CN114318317A - Inorganic passivation film forming solution for steel surface and preparation method and application thereof - Google Patents
Inorganic passivation film forming solution for steel surface and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to an inorganic passivation film-forming solution for steel surfaces, a preparation method and application thereof, wherein the inorganic passivation film-forming solution for steel surfaces comprises the following raw material components in percentage by mass: the weight percentage of the sodium metavanadate is 100%, the weight percentage of the sodium metavanadate is 2-5%, the weight percentage of the zirconium nitrate is 1-2%, the weight percentage of the sodium molybdate is 0.5-3%, the weight percentage of the sodium benzoate is 0.5-1%, and the balance is water. The sodium metavanadate and molybdate of the invention are dissolved in the metal on the surface of the steel in the anode area (M-2e ═ M)2+) The surface of the steel substrate can be oxidized by (M + V)5+/Mo6+＝M2++V4+/Mo5+) The steel substrate is partially passivated, active sites on the surface of steel are effectively covered, and the anti-corrosion performance is excellent.
Description
Technical Field
The invention relates to the technical field of steel surfaces, in particular to an inorganic passivation film-forming solution for a steel surface and a preparation method and application thereof.
Background
The preparation of a passivation film with anticorrosion capability on a metal surface is a metal anticorrosion technology with simple operation and low cost, but common passivation films, such as: hexavalent chromate passivation, while having good corrosion protection, is extremely hazardous and environmentally unfriendly and has been banned by various countries. Therefore, it is a matter of concern to find alternative chromate passivated products.
The steel material is a metal material which is widely applied and is extremely easy to corrode by corrosive media in the external environment. At present, the preparation of the conversion coating on the surface of steel is a good choice, but an organic solvent is needed, and the prepared conversion coating has relatively common corrosion resistance and is mainly used as an adhesive which can enhance the bonding force between metal and a coating. Therefore, the development of the inorganic passivation film forming technology which is simple to operate, green and environment-friendly and is applied to the steel material has very wide application prospect in the field of corrosion protection of the steel material.
Chinese patent document CN112301338A discloses a medium-low temperature fast-curing trivalent chromium passivation solution, which is characterized by comprising the following components in percentage by weight: 3-10% of a hydrolytic silane coupling agent; 3-10% of corrosion inhibitor; 0.5 to 5 percent of strong oxidizing acid; 15-30% of trivalent chromium salt solution; 0.5-5% of ligand complex; 0.1 to 1 percent of yttrium salt; 0.1 to 1 percent of fluoride; the balance being deionized water. The trivalent chromium passivation solution has the advantages of rapid and uniform film formation, and rapid drying at medium and low temperature, and meets the requirements of continuous and high-speed production in steel plants. The passivation solution provides excellent corrosion resistance and moisture and heat resistance.
Chinese patent document CN111455365A discloses an environment-friendly trivalent chromium cobalt-free color passivation solution for a zinc layer and a process thereof, and mainly relates to the technical field of metal surface treatment and protection. The passivation solution comprises the following raw materials in proportion: 50-500g/L of trivalent chromium salt; 0.1-100g/L of auxiliary film-forming agent; 10-200g/L of complexing agent; 10-150g/L of oxidant; pH regulator 10-100 g/L; the solvent is water. The invention has the advantages of no cobalt, low nitrate and iron impurity resistance, and has good corrosion resistance, bright and bright passivation film and simple passivation process operation.
The passivating agents are all passivated by using trivalent chromium, the harm of hexavalent chromium can be reduced to a certain degree, but the passivating agents still have a problem in waste liquid treatment, and the chromium-free passivation developed has a good application prospect in the future steel surface corrosion prevention.
Disclosure of Invention
In order to solve the technical problems, the invention provides an inorganic passivation film-forming solution for steel surfaces and a preparation method and application thereof.
