CN112853247A - Surface treatment process of anti-corrosion fastener - Google Patents

Surface treatment process of anti-corrosion fastener Download PDF

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Publication number
CN112853247A
CN112853247A CN202011569155.9A CN202011569155A CN112853247A CN 112853247 A CN112853247 A CN 112853247A CN 202011569155 A CN202011569155 A CN 202011569155A CN 112853247 A CN112853247 A CN 112853247A
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fastener
degreasing
corrosion
treatment process
surface treatment
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CN112853247B (en
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邱添
邱杰
周寰宇
肖沅均
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Sichuan Tianteng Technology Co ltd
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Sichuan Tianteng Technology Co ltd
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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
    • C23C2/00Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/04Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
    • C23C2/12Aluminium or alloys based thereon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24CABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
    • B24C1/00Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods
    • B24C1/08Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods for polishing surfaces, e.g. smoothing a surface by making use of liquid-borne abrasives
    • B24C1/086Descaling; Removing coating films
    • 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
    • C23C2/00Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/02Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • 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
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F17/00Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/026Anodisation with spark discharge
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/34Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Electrochemistry (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

The invention provides a surface treatment process for an anti-corrosion fastener, aiming at solving the problems of hydrogen embrittlement, poor anti-corrosion effect and influence on strength after the surface of the fastener is treated by zinc impregnation, cadmium plating, electro-galvanizing, hot galvanizing, chromate treatment, phosphating treatment, surface coating protection and other methods in the prior art. The process comprises the steps of degreasing the surface of the fastener, performing shot blasting treatment on the fastener, aluminizing the fastener, preparing a micro-arc oxidation film layer on the surface of the fastener and the like. According to the surface treatment process of the anti-corrosion fastener, firstly, degreasing and deoiling is carried out on the fastener, a through type shot blasting machine is adopted to carry out shot blasting on the surface of the fastener to remove iron oxide scales, then a layer of aluminum is plated on the surface of the fastener material to serve as a precursor of micro-arc oxidation, and a ceramic membrane with excellent corrosion resistance and mechanical property is prepared on the surface of the fastener through the micro-arc oxidation process, so that the corrosion resistance and the surface hardness of a fastener product are improved.

Description

Surface treatment process of anti-corrosion fastener
Technical Field
The invention relates to metal surface treatment, in particular to a surface treatment process of an anti-corrosion fastener.
Background
The fastener is a general name of a series of mechanical parts adopted when two or more parts (or components) are fastened and connected into a whole, is the most widely used universal part in industry at present, and is known as 'industrial rice'.
At present, the materials of the used fasteners generally comprise common carbon steel, high-strength steel, alloy steel and the like. In some special cases, a small amount of copper bolts is used, and although copper bolts have excellent corrosion resistance, it is difficult to use copper bolts in large amounts due to the control cost and the matching problem. In a humid environment, the corrosion resistance of a steel fastener is poor, so that the steel fastener must be treated by adopting an effective surface protection technology, otherwise, once the corrosion of the fastener fails, the normal use and safety of equipment and various engineering structures can be seriously influenced.
The corrosion prevention treatment on the surface of the steel fastener material adopted at the present stage is a relatively reasonable and practical approach. The conventional surface treatment methods adopted at home and abroad include zinc impregnation, cadmium plating, electrogalvanizing, hot galvanizing, chromate treatment, phosphating, surface coating protection and the like. The use effect in the actual environment shows that the anti-corrosion effect of the surface treatment processes such as cadmium plating, zinc plating and the like in the humid environment is not easy to meet the requirement, the high-strength steel is easy to generate hydrogen embrittlement danger in the electroplating process, and the cadmium and chromate used in the treatment processes can cause pollution to the environment, so the cadmium and chromate are gradually eliminated and forbidden to be used. The corrosion resistance of the steel fastener is improved mainly by adopting a powder zinc impregnation method in the original road engineering, and the method does not obtain the expected protection effect according to the practical application condition, and the expected protection service life requirement is difficult to achieve under the wet working condition because a hydrogen evolution environment exists in the zinc impregnation pretreatment process and the mechanical property of the high-strength fastener is possibly influenced in the zinc impregnation treatment process at higher temperature.
