CN113174593A - Production process of cold-drawn section steel - Google Patents
Production process of cold-drawn section steel Download PDFInfo
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- CN113174593A CN113174593A CN202110431165.4A CN202110431165A CN113174593A CN 113174593 A CN113174593 A CN 113174593A CN 202110431165 A CN202110431165 A CN 202110431165A CN 113174593 A CN113174593 A CN 113174593A
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- billet
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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
- C23C22/34—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 fluorides or complex fluorides
- C23C22/36—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 fluorides or complex fluorides containing also phosphates
- C23C22/364—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 fluorides or complex fluorides containing also phosphates containing also manganese 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
- C23C22/78—Pretreatment of the material to be coated
-
- 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
- C23C22/82—After-treatment
Abstract
The invention discloses a production process of cold-drawn section steel, which comprises the following steps: step 1: grinding a decarburized layer of the billet with the decarburized surface; step 2: alkaline washing to remove the steel billet after the carbon removal layer so as to remove oil stains and abrasive dust on the surface of the steel billet; and step 3: washing, phosphorizing, saponifying and drying the alkali-washed steel billet in sequence; and 4, step 4: the dried billet is subjected to pointing, drawing, annealing and straightening in sequence; the phosphating solution used in the phosphating process comprises the following components in parts by weight: 50-70g/L zinc dihydrogen phosphate, 70-90g/L zinc nitrate, 45-55g/L permanganate, 0.5-1.5g/L organic accelerator, 3-6g/L complexing agent, 1-3g/L film-forming aid, 1-2g/L emulsifying agent, 1-3ml/L emulsifying agent and the balance of water. The invention has the beneficial effects that: the cold-drawn steel produced by the production process has excellent corrosion resistance.
Description
Technical Field
The invention relates to steel, in particular to a production process of cold-drawn steel.
Background
Cold-drawn steel sections are steel products of various cross-sectional shapes and sizes produced by cold drawing, and may be classified into cold-drawn round steel, cold-drawn square steel, cold-drawn flat steel, cold-drawn hexagonal steel, cold-drawn deformed steel, and the like. In the production of cold-drawn steel, it is generally necessary to remove an oxide layer on the surface of a steel slab by pickling the steel slab with sulfuric acid. Therefore, not only the billet is easy to corrode, but also the environment is polluted.
Chinese patent publication No. CN111672927A discloses a method for manufacturing cold-drawn special steel round steel without decarburized layer on the surface. The manufacturing method comprises the following steps: (1) and (3) inspecting the steel blank before cold drawing: selecting a steel blank with qualified quality and hardness and decarburized surface; (2) completely grinding a decarburized layer on the surface of a steel blank; (3) alkaline washing to remove the steel blank of the decarburized layer and remove oil stains and abrasive dust on the surface; (4) sequentially carrying out phosphating, saponification and drying treatment on the steel blank after alkali washing; (5) and (3) performing pointing, drawing and straightening on the dried steel blank to obtain the cold-drawn special steel round steel without the decarburized layer on the surface. The manufacturing method omits the step of pickling, thereby avoiding the corrosion to the billet and reducing the pollution to the environment.
However, when the alkali-washed billet is phosphated and saponified, the phosphating solution component of the production method is zinc dihydrogen phosphate, and it is difficult to form an excellent phosphate film on the surface of the alkali-washed billet, so that the formed cold-drawn steel is likely to rust, and improvement is needed.
Disclosure of Invention
The invention aims to provide a production process of cold-drawn steel. The cold-drawn steel produced by the production process has excellent corrosion resistance.
