CN112410769A - Phosphating solution for drawing and preparation method thereof - Google Patents
Phosphating solution for drawing and preparation method thereof Download PDFInfo
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- CN112410769A CN112410769A CN202011227467.1A CN202011227467A CN112410769A CN 112410769 A CN112410769 A CN 112410769A CN 202011227467 A CN202011227467 A CN 202011227467A CN 112410769 A CN112410769 A CN 112410769A
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- phosphating
- nitrate
- calcium
- phosphate
- phosphating solution
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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
- C23C22/22—Orthophosphates containing alkaline earth metal cations
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- Chemical & Material Sciences (AREA)
- 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 invention discloses a preparation method of phosphating solution for drawing, which comprises 5-40g/L of zinc ions, 70-85g/L of phosphate radicals, 80-150g/L of calcium ions, 30-50g/L of nitrate radicals, 20-30g/L of organic acid and 0.1-0.5g/L of sodium nitrite, and a formed phosphating film with calcium phosphate as a component is more and more compact. The phosphate film formed by calcium phosphate is porous, is convenient for carrying lubricant, has strong binding force, and improves the drawing speed.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of chemical industry, in particular to a phosphating solution for drawing and a preparation method thereof.
[ background of the invention ]
The phosphating treatment is a process of treating metal in a solution containing phosphate to form a phosphate chemical conversion coating on the surface of the metal. The phosphating film can be applied to metals or alloys such as steel, aluminum, magnesium and the like for more than one hundred years, not only can improve corrosion resistance and adhesion between a matrix and a coating, but also can obviously improve the surface friction performance of a workpiece and improve the cold processing performance of the material. However, the existing phosphating films have poor bonding force, so that the drawing quality is poor.
Therefore, the problem to be solved in the art is to provide an improved phosphating solution for drawing.
[ summary of the invention ]
The invention provides a preparation method of a phosphating solution for drawing aiming at the problems.
In order to solve the problems, the preparation method of the phosphating solution for drawing comprises 5-40g/L of zinc ions, 70-85g/L of phosphate radical, 80-150g/L of calcium ions, 30-50g/L of nitrate radical, 20-30g/L of organic acid and 0.1-0.5g/L of sodium nitrite.
Further, the zinc ion is derived from at least one of zinc nitrate and zinc dihydrogen phosphate.
Further, the phosphate is derived from phosphoric acid.
Further, the calcium ions are derived from calcium nitrate and calcium dihydrogen phosphate, and the nitrates are derived from zinc nitrate and calcium nitrate.
Further, the organic acid may be derived from at least one of citric acid and tartaric acid.
Further, the nitrate is derived from zinc nitrate and calcium nitrate.
Compared with the prior art, the invention has the following advantages: the phosphating solution for drawing prepared by the invention contains two metal ions, namely zinc ions and calcium ions, wherein the content of the calcium ions is far greater than that of the zinc ions, so that a compact phosphating film with calcium phosphate as a component is formed, the phosphating film formed by the calcium phosphate is porous, is convenient for carrying a lubricant, has strong binding force, and improves the drawing speed. The content of nitrite is greatly reduced, so that the amount of phosphorization slag of the phosphorization liquid is greatly reduced, the period of the guide groove is prolonged, and the production efficiency is improved.
[ description of the drawings ]
Is free of
[ detailed description ] embodiments
One or more groups of adjustable direct current power supplies with 0-20V are selected to provide adjustable direct current. The anode is a titanium plate or a titanium mesh plated with an inert layer on the surface, the inert layer can be made of metals with strong inertia such as platinum, iridium and the like, and the phosphated steel wire is used as the cathode. In order to make the current distribution around the wire uniform, multiple power supplies may be used simultaneously, each connected to an anode, forming multiple electrode pairs with the wire. The steel wire or wire rod is treated by acid cleaning, water cleaning and surface conditioning, and then different formulas of phosphating solutions are selected. The phosphating solution for drawing comprises 5-40g/L of zinc ions, 70-85g/L of phosphate radicals, 80-150g/L of calcium ions, 30-50g/L of nitrate radicals, 20-30g/L of organic acids and 0.1-0.5g/L of sodium nitrite, wherein the zinc ions are derived from at least one of zinc nitrate and zinc dihydrogen phosphate, the phosphate radicals are derived from phosphoric acid, the calcium ions are derived from calcium nitrate and calcium dihydrogen phosphate, the nitrate radicals are derived from zinc nitrate and calcium nitrate, and the organic acids can be derived from at least one of citric acid and tartaric acid. The specific implementation case is as follows:
example 1:
a phosphating solution for drawing comprises 8g/L of zinc ions, 76g/L of phosphate radicals, 122g/L of calcium ions, 42g/L of nitrate radicals, 20g/L of organic acid and 0.1g/L of sodium nitrite, and is prepared by using a No. 70 steel wire with the specification of 3.6mm in wire diameter, the phosphating temperature of 60 ℃, the phosphating temperature of 100 seconds and the current density of 2A/dm2Film weight after phosphating of 8g/m2The phosphating film is complete and has grey and black color.
