CN111945099A - Preparation method of CoCrFeNi high-entropy alloy coating - Google Patents
Preparation method of CoCrFeNi high-entropy alloy coating Download PDFInfo
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- CN111945099A CN111945099A CN202010911375.9A CN202010911375A CN111945099A CN 111945099 A CN111945099 A CN 111945099A CN 202010911375 A CN202010911375 A CN 202010911375A CN 111945099 A CN111945099 A CN 111945099A
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/129—Flame spraying
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/08—Metallic material containing only metal elements
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Abstract
The invention relates to a preparation method of a CoCrFeNi high-entropy alloy coating, which comprises the following steps: the method comprises the steps of pretreating a substrate, fully melting CoCrFeNi high-entropy alloy powder in acetylene-oxygen combustion high-temperature flame by using a subsonic flame spraying technology, and spraying the molten CoCrFeNi high-entropy alloy on the surface of the pretreated substrate to obtain the CoCrFeNi high-entropy alloy coating. The method is simple in process and suitable for industrial production, and the obtained coating has the microhardness of Hv 400-600 and good wear-resistant and friction-reducing properties, overcomes the defects of the traditional single alloy, and has wide application prospects in the fields of wear resistance and corrosion resistance.
Description
Technical Field
The invention relates to the technical field of surface engineering, in particular to a preparation method of a CoCrFeNi high-entropy alloy coating.
Background
A substance having a metallic property, which is synthesized from two or more metals and metals or metals and nonmetals by a certain method, is called an alloy. Bronze (copper-tin alloy) is the earliest alloy, and as early as the business era (about 3000 years to date), the process for making bronze has been very developed. With the research of alloy systems approaching saturation in recent years, scholars have missed a novel alloy design concept in 1995, namely a multielement high-entropy alloy.
The multi-element high-entropy alloy generally consists of 5 or more than 5 main elements which are arranged in a nearly equal atomic ratio or atomic ratio mode. The high-entropy alloy has a high-entropy effect, a distortion effect, a delayed diffusion effect and a cocktail effect, and the effects enable the high-entropy alloy to form a simple solid solution structure, a nano structure or even an amorphous structure more easily, so that the high-entropy alloy has excellent mechanical properties (compression, tensile strength, hardness and the like), thermodynamic stability, excellent performances such as wear resistance, high-temperature oxidation resistance and corrosion resistance, which are incomparable with the traditional alloy. Currently, high entropy alloys have been used in a variety of fields, such as for tool manufacturing materials (cutters, golf club heads), aerospace materials, and high frequency soft magnetic materials. In recent years, researches on high-entropy alloy coating materials are widely concerned by researchers due to the fact that high-entropy alloy overall materials are high in material consumption and high in manufacturing cost.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a CoCrFeNi high-entropy alloy coating, which is simple in process and suitable for industrial production.
In order to solve the problems, the preparation method of the CoCrFeNi high-entropy alloy coating is characterized by comprising the following steps: the method comprises the steps of pretreating a substrate, fully melting CoCrFeNi high-entropy alloy powder in acetylene-oxygen combustion high-temperature flame by using a subsonic flame spraying technology, and spraying the molten CoCrFeNi high-entropy alloy on the surface of the pretreated substrate to obtain the CoCrFeNi high-entropy alloy coating.
The base body is made of steel with different grades.
The pretreatment is to remove oil on the surface of the base material by using a weakly acidic water-based oil removal agent, then sequentially perform polishing and rust removal, distilled water washing, acetone solution secondary washing and finally adopt corundum for sand blasting.
The CoCrFeNi high-entropy alloy powder is prepared by mixing Fe, Co, Cr and Ni raw materials with the purity higher than 99.9% according to the molar equivalent or the proportion that the atomic percentage of each element is between 5 and 35 percent and the total content is 100 percent, and preparing the powder with the granularity of 15 to 45 mu m through arc melting or vacuum induction melting and vacuum gas atomization cooling.