The invention aims to provide an inorganic passivation film-forming solution for a steel surface, which comprises the following raw material components in percentage by mass:
the weight percentage of the sodium metavanadate is 100%, the weight percentage of the sodium metavanadate is 2-5%, the weight percentage of the zirconium nitrate is 1-2%, the weight percentage of the sodium molybdate is 0.5-3%, the weight percentage of the sodium benzoate is 0.5-1%, and the balance is water.
Further, the inorganic passivation film-forming solution for the steel surface comprises the following raw material components in percentage by mass:
the weight percentage of the sodium metavanadate is 100%, the weight percentage of the sodium metavanadate is 3-5%, the weight percentage of the zirconium nitrate is 1-1.5%, the weight percentage of the sodium molybdate is 0.5-1.5%, the weight percentage of the sodium benzoate is 0.5-1%, and the balance is water.
Further, the inorganic passivation film-forming solution for the steel surface comprises the following raw material components in percentage by mass:
by mass percent of 100%, 3% of sodium metavanadate, 1% of zirconium nitrate, 0.5% of sodium molybdate, 0.5% of sodium benzoate and the balance of water.
Further, the inorganic passivation film-forming solution for the steel surface comprises the following raw material components in percentage by mass:
the weight percentage of the sodium metavanadate is 100%, the zirconium nitrate is 1.5%, the sodium molybdate is 1%, the sodium benzoate is 1%, and the balance is water.
Further, the inorganic passivation film-forming solution for the steel surface comprises the following raw material components in percentage by mass:
by mass percentage of 100%, sodium metavanadate 4%, zirconium nitrate 1.0%, sodium molybdate 1.5%, sodium benzoate 1%, and the balance of water.
Further, the pH value of the inorganic passivation film-forming solution on the surface of the steel is 3.5-5.0; preferably, the pH of the inorganic passivation film-forming solution is 4.5-5.0. The film cannot be formed or is a light yellow film when the pH is lower than 3.5, the pH is higher than 5, the self-assembly liquid is suspended by a trace amount of white floccules, and the film layer is slightly purple yellow.
The second purpose of the invention is to provide a preparation method of the inorganic passivation film-forming solution for the surface of the steel, which comprises the following steps of adding zirconium nitrate into water according to the proportion to dissolve, then adding sodium molybdate and sodium benzoate, stirring, dissolving, standing, then adding sodium metavanadate, and stirring until the sodium metavanadate is completely dissolved to obtain the inorganic passivation film-forming solution for the surface of the steel.
Further, the standing time is 20-30 min.
The third purpose of the invention is to apply the inorganic passivation film-forming solution on the surface of steel in the treatment of the surface of steel, which comprises the following steps,
(1) degreasing the surface of a steel workpiece to be treated, and washing the surface of the steel workpiece with water after oil stains on the surface of the steel are removed;
(2) soaking the steel workpiece treated in the step (1) in the inorganic passivation film-forming solution;
(3) and (3) washing the steel surface treated in the step (2) with water, washing with ethanol, and airing or drying in a natural environment to obtain an anticorrosive purple yellow or light blue inorganic passivation film layer on the steel surface.
Further, the soaking time is 5-8 min; preferably, the soaking time is 7 min. When the soaking time is less than 5min, the color of the film layer is lighter and uneven, and when the soaking time is more than 8min, the surface of the steel can generate a small degree of corrosion in the airing process.
The principle of the invention is as follows:
the sodium metavanadate adopted in the invention can cooperate with the zirconium salt to form a film on the surface of the steel in an in-situ self-assembly manner under a proper condition.
Sodium metavanadate and molybdate as oxidation type corrosion inhibitor can dissolve metal on the surface of steel in anode area under mild condition (M-2e ═ M)2+) The surface of the steel substrate can be oxidized by (M + V)5+/Mo6+＝M2++V4+/Mo5+). The steel substrate is partially passivated, so that the coverage of active sites on the surface of steel can be enhanced, pitting corrosion can be effectively inhibited, and the corrosion resistance of the self-assembled film can be enhanced.