Disclosure of Invention
The invention provides a surface treatment process of an anti-corrosion fastener, aiming at solving the problems of hydrogen embrittlement, poor anti-corrosion effect and influence on strength after the surface of the fastener is treated by adopting methods such as zinc impregnation, cadmium plating, electro-galvanizing, hot galvanizing, chromate treatment, phosphating treatment, surface coating protection and the like in the prior art,
the technical scheme adopted by the invention is as follows:
a surface treatment process of an anti-corrosion fastener comprises the following steps,
step 1, degreasing the surface of a fastener;
step 2, performing shot blasting treatment on the fastener in the previous step;
step 3, heating the industrial aluminum with the purity of more than 99.7wt% to 760 ℃ to obtain aluminum liquid; placing the fastener in the last step in aluminum liquid for 2-5 min; taking out, cleaning by using a mixed solution of nitric acid, phosphoric acid and water at 60 ℃, and cooling to room temperature;
step 3, adding aminosilane and fluoride into water, adjusting the pH value to be more than 10 by adopting hydroxide, standing for a period of time until hydrolysis is finished, and obtaining an electrolyte solution; placing the fastener in the last step as an anode or a cathode and stainless steel as a counter electrode in a prepared electrolyte solution, and performing micro-arc oxidation treatment by constant voltage or constant current or constant power control of a power supply; the power supply is an alternating current power supply or a direct current power supply, the temperature of the electrolyte solution is lower than 50 ℃, and the oxidation time is 3-20 min.
In one embodiment of the invention, in step 1, the fastener is pre-degreased and immersion-degreased sequentially.
In one embodiment of the invention, in step 1, water is used as a diluent, and 10 g/L of degreasing agent and 5 mL/L of surfactant OP-10 are stirred for 3-4 min by compressed air at normal temperature to obtain pre-degreasing liquid; and uniformly spraying or brushing the pre-degreasing liquid on the surface of the fastener to perform pre-degreasing.
In one embodiment of the invention, water is used as a diluent, degreasing fluid is prepared in a degreasing tank according to the concentration of 50 g/L of degreasing agent, the temperature of the degreasing fluid is controlled to be 70 +/-2 ℃, and the fastener after pre-degreasing is immersed in the degreasing fluid.
In one embodiment of the invention, in the step 2, when the fastener is made of alloy steel or stainless steel, steel shots with the diameter of 0.5-0.75 mm are adopted; when the fastener is made of low-carbon steel, steel shots with the diameter of 1.2-2 mm are adopted; after shot blasting treatment, the surface of the fastener reaches the standard Sa2.5.
In one embodiment of the present invention, in step 3, nitric acid, phosphoric acid and water are mixed in a volume ratio of 1: 1: 1, the concentration of nitric acid is 50-70 wt%, the concentration of phosphoric acid is 85wt%, and the thickness of the aluminum film after cleaning is controlled to be 200-300 mu m.
In one embodiment of the invention, in the step 4, the fluoride is one or two of sodium fluoride and potassium fluoride, and the preparation concentration is 1-3 g/L.
In one embodiment of the present invention, in step 4, the hydroxide is one or both of sodium hydroxide and potassium hydroxide.
In one embodiment of the present invention, in step 4, the aminosilane has a general molecular formula of R4-xSi (OR ') x, wherein x is a number of 1, 2 OR 3, R is an amino group, R' is a methyl group OR an ethyl group, and the prepared concentration is 0.1 to 50 ml/L.
In one embodiment of the present invention, in step 4, the voltage range is 230V to 450V during the constant voltage control; when the current is controlled by constant current, the current density range is 5-30 mA/cm2
The invention has the beneficial effects that:
the invention provides a surface treatment process for an anti-corrosion fastener, aiming at solving the problems of hydrogen embrittlement, poor anti-corrosion effect and influence on strength after the surface of the fastener is treated by zinc impregnation, cadmium plating, electro-galvanizing, hot galvanizing, chromate treatment, phosphating treatment, surface coating protection and other methods in the prior art. The process comprises the steps of degreasing the surface of the fastener, performing shot blasting treatment on the fastener, aluminizing the fastener, preparing a micro-arc oxidation film layer on the surface of the fastener and the like. According to the invention, firstly, the fastener is degreased and degreased, the surface of the fastener is shot-blasted by using a through type shot blasting machine to remove iron scales, then a layer of aluminum is plated on the surface of the fastener material to be used as a precursor of micro-arc oxidation, and a ceramic membrane with excellent corrosion resistance and mechanical property is prepared on the surface of the fastener by a micro-arc oxidation process, so that the corrosion resistance and the surface hardness of the fastener product are improved. Compared with the traditional dacromet and galvanizing process, the fastener product developed by the project has the advantages of good corrosion resistance, higher surface hardness, strong scratch resistance, no use of virulent Cr6+, environmental protection, safety and huge market popularization potential.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a process flow diagram of a surface treatment process for a corrosion resistant fastener according to an embodiment.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention.