The subsonic flame spraying conditions comprise that the acetylene pressure is 0.06-0.09 MPa, the oxygen pressure is 0.01-0.04 MPa, the powder feeding pressure is 0.05-0.09 MPa, an intermittent spraying mode is adopted, the spraying frequency is 4-8 times, and the interval between the previous spraying and the next spraying is 2-6 seconds.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, CoCrFeNi powder containing an FCC-CoCrFeNi phase, with the granularity of 15-45 mu m and the purity of more than 99.9% is used as a raw material (as shown in figure 1), and a CoCrFeNi high-entropy alloy coating containing the FCC-CoCrFeNi phase is prepared by a subsonic flame spraying technology, and a chromium oxide ceramic phase structure is compounded in situ, so that the wear resistance of the coating under a boundary lubrication condition is enhanced (as shown in figure 2).
2. The main body phase of the high-entropy alloy coating prepared by the invention has a face-centered cubic structure, contains an oxide ceramic reinforcing phase, has the microhardness of Hv 400-600 and good wear-resistant and friction-reducing properties, makes up for the defects of the traditional single alloy, and has wide application prospects in the fields of wear resistance and corrosion resistance.
[ evaluation of Properties ]
The CoCrFeNi high-entropy alloy coating obtained by the invention is subjected to a friction wear test:
a fretting friction wear testing machine is adopted, and a ball-disc reciprocating mode is adopted as a friction condition. The CoCrFeNi high-entropy alloy coating and a commercially available GCr15 steel ball with the diameter of 10mm form a friction matching pair as a dual ball, the test environment is atmosphere, and the test conditions are as follows: the load was 25N, the reciprocation frequency was 45 Hz, the amplitude was 1 mm, and the lubricant was liquid paraffin.
The test results are shown in FIGS. 3 to 4. As can be seen from FIG. 3, the initial coefficient of friction of the coating was 0.18, then rapidly became 0.14, then exhibited a slow decline of 0.12 to 0.13 at a friction time of 25min, and the lowest average coefficient of friction of the coating under paraffin lubrication was 0.124643. As can be seen from FIG. 4, the coating has shallow grinding marks and better abrasion resistance, and is lubricated under the condition of paraffinThe loss volume of the coating is as low as 4.91761 x 10-4 mm3. Therefore, under the condition of paraffin lubrication, the CoCrFeNi high-entropy alloy coating obtained by the invention has a low friction coefficient and excellent wear resistance.
3. The method is simple and easy to realize, can be sprayed on the surfaces of different parts, is suitable for industrial production, and has potential application prospect in the environment of wear resistance and friction reduction of a mechanical motion system.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is an XRD spectrum of a raw material CoCrFeNi powder for spraying a CoCrFeNi high-entropy alloy coating.
FIG. 2 is an XRD spectrum of the CoCrFeNi high-entropy alloy coating.
FIG. 3 is a graph of the change of the friction coefficient of the CoCrFeNi high-entropy alloy coating with time under the condition of liquid paraffin lubrication.
FIG. 4 is a 3D topography of a grinding crack of the CoCrFeNi high-entropy alloy coating under the condition of liquid paraffin lubrication.
Detailed Description
A preparation method of a CoCrFeNi high-entropy alloy coating comprises the following steps: the method comprises the steps of pretreating a substrate, fully melting CoCrFeNi high-entropy alloy powder in acetylene-oxygen combustion high-temperature flame by using a subsonic flame spraying technology, and spraying the molten CoCrFeNi high-entropy alloy on the surface of the pretreated substrate to obtain the CoCrFeNi high-entropy alloy coating.
Wherein: the material of the substrate is steel with various grades, such as 45-grade steel, 30CrMo, 1Cr18Ni9Ti and the like.
The pretreatment comprises removing oil on the surface of the base material by using a weakly acidic water-based oil removing agent, polishing, removing rust, washing with distilled water, washing with acetone solution for the second time, and finally using corundum (the main component is molten white Al)2O3Particles) are blasted.
The CoCrFeNi high-entropy alloy powder is commercial powder with the granularity of 15-45 mu m prepared by mixing Fe, Co, Cr and Ni raw materials with the purity higher than 99.9% according to the molar equivalent or the proportion that the atomic percentage of each element is between 5-35% and the total content is 100%, and carrying out arc melting or vacuum induction melting and vacuum gas atomization cooling. The specific preparation method can be carried out according to a method published by a literature: https:// cn. made-in-china. com/gongying/bjyb321-kvumwqxAJTYC. html; http:// www.bjybxc.com/; http:// www.xincailiao.com/news/news _ detail. aspx _ id = 562927. As shown in figure 1, the main phase of the CoCrFeNi high-entropy alloy powder is a single face-centered cubic structure high-entropy alloy solid solution which contains an FCC-CoCrFeNi phase and has the purity of more than 99.9 percent.