The technical purpose of the invention is realized by the following technical scheme:
a production process of cold-drawn steel comprises the following steps:
step 1: grinding a decarburized layer of the billet with the decarburized surface;
step 2: alkaline washing to remove the steel billet after the carbon removal layer so as to remove oil stains and abrasive dust on the surface of the steel billet;
and step 3: washing, phosphorizing, saponifying and drying the alkali-washed steel billet in sequence;
and 4, step 4: the dried billet is subjected to pointing, drawing, annealing and straightening in sequence;
the phosphating solution used in the phosphating process comprises the following components in parts by weight:
50-70g/L zinc dihydrogen phosphate
70-90g/L zinc nitrate
Permanganate 45-55g/L
Chlorate 0.5-1.5g/L
3-6g/L of organic accelerator
1-3g/L complexing agent
1-2g/L of film-forming additive
Emulsifier 1-3ml/L
The balance being water.
The invention is further configured to: the organic accelerator comprises a m-nitro compound and hydroxylamine sulfate, wherein the weight ratio of the m-nitro compound to the hydroxylamine sulfate is 1: 1-3.
The invention is further configured to: the m-nitro compound is sodium m-nitrobenzenesulfonate.
The invention is further configured to: the complexing agent is citric acid.
The invention is further configured to: the film-forming aid is sodium fluoride.
The invention is further configured to: the emulsifier is OP-10.
The invention is further configured to: the permanganate is sodium permanganate.
The invention is further configured to: the chlorate is sodium chlorate.
The invention is further configured to: the preparation method of the phosphating solution comprises the following steps: zinc dihydrogen phosphate, zinc nitrate, permanganate, chlorate, organic accelerator, complexing agent, film-forming assistant, emulsifier and water are obtained according to the proportion and then are mixed and stirred evenly.
The invention is further configured to: the phosphorization comprises the following steps:
and (3) soaking the washed steel billet into the phosphating solution for 5-10min at the temperature of 20-40 ℃, taking out the steel billet, naturally airing the steel billet, and then washing the steel billet with water.
In conclusion, the invention has the following beneficial effects:
1. zinc dihydrogen phosphate is one of basic components for phosphating film forming, can ensure the pH stability of a phosphating solution system, and mainly plays a role in regulating total acid and free acid. When the consumption of zinc dihydrogen phosphate is too low, the free acidity is low, the anode is slowly dissolved, the phosphating capability is weak, a phosphating film is too thin and even does not form a film, and meanwhile, the stability of the phosphating solution is poor, and extra sediments are generated. When the content of zinc dihydrogen phosphate is too high, the free acidity is high, so that the dissolution speed of the anode is higher than the deposition speed of a phosphating film, the film forming is too slow, and the film layer is rough and loose;
2. the zinc nitrate mainly plays a stabilizing role in the phosphating process, stabilizes the components of the phosphating solution, has the function of primary oxidation balance and inhibits the zinc dihydrogen phosphate from being changed into suspended sediment of zinc phosphate in the reaction process. Zinc nitrate can adjust the total acidity and also provide nitrate ions. Nitrate ions have oxidizability, and can promote the formation of a phosphating film, accelerate the phosphating speed and reduce the phosphating temperature. Under proper conditions, the nitrate ions and the steel billet react to generate a small amount of nitric oxide, so that divalent iron ions are stabilized. The zinc nitrate concentration is too low, the phosphorization film forming speed is slow, and the phosphorization film is loose and dark; the concentration of zinc nitrate is too high, the phosphorization film forming speed is too high, the phosphorization film is coarse and thick in crystallization, the film layer is coarse and loose, the adhesive force is poor, and floating ash exists on the surface;
3. the permanganate is beneficial to generating crystal nucleus and refining crystal grains, and the deposition speed of the phosphating film at normal temperature is accelerated. Meanwhile, manganese also participates in the phosphating film formation to generate manganese phosphate with excellent corrosion resistance in the phosphating film. The permanganate is used as a strong oxidant, can directly oxidize nascent hydrogen atoms and iron generated in the phosphorization process, and has a quick promotion effect;
