CN112301385A - Method for improving corrosion resistance of chromium layer deposited on H13 steel surface - Google Patents
Method for improving corrosion resistance of chromium layer deposited on H13 steel surface Download PDFInfo
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- CN112301385A CN112301385A CN201910713797.2A CN201910713797A CN112301385A CN 112301385 A CN112301385 A CN 112301385A CN 201910713797 A CN201910713797 A CN 201910713797A CN 112301385 A CN112301385 A CN 112301385A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/04—Electroplating: Baths therefor from solutions of chromium
- C25D3/08—Deposition of black chromium, e.g. hexavalent chromium, CrVI
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/12—Oxidising using elemental oxygen or ozone
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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Abstract
The invention discloses a method for improving corrosion resistance of a chromium layer deposited on the surface of H13 steel, which comprises the steps of taking an H13 steel sample and a lead-antimony alloy containing 7 wt.% of antimony as an electroplating cathode and an electroplating anode, and electroplating at a current density of 10-90A/dm2The temperature of the plating solution is 25-65 ℃, the electroplating time is 15-120 min, the content of chromic anhydride in the chromium plating solution is 100-400 g/L, the content of strontium sulfate is 1-9 g/L, and the content of potassium fluosilicate is 1-25 g/L; after electroplating, the obtained Cr coating sample is annealed in an annealing furnace to remove hydrogen and generate compact Cr on the surface of the Cr coating2O3Protecting the layer to improve its corrosion resistance.
Description
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to a method for improving corrosion resistance of a chromium layer deposited on the surface of H13 steel.
Background
H13 steel is used for manufacturing dies such as rolls and mandrels because of its high strength, toughness, wear resistance, and the like. These dies are prone to severe wear, corrosion and other damages during service, and the surfaces thereof are required to have high hardness, wear resistance, corrosion resistance and the like. A method of electrodepositing a metal or alloy layer having high hardness, wear resistance, and corrosion resistance on the surface thereof has received much attention from researchers. The Cr plating layer has beautiful surface, higher hardness, excellent wear resistance, heat resistance and corrosion resistance, and is widely applied to the fields of mold manufacturing, automobiles, aviation, navigation and the like. In the hexavalent chromium electroplating process, the side reaction on the surface of the cathode is serious, so that the cathode current efficiency is extremely low. One part of hydrogen generated by the side reaction escapes from the surface of the coating in the form of hydrogen, and the other part of hydrogen permeates into the substrate and the coating in the form of hydrogen atoms, so that the internal stress of the substrate and the coating is improved, the brittleness of the coating is increased, and the service life of the coating is greatly shortened. In addition, excessive internal stress causes cracking of the surface of the Cr plating layer, forming a microcrack structure. The micro cracks have the function of storing lubricating media in the service process of the dies such as the chromium-plated core rod or the roller and the like, and the wear resistance of the plating layer is enhanced. However, these microcracks also lead to the penetration of corrosive agents such as water molecules, oxygen, halide ions, salts, and the like, reducing the corrosion resistance of the coating. Therefore, it is necessary to adopt a method of protecting the plating layer to improve the corrosion resistance of the plating layer.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for improving the corrosion resistance of a chromium layer deposited on the surface of H13 steel by utilizing heat treatment, so as to achieve the aim of removing hydrogen and generate compact Cr on the surface of a Cr coating2O3Protecting the layer to improve its corrosion resistance.
The technical purpose of the invention is realized by the following technical scheme.
A method for improving the corrosion resistance of a chromium layer deposited on the surface of H13 steel comprises the following steps:
step 1, carrying out deposition preparation of chromium plating on the surface of H13 steel
With H13Steel is used as a cathode, lead-antimony alloy containing 7 wt% (mass percentage) of antimony is used as an electroplating anode, the electroplating anode is immersed in prepared chromium plating solution, and the electroplating solution is electrified to carry out deposition preparation of a chromium plating layer; the chromium plating solution consists of chromic anhydride, strontium sulfate, potassium fluosilicate and water, wherein the solvent is water, the content of chromic anhydride is 100-400 g/L, the content of strontium sulfate is 1-10 g/L, and the content of potassium fluosilicate is 1-25 g/L; the current density is 10-90A/dm2The temperature of the plating solution is 25-65 ℃, and the electroplating time is 15-120 min;
in step 1, the lead-antimony alloy is a clean lead-antimony alloy containing 7 wt% (mass percent) antimony.
In step 1, the area ratio of the cathode to the anode is 1:2, the distance between the cathode and the anode is 1-3 cm.
In the step 1, after the electroplating is finished, washing with tap water, then putting into absolute ethyl alcohol for ultrasonic oscillation, taking out, drying and weighing.
In step 1, the solvent in the chromium plating solution is deionized water.
