CN111235561A - Preparation method of high-performance Pb/Al coating - Google Patents
Preparation method of high-performance Pb/Al coating Download PDFInfo
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- CN111235561A CN111235561A CN201911340201.5A CN201911340201A CN111235561A CN 111235561 A CN111235561 A CN 111235561A CN 201911340201 A CN201911340201 A CN 201911340201A CN 111235561 A CN111235561 A CN 111235561A
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
Abstract
The invention relates to the technical field of aluminum alloy surface modification, in particular to a method for realizing surface lead alloying of a Pb/Al coating prepared by electron beam irradiation ball milling. Specifically, an Al block and Pb powder to be coated are put into a ball mill together for mixing and ball milling, a coating is prepared on the surface, and then an alloying layer with higher hardness and excellent wear resistance is prepared on the Al surface by adopting a method of combining a high-current pulse electron beam irradiation technology.
Description
Technical Field
The invention relates to the technical field of aluminum alloy surface modification, in particular to a method for realizing surface lead alloying of a Pb/Al coating prepared by electron beam irradiation ball milling. Specifically, an Al block and Pb powder to be coated are put into a ball mill together for mixing and ball milling, a coating is prepared on the surface, and then an alloying layer with higher hardness and excellent wear resistance is prepared on the Al surface by adopting a method of combining a high-current pulse electron beam irradiation technology.
Background
Because of high specific strength, good ductility, low density, excellent thermal and electrical conductivity, aluminum (Al) and its alloys have been widely used in various industries such as automotive, sports, aerospace, and electronics. However, low hardness, poor wear and corrosion resistance, etc. hinder further applications. To overcome these problems, surface alloying of Al with other metal elements is considered to be an effective method. As is well known, the homogeneous Al-Pb alloy is a common Al-based bearing alloy which takes a Pb phase as a lubricant component, has the characteristics of high specific strength and excellent frictional wear performance, is widely used as a substitute material of the Al-Sn bearing alloy, and is also an ideal material of a bearing bush of an automobile, a tractor and an internal combustion engine. The segregation problem in the aspect of Al-Pb alloy metallurgy caused by the wide liquid immiscible interval and large component density difference causes that the homogeneous Al-Pb alloy is difficult to synthesize by the conventional metallurgy method such as casting. Some studies show that the MA coating preparation method improves the Pb segregation to a certain extent, but the prepared coating is loose and porous, and meanwhile, the surface roughness is inevitably large, and the prepared coating is not metallurgically combined with a substrate. Therefore, the surface alloying process is only realized by non-equilibrium methods such as vapor deposition, ion implantation, laser beam, and the like. At present, vapor deposition, ion implantation, laser beam surface alloying technology and the like are all advanced on Al-Pb alloy to a certain extent, however, the vapor deposition has low bonding strength and certain air holes, the ion beam implantation has low production efficiency and the implantation system is complex and expensive, and the laser surface alloying technology has the problems of low energy utilization rate, high equipment running cost and the like.
Among various surface modification techniques, High Current Pulsed Electron Beam (HCPEB), which is a novel energy-carrying beam surface modification technique for materials, has recently proven to be an effective means for surface treatment of materials and has received a great deal of attention from material scientists, is higher in energy (10) during the transient period of pulsed electron beam bombardment of materials8-109W/cm2) In a very short time (nanoseconds to microseconds) on the surface of the material, causing extremely rapid heating and cooling of the material surface, even melting, evaporation and rapid solidification of the material surface, in the course of which induced stressesThe force field can cause rapid and intense deformation of the material surface, resulting in a particular modification effect. At the same time, many non-equilibrium microstructures such as supersaturated solid solutions, nanocrystals and amorphous phases can be formed in the modification layer, which is generally not possible with conventional methods. Extensive research has been conducted by many researchers using HCPEB radiation-induced surface alloying of thin film-substrate systems. Zou et Al found that after the surface alloying treatment of AISI H13 with Al, part of the pre-coat Al dissolved into the substrate to form a saturated surface alloy layer, and the high temperature oxidation resistance was greatly improved. Allain-Bonasso et Al studied the Ti/Al system, indicating that fairly good surface chemical uniformity was obtained after HCPEB irradiation. It was found by the inventors that the corrosion resistance of the irradiated W/Al system is significantly improved due to the W addition and the improved microstructure to form a more stable passivation film. Therefore, the HCPEB technology is a promising surface alloying method, can improve the properties of alloy surface hardness, wear resistance and the like, and has important effect on the application value of Al-Pb alloy.