Example 2:
a phosphating solution for drawing comprises 5g/L of zinc ions, 70g/L of phosphate radicals, 150g/L of calcium ions, 50g/L of nitrate radicals, 30g/L of organic acid and 0.1g/L of sodium nitrite, and is prepared by using a No. 70 steel wire with the specification of 3.6mm in wire diameter, the phosphating temperature of 60 ℃, the phosphating temperature of 100 seconds and the current density of 2A/dm2The film after phosphating weighs 10g/m2The phosphating film is complete and dark in color.
Example 3:
a phosphating solution for drawing contains 30g/L of zinc ions, 80g/L of phosphate radicals, 90g/L of calcium ions, 30g/L of nitrate radicals, 25g/L of organic acid and 0.5g/L of sodium nitrite, and uses a No. 70 steel wire with the specification of 3.6mm in wire diameter, the phosphating temperature is 60 ℃, the phosphating temperature is 100 seconds, and the current density is 2A/dm2Film weight after phosphating 4g/m2The phosphating film is complete and has grey and black color.
Example 4:
a phosphating solution for drawing comprises 8g/L of zinc ions, 76g/L of phosphate radicals, 122g/L of calcium ions, 42g/L of nitrate radicals, 20g/L of organic acid and 0.1g/L of sodium nitrite, and is prepared by using a No. 70 steel wire with the specification of 3.6mm in wire diameter, the phosphating temperature of 60 ℃, the phosphating temperature of 100 seconds and the current density of 2A/dm2Film weight after phosphating of 8g/m2The phosphating film is complete and dark in color.
Comparative example
A phosphating solution for drawing comprises 5g/L of zinc ions, 85g/L of phosphate radicals, 60g/L of calcium ions, 50g/L of nitrate radicals, 20g/L of organic acid and 0.1g/L of sodium nitrite, and is prepared by using a No. 70 steel wire with the specification of 3.6mm in wire diameter, the phosphating temperature of 60 ℃, the phosphating temperature of 100 seconds and the current density of 2A/dm2The film after phosphating weighs 3g/m2The phosphating film is complete and is grey and black.
Examples of the experiments
The phosphating solutions for drawing prepared in examples 1 to 4 and comparative example were respectively subjected to performance tests, mainly considering the drawing speed for metal wire rods, taking steel wires as an example.
And (3) testing: the drawing test was carried out using a drawing machine, and the drawing speed of the drawing phosphating solutions prepared in examples and comparative examples was measured.
TABLE 1 Performance data of the phosphating solutions for drawing and comparative examples prepared in the examples
Item | Drawing speed (m/s) |
Example 1 | 8 |
Example 2 | 6 |
Example 3 | 8 |
Example 4 | 7 |
Comparative example | 5 |
As is clear from Table 1, the calcium ion content of the phosphating solutions for drawing prepared in examples 1 to 4 was much larger than that of the comparative examples, and more compact phosphating films containing calcium phosphate were formed. The phosphate film formed by calcium phosphate is porous, is convenient for carrying lubricant, has strong binding force, and improves the drawing speed. The drawing speeds of the drawing phosphatizing solutions prepared in examples 1 to 4 were much higher than those of the comparative examples.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. The preparation method of the phosphating solution for drawing is characterized in that the phosphating solution for drawing comprises 5-40g/L of zinc ions, 70-85g/L of phosphate radicals, 80-150g/L of calcium ions, 30-50g/L of nitrate radicals, 20-30g/L of organic acid and 0.1-0.5g/L of sodium nitrite.
2. The method of preparing a phosphating solution for drawing according to claim 1, characterized in that: the zinc ion is derived from at least one of zinc nitrate and zinc dihydrogen phosphate.
3. The method of preparing a phosphating solution for drawing according to claim 1, characterized in that: the phosphate radical is derived from phosphoric acid.
4. The method of preparing a phosphating solution for drawing according to claim 1, characterized in that: the calcium ions are from calcium nitrate and calcium dihydrogen phosphate, and the nitrate radicals are from zinc nitrate and calcium nitrate.
5. The method of preparing a phosphating solution for drawing according to claim 1, characterized in that: the organic acid can be derived from at least one of citric acid and tartaric acid.
6. The method of preparing a phosphating solution for drawing according to claim 1, characterized in that: the nitrate radical is derived from zinc nitrate and calcium nitrate.
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CN202011227467.1A CN112410769A (en) | 2020-11-06 | 2020-11-06 | Phosphating solution for drawing and preparation method thereof |
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CN202011227467.1A CN112410769A (en) | 2020-11-06 | 2020-11-06 | Phosphating solution for drawing and preparation method thereof |
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109056034A (en) * | 2018-08-03 | 2018-12-21 | 南京派诺金属表面处理技术有限公司 | Room temperature electrolytic phosphating process and phosphating solution |
CN109468623A (en) * | 2018-12-29 | 2019-03-15 | 南京派诺金属表面处理技术有限公司 | Low slag, inexpensive high speed drawing phosphating solution and use technique |
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- 2020-11-06 CN CN202011227467.1A patent/CN112410769A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109056034A (en) * | 2018-08-03 | 2018-12-21 | 南京派诺金属表面处理技术有限公司 | Room temperature electrolytic phosphating process and phosphating solution |
CN109468623A (en) * | 2018-12-29 | 2019-03-15 | 南京派诺金属表面处理技术有限公司 | Low slag, inexpensive high speed drawing phosphating solution and use technique |
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Application publication date: 20210226 |