CN109338362B - Method for preparing wear-resistant ceramic layer on surface of high-phosphorus cast iron - Google Patents

Method for preparing wear-resistant ceramic layer on surface of high-phosphorus cast iron Download PDF

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CN109338362B
CN109338362B CN201811264303.9A CN201811264303A CN109338362B CN 109338362 B CN109338362 B CN 109338362B CN 201811264303 A CN201811264303 A CN 201811264303A CN 109338362 B CN109338362 B CN 109338362B
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cast iron
micro
aluminum
arc oxidation
ceramic layer
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CN109338362A (en
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马瑞娜
张余
杜安
范永哲
赵雪
曹晓明
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Hebei University of Technology
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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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • 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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
    • C23C2/12—Aluminium or alloys based thereon
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/026—Anodisation with spark discharge
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires

Abstract

The invention relates to a method for preparing a wear-resistant ceramic layer on the surface of high-phosphorus cast iron, which comprises the following steps: (1) pretreating the high-phosphorus cast iron workpiece, and obtaining an aluminum-plated layer on the surface of the high-phosphorus cast iron workpiece by adopting a hot-dip aluminum plating mode; (2) polishing the aluminized sample, ultrasonically cleaning the aluminized sample in alcohol, and drying the aluminized sample for later use; immersing the dried aluminum-plated sample into micro-arc oxidation electrolyte for micro-arc oxidation treatment to form an aluminum oxide ceramic layer on the surface of the aluminum-plated sample; the specific process of the micro-arc oxidation treatment comprises the following steps: an alternating current pulse power supply is adopted, positive voltage is controlled to be boosted to 400V from a 100V stage, negative voltage is controlled to be boosted to 140V from a 10V stage, processing time is 30-60min, frequency is 200Hz, and duty ratio is 40-60%. According to the method, a thicker wear-resistant ceramic layer is formed on the surface of the high-phosphorus cast iron by combining a hot dip aluminum plating technology and a micro-arc oxidation technology, the coating and a matrix are combined to form metallurgical bonding, the bonding force is good, and the wear resistance of the high-phosphorus cast iron is remarkably improved.

