CN110592570A - Magnesium alloy surface black chemical conversion process - Google Patents

Magnesium alloy surface black chemical conversion process Download PDF

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Publication number
CN110592570A
CN110592570A CN201910920424.2A CN201910920424A CN110592570A CN 110592570 A CN110592570 A CN 110592570A CN 201910920424 A CN201910920424 A CN 201910920424A CN 110592570 A CN110592570 A CN 110592570A
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China
Prior art keywords
magnesium alloy
washing
namely
temperature
degreasing
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CN201910920424.2A
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Chinese (zh)
Inventor
贺东奎
封居刚
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AMGAIN SHANDONG MAGNESIUM Co Ltd
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AMGAIN SHANDONG MAGNESIUM Co Ltd
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Priority to CN201910920424.2A priority Critical patent/CN110592570A/en
Publication of CN110592570A publication Critical patent/CN110592570A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/48Chemical 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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/57Treatment of magnesium or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/78Pretreatment of the material to be coated

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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 magnesium alloy surface black chemical conversion process, which belongs to the field of magnesium alloy processing and comprises the steps of degreasing, washing, activating, washing, descaling, washing, oxidizing black, washing and drying; the process is mainly suitable for various grades of magnesium alloys, a uniform and compact oxide film layer is generated on the surface of the magnesium alloy in a chemical conversion mode, and the surface substances of the magnesium alloy can play the technical characteristics of optical infrared ray resistance and no falling of organic coatings, so that the limitation blank of the technical field in China at present is filled; solves the problem that the original black film of the organic coating is easy to age, discolor and fall off in the using process.

