CN114839030A - Cold pickling solution for identifying surface defects of high-nitrogen stainless steel and application thereof - Google Patents
Cold pickling solution for identifying surface defects of high-nitrogen stainless steel and application thereof Download PDFInfo
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Abstract
The invention relates to a cold pickling solution for identifying surface defects of high-nitrogen stainless steel and application thereof, belonging to the technical field of alloy surface defect identification. The cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel consists of the following components in percentage by mass: HCl 2.1-4.3%, H 3 PO 4 19.5～25.5％，FeCl 3 8-17% and the balance of water. The formula of the cold pickling solution can rapidly corrode the surface of the high-nitrogen stainless steel, the corrosion time only needs 1-2 min, the pickling amount after corrosion is below 2 mu m, the surface quality of a part cannot be excessively damaged, the identification accuracy rate of the grinding burn defect of the surface of the high-nitrogen stainless steel bearing can reach 100%, in addition, the long-term stable storage of the cold pickling solution can be ensured, and the effective service life is more than three months.
Description
Technical Field
The invention belongs to the technical field of alloy surface defect identification, and particularly relates to cold pickling solution for identifying high-nitrogen stainless steel surface defects and application thereof.
Background
The grinding burn is that the local metallographic structure of the surface layer of the part is changed due to the instantaneous high temperature during grinding, so that the part has the defects of reduced hardness, fine cracks and the like, and the quality of the part is seriously damaged. In order to identify whether the surface of the part has the defect of grinding burn, the chemical cold pickling technology is a simple, visual, high-accuracy and low-cost method. The chemical cold pickling is to corrode the surface of the part by acid, and because different metallographic structures have different sensitivities to the acid corrosion, the color difference presented by the surface corrosion of different degrees is utilized to judge the defect of grinding burn.
The high-nitrogen stainless steel bearing has high strength, good wear resistance and stronger corrosion resistance, is more and more widely applied in the industries of aerospace, precision machine tools, automobile manufacturing, wind power generation and the like, and can play an important role particularly in specific environments such as oceans and the like. But at the same time, the stronger corrosion resistance of the high-nitrogen stainless steel causes difficulty to the inspection procedure of the grinding burn defect on the surface of the bearing part.
The cold pickling operation specification of appendix C of technical conditions JB/T1460-2011 for heat treatment of high-carbon chromium stainless steel bearing parts of rolling bearings is adopted to carry out cold pickling on the high-nitrogen stainless steel bearing parts, and the results show that the parts have strong corrosion resistance on the cold pickling solution, the surface color has no change for a long time, and the defect of surface grinding burn cannot be effectively identified, so that the surface quality of the product has hidden danger, and the performance and the service life of the bearing are influenced.
In the prior art, for detecting the processing defects of high-nitrogen corrosion-resistant bearing parts, 25-30% of nitric acid, 10-15% of hydrochloric acid, 2-4% of ferric trichloride and 51-63% of water are compounded to be used as a pickling solution. Although the pickling solution with the formula can be used for detecting the surface defects of the high-nitrogen corrosion-resistant steel, the effective use frequency of the pickling solution is extremely low in practical application, a large amount of pickling solution needs to be prepared continuously when batch detection is carried out, and the cost is high.
Disclosure of Invention
The invention aims to provide a cold pickling solution for identifying surface defects of high-nitrogen stainless steel, which has the advantage of long service cycle.
Another object of the present invention is to provide a use of a cold pickling solution for identifying surface defects of high nitrogen stainless steel.
The technical scheme adopted by the cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel is as follows:
the cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel comprises the following components in percentage by mass: HCl 2.1-4.3%, H 3 PO 4 19.5～25.5％，FeCl 3 8-17% and the balance of water.
The cold pickling solution disclosed by the invention adopts 2.1-4.3% of hydrochloric acid by mass, so that the corrosion resistance of the high-nitrogen stainless steel can be resisted, the corrosion of the steel surface can reach an expected effect, and the corrosion time is short. Phosphoric acid with the mass fraction of 19.5-25.5% is adopted, and the passivation effect can be exerted, so that a passivation film is formed on the surface of the steel part to protect the part, and excessive corrosion in acid washing or a subsequent procedure is avoided. The acidity of the phosphoric acid is relatively weak, the phosphoric acid and the hydrochloric acid are mixed to generate a synergistic effect, the complete ionization of the phosphoric acid and the hydrochloric acid is promoted, hydrogen ions in the solution are increased, the phosphoric acid and the hydrochloric acid are more fully combined with chloride ions decomposed by ferric trichloride in the solution, the corrosivity is enhanced, the phosphoric acid is not easy to volatilize, the mass concentration change is small, and the effect of prolonging the effective service life of the pickling solution is achieved. In addition, the characteristic that the phosphoric acid is not easy to volatilize is utilized, so that the harm to the environment and the human body can be reduced. The ferric trichloride with the mass fraction of 8-17% is adopted to have a strong oxidation effect in the cold pickling solution, and the ferric trichloride and hydrogen ions separated from the solution generate hydrochloric acid to promote the corrosion effect of the cold pickling solution on the steel surface, so that the corrosion speed is further increased, and the pickling efficiency is accelerated.