Embodiments of the invention are described in detail below with reference to the accompanying drawings.
The conventional surface treatment methods adopted at home and abroad include zinc impregnation, cadmium plating, electrogalvanizing, hot galvanizing, chromate treatment, phosphating, surface coating protection and the like. The use effect in the actual environment shows that the anti-corrosion effect of the surface treatment processes such as cadmium plating, zinc plating and the like in the humid environment is not easy to meet the requirement, the high-strength steel is easy to generate hydrogen embrittlement danger in the electroplating process, and the cadmium and chromate used in the treatment processes can cause pollution to the environment, so the cadmium and chromate are gradually eliminated and forbidden to be used. The corrosion resistance of the steel fastener is improved mainly by adopting a powder zinc impregnation method in the original road engineering, and the method does not obtain the expected protection effect according to the practical application condition, and the expected protection service life requirement is difficult to achieve under the wet working condition because a hydrogen evolution environment exists in the zinc impregnation pretreatment process and the mechanical property of the high-strength fastener is possibly influenced in the zinc impregnation treatment process at higher temperature.
In order to solve the problems of hydrogen embrittlement, poor corrosion prevention effect and influence on strength after the surface of a fastener is treated by adopting methods such as zinc impregnation, cadmium plating, electrogalvanizing, hot galvanizing, chromate treatment, phosphating treatment, surface coating protection and the like in the prior art, the embodiment provides a surface treatment process of a corrosion-prevention fastener, and the process flow is shown in figure 1.
Specifically, the surface treatment process of the anti-corrosion fastener comprises the following steps:
1. fastener surface degreasing
And (2) stirring 10 g/L of degreasing agent and 5 mL/L of surfactant OP-10 for 3-4 min by compressed air at normal temperature by taking water as a diluent to obtain the pre-degreasing solution.
And uniformly spraying or brushing the pre-degreasing liquid on the surface of the fastener to perform pre-degreasing.
Water is used as a diluent, degreasing fluid is prepared in a degreasing tank according to the concentration of 50 g/L degreasing agent, and the temperature of the degreasing fluid is controlled at 70 +/-2 ℃.
And (4) transferring the fastener into a degreasing tank after the fastener is subjected to pre-degreasing treatment. A grid barrel frame is arranged at the bottom of the degreasing tank and is 3cm away from the bottom of the degreasing tank, and a fastening piece is ensured to be arranged on the grid barrel frame to prevent sediment from being attached to the fastening piece. The total degreasing time is controlled to be 3-4 min.
After the fastener is subjected to pre-degreasing treatment, washing the residual degreasing fluid on the surface of the fastener with clear water for 2-3 times, and drying for later use.
2. Fastener shot blasting treatment
And adding 75-125 kg of specified mixed shot into the shot blasting cleaning chamber. The fastener is installed in the cleaning chamber, and the cleaning chamber door is closed. And (4) pressing buttons such as a dust removal button, a shot blasting button, a lifting button and a roller in sequence, and operating the shot blasting machine at the moment. And (4) observing whether the working current is normal or not, if the working current is less than 12A, indicating that the shot amount is insufficient, adding the shots immediately to enable the current to reach the range of 12-15A. And (4) setting shot blasting time in advance, and automatically stopping when the preset time is up. Slightly waiting for a moment after the machine is stopped, opening the cleaning room door, pressing a roller reversing switch, and automatically discharging. After shot blasting treatment by a through type shot blasting machine, the surface of the fastener reaches the standard Sa2.5.