In the step 1, in the chromium plating solution, the content of chromic anhydride is 200-300 g/L, the content of strontium sulfate is 4-8 g/L, and the content of potassium fluosilicate is 10-20 g/L.
In the step 1, electrifying to prepare the chromium coating by deposition, wherein the current density is 30-80A/dm2The temperature of the plating solution is 30-50 ℃, and the electroplating time is 50-100 min.
And 2, carrying out heat treatment on the H13 steel deposited with the chromium coating and prepared in the step 1, heating the steel from the room temperature of 20-25 ℃ to the annealing heat treatment temperature of 100-800 ℃ at the heating rate of 1-50 ℃/min in the air atmosphere, keeping the temperature for 0.5-8H, taking out the steel, and air-cooling the steel to the room temperature of 20-25 ℃.
In step 2, after air cooling, the surface is cleaned by absolute ethyl alcohol and dried for standby.
In step 2, an annealing furnace is selected for the annealing heat treatment.
In the step 2, the temperature is raised from the room temperature of 20-25 ℃ to the annealing heat treatment temperature of 300-600 ℃ at the temperature raising speed of 10-20 ℃/min, and the temperature is kept for 3-6 h, and then the material is taken out and air-cooled to the room temperature of 20-25 ℃.
In the technical scheme of the invention, the pretreatment of the matrix is firstly carried out: polishing an H13 steel sample with the size of 20mm multiplied by 15mm multiplied by 3mm to a bright mirror surface by using metallographic abrasive paper, then ultrasonically cleaning the sample in a 5-10% sodium hydroxide aqueous solution for 10-15 minutes to remove grease on the surface of the sample, then immersing the sample in 5-10% diluted hydrochloric acid for activation for 5-10 seconds, taking out the sample, washing the sample by using deionized water, ultrasonically oscillating the sample by using absolute ethyl alcohol, and drying the sample for later use.
In the technical scheme of the invention, after heat treatment, the surface Cr is2O3The content is increased, and the corrosion resistance of the plating layer is obviously improved. Compared with the prior art, the invention has the advantages that: the patent provides a method for improving the corrosion resistance of a chromium layer deposited on the surface of H13 steel by utilizing heat treatment according to the protection principle of a metal passive film, and achieves the aim of removing hydrogen by adjusting the heat treatment process, and simultaneously generates compact Cr on the surface of a Cr coating2O3Protecting the layer to improve its corrosion resistance.
Drawings
FIG. 1 is an SEM photograph of the surface topography of an as-plated chromium layer of the present invention.
FIG. 2 is an XRD spectrum of an as-plated chromium layer according to the present invention.
FIG. 3 is a photograph showing the appearance of the corrosion caused by the salt fog of the as-coated chromium layer according to the present invention.
FIG. 4 is an SEM photograph of the surface morphology of the chromium plating layer after the heat treatment in example 1 of the present invention.
FIG. 5 is an XRD spectrum of a chromium deposit after heat treatment according to example 1 of the present invention.
FIG. 6 is a photograph showing the appearance and appearance of salt spray corrosion of the heat-treated chromium plating layer in example 1 of the present invention.
FIG. 7 is an SEM photograph of the surface morphology of the chromium plating layer after the heat treatment in example 2 of the present invention.
FIG. 8 is an XRD spectrum of a chromium deposit after heat treatment in accordance with example 2 of the present invention.
FIG. 9 is a photograph showing the appearance and appearance of salt spray corrosion of the chromium plating layer after heat treatment in example 2 of the present invention.
FIG. 10 is an SEM photograph of the surface morphology of the chromium plating layer after the heat treatment in example 3 of the present invention.
FIG. 11 is an XRD spectrum of a chromium deposit after heat treatment according to example 3 of the present invention.
FIG. 12 is a photograph showing the appearance and appearance of salt spray corrosion of the chromium plating layer after heat treatment in example 3 of the present invention.
FIG. 13 is an SEM photograph of the surface morphology of the chromium deposit after heat treatment in example 4 of the present invention.
FIG. 14 is an XRD spectrum of a chromium deposit after heat treatment according to example 4 of the present invention.
FIG. 15 is a photograph of the appearance and appearance of salt spray corrosion of the heat-treated chromium deposit of example 4 of the present invention.
Detailed Description
To further illustrate the features and advantages of the present invention, the following description is given in conjunction with the examples, but the present invention is not limited to the examples. And observing the surface morphology of the coating by adopting an S-4800 type field emission Scanning Electron Microscope (SEM) and an SU1510 type tungsten filament SEM. The phase structure of the coating was characterized by means of an X-ray diffractometer (XRD) type Brook D8, Cu ka radiation, λ 0.1542nm, scan rate 0.02 °/s. The corrosion performance test is carried out in a simulated accelerated corrosion test box of model MNFS-1 by referring to the standard of GB/T10125-1997 salt spray test for artificial atmosphere corrosion test. The corrosion medium is NaCl aqueous solution with the mass fraction of 5 wt%. The effective area of the sample is 15mm multiplied by 15mm, and other parts are sealed by hot melt adhesive. After the test for 96h, the protection rating is carried out on the surface of the sample after corrosion according to GB/T6461-.