Description

Method for preparing wear-resistant ceramic layer on surface of high-phosphorus cast iron
Technical Field
The invention relates to a new technology for surface protection and wear-resistant treatment of high-phosphorus cast iron, in particular to a method for preparing a wear-resistant ceramic layer on the surface of a high-phosphorus cast iron material.
Background
In recent years, the rapidly growing transportation industry has become one of the national economic shoring industries. In the transportation industry, heavy-duty vehicles are responsible for major transportation tasks. Among them, heavy-duty automobile engines as key parts must be stably and reliably operated in a high-speed running state, and thus, higher demands are made on the performance of internal parts of the engines. The valve guide is an important part and needs to be stable under high-speed motion, so that the requirement on the wear resistance is high. The traditional method adopts high-phosphorus cast iron materials (when the phosphorus content is higher than the solubility of phosphorus in cast iron, phosphorus eutectic is generated, and the phosphorus eutectic can improve the wear resistance of the cast iron), but the development of times can not be met gradually. Therefore, the surface modification of the material is considered to improve the wear resistance of the material. Common methods include thermal spraying, surface heat treatment, powder embedding, micro-arc oxidation, and the like.
The coating prepared by the thermal spraying method is physically combined with the substrate and is easy to fall off. The surface heat treatment is not suitable for cast iron because graphite in cast iron is oxidized due to the surface heat treatment process. The powder embedding process is relatively complex, has low success rate, so the cost is high, and is not suitable for industrial production.
Disclosure of Invention
The invention aims to provide a method for preparing a wear-resistant ceramic layer on the surface of high-phosphorus cast iron, which forms a thicker wear-resistant ceramic layer on the surface of the high-phosphorus cast iron by combining a hot dip aluminizing technology and a micro-arc oxidation technology, and the coating and a matrix are combined to form metallurgical bonding, so that the bonding force is good, the wear resistance of the high-phosphorus cast iron is obviously improved, the process is relatively simple, the cost rate is high, and the method is suitable for industrial production. Meanwhile, the coating can well protect the graphite in the cast iron.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing a wear-resistant ceramic layer on the surface of high-phosphorus cast iron comprises the following steps:
(1) pretreating the high-phosphorus cast iron workpiece, and obtaining an aluminum-plated layer on the surface of the high-phosphorus cast iron workpiece by adopting a hot-dip aluminum plating mode; the specific process of the hot dip aluminum plating mode is as follows: the aluminum plating temperature is 710-770 ℃, the immersion plating time is 1-5min, the plating assistant agent adopts 7-10% of KF and 5-8% of NaCl aqueous solution by mass fraction, the plating assistant temperature is 95-100 ℃, and the plating assistant time is 2-5 min.
(2) Polishing the aluminized sample, ultrasonically cleaning the aluminized sample in alcohol, and drying the aluminized sample for later use; immersing the dried aluminum-plated sample into micro-arc oxidation electrolyte for micro-arc oxidation treatment to form an aluminum oxide ceramic layer on the surface of the aluminum-plated sample; the specific process of the micro-arc oxidation treatment comprises the following steps: an alternating current pulse power supply is adopted, positive voltage is controlled to be boosted to 400V from a 100V stage, negative voltage is controlled to be boosted to 140V from a 10V stage, processing time is 30-60min, frequency is 200Hz, and duty ratio is 40-60%; the electrolyte is prepared by mixing sodium silicate, sodium hexametaphosphate and potassium hydroxide according to the mass ratio of 5: 3: 2 in distilled water.
Compared with the prior art, the invention has the beneficial effects that:
the object of the coating prepared by the invention is high-phosphorus cast iron, which aims to improve the wear resistance of the high-phosphorus cast iron, the high-phosphorus cast iron workpiece is subjected to hot dip aluminum plating treatment, then the workpiece is subjected to micro-arc oxidation, and the technological parameters in the micro-arc oxidation process are strictly controlled, so that the aim of combining the high-phosphorus cast iron and the oxidized ceramic into a whole is fulfilled, the advantages of the high-phosphorus cast iron material are retained, and the advantages of the high hardness and the high wear resistance of the ceramic are applied to the invention; meanwhile, the method has the advantages of simple process, convenient operation, environmental protection and no pollution, and is suitable for the trend of social development. The micro-arc oxidation electrolyte is preferably added with a dispersion liquid prepared from nano BN and ethanol, and in the micro-arc oxidation process, the nano BN mainly enters the ceramic layer in a mode of solid solution with molten aluminum oxide and dispersion deposition on film layer holes and cracks, so that a composite ceramic layer containing nano BN particles is generated, and the wear resistance of the composite ceramic layer is obviously improved.
In addition, the hot dip aluminizing temperature in the method needs to be strictly controlled, and since the melting point of pure aluminum is about 670 ℃, the fluidity of aluminum liquid is poor at the temperature (710 ℃) slightly higher than the melting point, the viscosity is large, the diffusion capacity of aluminum atoms is weak, the alloy is thin, and the adhesion effect on the aluminum liquid is poor. The thickness of the aluminum layer is the largest at 730 ℃, when the temperature is continuously increased, the limitation of the alloy layer on the thickness of the aluminum layer is eliminated, the fluidity of the aluminum liquid is enhanced when the temperature is increased, the viscosity is reduced, and the aluminum liquid flows back to the crucible in the pulling process, so that the thickness of the aluminum layer is reduced. The immersion plating time is preferably 3min, the aluminum layer thickness increasing speed reaches the maximum at the time, the aluminum layer thickness increases along with the increase of the time, but the increasing speed decreases, because when the aluminum layer thickness reaches a certain value, the adhesion effect of the aluminum liquid on the matrix begins to decrease, and when the aluminum plated part is lifted out of the aluminum liquid, the carried-out aluminum liquid flows back into the aluminum liquid. The micro-arc oxidation time determines the thickness and quality of the oxidized ceramic layer, and further influences the wear resistance, so the micro-arc oxidation time in the method needs to be strictly controlled.
The method can prepare a thicker composite ceramic oxide layer containing nano BN particles on the surface of the high-phosphorus cast iron by adopting a method of combining hot dip aluminum plating and micro-arc oxidation, and after a friction and wear experiment, the wear rate of the composite ceramic oxide layer containing the nano BN particles is 0.852 × 10-4mm3/(N × m), whereas the wear rate of the ceramic oxide layer without nano BN particles was 1.25 × 10-4mm3/(N × m), the wear rate of the high phosphorus cast iron was 3.22 × 10-4mm3And (N × m) under the same abrasion condition, the abrasion rate of the composite ceramic oxide layer containing the nanometer BN particles is the lowest, so the method obviously improves the abrasion resistance of the high-phosphorus cast iron, and the coating and the substrate are combined into metallurgical bonding with good bonding force.
Drawings