4. chlorate is a strengthening oxidant, can directly oxidize nascent hydrogen atoms and iron generated in the phosphating process, and has the advantages of quick promotion effect, compact phosphating film and good protection. However, chlorate is reduced to generate chloride ions, which not only corrode the substrate, but also can be absorbed by the phosphating film to participate in crystallization, so that the phosphating film generates a white spot phenomenon. In the presence of permanganate, chlorate can be reduced, thereby reducing the generation of chloride ions and the corresponding negative effects. In addition, manganese ions generated by permanganate can also accelerate the oxidation of nascent hydrogen atoms and iron;
5. the sodium m-nitrobenzenesulfonate has the effects of depolarization and anode area blockage, the anode area can be converted into the cathode area in the phosphating treatment, and the area ratio of the cathode area to the anode area is increased, so that the effect of accelerating the phosphating is achieved, and a uniform and compact phosphating film is quickly formed;
6. the hydroxylamine sulfate can generate higher reduction potential after being compounded with chlorate and sodium m-nitrobenzenesulfonate, and iron is quickly oxidized into ferrous ions to form a phosphating film with higher corrosion resistance. Hydroxylamine sulphate can reduce the ferric iron produced during the phosphating process to ferrous iron on the one hand and can formThe coordination adsorption reduces the electrode potential of iron, accelerates the dissolution of matrix iron, finally accelerates the generation of ferrous iron in the solution, and is beneficial to a P film (Zn)2Fe(PO4)2H2O) to greatly improve the corrosion resistance of the phosphating film, and the extremely strong depolarization capacity of the hydroxylamine sulfate greatly shortens the progress of the phosphating reaction and accelerates the reaction speed;
7. the action mechanism of the complexing agent is to form a soluble complex with iron ions, thereby reducing the generation of the sediment of the phosphating solution and prolonging the service life of the phosphating solution. The complexing agent reduces the concentration of ferrous iron on the surface of the billet in the phosphating process, thereby playing a role in depolarization and accelerating the phosphating film-forming process. Meanwhile, citric acid as organic weak acid can be cooperated with phosphoric acid to increase cathode polarization, so that the crystal boundary on the surface of the billet is fully exposed, a large number of active points are provided for phosphorization nucleation, a uniformly and compactly crystallized phosphorized film is formed, the porosity of the phosphorized film is reduced, and the binding force between the phosphorized film and a substrate is improved. Compared with tartaric acid, the citric acid has more carboxyl groups in molecules and can provide more hydrogen ions, so that on one hand, more alkali remained on the surface of a steel billet after water washing can be neutralized, on the other hand, hydrogen ions can be provided for oxidation of permanganate, and the oxidation performance of the steel billet is enhanced;
8. the fluoride is used as a film forming aid, can improve the uniformity of a phosphating film and can also accelerate the phosphating film forming speed. Because the fluorine ions have large electronegativity and large electron affinity, the hydrogen overpotential is reduced, and the cathode depolarization effect is achieved, so that the cathode surface presents an active region which is favorable for phosphate crystal nucleation, the phosphating process is accelerated, and the crystallization is refined. The fluorine ions are easy to combine with the hydrogen ions to form hydrofluoric acid, and when the free acidity of the solution is reduced, the hydrogen ions are released to adjust the acidity of the phosphating solution. The fluoride and the citric acid are matched, so that the pH of the phosphating solution is stable in the using process, and the service life of the phosphating solution is prolonged. The fluorinion also has stronger complexing ability to ferric iron and is easy to form a complex with a stable regular octahedral structure;
9. OP-10 is a nonionic surfactant, which can reduce the surface tension of the phosphating solution in the phosphating process, is beneficial to the escape of hydrogen in the phosphating reaction and enhances the depolarization of a cathode, thereby accelerating the phosphating film-forming process, has the functions of emulsifying and solubilizing oil stains adhered to the metal surface, can prevent the redeposition of the dirt, enables the solution to be wetted and permeated, and is beneficial to the contact between the phosphating solution and the surface of a billet. The OP-10 can also reduce the porosity and water absorption of the phosphating film, promote the metal surface to form a hard and compact phosphating film and improve the uniformity and corrosion resistance of the phosphating film;
10. the steel billet taken out from the phosphating solution is washed by water to remove residues on a phosphating film, so that the corrosion and ash hanging of the phosphating film are avoided. And the steel billet is naturally dried before being washed by water, so that the film forming reaction of the phosphating solution on the surface of the steel billet is avoided.