Description

Magnesium alloy surface black chemical conversion process
Technical Field
The invention belongs to the technical field of magnesium alloy processing, and particularly relates to a black chemical conversion process for a magnesium alloy surface.
Background
At present, because the application of magnesium alloy materials in military optics can not realize the technique of matte black oxidation treatment of inorganic salt film layers, the application in the field is always subjected to the bottleneck of great technical difficulty, and the technique is born; the biggest technical advantages are that; the technology is environment-friendly, easy to control and low in cost, and the greatest technical advantage is that the disposable investment equipment is few;
at present, the treatment method of the magnesium alloy in the technical field is mainly carried out by organic coating and non-environment-friendly potassium dichromate in China, and the biggest defect of the original technology is that; the environment is not protected, the ultraviolet resistance is poor, the color uniformity is not easy to control, and the like;
the original technology is required to be processed at high temperature in the using process, the solution is easy to volatilize, a large amount of energy is consumed, and the like, and the technical advantages of low-temperature operation, low energy consumption and the like are the biggest advantages of the prior art;
the prior art invention needs mass production verification and technical consolidation of corrosion resistance improvement and the like.
Disclosure of Invention
The invention aims to provide a magnesium alloy surface black chemical conversion process to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a magnesium alloy surface black chemical conversion process comprises the following steps:
1) degreasing, namely soaking the magnesium alloy in degreasing liquid at a certain temperature for a period of time to remove dirt on the surface of the magnesium alloy;
2) washing, namely, putting the magnesium alloy soaked by the degreasing solution into clear water, and washing the residual degreasing solution on the surface;
3) activating, namely soaking the magnesium alloy washed in the step 2) in an activating agent at a certain temperature for a period of time to remove an oxide film and impurities on the surface of the magnesium alloy;
4) washing, namely putting the magnesium alloy activated in the step 3) into clear water, and washing the activator remained on the surface;
5) descaling, namely soaking the magnesium alloy washed in the step 4) in descaling liquid at a certain temperature for a period of time to remove dirt on the surface of the magnesium alloy;
6) washing, namely putting the magnesium alloy descaled in the step 5) into clear water, and washing residual dirt and descaling liquid on the surface;
7) black oxidation, namely soaking the magnesium alloy washed by water in the step 6) in an oxidant solution at a certain temperature for a period of time to oxidize and blacken the surface of the magnesium alloy;
8) washing, namely placing the magnesium alloy oxidized in the step 7) in clear water to wash away the residual oxidant solution on the surface;
9) drying, the magnesium alloy cleaned in the step 8) is placed in a drying device with the temperature of 120-.
Preferably, in step 1), the degreasing fluid comprises the following components in concentration:
5-10g/L of sodium hydroxide, 1-7g/L of sodium tripolyphosphate and 0.5-1.0g/L of organic emulsion solution.
Preferably, in step 3), the activator comprises the following components in concentration:
3.0-5.3g/L of phosphate, 0.3-20g/L of oxalic acid and 0.5-1.0g/L of EDTA.
Preferably, in step 5), the scale remover comprises the following components in concentration:
10-25g/L of potassium hydroxide and 5-12g/L of nitrite.
Preferably, the oxidizing agent comprises the following components in concentrations:
acetate 0.13-2.35g/L, molybdate 2.0-5.5g/L, sodium m-nitrobenzenesulfonate 0.10-2.30g/L, phosphoric acid 0.5-3.0g/L and acetic acid 3-7 g/L.
Preferably, in the step 1), the temperature of the degreasing fluid is 60-65 ℃, and the soaking time is 240-300 s.
Preferably, in the step 3), the temperature of the activating agent is 40-45 ℃, and the soaking time is 45-60 s.
Preferably, in the step 5), the temperature of the scale remover is 40-45 ℃, and the soaking time is 180-300 s.
Preferably, in the step 7), the temperature of the oxidant is 30-35 ℃, and the soaking time is 240-300 s.
Compared with the prior art, the invention has the beneficial effects that: the process is mainly suitable for various grades of magnesium alloys, a uniform and compact oxide film layer is generated on the surface of the magnesium alloy in a chemical conversion mode, and the surface substances of the magnesium alloy can play the technical characteristics of optical infrared ray resistance and no falling of organic coatings, so that the limitation blank of the technical field in China at present is filled; solves the problem that the original black film of the organic coating is easy to age, discolor and fall off in the using process.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The conditions in the embodiments can be further adjusted according to specific conditions, and simple modifications of the method of the present invention based on the concept of the present invention are within the scope of the claimed invention.
Example 1