In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, a brief description is given below of the drawings used in describing the embodiments. It should be clear that the described figures are only views of some of the embodiments of the invention to be described, not all, and that for a person skilled in the art, other figures can be derived from these figures without inventive effort.
FIG. 1 is a schematic wear rate diagram.
Detailed Description
The invention discloses a method for preparing a wear-resistant ceramic layer on the surface of high-phosphorus cast iron, which comprises the following steps:
(1) pretreating the high-phosphorus cast iron workpiece, and obtaining an aluminum-plated layer on the surface of the high-phosphorus cast iron workpiece by adopting a hot-dip aluminum plating mode; the specific process of the hot dip aluminum plating mode is as follows: acid washing treatment, namely adopting a hydrochloric acid solution with the concentration of 40%, wherein the acid washing time is 4 min; the hot dip aluminum plating component is industrial pure aluminum (the purity is more than 99.7%), the aluminum plating equipment is a well-type resistance furnace, the aluminum plating temperature is 710-770 ℃, the dip plating time is 1-5min, the plating assistant agent adopts KF with the mass fraction of 7-10% and NaCl aqueous solution with the mass fraction of 5-8%, the plating assistant temperature is 95-100 ℃, and the plating assistant time is 2-5 min;
(2) polishing the aluminized sample, ultrasonically cleaning the aluminized sample in alcohol for 10min, and drying the aluminized sample for later use; immersing the dried aluminum-plated sample into micro-arc oxidation electrolyte for micro-arc oxidation treatment to form an aluminum oxide ceramic layer on the surface of the aluminum-plated sample; the specific process of the micro-arc oxidation treatment comprises the following steps: an alternating current pulse power supply is adopted, positive voltage is controlled to be boosted to 400V from a 100V stage, negative voltage is controlled to be boosted to 140V from a 10V stage, processing time is 30-60min, frequency is 200Hz, and duty ratio is 40-60%; the electrolyte is prepared by mixing sodium silicate, sodium hexametaphosphate and potassium hydroxide according to the mass ratio of 5: 3: 2 in distilled water.
And a dispersion prepared from nano BN and ethanol is also added into the electrolyte in the micro-arc oxidation treatment process. The concentration of the dispersion liquid is 40-60 g/mL.
The pretreatment process in the step (1) of the invention is to carry out oil and rust removal treatment, then polish and polish, ultrasonically clean in alcohol for 10min, and finally dry for later use. The invention carries out polishing treatment twice to ensure that the surfaces of the workpiece and the aluminum layer have no defects.
In the invention, the aluminum plating temperature is preferably 730 ℃, and the dip plating time is preferably 3 min. The electrolyte during micro-arc oxidation is an aqueous solution consisting of 2g/L potassium hydroxide, 3g/L sodium hexametaphosphate and 5g/L sodium silicate; the concentration of the dispersion is 50 g/mL; the micro-arc oxidation treatment temperature is 25 +/-10 ℃.
Example 1
The embodiment of the method for preparing the wear-resistant ceramic layer on the surface of the high-phosphorus cast iron adopts an alternating-current pulse power supply, takes aluminized cast iron as an anode and a steel plate as a cathode, and comprises the following specific steps:
(1) pretreating the high-phosphorus cast iron workpiece, and obtaining an aluminum-plated layer on the surface of the high-phosphorus cast iron workpiece by adopting a hot-dip aluminum plating mode; the specific process of the hot dip aluminum plating mode is as follows: acid washing treatment, namely adopting a hydrochloric acid solution with the concentration of 40%, wherein the acid washing time is 4 min; the hot dip aluminum plating component is industrial pure aluminum (the purity is more than 99.7%), the aluminum plating equipment is a well-type resistance furnace, the aluminum plating temperature is 730 ℃, the dip plating time is 3min, the plating assistant agent adopts KF with the mass fraction of 8% and NaCl aqueous solution with the mass fraction of 6%, the plating assistant temperature is 98 ℃, and the plating assistant time is 3 min.
(2) Polishing the aluminized sample, ultrasonically cleaning the aluminized sample in alcohol for 10min, and drying the aluminized sample for later use; immersing the dried aluminum-plated sample into micro-arc oxidation electrolyte for micro-arc oxidation treatment to form an aluminum oxide ceramic layer on the surface of the aluminum-plated sample; the specific process of the micro-arc oxidation treatment comprises the following steps: immersing an anode sample into electrolyte, performing micro-arc oxidation treatment by adopting a processing mode of stage constant voltage, controlling the positive voltage to be boosted to 400V from a 100V stage and the negative voltage to be boosted to 140V from a 10V stage at the processing temperature of 25 ℃, wherein the processing time is 30min, the frequency is 200Hz, and the duty ratio is 45%; the electrolyte is a mixture of 2g/L potassium hydroxide, 3g/L sodium hexametaphosphate, 5g/L sodium silicate and the balance of water, the residual electrolyte on the surface of the sample is washed by distilled water, and the sample is air-dried at room temperature.
The micro-arc oxidation film obtained by the embodiment has the thickness of 20 mu m, the hardness of 500HV, the friction coefficient of 0.4 and the wear rate of 2.725 × 10-4mm3/(N×m)。
Example 2
The method of this embodiment is the same as embodiment 1 except that the energization time is 40 min.
The micro-arc oxidation film obtained by the embodiment has the thickness of 40 mu m, the hardness of 650HV, the friction coefficient of 0.45 and the wear rate of 1.725 × 10-4mm3/(N×m)。
Example 3
The method of this embodiment is the same as embodiment 1 except that the energization time is 50 min.
The micro-arc oxidation film obtained by the embodiment has the thickness of 60 mu m, the hardness of 950HV, the friction coefficient of 0.5 and the wear rate of 1.25 × 10-4mm3/(N×m)。
Example 4
The method of this embodiment is the same as embodiment 1 except that the energization time is 60 min.
The micro-arc oxidation film obtained by the embodiment has the thickness of 70 mu m, the hardness of 800HV, the friction coefficient of 0.6 and the wear rate of 2.125 × 10-4mm3/(N×m)。
The embodiment shows that the method can obviously improve the wear resistance of the surface of the high-phosphorus cast iron, and when the electrifying time is 50min, the wear rate is the lowest, so that the wear resistance can be greatly improved.
Example 5
The method of this example is the same as example 1, except that the energization time is 50min, a dispersion prepared from nano BN and ethanol is added to the electrolyte, and the concentration of nano BN in the dispersion is 50 g/mL.
The micro-arc oxidation film obtained by the embodiment has the thickness of 65 mu m, the hardness of 1050HV, the friction coefficient of 0.4 and the wear rate of 0.852 × 10-4mm3/(N×m)。
From the comparison of the wear rates of examples 3 and 5 with the matrix, it can be seen that the wear rate of example 5 is the smallest, and that the matrix is the largest after 3 applications. Therefore, the wear resistance of the high-phosphorus cast iron is really improved after hot dip aluminum plating and micro-arc oxidation treatment. The composite ceramic layer prepared by adding the dispersion prepared by nano BN and ethanol into the electrolyte has better wear resistance than a pure ceramic layer.
It is to be noted that the foregoing is only illustrative of the preferred embodiments of the present invention and the technical principles employed. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, although the present invention has been described in more detail by the above embodiments, the present invention is not limited to the above embodiments, and may include more other embodiments without departing from the spirit of the present invention, and the scope of the present invention is determined by the scope of the appended claims.
The invention is applicable to the prior art.