Detailed Description
Examples 1-5 are provided to illustrate the components of the phosphating solutions. The components of the phosphating solutions of examples 1 to 5 are shown in the table below.
TABLE 1, composition of phosphating solutions of examples 1-5
Note: the organic accelerant comprises a m-nitro compound and hydroxylamine sulfate, wherein the m-nitro compound is sodium m-nitrobenzenesulfonate. The complexing agent is citric acid, the film-forming additive is sodium fluoride, and the emulsifier is OP-10.
The following will describe in detail the preparation of the phosphating solutions of examples 1 to 5 with reference to Table 1.
A preparation method of phosphating solution comprises the following steps:
zinc dihydrogen phosphate, zinc nitrate, permanganate, chlorate, organic accelerator, complexing agent, film-forming assistant, emulsifier and water are obtained according to the proportion and then are mixed and stirred evenly.
Examples 6 to 10 are provided to illustrate the production process of cold drawn steel.
Example 6
A production process of cold-drawn steel comprises the following steps:
step 1: grinding a decarburized layer of the billet with the decarburized surface;
step 2: alkaline washing to remove the steel billet after the carbon removal layer so as to remove oil stains and abrasive dust on the surface of the steel billet;
and step 3: washing, phosphorizing, saponifying and drying the alkali-washed steel billet in sequence;
and 4, step 4: and (3) sequentially carrying out pointing, drawing, annealing and straightening on the dried billet.
Wherein, the phosphorization comprises the following steps:
the water-washed steel slab was immersed in the phosphating solution prepared in example 1 at 20 ℃ for 10min, taken out, naturally dried, and then water-washed.
Example 7
Example 7 differs from example 6 in the phosphating.
In example 7, the phosphating comprises the following steps:
the water-washed steel slab was immersed in the phosphating solution prepared in example 2 at 25 ℃ for 10min, taken out, naturally dried, and then water-washed.
Example 8
Example 8 differs from example 6 in the phosphating.
In example 8, the phosphating comprised the following steps:
the water-washed steel slab was immersed in the phosphating solution prepared in example 3 at 30 ℃ for 8min, taken out, naturally dried, and then water-washed.
Example 9
Example 9 differs from example 6 in the phosphating.
In example 9, the phosphating comprises the following steps:
the water-washed steel slab was immersed in the phosphating solution prepared in example 4 at 35 c for 8min, taken out, naturally dried, and then water-washed.
Example 10
Example 10 differs from example 6 in the phosphating.
In example 10, the phosphating comprises the following steps:
the water-washed steel slab was immersed in the phosphating solution prepared in example 5 at 40 ℃ for 5min, taken out, naturally dried, and then water-washed.
Test for Corrosion resistance
The cold-drawn steel prepared in examples 6 to 10 was subjected to a corrosion resistance test with reference to "salt spray test for GB/T10125-2012 Artificial atmosphere Corrosion test".
TABLE 2, and the test record tables of examples 6 to 10 for corrosion resistance
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications without inventive contribution to the present embodiment as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (10)
1. A production process of cold-drawn steel is characterized by comprising the following steps: the method comprises the following steps:
step 1: grinding a decarburized layer of the billet with the decarburized surface;
step 2: alkaline washing to remove the steel billet after the carbon removal layer so as to remove oil stains and abrasive dust on the surface of the steel billet;
and step 3: washing, phosphorizing, saponifying and drying the alkali-washed steel billet in sequence;
and 4, step 4: the dried billet is subjected to pointing, drawing, annealing and straightening in sequence;
the phosphating solution used in the phosphating process comprises the following components in parts by weight:
50-70g/L zinc dihydrogen phosphate
70-90g/L zinc nitrate
Permanganate 45-55g/L
Chlorate 0.5-1.5g/L
3-6g/L of organic accelerator
1-3g/L complexing agent
1-2g/L of film-forming additive
Emulsifier 1-3ml/L
The balance being water.