Through the matching of the components, the cold pickling solution provided by the invention can quickly corrode the surface of the high-nitrogen stainless steel, the corrosion time is only 1-2 min, and the detection efficiency of surface defects is improved; after corrosion, the pickling amount meets the related requirements below 2 mu m, the surface quality such as the surface roughness of parts and the like is not excessively damaged, and the identification accuracy of the grinding burn defects on the surface of the high-nitrogen stainless steel bearing reaches 100 percent; in addition, the cold pickling solution can be stably stored for a long time, the effective service life is more than three months, the excellent corrosion effect can be maintained, the effective service life is long, and the frequency of effective cold pickling is more than 5 times that of the conventional formula of the cold pickling solution.
Further, the cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel comprises the following components in percentage by mass: HCl 3.6-4.3%, H 3 PO 4 22.9～25.5％，FeCl 3 8-12% of water, and the balance of water. The formula of the cold pickling solution has the advantages of ensuring the corrosion effect on the high-nitrogen stainless steel, along with higher corrosion speed, improving the pickling efficiency, long service cycle and being beneficial to saving the pickling process cost.
Further, the cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel comprises the following components in percentage by mass: HCl 4.3%, H 3 PO 4 25.5％，FeCl 3 8 percent and the balance of water. The cold pickling solution with the formula has high corrosion speed on high-nitrogen stainless steel parts and low pickling amount, can better protect the surface of the high-nitrogen stainless steel, and avoids excessive corrosion of the high-nitrogen stainless steel.
The cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel can be prepared by adopting a method comprising the following steps of: at normal temperature, taking hydrochloric acid, phosphoric acid, ferric trichloride and water, sequentially pouring the hydrochloric acid and the phosphoric acid into the water, and adding the ferric trichloride to completely dissolve after uniformly dissolving to obtain the compound.
The technical scheme adopted by the application of the cold pickling solution in identifying the surface defects of the high-nitrogen stainless steel is as follows:
the application of the cold pickling solution in identifying the surface defects of the high-nitrogen stainless steel.
The application of the cold pickling solution in identifying the surface defects of the high-nitrogen stainless steel improves the corrosion efficiency of the high-nitrogen stainless steel, is simple and convenient to operate, is intuitive to observe and distinguish, has high accuracy, does not cause excessive damage to the surface quality of parts, and better solves the problem of identifying the surface grinding burn defects of the high-nitrogen stainless steel.
Further, the application of the cold pickling solution provided by the invention in identifying the surface defects of the high-nitrogen stainless steel comprises the following steps: immersing the degreased and cleaned high-nitrogen stainless steel part in cold pickling solution, moving the part up and down for 1-2 min until the surface of the part is gray and has no obvious metallic luster, and then performing brightening and neutralizing treatment.
Further, the cold pickling solution provided by the invention is applied to identifying the surface defects of the high-nitrogen stainless steel, and parts are moved up and down at intervals of 20 seconds for about 5 seconds at a speed of 2-3 times/second.
It can be understood that the application of the cold pickling solution provided by the invention in identifying the surface defects of the high-nitrogen stainless steel, the degreasing and cleaning steps adopted before pickling, and the brightening and neutralizing treatment steps adopted after pickling can adopt conventional treatment methods in the prior art, such as a method specified in appendix C of technical conditions JB/T1460-2011 for heat treatment of rolling bearing high-carbon chromium stainless steel bearing parts.
Drawings
FIG. 1 is a surface topography map of a high nitrogen stainless steel part of example 5 before and after cold pickling;
FIG. 2 is a surface topography of a high nitrogen stainless steel part identified after cold pickling in example 3 as having a grinding burn defect.
Detailed Description
The following provides a supplementary explanation of the technical effects of the present invention with reference to specific embodiments.
The raw materials in the following examples and comparative examples are all conventional commercial products, wherein the concentration of hydrochloric acid is 35.5%, and the concentration of phosphoric acid is 85%; the material of the high-nitrogen stainless steel part is X30 CrMoVN-15.