The subsonic flame spraying conditions comprise that the acetylene pressure is 0.06-0.09 MPa, the oxygen pressure is 0.01-0.04 MPa, the powder feeding pressure is 0.05-0.09 MPa, an intermittent spraying mode is adopted, the spraying frequency is 4-8 times, and the interval between the previous spraying and the next spraying is 2-6 seconds.
Embodiment 1 a method for preparing a CoCrFeNi high-entropy alloy coating:
the 45# steel substrate was processed into round block specimens with dimensions Φ 24mm × 8mm, followed by pretreatment. The specific process is as follows: the method comprises the steps of firstly removing oil from a base material by using a weakly acidic water-based oil removal agent, then sequentially carrying out polishing rust removal, washing by using distilled water, washing by using an acetone solvent for the second time, and finally carrying out sand blasting by using corundum. The whole washing process is carried out under ultrasonic oscillation.
After pretreatment, high-purity CoCrFeNi powder is melted by a Y16258 type spray gun by using a subsonic flame spraying technology and sprayed to the surface of the matrix in an atmospheric environment. The main spraying gas is acetylene and the auxiliary gas is oxygen; the purity of the introduced acetylene and oxygen is more than 99.99 percent, and the powder feeding gas is compressed air. The acetylene pressure used for spraying is 0.07-0.08 MPa, the oxygen pressure is 0.02-0.03 MPa, the powder feeding pressure is 0.06-0.07 MPa, the spraying distance is 150-350 mm, an intermittent spraying mode is adopted, the spraying frequency is 6 times, and the interval between the front spraying and the back spraying is 2-6 s. And (5) obtaining the CoCrFeNi high-entropy alloy coating after spraying, as shown in figure 2. From FIG. 2, it can be found that the main phases of the coating are a face-centered cubic structure high-entropy alloy solid solution and an oxide ceramic phase of the high-entropy alloy.
Embodiment 2 a method for preparing a CoCrFeNi high-entropy alloy coating:
the substrate was pretreated in the same manner as in example 1.
After pretreatment, high-purity CoCrFeNi powder is melted by a Y16258 type spray gun by using a subsonic flame spraying technology and sprayed to the surface of the matrix in an atmospheric environment. The main spraying gas is acetylene and the auxiliary gas is oxygen; the purity of the introduced acetylene and oxygen is more than 99.99 percent, and the powder feeding gas is compressed air. The acetylene pressure used for spraying is 0.06-0.07 MPa, the oxygen pressure is 0.01-0.02 MPa, the powder feeding pressure is 0.05-0.06 MPa, the spraying distance is 150-350 mm, an intermittent spraying mode is adopted, the spraying frequency is 8 times, and the interval between the front spraying and the back spraying is 2-6 s. And obtaining the CoCrFeNi high-entropy alloy coating after spraying.
Embodiment 3 a method for preparing a CoCrFeNi high-entropy alloy coating:
the substrate was pretreated in the same manner as in example 1.
After pretreatment, high-purity CoCrFeNi powder is melted by a Y16258 type spray gun by using a subsonic flame spraying technology and sprayed to the surface of the matrix in an atmospheric environment. The main spraying gas is acetylene and the auxiliary gas is oxygen; the purity of the introduced acetylene and oxygen is more than 99.99 percent, and the powder feeding gas is compressed air. The acetylene flow rate used for spraying is 0.08-0.09 MPa, the oxygen flow rate is 0.03-0.04 MPa, the powder feeding pressure is 0.07-0.09 MPa, the spraying distance is 150-350 mm, an intermittent spraying mode is adopted, the spraying frequency is 4 times, and the interval between the previous spraying and the next spraying is 2-6 s. And obtaining the CoCrFeNi high-entropy alloy coating after spraying.