In order to ensure the reduction of the surface roughness value of the fastener after shot blasting and the reasonable service life of the steel shots, the steel shots with the diameter of 0.5-0.75 mm are generally adopted. If the raw material of the fastener is low-carbon steel, adjusting and selecting steel shots with the diameter of 1.2-2 mm. The shot blasting amount per minute of each throwing head is controlled to be 15 kg/kW.
The surface of the fastener is usually provided with a layer of thinner iron oxide scale, which affects the lubrication effect on one hand, and on the other hand, during cold drawing, the hardness of the iron oxide scale is higher, so that surface defects such as scratches and the like are easily caused, and simultaneously, the drawing force is increased, so that the abrasion of a die is aggravated, the drawing is difficult, and the requirement of the smooth surface of the cold-drawn steel cannot be met. Therefore, in the traditional production process of the fastener, the iron oxide sheet of the fastener needs to be removed by an acid washing process. However, the process has the defects of easy hydrogen embrittlement of the fastener, aggravated die abrasion, large water consumption, high environmental-friendly disposal cost of the pickling waste liquid and the like.
In this embodiment, the steel shot is thrown to the surface of the steel material by the impeller rotating at a high speed to remove the iron scale. According to the ISO8501-1 standard, the diameter of a steel shot used for shot blasting, shot blasting amount per minute of the steel shot in the shot blasting process and the like are optimized, and finally the surface cleaning quality of the fastener is ensured to reach more than Sa2.5 grade.
And after shot blasting treatment of the fastener, washing the fastener for 2-3 times by using clear water, and drying.
3. Surface aluminizing of fastener
Selecting industrial aluminum with the purity of more than 99.7wt%, placing the industrial aluminum in a melting furnace, and heating to about 760 ℃ to obtain aluminum liquid. And (5) placing the fastener subjected to shot blasting in aluminum liquid for 2-5 min. Taking out, cleaning by using a mixed solution of nitric acid, phosphoric acid and water at about 60 ℃, cooling to room temperature, and forming an aluminum film precursor on the surface of the fastener. Wherein, the volume ratio of nitric acid, phosphoric acid and water is 1: 1: 1, the concentration of nitric acid is 50-70 wt%, and the concentration of phosphoric acid is 85 wt%.
In this embodiment, an aluminum film precursor is formed on the surface of the fastener by optimizing the process. Meanwhile, after the aluminum film precursor is cleaned by the mixed solution of nitric acid, phosphoric acid and water, the thickness of the aluminum film precursor is adjusted to be 200-300 mu m. Meanwhile, the pickling operation makes the surface of the aluminum film precursor uneven, so as to be beneficial to subsequent treatment.
4. Preparation of micro-arc oxidation film layer on surface of fastener
Adding aminosilane and fluoride into water, adjusting the pH value to be more than 10 by adopting hydroxide, standing for a period of time until hydrolysis is finished, and obtaining the electrolyte solution. Wherein the fluoride is one or two of sodium fluoride and potassium fluoride, and the preparation concentration is 1-3 g/L. The hydroxide is one or two of sodium hydroxide or potassium hydroxide. The molecular general formula of the aminosilane is R4-xSi (OR ') x, wherein x is a number 1, 2 OR 3, R is amino, R' is methyl OR ethyl, and the preparation concentration is 0.1-50 ml/L.
The fastener after aluminizing is used as an anode or a cathode, stainless steel is used as a counter electrode, the aluminum-plated fastener is placed in a prepared electrolyte solution, and micro-arc oxidation is carried out through the constant voltage or constant current or constant power control of a power supplyAnd (6) processing. The power supply is an alternating current power supply or a direct current power supply, the temperature of the electrolyte solution is lower than 50 ℃, and the oxidation time is 3-20 min. Wherein, the voltage range is 230V-450V when the constant voltage control is performed. When the current is controlled by constant current, the current density range is 5-30 mA/cm2
And after the oxidation is finished, taking out the fastener, washing and drying the fastener, and obtaining the micro-arc oxidation film layer on the surface of the fastener.
In the embodiment, the aluminum film precursor is already formed on the surface of the fastener, and the surface of the aluminum film precursor is rough, so that the contact area between the micro-arc oxidation film layer and the aluminum film precursor is increased, and the improvement of the reliability of combination is facilitated.