Zirconium nitrate may be in the cathode region (H) during etching++2e-＝H2) The zirconium dioxide nanoparticles converted in the process of increasing the pH value are deposited on the surface of the steel, so that the coverage of inorganic matters on the surface of the steel can be further enhanced, the whole passivation film layer is thickened, and the corrosion resistance is improved.
Sodium benzoate is a food preservative having excellent effect under acidic conditions, and can inhibit the growth of bacteria. Therefore, the storage period of the film forming liquid can be effectively prolonged by adding a proper amount of sodium benzoate into the film forming liquid, and the applicability of the film forming liquid is improved.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) the inorganic passivation film-forming solution sodium metavanadate and zirconium salt can form a passivation film on the surface of a cold-rolled steel plate in a chemical adsorption mode, effectively cover active sites on the surface of steel and has excellent corrosion resistance. Compared with the traditional passivation film forming technology, the method avoids the use of chromium salt and has excellent anticorrosion capability.
(2) The inorganic passivation film-forming solution has simple operation and low price, and forms a better corrosion-resistant film layer on the surface of steel.
Detailed Description
The present invention is further described below in conjunction with specific examples to enable those skilled in the art to better understand the present invention and to practice it, but the examples are not intended to limit the present invention.
The raw materials described in the examples are all conventional raw materials and are commercially available products.
Example 1
An inorganic passivation film-forming solution for a steel surface comprises the following raw materials in percentage by mass:
by mass percent of 100%, 3% of sodium metavanadate, 1% of zirconium nitrate, 0.5% of sodium molybdate, 0.5% of sodium benzoate and the balance of water, wherein the pH value is 4.0.
Treating the surface of steel by using the inorganic passivation film-forming solution for the surface of steel, and comprises the following steps:
(1) washing the surface of steel with water, pre-degreasing with acetone, degreasing with a commercial degreasing agent, and washing with ultrapure water;
(2) placing the steel plate treated in the step (1) in a water phase at normal temperature for self-assembly for 7 minutes;
(3) and (3) washing the steel surface treated in the step (2) with ultrapure water, washing with ethanol, and naturally drying to finish the inorganic passivation process.
Example 2
An inorganic passivation film-forming solution for a steel surface comprises the following raw materials in percentage by mass:
by mass percent of 100%, sodium metavanadate 4%, zirconium nitrate 1.5%, sodium molybdate 1%, sodium benzoate 1%, and the balance of water, and the pH value is 4.5.
Treating the surface of steel by using the inorganic passivation film-forming solution for the surface of steel, and comprises the following steps:
(1) washing the surface of steel with water, pre-degreasing with acetone, degreasing with a commercial degreasing agent, and washing with ultrapure water;
(2) placing the steel plate treated in the step (1) in a water phase at normal temperature for self-assembly for 7 minutes;
(3) and (3) washing the steel surface treated in the step (2) with ultrapure water, washing with ethanol, and naturally drying to finish the inorganic passivation process.
Example 3
An inorganic passivation film-forming solution for a steel surface comprises the following raw materials in percentage by mass:
by mass percent of 100%, sodium metavanadate 4%, zirconium nitrate 1.0%, sodium molybdate 1.5%, sodium benzoate 1%, and the balance of water, and the pH value is 4.8.
Treating the surface of steel by using the inorganic passivation film-forming solution for the surface of steel, and comprises the following steps:
(1) washing the surface of steel with water, pre-degreasing with acetone, degreasing with a commercial degreasing agent, and washing with ultrapure water;
(2) placing the steel plate treated in the step (1) in a water phase at normal temperature for self-assembly for 7 minutes;
(3) and (3) washing the steel surface treated in the step (2) with ultrapure water, washing with ethanol, and naturally drying to finish the inorganic passivation process.
Example 4
An inorganic passivation film-forming solution for a steel surface comprises the following raw materials in percentage by mass:
by mass percent of 100%, sodium metavanadate 5%, zirconium nitrate 1.0%, sodium molybdate 2.0%, sodium benzoate 1%, and the balance of water, and the pH value is 5.0.