Example 1
1. Matrix pretreatment: h13 steel with the size of 20mm multiplied by 15mm multiplied by 3mm is cut out as a plating base by a wire cutting machine. The matrix sample is polished to a bright mirror surface by metallographic abrasive paper of 400 meshes, 600 meshes, 800 meshes, 1000 meshes, 1200 meshes and 1500 meshes, then is ultrasonically cleaned for 15 minutes in sodium hydroxide with the mass fraction of 10% to remove grease on the surface of the sample, then the sample is immersed in dilute hydrochloric acid with the mass fraction of 5% to be activated for 5 seconds, and is washed by deionized water after being taken out, ultrasonically vibrated by absolute ethyl alcohol and dried for later use.
2. The preparation process of the chromium plating comprises the following steps: by cleanLead-antimony alloy containing 7% of antimony by mass is used as an electroplating anode, the area ratio of the cathode to the anode is 1:2, and the distance between the cathode and the anode is 2 cm. Immersing the treated cathode and anode into the prepared chromium plating solution, and electrifying. The current density is 90A/dm2The temperature of the plating solution is 65 ℃ and the electroplating time is 30 min. And after the electroplating is finished, washing with tap water, then putting into absolute ethyl alcohol for ultrasonic oscillation, taking out, drying and weighing. The prepared chromium plating solution contains 250g/L of chromic anhydride, 1g/L of strontium sulfate and 10g/L of potassium fluosilicate, and the water used for preparing the chromium plating solution is deionized water.
3. The heat treatment process comprises the following steps: and (3) respectively heating the Cr coating samples obtained in the step (2) to 400 ℃ in an annealing furnace, preserving the heat for 1h, wherein the heating rate is 10 ℃/min, cleaning the surface with absolute ethyl alcohol after air cooling, and drying for later use.
4. The chromium plating layer prepared by the steps 1 and 2 has a uniform and compact surface and is distributed with fine microcracks (as shown in figure 1). As can be seen from the XRD spectrum (as shown in fig. 2), three distinct diffraction peaks appear at the positions of 44.4 °, 64.6 ° and 81.7 ° 2 θ, corresponding to the (110), (200) and (211) crystal planes, respectively, and the crystal grain size corresponding to the (200) crystal plane with the highest diffraction peak intensity is calculated to be only 54.3 nm. The plated Cr layer is composed of nanocrystalline chromium with a body-centered cubic structure. After 96h of salt spray corrosion, the surface corrosion area of the coating was 40% (as shown in FIG. 3), and the protection rating was 1. After the heat treatment in the step 3. The grain size and crack size of the plating layer are increased compared with the plating state (as shown in figure 4), and Cr begins to appear on the surface2O3And (3) as shown in figure 5, after 96h of salt spray corrosion, the corrosion area of the surface of the coating is 1 percent (as shown in figure 6), the protection rating is 6, and the corrosion resistance of the coating is remarkably improved under the heat treatment process.
Example 2
3. The heat treatment process comprises the following steps: and (3) respectively heating the Cr coating samples obtained in the step (2) to 400 ℃ in an annealing furnace, preserving the heat for 2h, wherein the heating rate is 10 ℃/min, cleaning the surface with absolute ethyl alcohol after air cooling, and drying for later use.
4. After the heat treatment in the step 3. The grain size and crack size of the coating were increased compared to example 1 (see FIG. 7)Shown), surface Cr2O3The content is increased (as shown in figure 8), after 96h of salt spray corrosion, the corrosion area of the surface of the plating is 0.5% (as shown in figure 9), the protection rating is 7, and the corrosion resistance of the plating is obviously improved under the heat treatment process.
Example 3
3. The heat treatment process comprises the following steps: and (3) respectively heating the Cr coating samples obtained in the step (2) to 500 ℃ in an annealing furnace, preserving the heat for 1h, heating at a speed of 10 ℃/min, cooling in air, cleaning the surface with absolute ethyl alcohol, and drying for later use.
4. After the heat treatment in the step 3. The grain size and crack size of the coating were increased compared to example 1 (as shown in FIG. 10), and the surface Cr was increased2O3The content is increased (as shown in figure 11), after 96h of salt spray corrosion, the surface of the plating layer is not obviously corroded (as shown in figure 12), the protection rating is 10, and the corrosion resistance of the plating layer under the heat treatment process is obviously improved.