Meanwhile, during the subsequent micro-arc oxidation process, due to the local high temperature, Si and O diffuse from the surface to the base of the fastener, and Fe and Al diffuse to the surface, thereby generating a complex A1-Fe-Si alloy phase. The mutual diffusion among elements can ensure that the substrate and the surface film layer have good adhesion performance, thereby being convenient for the subsequent micro-arc oxidation process operation. Meanwhile, gradient distribution of hardness is formed between the oxide ceramic and the substrate material, so that the brittle fracture of the surface can be effectively reduced, the surface stress is relieved, and the comprehensive performance of the fastener is improved.
In addition, the local tip discharge of the surface of the fastener is accompanied by strong spark or micro-arc discharge in the traditional micro-arc oxidation process, a large amount of heat is released in the treatment process, the local temperature is too high, the fastener ablation is easy to generate, large-scale cooling equipment is needed in production, the production cost is increased, and potential safety hazards are brought to the surface treatment of the fastener. In the embodiment, aminosilane with excellent hydrolyzable performance is introduced into the micro-arc oxidation electrolyte, the number of amino functional groups on a silane chain segment is controlled in a focused manner, and the silanol hydrolyzed by the silane coupling agent is adsorbed on the metal surface to inhibit the point discharge in the micro-arc oxidation process of the fastener, so that the effects of arc suppression and pressure reduction are achieved.
Moreover, the prepared micro-arc oxidation film has a controllable structure, such as a micro-arc oxidation film with uniformly distributed micropores, and has better corrosion resistance and wear resistance.
Moreover, the adsorption of the long carbon chain organic silanol is beneficial to strengthening the adhesion performance of the micro-arc oxidation film and subsequent coating or other coatings. The surface can be prepared according to the requirements of the surface composite coating, and the excellent transition performance is provided for the composite coating.
Finally, the long carbon chain structure has a hydrophobic function, hydrolyzed silanol is adsorbed on the surface of the micro-arc oxidation film after micro-arc oxidation is finished, the micro-arc oxidation film can be endowed with the characteristics of hydrophobic function and the like, and the corrosion resistance of the micro-arc oxidation film is further improved.
The hexagon head bolts of a certain batch are processed and tested by the method, and the test results are shown as follows.
And (3) carrying out a sample tensile test by adopting a WDW-200 universal testing machine, wherein the test conditions are strictly executed according to the national standard GB/T3098.6-2010.
The bending fatigue test is carried out on a PQ-6 type bending fatigue testing machine, the load on a sample is realized by a mode of directly adding weights, the weights are hung on a pull rod penetrating through a screw rod, and the pull rod is connected with a connecting plate through a spring, so that the stability of loading and unloading is ensured.
The change rule of the hardness of the micro-arc oxidation layer is measured by adopting micro Vickers hardness, and the hardness test standard is strictly executed according to GB/T4340.1-1999.
The corrosion resistance test of the fastener is carried out by adopting a neutral salt spray corrosion test according to the national standard GB/T10125-1997.
Numbering Diameter/mm Yield strength/MPa Tensile strength/MPa Vickers hardness
1# 11.90 980 1000 206
2# 12.44 1060 1110 235
3# 12.32 1060 1140 245
4# 12.52 1080 1200 240
5# 12.46 1080 1180 240
6# 11.88 970 990 192
Wherein, the No. 1 finishes surface degreasing and shot blasting treatment only;
2# and 3# were processed with reference to the methods in the above examples;
4# and 5# were treated according to the method in the above examples and then placed in a salt spray box for 96 hours;
and 6# only finishes surface degreasing and shot blasting treatment, and then is placed in a salt spray box for 96 hours.
From the test results of # 1, # 2 and # 2, it can be seen that by adopting the method in the embodiment, the mechanical properties of the hexagon head bolt before and after the treatment, the diameter of the hexagon head bolt is increased due to the addition of the aluminum layer and the micro-arc oxidation film layer on the surface, and the tensile strength and the yield strength of the hexagon head bolt are also superior to those before the treatment.
From the comparison test results of # 2, # 3, # 4, # 5 and # 6, it can be seen that the corrosion resistance of the hexagonal bolt is significantly improved after the aluminum layer and the micro-arc oxide film layer are added on the surface of the hexagonal bolt by the method in the embodiment.