Treating the surface of steel by using the inorganic passivation film-forming solution for the surface of steel, and comprises the following steps:
(1) washing the surface of steel with water, pre-degreasing with acetone, degreasing with a commercial degreasing agent, and washing with ultrapure water;
(2) placing the steel plate treated in the step (1) in a water phase at normal temperature for self-assembly for 7 minutes;
(3) and (3) washing the steel surface treated in the step (2) with ultrapure water, washing with ethanol, and naturally drying to finish the inorganic passivation process.
Comparative example 1
An inorganic passivation film-forming solution for a steel surface comprises the following raw materials in percentage by mass:
by mass percent of 100%, zirconium nitrate 1%, sodium molybdate 0.5%, sodium benzoate 0.5%, and the balance of water, and the pH value is 4.0.
The steel surface was treated in the same manner as in example 1.
Comparative example 2
An inorganic passivation film-forming solution for a steel surface comprises the following raw materials in percentage by mass:
by mass percent of 100%, sodium metavanadate 3%, sodium molybdate 0.5%, sodium benzoate 0.5%, and the balance of water, and the pH value is 4.0.
The steel surface was treated in the same manner as in example 1.
Comparative example 3
An inorganic passivation film-forming solution for a steel surface comprises the following raw materials in percentage by mass:
by mass percent of 100%, sodium metavanadate 10%, zirconium nitrate 1%, sodium molybdate 0.5%, sodium benzoate 0.5%, and the balance of water, and the pH value is 4.0.
The steel surface was treated in the same manner as in example 1.
Comparative example 4
An inorganic passivation film-forming solution for a steel surface comprises the following raw materials in percentage by mass:
by mass percent of 100%, sodium metavanadate is 0.5%, zirconium nitrate is 1%, sodium molybdate is 0.5%, sodium benzoate is 0.5%, the balance is water, and the pH value is 4.0.
The steel surface was treated in the same manner as in example 1.
Test example
The steel surfaces after surface treatment in examples 1 to 4 and comparative examples 1 to 4 were subjected to performance tests, and the test items and results were as follows:
(a) appearance: in the examples 1 to 4, a uniform light purple chemical conversion coating is formed on the surface of the steel after the surface treatment. Comparative example 1, no apparent change in surface; comparative example 2, the surface was yellowish and had a little corrosion rust; comparative example 3, the surface was light yellow with little corrosion rust; in comparative example 4, the surface was blue-yellow and had little corrosion rust.
(b) And (3) electrochemical performance testing:
the polarization and impedance curves were tested for passivation film performance. The corrosion current icorr can be calculated on the polarization curve, and the decrease of the corrosion current is calculated to show that the corrosion of the passivation film is reduced. Similarly, the polarization resistance can be calculated by using the impedance diagram, and the corrosion inhibition rate can be obtained by calculating the change of the polarization resistance Rct.
(1) Polarization curve:
open circuit time: 1200s
Scanning voltage: open circuit potential 300mv
Scanning rate: 0.2mv/s
Sensitivity: 10-3
The corrosion inhibition efficiency IE (icorr-i)/icorr of the steel surface treated by the inorganic passivation solution is as follows:
example 1: 82.3% example 2: 83.1% example 3: 90.6% example 4: 83.7 percent
Comparative example 1: 60.1% comparative example 2: 71.3% comparative example 3: 68.2% comparative example 4: 64.1 percent
(2) Impedance curve:
open circuit time: 1200s
Scanning frequency: 106Hz-50mHz
The corrosion inhibition efficiency IE% of the steel surface treated by the inorganic passivation solution is (Rct '-Rct)/Rct':
example 1: 73.4% example 2: 75.2% example 3: 71.6% example 4: 76.6 percent
Comparative example 1: 42.9% comparative example 2: 49.3% comparative example 3: 41.6% comparative example 4: 43.3 percent
(c)3.5 wt% brine soak experiment:
the surface of the steel plate treated by the inorganic passivation solution is subjected to a 3.5 wt% brine soaking experiment:
example 1: no large amount of rust spots appeared within 1 hour
Example 2: no large amount of rust spots appeared within 1 hour
Example 3: no large amount of rust spots appeared within 1 hour
Example 4: no large amount of rust spots appeared within 1 hour
The saline soaking time reaches the national standard.