2. A process for producing cold drawn steel according to claim 1, wherein: the organic accelerator comprises a m-nitro compound and hydroxylamine sulfate, wherein the weight ratio of the m-nitro compound to the hydroxylamine sulfate is 1: 1-3.
3. A process for producing cold drawn steel according to claim 2, wherein: the m-nitro compound is sodium m-nitrobenzenesulfonate.
4. A process for producing cold drawn steel according to claim 1, wherein: the complexing agent is citric acid.
5. A process for producing cold drawn steel according to claim 1, wherein: the film-forming aid is sodium fluoride.
6. A process for producing cold drawn steel according to claim 1, wherein: the emulsifier is OP-10.
7. A process for producing cold drawn steel according to claim 1, wherein: the permanganate is sodium permanganate.
8. A process for producing cold drawn steel according to claim 1, wherein: the chlorate is sodium chlorate.
9. A process for producing cold drawn steel according to claim 1, wherein: the preparation method of the phosphating solution comprises the following steps: zinc dihydrogen phosphate, zinc nitrate, permanganate, chlorate, organic accelerator, complexing agent, film-forming assistant, emulsifier and water are obtained according to the proportion and then are mixed and stirred evenly.
10. A process for producing cold drawn steel according to claim 1, wherein: the phosphorization comprises the following steps:
and (3) soaking the washed steel billet into the phosphating solution for 5-10min at the temperature of 20-40 ℃, taking out the steel billet, naturally airing the steel billet, and then washing the steel billet with water.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703889A (en) * | 2012-05-28 | 2012-10-03 | 武汉永正科技发展有限公司 | Low-temperature single-component zinc series phosphating solution and preparation method thereof |
| CN103757620A (en) * | 2014-02-07 | 2014-04-30 | 蚌埠市钰诚新材料科技有限公司 | Phosphating solution for drawing of low-carbon and medium-carbon steel wire rod |
| CN104498921A (en) * | 2014-12-11 | 2015-04-08 | 国家电网公司 | Special treating agent for galvanizing surface chemical conversion and treating technique thereof |
| CN104988477A (en) * | 2015-07-14 | 2015-10-21 | 武汉富诗特科技有限公司 | Normal-temperature phosphating fluid for drawing steel |
| CN105543826A (en) * | 2015-12-29 | 2016-05-04 | 钢铁研究总院 | Normal-temperature phosphating solution forming phosphating film highly resistant to corrosion, preparing method and phosphating technology |
| CN111672927A (en) * | 2020-05-28 | 2020-09-18 | 大冶特殊钢有限公司 | Method for manufacturing cold-drawn special steel round steel without decarburized layer on surface |
-
2021
- 2021-04-21 CN CN202110431165.4A patent/CN113174593A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703889A (en) * | 2012-05-28 | 2012-10-03 | 武汉永正科技发展有限公司 | Low-temperature single-component zinc series phosphating solution and preparation method thereof |
| CN103757620A (en) * | 2014-02-07 | 2014-04-30 | 蚌埠市钰诚新材料科技有限公司 | Phosphating solution for drawing of low-carbon and medium-carbon steel wire rod |
| CN104498921A (en) * | 2014-12-11 | 2015-04-08 | 国家电网公司 | Special treating agent for galvanizing surface chemical conversion and treating technique thereof |
| CN104988477A (en) * | 2015-07-14 | 2015-10-21 | 武汉富诗特科技有限公司 | Normal-temperature phosphating fluid for drawing steel |
| CN105543826A (en) * | 2015-12-29 | 2016-05-04 | 钢铁研究总院 | Normal-temperature phosphating solution forming phosphating film highly resistant to corrosion, preparing method and phosphating technology |
| CN111672927A (en) * | 2020-05-28 | 2020-09-18 | 大冶特殊钢有限公司 | Method for manufacturing cold-drawn special steel round steel without decarburized layer on surface |
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Application publication date: 20210727 |