Disclosure of Invention
In order to solve the problems in the background art, the invention aims to provide an Al-Pb alloy surface modification technology, so as to improve the surface property of the Al alloy and prolong the service life of the Al alloy in special environments.
The Al block and the required pure lead powder are put into a ball mill together for mixing and ball milling, and a layer of coating is prepared on the surface. The combined process can obviously improve the formation rate of a Pb film and the bonding strength with the matrix, also homogenize the distribution of Pb, solve the problem of serious segregation of Pb elements and finally improve the friction service life of the Al-Pb layer.
The technical scheme of the invention is as follows:
a treatment method for improving the alloying Al content and the frictional wear performance of the surface of a Pb/Al coating is characterized in that a combined process combining mechanical ball milling and electron beam treatment is combined to prepare a high-performance wear-resistant Pb/Al coating, a Pb coating is preset on the surface of an Al matrix through a mechanical mixing ball milling method of an Al block and Pb powder, then electron beam treatment is utilized to improve the surface density of the coating, metallurgical bonding of Al and Pb is realized, meanwhile, residual stress generated in the ball milling process is eliminated, and the hardness and the wear resistance of the material are improved.
The method specifically comprises the following steps:
(1) pretreatment of the surface of a substrate:
the present invention selects 1060 block pure aluminum as the substrate, cuts into aluminum block samples, all of which are mechanically polished with sandpaper and polished with diamond gypsum and ultrasonically cleaned in acetone, and then dries the aluminum block samples with a blower.
(2) Pre-setting a Pb coating:
the method adopts the powder raw material for preparing the coating as Pb powder, and under the protection of high-purity argon (Ar), the aluminum block sample prepared in the step (1) and the Pb powder are uniformly mixed and subjected to ball milling, so that the Pb powder is adhered to the surface of the aluminum block sample serving as the substrate to prepare the pure Pb coating. The MA process was carried out at a rotational speed of 250 r/min. At the same time, high purity argon is used as a shielding gas to avoid oxidation and contamination. The mixed system was ball milled at room temperature for 1 h. The milling time should not be too long in order to avoid damaging the matrix surface during the milling process. In addition, each ball milling is carried out for 20min, and then 10min is carried out, so as to prevent the temperature in the ball milling tank from being overhigh.
(3) Irradiation treatment by a high-current pulse electron beam:
fixing an aluminum block sample with a pure Pb coating prepared on the surface on an objective table, and vertically irradiating the surface of the Pb coating by using a HOPE-1 type high-current pulse electron beam device to obtain a Pb/Al alloy layer on the surface of an Al matrix sample.
The mechanical polishing in the step (1) sequentially adopts SiC sand paper with the specification of 150-3000 meshes, and the diamond gypsum polishing agent with the particle size of 0.5 mu m is selected as the polishing agent; the size of the aluminum block is 10 multiplied by 5 mm.
In the step (2), the ball milling process comprises the following steps: quenching steel balls and a stainless steel tank are adopted, the mass ratio of the ball materials is 10: 1-1.5, the rotating speed is 250r/min, and the ball milling time is 1 h; the purity of the Pb powder is 99.9 wt%, and the granularity is 200 meshes; the thickness of the prepared pure Pb coating was 10 μm.
The technical parameters of the irradiation of the high-current pulse electron beam in the step (3) are as follows: the electron beam acceleration voltage is 23.4kV, and the energy density is 3-4J/cm2The distance between the target source and the target source is 12-15cm, the pulse width is 0.5-5 mu s, and the vacuum degree is 3.5 multiplied by 10-3-5×10-3Pa, the irradiation times are 10-30 times.
Compared with the prior art, the invention has the following advantages:
first, the technical scheme of the invention has the advantages of low cost, short period, high efficiency and simple operation process, and plays an extremely important role in the practical application of Pb/Al alloy.
Secondly, the surface alloying of the high-current pulse electron beam is used as a novel surface modification technology, and has the unique advantages of high efficiency, simple operation steps, strong controllability and the like. Compared with the traditional manual coating, the distribution of the ball-milling powder is more uniform, and the surface bonding force between the coating and the surface of the substrate is larger and the coating is not easy to fall off. The HCPEB alloying is realized by utilizing the characteristic of HCPEB irradiation technology to cause chemical reaction between a matrix and alloying elements. After the action of the pulsed electron beam and the material, the temperature of the surface layer is rapidly raised, the substrate and the preset coating are simultaneously melted to form a remelting mixing layer, and then an alloy layer can be formed after rapid solidification, so that the surface mechanical, physical or chemical properties of the substrate, such as surface hardness, wear resistance, corrosion resistance and the like, are improved.