After the surface of the 2# hexagon head bolt is aluminized, the aluminum film layer is detected through SME and XRD. The main components of the XRD result of the film layer are solid solution (Fe, Cr, Ni)2Al5 with matrix of Fe2A15 and solid solution (Fe, Cr, Ni) Al3 with matrix of FeAl3, namely, the film layer shows that a complex intermetallic compound intermediate layer is formed between the aluminum film and the substrate, and a good transition layer is provided between the subsequent micro-arc oxidation film layer and the substrate. The SME structure shows an aluminum layer thickness of about 255 μm.

Claims (10)

1. A surface treatment process of an anti-corrosion fastener is characterized by comprising the following steps,
step 1, degreasing the surface of a fastener;
step 2, performing shot blasting treatment on the fastener in the previous step;
step 3, heating the industrial aluminum with the purity of more than 99.7wt% to 760 ℃ to obtain aluminum liquid; placing the fastener in the last step in aluminum liquid for 2-5 min; taking out, cleaning by using a mixed solution of nitric acid, phosphoric acid and water at 60 ℃, and cooling to room temperature;
step 3, adding aminosilane and fluoride into water, adjusting the pH value to be more than 10 by adopting hydroxide, standing for a period of time until hydrolysis is finished, and obtaining an electrolyte solution; placing the fastener in the last step as an anode or a cathode and stainless steel as a counter electrode in a prepared electrolyte solution, and performing micro-arc oxidation treatment by constant voltage or constant current or constant power control of a power supply; the power supply is an alternating current power supply or a direct current power supply, the temperature of the electrolyte solution is lower than 50 ℃, and the oxidation time is 3-20 min.
2. The surface treatment process for an anti-corrosion fastener according to claim 1, characterized in that in step 1, the fastener is subjected to pre-degreasing and immersion degreasing in sequence.
3. The surface treatment process of the anti-corrosion fastener according to claim 2, characterized in that in the step 1, water is used as a diluent, 10 g/L of degreasing agent and 5 mL/L of surfactant OP-10 are stirred for 3-4 min by compressed air at normal temperature, and pre-degreasing liquid is obtained; and uniformly spraying or brushing the pre-degreasing liquid on the surface of the fastener to perform pre-degreasing.
4. The surface treatment process of an anti-corrosion fastener according to claim 2 or 3, characterized in that water is used as a diluent, degreasing fluid is prepared in a degreasing tank at a concentration of 50 g/L of degreasing agent, the temperature of the degreasing fluid is controlled at 70 ± 2 ℃, and the pre-degreased fastener is immersed in the degreasing fluid.
5. The surface treatment process of the anti-corrosion fastener according to claim 1, wherein in the step 2, when the fastener is made of alloy steel or stainless steel, steel shots with the diameter of 0.5-0.75 mm are adopted; when the fastener is made of low-carbon steel, steel shots with the diameter of 1.2-2 mm are adopted; after shot blasting treatment, the surface of the fastener reaches the standard Sa2.5.
6. The surface treatment process for an anti-corrosion fastener according to claim 1, wherein in the step 3, nitric acid, phosphoric acid and water are mixed in a volume ratio of 1: 1: 1, the concentration of nitric acid is 50-70 wt%, the concentration of phosphoric acid is 85wt%, and the thickness of the aluminum film after cleaning is controlled to be 200-300 mu m.
7. The surface treatment process for an anti-corrosion fastener according to claim 1, wherein in the step 4, the fluoride is one or two of sodium fluoride and potassium fluoride, and the preparation concentration is 1-3 g/L.
8. The surface treatment process for an anti-corrosion fastener according to claim 1, wherein in step 4, the hydroxide is one or both of sodium hydroxide and potassium hydroxide.
9. The surface treatment process for an anti-corrosion fastener according to claim 1, characterized in that in step 4, the aminosilane has a general molecular formula of R4-xSi (OR ') x, wherein x is a number 1, 2 OR 3, R is an amino group, and R' is a methyl group OR an ethyl group, and the preparation concentration is 0.1 to 50 ml/L.
10. The surface treatment process for an anti-corrosion fastener according to claim 1, wherein in the step 4, the voltage range is 230V to 450V during constant voltage control; when the current is controlled by constant current, the current density range is 5-30 mA/cm2
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