Comparative example 1: no large amount of rust spots appear within 15 minutes
Comparative example 2: no large amount of rust spots appear within 32 minutes
Comparative example 3: no large amount of rust spots appear within 25 minutes
Comparative example 4: no significant rust spots appeared within 20 minutes.
Comparing examples 1-4 with comparative examples 1-4, it can be seen that the corrosion inhibition rate of the examples is obviously better than that of the comparative examples, because the components of the examples can form a synergistic effect to form an inorganic passivation film on the surface of steel, and the corrosion resistance of the steel is greatly improved.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications can be made without departing from the scope of the invention.
Claims (10)
1. The inorganic passivation film-forming solution for the steel surface is characterized by comprising the following raw material components in percentage by mass:
the weight percentage of the sodium metavanadate is 100%, the weight percentage of the sodium metavanadate is 2-5%, the weight percentage of the zirconium nitrate is 1-2%, the weight percentage of the sodium molybdate is 0.5-3%, the weight percentage of the sodium benzoate is 0.5-1%, and the balance is water.
2. The inorganic passivation film-forming solution for the steel surface according to claim 1, characterized by comprising the following raw material components by mass percent:
the weight percentage of the sodium metavanadate is 100%, the weight percentage of the sodium metavanadate is 3-5%, the weight percentage of the zirconium nitrate is 1-1.5%, the weight percentage of the sodium molybdate is 0.5-1.5%, the weight percentage of the sodium benzoate is 0.5-1%, and the balance is water.
3. The inorganic passivation film-forming solution for the steel surface according to claim 1, characterized by comprising the following raw material components by mass percent:
by mass percent of 100%, 3% of sodium metavanadate, 1% of zirconium nitrate, 0.5% of sodium molybdate, 0.5% of sodium benzoate and the balance of water.
4. The process according to claim 1, wherein the raw materials comprise the following components in percentage by mass:
the weight percentage of the sodium metavanadate is 100%, the zirconium nitrate is 1.5%, the sodium molybdate is 1%, the sodium benzoate is 1%, and the balance is water.
5. The inorganic passivation film-forming solution for the steel surface according to claim 1, characterized by comprising the following raw material components by mass percent:
by mass percentage of 100%, sodium metavanadate 4%, zirconium nitrate 1.0%, sodium molybdate 1.5%, sodium benzoate 1%, and the balance of water.
6. The method of claim 1, wherein: the pH value of the inorganic passivation film-forming solution on the surface of the steel is 3.5-5.0.
7. The method for preparing the inorganic passivation film-forming solution for the steel surface according to any one of claims 1 to 6, wherein the method comprises the following steps: adding zirconium nitrate into water according to a ratio to dissolve, then adding sodium molybdate and sodium benzoate, stirring, dissolving and standing, then adding sodium metavanadate, and stirring until the sodium metavanadate is completely dissolved to obtain the inorganic passivation film-forming solution for the surface of the steel.
8. The method for preparing the inorganic passivation film-forming solution for the steel surface according to claim 7, which is characterized in that: the standing time is 20-30 min.
9. The use of the inorganic passivation deposition solution according to any one of claims 1 to 8 in the surface treatment of steel, characterized in that:
(1) degreasing the surface of a steel workpiece to be treated, and washing the surface of the steel workpiece with water after oil stains on the surface of the steel are removed;
(2) soaking the steel workpiece treated in the step (1) in the inorganic passivation film-forming solution;
(3) and (3) washing the steel surface treated in the step (2) with water and ethanol, and airing or drying to obtain an anticorrosive purple yellow or light blue inorganic passivation film layer on the steel surface.
10. The use of the inorganic passivation deposition solution according to claim 9 in steel surface treatment, characterized in that: the soaking time is 5-8 min.
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