When the coating is applied, once the acetylene pressure, the oxygen pressure and the powder feeding gas pressure exceed the ranges described in the invention, although the main structure of the obtained coating is kept unchanged, the structural characteristics such as pore distribution, lattice distortion and the like and the wear resistance of the coating are greatly changed under the influence of the molten state and the content of oxides, and under the same friction and wear experimental conditions, the wear rate of the coating is increased to 5-8 times or more of that of the coating obtained in the above example.
Claims (5)
1. A preparation method of a CoCrFeNi high-entropy alloy coating is characterized by comprising the following steps: the method comprises the steps of pretreating a substrate, fully melting CoCrFeNi high-entropy alloy powder in acetylene-oxygen combustion high-temperature flame by using a subsonic flame spraying technology, and spraying the molten CoCrFeNi high-entropy alloy on the surface of the pretreated substrate to obtain the CoCrFeNi high-entropy alloy coating.
2. The preparation method of the CoCrFeNi high-entropy alloy coating as claimed in claim 1, characterized in that: the base body is made of steel with different grades.
3. The preparation method of the CoCrFeNi high-entropy alloy coating as claimed in claim 1, characterized in that: the pretreatment is to remove oil on the surface of the base material by using a weakly acidic water-based oil removal agent, then sequentially perform polishing and rust removal, distilled water washing, acetone solution secondary washing and finally adopt corundum for sand blasting.
4. The preparation method of the CoCrFeNi high-entropy alloy coating as claimed in claim 1, characterized in that: the CoCrFeNi high-entropy alloy powder is prepared by mixing Fe, Co, Cr and Ni raw materials with the purity higher than 99.9% according to the molar equivalent or the proportion that the atomic percentage of each element is between 5 and 35 percent and the total content is 100 percent, and preparing the powder with the granularity of 15 to 45 mu m through arc melting or vacuum induction melting and vacuum gas atomization cooling.
5. The preparation method of the CoCrFeNi high-entropy alloy coating as claimed in claim 1, characterized in that: the subsonic flame spraying conditions comprise that the acetylene pressure is 0.06-0.09 MPa, the oxygen pressure is 0.01-0.04 MPa, the powder feeding pressure is 0.05-0.09 MPa, an intermittent spraying mode is adopted, the spraying frequency is 4-8 times, and the interval between the previous spraying and the next spraying is 2-6 seconds.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113430513A (en) * | 2021-06-28 | 2021-09-24 | 山东理工大学 | Preparation method of magnesium alloy surface cold spraying high-entropy alloy coating |
| CN113444960A (en) * | 2021-06-29 | 2021-09-28 | 哈尔滨工业大学 | Unequal atomic ratio CoCrFeNiMoxHigh-entropy alloy and preparation method thereof |
| CN113445041A (en) * | 2021-07-15 | 2021-09-28 | 山东理工大学 | Preparation method of low-cost light high-entropy alloy/aluminum oxide composite coating on surface of magnesium alloy |
| CN115418595A (en) * | 2022-08-18 | 2022-12-02 | 中国科学院兰州化学物理研究所 | Cavitation-corrosion-resistant high-entropy alloy coating and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113430513A (en) * | 2021-06-28 | 2021-09-24 | 山东理工大学 | Preparation method of magnesium alloy surface cold spraying high-entropy alloy coating |
| CN113444960A (en) * | 2021-06-29 | 2021-09-28 | 哈尔滨工业大学 | Unequal atomic ratio CoCrFeNiMoxHigh-entropy alloy and preparation method thereof |
| CN113445041A (en) * | 2021-07-15 | 2021-09-28 | 山东理工大学 | Preparation method of low-cost light high-entropy alloy/aluminum oxide composite coating on surface of magnesium alloy |
| CN113445041B (en) * | 2021-07-15 | 2022-02-25 | 山东理工大学 | Preparation method of low-cost light high-entropy alloy/aluminum oxide composite coating on surface of magnesium alloy |
| CN115418595A (en) * | 2022-08-18 | 2022-12-02 | 中国科学院兰州化学物理研究所 | Cavitation-corrosion-resistant high-entropy alloy coating and preparation method thereof |
| CN115418595B (en) * | 2022-08-18 | 2023-11-07 | 中国科学院兰州化学物理研究所 | Cavitation erosion-corrosion resistant high-entropy alloy coating and preparation method thereof |
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