Claims (4)

1. A method for preparing a wear-resistant ceramic layer on the surface of high-phosphorus cast iron comprises the following steps:
(1) pretreating the high-phosphorus cast iron workpiece, and obtaining an aluminum-plated layer on the surface of the high-phosphorus cast iron workpiece by adopting a hot-dip aluminum plating mode; the specific process of the hot dip aluminum plating mode is as follows: the aluminum plating temperature is 710-;
(2) polishing the aluminized sample, ultrasonically cleaning the aluminized sample in alcohol, and drying the aluminized sample for later use; immersing the dried aluminum-plated sample into micro-arc oxidation electrolyte for micro-arc oxidation treatment to form an aluminum oxide ceramic layer on the surface of the aluminum-plated sample; the specific process of the micro-arc oxidation treatment comprises the following steps: an alternating current pulse power supply is adopted, positive voltage is controlled to be boosted to 400V from a 100V stage, negative voltage is controlled to be boosted to 140V from a 10V stage, processing time is 30-60min, frequency is 200Hz, and duty ratio is 40-60%; the electrolyte is prepared by mixing sodium silicate, sodium hexametaphosphate and potassium hydroxide according to the mass ratio of 5: 3: 2 dissolving in distilled water to obtain an aqueous solution;
the electrolyte during micro-arc oxidation is an aqueous solution consisting of 2g/L potassium hydroxide, 3g/L sodium hexametaphosphate and 5g/L sodium silicate.
2. The method for preparing the wear-resistant ceramic layer on the surface of the high-phosphorus cast iron according to claim 1, wherein a dispersion prepared from nano BN and ethanol is added into the electrolyte during the micro-arc oxidation treatment.
3. The method for preparing the wear-resistant ceramic layer on the surface of the high-phosphorus cast iron according to claim 1 or 2, wherein the aluminizing temperature is 730 ℃ and the immersion plating time is 3 min; the micro-arc oxidation treatment temperature is 25 +/-10 ℃.
4. The method for preparing a wear-resistant ceramic layer on the surface of high-phosphorus cast iron according to claim 2, wherein the concentration of the dispersion is 40-60 g/mL.
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