Example 4
3. The heat treatment process comprises the following steps: and (3) respectively heating the Cr coating samples obtained in the step (2) to 600 ℃ in an annealing furnace, preserving the heat for 1h, heating at a speed of 10 ℃/min, cooling in air, cleaning the surface with absolute ethyl alcohol, and drying for later use.
4. After the heat treatment in the step 3. The grain size and crack size of the coating were increased compared to example 3 (as shown in FIG. 13), and the surface Cr was increased2O3The content is increased (as shown in figure 14), after 96h of salt spray corrosion, the surface of the plating layer is not obviously corroded (as shown in figure 15), the protection rating is 10, and the corrosion resistance of the plating layer under the heat treatment process is obviously improved.
The preparation of the chromium layer deposited on the surface of the H13 steel can be realized by adjusting the process parameters according to the content of the invention, the performance which is basically consistent with the invention is shown by tests, and the Cr layer on the surface is subjected to heat treatment2O3The content is increased, and the corrosion resistance of the plating layer is obviously improved. The invention being thus described by way of example, it will be obvious to those skilled in the art that various changes, modifications and alterations can be made therein without departing from the spirit and scope of the inventionEquivalents which do not entail any inventive step are intended to fall within the scope of the invention.
Claims (7)
1. A method for improving the corrosion resistance of a chromium layer deposited on the surface of H13 steel is characterized by comprising the following steps:
step 1, carrying out deposition preparation of chromium plating on the surface of H13 steel
H13 steel is taken as a cathode, lead-antimony alloy containing 7 wt% (mass percent) of antimony is taken as an electroplating anode, the electroplating anode is immersed into prepared chromium plating solution, and the electroplating solution is electrified to carry out deposition preparation of a chromium plating layer; the chromium plating solution consists of chromic anhydride, strontium sulfate, potassium fluosilicate and water, wherein the solvent is water, the content of chromic anhydride is 100-400 g/L, the content of strontium sulfate is 1-10 g/L, and the content of potassium fluosilicate is 1-25 g/L; the current density is 10-90A/dm2The temperature of the plating solution is 25-65 ℃, and the electroplating time is 15-120 min;
and 2, carrying out heat treatment on the H13 steel deposited with the chromium coating and prepared in the step 1, heating the steel from the room temperature of 20-25 ℃ to the annealing heat treatment temperature of 100-800 ℃ at the heating rate of 1-50 ℃/min in the air atmosphere, keeping the temperature for 0.5-8H, taking out the steel, and air-cooling the steel to the room temperature of 20-25 ℃.
2. The method for improving the corrosion resistance of the Cr layer deposited on the surface of the H13 steel as claimed in claim 1, wherein in step 1, the area ratio of the cathode to the anode is 1:2, the distance between the cathode and the anode is 1-3 cm.
3. The method for improving the corrosion resistance of the chromium layer deposited on the surface of the H13 steel according to claim 1, wherein in step 1, the solvent in the chromium plating solution is deionized water, and in the chromium plating solution, the content of chromic anhydride is 200-300 g/L, the content of strontium sulfate is 4-8 g/L, and the content of potassium fluosilicate is 10-20 g/L.
4. The method for improving the corrosion resistance of the chromium layer deposited on the H13 steel surface according to claim 1, wherein in step 1, the method is characterized in that electricity is applied to prepare the chromium coating by deposition, and the current density is 30-80A/dm2The temperature of the plating solution is 30-50 ℃, and the electroplating time is 50-100 min.
5. The method for improving the corrosion resistance of the Cr layer deposited on the surface of the H13 steel as claimed in claim 1, wherein in step 2, an annealing furnace is selected for annealing heat treatment, the temperature is raised from room temperature 20-25 ℃ to the annealing heat treatment temperature 300-600 ℃ at a temperature rise rate of 10-20 ℃/min, and the temperature is kept for 3-6H, and then the steel is taken out and air-cooled to room temperature 20-25 ℃.
6. The method for improving the corrosion resistance of the chromium layer deposited on the H13 steel surface as claimed in claim 1, wherein the pretreatment of the matrix is carried out firstly: polishing an H13 steel sample with the size of 20mm multiplied by 15mm multiplied by 3mm to a bright mirror surface by using metallographic abrasive paper, then ultrasonically cleaning the sample in a 5-10% sodium hydroxide aqueous solution for 10-15 minutes to remove grease on the surface of the sample, then immersing the sample in 5-10% diluted hydrochloric acid for activation for 5-10 seconds, taking out the sample, washing the sample by using deionized water, ultrasonically oscillating the sample by using absolute ethyl alcohol, and drying the sample for later use.
7. A Cr coating obtained by the method as claimed in any one of claims 1 to 6, wherein dense Cr is formed on the surface of the Cr coating2O3Protecting the layer to improve its corrosion resistance.
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Application publication date: 20210202 |