Example 1
The cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel comprises the following components in percentage by mass: HCl 2.1%, H 3 PO 4 19.5％，FeCl 3 17 percent and the balance of water.
Example 2
The cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel comprises the following components in percentage by mass: HCl 4.3%, H 3 PO 4 25.5％，FeCl 3 8 percent and the balance of water.
Example 3
The cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel comprises the following components in percentage by mass: HCl 3.6%, H 3 PO 4 22.9％，FeCl 3 12 percent and the balance of water.
Example 4
The cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel comprises the following components in percentage by mass: HCl 2.9%, H 3 PO 4 21.2％，FeCl 3 14 percent and the balance of water.
The cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel in the above embodiments 1 to 4 is prepared by a method including the following steps: at normal temperature, hydrochloric acid, phosphoric acid, ferric trichloride and water are taken, the hydrochloric acid and the phosphoric acid are poured into the water in sequence, after the hydrochloric acid and the phosphoric acid are dissolved uniformly, the ferric trichloride is added and mechanically stirred until the hydrochloric acid and the phosphoric acid are completely dissolved, and the mixture is uniformly mixed, so that the cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel is obtained.
Example 5
The application of the cold pickling solution in the embodiment in identifying the surface defects of the high-nitrogen stainless steel adopts the cold pickling solution in any one of embodiments 1 to 4, and comprises the following steps:
1) degreasing the high-nitrogen stainless steel part in degreasing liquid at the temperature of 75-85 ℃ for more than 2min, cleaning the high-nitrogen stainless steel part in hot water at the temperature of 75-85 ℃ for 1min after degreasing is completed, and then cleaning the high-nitrogen stainless steel part in a flowing cold water tank for 1 min;
2) immersing the high-nitrogen stainless steel part cleaned by flowing cold water in the step 1) in cold pickling solution at room temperature, moving the part up and down at the speed of 2-3 times/second at intervals of 20 seconds for about 5 seconds, wherein the pickling time is not more than 2min until the surface of the part is gray and has no obvious metallic luster, and then cleaning the part in a flowing cold water tank for 1 min;
3) placing the parts cleaned by the flowing cold water in the step 2) into a 1 st brightening tank, brightening the parts at room temperature for 1-2 min, and cleaning the parts for 1-2 min by the flowing cold water; then putting the mixture into a 2 nd brightening tank, brightening the mixture for 30 to 90 seconds at room temperature, washing the mixture for 1 to 2 minutes by flowing cold water, and then neutralizing the mixture for 1 minute at room temperature.
Note: a) the bearing parts are moved in a degreasing, cleaning, brightening and neutralizing tank solution in a vertically oscillating mode, and the oscillating speed is 60-70 times/min;
b) the washing of the flowing cold water tank of the bearing part ensures that the solution in the upper tank is washed clean so as to avoid polluting the solution in the lower tank.
The cold pickling solution of the embodiment is applied to identifying the surface defects of the high-nitrogen stainless steel, and the surface topography of the high-nitrogen stainless steel part before and after cold pickling is shown in fig. 1.
Comparative example 1
The cold pickling solution of the comparative example consists of the following components in percentage by weight: nitric acid (HNO) 3 ) 27.5%, hydrochloric acid (HCl) 12.5%, ferric chloride (FeCl) 3 ) 3% and 57% of water.
Comparative example 2
The cold pickling solution of the comparative example is prepared by mixing the following raw materials in parts by weight according to a formula of a pickling solution specified in C.1.1.4 in appendix C of technical conditions JB/T1460-2011 for heat treatment of high-carbon chromium stainless steel bearing parts of rolling bearings: nitric acid (HNO) 3 )25.1 parts of phosphoric acid (H) 3 PO 4 )7.6 parts of ferric chloride (FeCl) 3 ·6H 2 O)4.5 parts and water 62.8 parts.
Comparative example 3
The cold pickling liquid of this comparative example differs from the cold pickling liquid of example 3 only in that: in this comparative example, the use of HCl was omitted and 2 times the mass fraction of H was used 3 PO 4 。
Comparative example 4
The cold pickling liquid of this comparative example differs from the cold pickling liquid of example 3 only in that: in this comparative example, H is omitted 3 PO 4 2 times the mass fraction of HCl was used.
Comparative example 5
The cold pickling liquid of this comparative example differs from the cold pickling liquid of example 1 only in that: this comparative example omits the use of HCl and employs FeCl at 2 times the mass fraction 3 。
Comparative example 6
Cold pickling solution of this comparative example, and Cold pickling solution of example 1The liquids differ only in that: this comparative example omits FeCl 3 2 times the mass fraction of HCl was used.