A magnesium alloy surface black chemical conversion process comprises the following steps:
1) degreasing, namely soaking the magnesium alloy in degreasing liquid at the temperature of 60 ℃ for 300s to remove dirt on the surface of the magnesium alloy;
the degreasing fluid comprises the following components in concentration:
5-10g/L of sodium hydroxide, 1-7g/L of sodium tripolyphosphate and 0.5-1.0g/L of organic emulsion solution.
2) And (3) water washing, namely, putting the magnesium alloy soaked in the degreasing solution into clear water, and washing the residual degreasing solution on the surface.
3) Activating, namely soaking the magnesium alloy washed in the step 2) in an activating agent at the temperature of 40 ℃ for 60s to remove an oxide film and impurities on the surface of the magnesium alloy;
the activator comprises the following components in concentration:
3.0-5.3g/L of phosphate, 0.3-20g/L of oxalic acid and 0.5-1.0g/L of EDTA.
4) Washing, namely putting the magnesium alloy activated in the step 3) into clear water, and washing the activator remained on the surface;
5) descaling, namely soaking the magnesium alloy washed in the step 4) in descaling liquid at the temperature of 40 ℃ for 300s to remove dirt on the surface of the magnesium alloy;
the descaling agent comprises the following components in concentration:
10-25g/L of potassium hydroxide and 5-12g/L of nitrite.
6) Washing, namely putting the magnesium alloy descaled in the step 5) into clear water, and washing residual dirt and descaling liquid on the surface;
7) black oxidation, namely soaking the magnesium alloy washed by water in the step 6) in an oxidant solution at the temperature of 30 ℃ for 300s to oxidize and blacken the surface of the magnesium alloy;
the oxidant comprises the following components in concentration:
acetate 0.13-2.35g/L, molybdate 2.0-5.5g/L, sodium m-nitrobenzenesulfonate 0.10-2.30g/L, phosphoric acid 0.5-3.0g/L and acetic acid 3-7 g/L.
8) Washing, namely placing the magnesium alloy oxidized in the step 7) in clear water to wash away the residual oxidant solution on the surface;
9) and (3) drying, namely, placing the magnesium alloy cleaned in the step 8) into a drying device with the temperature of 120 ℃ for baking for 1800s to dry the magnesium alloy.
Example 2
A magnesium alloy surface black chemical conversion process comprises the following steps:
1) degreasing, namely soaking the magnesium alloy in degreasing liquid at the temperature of 63 ℃ for 270s to remove dirt on the surface of the magnesium alloy;
the degreasing fluid comprises the following components in concentration:
5-10g/L of sodium hydroxide, 1-7g/L of sodium tripolyphosphate and 0.5-1.0g/L of organic emulsion solution.
2) And (3) water washing, namely, putting the magnesium alloy soaked in the degreasing solution into clear water, and washing the residual degreasing solution on the surface.
3) Activating, namely soaking the magnesium alloy washed in the step 2) in an activating agent at the temperature of 43 ℃ for 52s to remove an oxide film and impurities on the surface of the magnesium alloy;
the activator comprises the following components in concentration:
3.0-5.3g/L of phosphate, 0.3-20g/L of oxalic acid and 0.5-1.0g/L of EDTA.
4) Washing, namely putting the magnesium alloy activated in the step 3) into clear water, and washing the activator remained on the surface;
5) descaling, namely soaking the magnesium alloy washed in the step 4) in descaling solution at the temperature of 43 ℃ for 240 seconds to remove dirt on the surface of the magnesium alloy;
the descaling agent comprises the following components in concentration:
10-25g/L of potassium hydroxide and 5-12g/L of nitrite.
6) Washing, namely putting the magnesium alloy descaled in the step 5) into clear water, and washing residual dirt and descaling liquid on the surface;
7) black oxidation, namely soaking the magnesium alloy washed by water in the step 6) in an oxidant solution at the temperature of 33 ℃ for 270s to oxidize and blacken the surface of the magnesium alloy;
the oxidant comprises the following components in concentration:
acetate 0.13-2.35g/L, molybdate 2.0-5.5g/L, sodium m-nitrobenzenesulfonate 0.10-2.30g/L, phosphoric acid 0.5-3.0g/L and acetic acid 3-7 g/L.
8) Washing, namely placing the magnesium alloy oxidized in the step 7) in clear water to wash away the residual oxidant solution on the surface;
9) and (3) drying, namely, placing the magnesium alloy cleaned in the step 8) into a drying device with the temperature of 135 ℃ for baking for 1200s, so that the magnesium alloy is dried.
Example 3
A magnesium alloy surface black chemical conversion process comprises the following steps:
1) degreasing, namely soaking the magnesium alloy in degreasing liquid at the temperature of 65 ℃ for 240s to remove dirt on the surface of the magnesium alloy;
the degreasing fluid comprises the following components in concentration:
5-10g/L of sodium hydroxide, 1-7g/L of sodium tripolyphosphate and 0.5-1.0g/L of organic emulsion solution.
2) And (3) water washing, namely, putting the magnesium alloy soaked in the degreasing solution into clear water, and washing the residual degreasing solution on the surface.
3) Activating, namely soaking the magnesium alloy washed in the step 2) in an activating agent at the temperature of 45 ℃ for 45s to remove an oxide film and impurities on the surface of the magnesium alloy;
the activator comprises the following components in concentration:
3.0-5.3g/L of phosphate, 0.3-20g/L of oxalic acid and 0.5-1.0g/L of EDTA.
4) Washing, namely putting the magnesium alloy activated in the step 3) into clear water, and washing the activator remained on the surface;
5) descaling, namely soaking the magnesium alloy washed in the step 4) in descaling liquid at the temperature of 45 ℃ for 180s to remove dirt on the surface of the magnesium alloy;
the descaling agent comprises the following components in concentration:
10-25g/L of potassium hydroxide and 5-12g/L of nitrite.
6) Washing, namely putting the magnesium alloy descaled in the step 5) into clear water, and washing residual dirt and descaling liquid on the surface;
7) black oxidation, namely soaking the magnesium alloy washed by water in the step 6) in an oxidant solution at the temperature of 35 ℃ for 240s to oxidize and blacken the surface of the magnesium alloy;
the oxidant comprises the following components in concentration:
acetate 0.13-2.35g/L, molybdate 2.0-5.5g/L, sodium m-nitrobenzenesulfonate 0.10-2.30g/L, phosphoric acid 0.5-3.0g/L and acetic acid 3-7 g/L.
8) Washing, namely placing the magnesium alloy oxidized in the step 7) in clear water to wash away the residual oxidant solution on the surface;
9) and (3) drying, namely, placing the magnesium alloy cleaned in the step 8) into a drying device at the temperature of 150 ℃ for baking for 600s to dry the magnesium alloy.
The process is mainly suitable for various grades of magnesium alloys, a uniform and compact oxide film layer is generated on the surface of the magnesium alloy in a chemical conversion mode, and the surface substances of the magnesium alloy can play the technical characteristics of optical infrared ray resistance and no falling of organic coatings, so that the limitation blank of the technical field in China at present is filled; solves the problem that the original black film of the organic coating is easy to age, discolor and fall off in the using process.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. A magnesium alloy surface black chemical conversion process is characterized by comprising the following steps:
1) degreasing, namely soaking the magnesium alloy in degreasing liquid at a certain temperature for a period of time to remove dirt on the surface of the magnesium alloy;
2) washing, namely, putting the magnesium alloy soaked by the degreasing solution into clear water, and washing the residual degreasing solution on the surface;
3) activating, namely soaking the magnesium alloy washed in the step 2) in an activating agent at a certain temperature for a period of time to remove an oxide film and impurities on the surface of the magnesium alloy;
4) washing, namely putting the magnesium alloy activated in the step 3) into clear water, and washing the activator remained on the surface;
5) descaling, namely soaking the magnesium alloy washed in the step 4) in descaling liquid at a certain temperature for a period of time to remove dirt on the surface of the magnesium alloy;
6) washing, namely putting the magnesium alloy descaled in the step 5) into clear water, and washing residual dirt and descaling liquid on the surface;
7) black oxidation, namely soaking the magnesium alloy washed by water in the step 6) in an oxidant solution at a certain temperature for a period of time to oxidize and blacken the surface of the magnesium alloy;
8) washing, namely placing the magnesium alloy oxidized in the step 7) in clear water to wash away the residual oxidant solution on the surface;
9) drying, the magnesium alloy cleaned in the step 8) is placed in a drying device with the temperature of 120-.
2. The process of claim 1, wherein in the step 1), the degreasing fluid comprises the following components in concentration:
5-10g/L of sodium hydroxide, 1-7g/L of sodium tripolyphosphate and 0.5-1.0g/L of organic emulsion solution.
3. The process of claim 1, wherein in step 3), the activator comprises the following components in concentration:
3.0-5.3g/L of phosphate, 0.3-20g/L of oxalic acid and 0.5-1.0g/L of EDTA.
4. The process of claim 1, wherein in the step 5), the scale remover comprises the following components in concentration:
10-25g/L of potassium hydroxide and 5-12g/L of nitrite.
5. The process of claim 1, wherein in step 7), the oxidizing agent comprises the following components in concentration:
acetate 0.13-2.35g/L, molybdate 2.0-5.5g/L, sodium m-nitrobenzenesulfonate 0.10-2.30g/L, phosphoric acid 0.5-3.0g/L and acetic acid 3-7 g/L.
6. The process of claim 1, wherein in the step 1), the temperature of the degreasing solution is 60-65 ℃, and the soaking time is 240-300 s.
7. The process of claim 1, wherein in the step 3), the temperature of the activator is 40-45 ℃ and the soaking time is 45-60 s.
8. The process as claimed in claim 1, wherein the temperature of the detergent in step 5) is 40-45 ℃ and the soaking time is 180-300 s.
9. The process as claimed in claim 1, wherein the temperature of the oxidant in step 7) is 30-35 ℃ and the soaking time is 240-300 s.
CN201910920424.2A 2019-09-27 2019-09-27 Magnesium alloy surface black chemical conversion process Pending CN110592570A (en)

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Cited By (1)

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CN115283309B (en) * 2022-07-06 2024-04-02 中船重工龙江广瀚燃气轮机有限公司 Method for removing residual scale and paint layer on surface of gas turbine casing by chemical method

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Application publication date: 20191220