.
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| CN201811245501.0A CN109338346A (en) | 2018-10-24 | 2018-10-24 | A kind of steel normal temperature phosphating method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111155076A (en) * | 2020-01-14 | 2020-05-15 | 山东建筑大学 | Process for preparing metal phosphating film based on ultrasonic waves |
| CN113046737A (en) * | 2021-03-11 | 2021-06-29 | 廊坊师范学院 | Method for treating metal surface by using hydroxylamine zinc phosphating solution |
| CN117358558A (en) * | 2023-09-09 | 2024-01-09 | 新疆八一钢铁股份有限公司 | Medium plate surface protection treatment method |
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|---|---|---|---|---|
| CN104651820A (en) * | 2015-02-16 | 2015-05-27 | 天津大学 | Ultrasonic phosphating solution for carbon steel, preparation method thereof and method for phosphating carbon steel by adopting phosphating solution |
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2018
- 2018-10-24 CN CN201811245501.0A patent/CN109338346A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104651820A (en) * | 2015-02-16 | 2015-05-27 | 天津大学 | Ultrasonic phosphating solution for carbon steel, preparation method thereof and method for phosphating carbon steel by adopting phosphating solution |
Non-Patent Citations (1)
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| 孙秀秀: "碳钢超声磷化膜和涂层封孔膜在模拟干热岩地热水中的耐蚀性能", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111155076A (en) * | 2020-01-14 | 2020-05-15 | 山东建筑大学 | Process for preparing metal phosphating film based on ultrasonic waves |
| CN113046737A (en) * | 2021-03-11 | 2021-06-29 | 廊坊师范学院 | Method for treating metal surface by using hydroxylamine zinc phosphating solution |
| CN117358558A (en) * | 2023-09-09 | 2024-01-09 | 新疆八一钢铁股份有限公司 | Medium plate surface protection treatment method |
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Application publication date: 20190215 |