Experimental example 1
Respectively taking the cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel in the embodiments 1-4 and the cold pickling solution in the comparative examples 1-6 with the same total weight, and carrying out cold pickling on the high-nitrogen stainless steel part after grinding, wherein the cold pickling method comprises the following steps:
1) degreasing the high-nitrogen stainless steel part in degreasing liquid at the temperature of 75-85 ℃ for more than 2min, cleaning the high-nitrogen stainless steel part in hot water at the temperature of 75-85 ℃ for 1min after degreasing is completed, and then cleaning the high-nitrogen stainless steel part in a flowing cold water tank for 1 min;
2) immersing the high-nitrogen stainless steel part cleaned by flowing cold water in the step 1) in cold pickling solution at room temperature, moving the part up and down at the speed of 2-3 times/second at intervals of 20 seconds for about 5 seconds, wherein the pickling time is not more than 2min until the surface of the part is gray and has no obvious metallic luster, recording the cold pickling time as shown in the following table 1, and then cleaning the part in a flowing cold water tank for 1 min;
3) placing the parts cleaned by the flowing cold water in the step 2) into a 1 st brightening tank, brightening the parts at room temperature for 1-2 min, and cleaning the parts for 1-2 min by the flowing cold water; then putting the mixture into a 2 nd brightening tank, brightening the mixture for 30 to 90 seconds at room temperature, washing the mixture for 1 to 2 minutes by flowing cold water, and then neutralizing the mixture for 1 minute at room temperature.
Note: a) the bearing parts are moved in a degreasing, cleaning, brightening and neutralizing tank solution in a vertically oscillating mode, and the oscillating speed is 60-70 times/min;
b) the washing of the flowing cold water tank of the bearing part ensures that the solution in the upper tank is washed clean so as to avoid polluting the solution in the lower tank.
After passing the above treatment, the acid pickling amount was measured, and the results are shown in the following table 1:
TABLE 1 results of acid etching time and acid etching amount for examples and comparative examples of the present application
| Cold pickling time/min | Pickling amount/. mu.m | |
| Example 1 | 2 | 1.8 |
| Example 2 | 1.7 | 1.5 |
| Example 3 | 1.7 | 1.8 |
| Example 4 | 2 | 2 |
| Comparative example 1 | 2 | 2 |
| Comparative example 2 | No obvious change in 30min | \ |
| Comparative example 3 | No obvious change in 30min | \ |
| Comparative example 4 | 5 | 8 |
| Comparative example 5 | No obvious change in 30min | \ |
| Comparative example 6 | No obvious change in 30min | \ |
As shown in table 1, the cold pickling solution for identifying surface defects of high-nitrogen stainless steel in embodiments 1 to 4 of the present application can rapidly corrode the surface of a high-nitrogen stainless steel part, the pickling time is 1.7 to 2min, and the pickling amount of the part surface is 1.5 to 2 μm, so that the surface quality of the part can be effectively protected from excessive damage, the pickling amount is ensured to be less than 2 μm to 4 μm, and the cold pickling solution meets the "JB 1460-2011" of the industrial standard.
And the comparative example 2 adopting the formula of the cold pickling solution of JB/T1460-2011 cannot generate corrosion effect on the high-nitrogen stainless steel parts. After the part is subjected to cold pickling for 30min, the surface of the part is not obviously changed. Similarly, comparative examples 3, 5 and 6 show no significant change for 30min when the high nitrogen stainless steel parts are cold pickled. The excellent corrosion resistance of the high-nitrogen stainless steel part can be seen, so that the conventional cold pickling solution cannot effectively corrode the high-nitrogen stainless steel part and cannot detect surface defects. And in the comparative example 4, although the high-nitrogen stainless steel part can be corroded, the pickling process can be completed within 5min, and the pickling amount is up to 8 mu m, so that the part surface is greatly damaged and does not meet the industrial standard.
The comparison of the results of the example 1 and the comparative examples 5 and 6 shows that no ferric trichloride participates, no reaction occurs on the surface of the high-nitrogen stainless steel part in the mixed solution of hydrochloric acid or hydrochloric acid and phosphoric acid, and the iron trichloride in the formula of the cold pickling solution has an excellent promotion effect on the corrosion effect and the phosphoric acid has a protection effect on the high-nitrogen stainless steel part; comparing the results of example 3 with those of comparative examples 3 and 4, it can be seen that the combination of phosphoric acid and hydrochloric acid according to the present invention produces a synergistic effect that enhances the corrosiveness of the cold pickling solution formulation.
Experimental example 2
The high-nitrogen stainless steel parts after grinding are subjected to cold pickling in example 3, 8 parts are subjected to cold pickling, surface burn is found in 1 part, and the surface appearance after cold pickling is shown in figure 2. After acid washing, the inner diameter surface of the high-nitrogen stainless steel part with surface burn has clear and obvious dark columnar marks, which shows that the surface of the high-nitrogen stainless steel part has columnar grinding burn defects, and the cold acid washing solution formula in the embodiment 3 can be used for easily identifying the surface burn and wear defects of the high-nitrogen stainless steel part.
The hardness values of the burnt part and the normal part on the surface of the part are tested by a DM-8 type micro Vickers hardness tester, and the test results are shown in a table 2.
TABLE 2 grinding hardness values of burned and normal part surfaces
As can be seen from table 2, when the high nitrogen stainless steel bearing part had a defect of grinding burn, the burned part had a problem of low hardness. The cold pickling solution disclosed by the invention is used for identifying and picking out the defective parts, so that the product quality is favorably ensured, and the risk caused by the quality defects of the parts is avoided.
Experimental example 3
The cold pickling solution of the embodiment 1-4 is adopted to identify defective parts, 1 high-nitrogen stainless steel bearing part with the grinding burn defect on the surface is selected, the hardness of the part is tested, and the test result shows that the identification is accurate.
Experimental example 4
50mL of each of the formulated solutions of example 3 and comparative example 1 were used to simultaneously perform a parallel pickling experiment, each time pickling a high nitrogen steel bearing part, comparing the effective use frequency of the two pickups, and the results are shown in Table 3 below.
Table 3 effective use period/frequency comparison of example 3 and comparative example 1
As can be seen from table 3, through the parallel pickling test, the cold pickling frequency of the cold pickling solution formulation in example 3 capable of maintaining excellent corrosion effect can reach 66-70 times, compared to that, in comparative example 1, the corrosion effect cannot be generated only through 11-13 times of cold pickling tests, and the pickling effect is lost. The formula of the cold pickling solution has the advantage of long service cycle, can clean more high-nitrogen stainless steel parts, is beneficial to reducing the solution preparation process, and saves the raw materials and time cost.
Claims (4)
1. The cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel is characterized by comprising the following components in percentage by mass: HCl 2.1-4.3%, H 3 PO 4 19.5～25.5％，FeCl 3 8-17% and the balance of water.
2. The cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel as claimed in claim 1, wherein the cold pickling solution consists of the following components in percentage by mass: HCl 3.6-4.3%, H 3 PO 4 22.9～25.5％，FeCl 3 8-12% of water, and the balance of water.
3. The cold pickling solution for identifying the surface defects of the high-nitrogen stainless steel according to claim 1 or 2, wherein the cold pickling solution consists of the following components in percentage by mass: HCl 4.3%, H 3 PO 4 25.5％，FeCl 3 8 percent and the balance of water.
4. Use of a cold pickling solution according to any one of claims 1 to 3 for identifying surface defects of high nitrogen stainless steel.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1690249A (en) * | 2004-04-30 | 2005-11-02 | 洛阳轴承集团有限公司 | Acid pickle for detecting processing deficiency of bearing parts made of carbonized steel |
| CN105241889A (en) * | 2015-11-13 | 2016-01-13 | 中航工业哈尔滨轴承有限公司 | Acid pickling method for inspecting surface grinding burns of bearing steel bearing part |
| CN106124426A (en) * | 2016-08-03 | 2016-11-16 | 中国人民解放军第五七九工厂 | A kind of pickling test method of grinding burn |
| CN108844962A (en) * | 2018-08-22 | 2018-11-20 | 洛阳Lyc轴承有限公司 | A method of for detecting the anti-corrosion steel bearing parts manufacturing deficiency of high nitrogen |
-
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- 2022-03-21 CN CN202210281400.9A patent/CN114839030B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1690249A (en) * | 2004-04-30 | 2005-11-02 | 洛阳轴承集团有限公司 | Acid pickle for detecting processing deficiency of bearing parts made of carbonized steel |
| CN105241889A (en) * | 2015-11-13 | 2016-01-13 | 中航工业哈尔滨轴承有限公司 | Acid pickling method for inspecting surface grinding burns of bearing steel bearing part |
| CN106124426A (en) * | 2016-08-03 | 2016-11-16 | 中国人民解放军第五七九工厂 | A kind of pickling test method of grinding burn |
| CN108844962A (en) * | 2018-08-22 | 2018-11-20 | 洛阳Lyc轴承有限公司 | A method of for detecting the anti-corrosion steel bearing parts manufacturing deficiency of high nitrogen |
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