Drawings
FIG. 1 is an OM diagram of the sample surface before and after alloying by a high current pulsed electron beam according to the present invention; (a)10 times (b), 20 times (c) and 30 times.
FIG. 2 is a surface SEM image of 30 times of irradiation with high current pulsed electron beam according to the present invention;
FIG. 3 is a cross-sectional Scanning Electron Microscopy (SEM) analysis and EDS map of the present invention with high current pulsed electron beam irradiation 30 times;
FIG. 4 surface hardness of samples before and after HCPEB alloying;
FIG. 5 shows the friction coefficient and wear rate of the sample before and after alloying with the high current pulsed electron beam of the present invention: (a) coefficient of friction; (b) the rate of wear;
Detailed Description
In order that the invention may be more clearly understood, reference will now be made in detail to the following examples.
Example 1
(1) Preparing an alloy layer:
firstly, after cutting, pre-grinding, cleaning and polishing treatment are carried out on bulk pure aluminum of a substrate 1060, a pure Pb coating is deposited on the surface of the substrate 1060 by utilizing a mechanical coating technology, and the thickness of the Pb coating is 10 microns; selecting the ball material mass ratio as 10 according to the technical requirements of mechanical coating equipment: 1, the rotating speed is 250r/min, the time is 1h, and the coating thickness is 10 mu m.
Fixing the sample to be irradiated on an objective table, and vertically irradiating the surface of the preset coating by using a HOPE-1 type high-current pulse electron beam device so as to obtain a Pb/Al alloy layer on the surface of the Al matrix sample. Wherein, the irradiation technical parameters of the high current pulse electron beam are as follows: the electron beam energy was 23.4KeV and the energy density was 3.5J/cm2Target source distance 15cm, pulse width 1.5 mus, vacuum degree 5X 10-3Pa, and the irradiation times are 10 times.
(2) Alloy layer microstructure characterization and performance testing
The surface appearance of the treated sample is observed by a metallographic microscope (OM), and a small number of raised nodules and a small number of crater-shaped melting pits appear on the surface of the sample after the sample is irradiated by HCPEB for 10 times, the average size of the crater-shaped melting pits is about 30 mu m, shrinkage holes exist in the center of the melting pits, and in addition, some black pure Pb particles also exist.
The surface microhardness values of the sample before and after irradiation are tested by using a Vickers microhardness tester, and the test result shows that the hardness value of the surface of the sample after irradiation alloying is improved to some extent and is about 1.57 times of that of the original sample. The friction wear resistance of the samples before and after alloying is tested by a friction wear tester, and the friction coefficient of 10 times of radiation alloying samples is reduced from 0.95 of the original sample to 0.19, and the wear rate is reduced from 9.62 multiplied by 10-3mm3the/Nm is reduced to 6.38 multiplied by 10-3mm3the/Nm is obviously reduced compared with that before treatment. The size of the friction coefficient and the wear rate reflect the difficulty of the material in friction and wear, and the smaller the friction coefficient is, the lower the wear rate is, and the less the material is prone to wear. Therefore, the HCPEB surface alloying treatment improves the frictional wear performance of the Pb/Al alloy surface.
Example 2
(1) Preparing an alloy layer:
firstly, after cutting, pre-grinding, cleaning and polishing treatment are carried out on bulk pure aluminum of a substrate 1060, a pure Pb coating is deposited on the surface of the substrate 1060 by utilizing a mechanical coating technology, and the thickness of the Pb coating is 10 microns; selecting the ball material mass ratio as 10 according to the technical requirements of mechanical coating equipment: 1, the rotating speed is 250r/min, the time is 1h, and the coating thickness is 10 mu m.
Fixing the sample to be irradiated on an objective table, and vertically irradiating the surface of the preset coating by using a HOPE-1 type high-current pulse electron beam device so as to obtain a Pb/Al alloy layer on the surface of the Al matrix sample. Wherein, the irradiation technical parameters of the high current pulse electron beam are as follows: the electron beam energy was 23.4KeV and the energy density was 3.5J/cm2Target source distance 15cm, pulse width 1.5 mus, vacuum degree 5X 10-3Pa, and the irradiation times are 20 times.
(2) Alloy layer microstructure characterization and performance testing
And observing the surface appearance of the treated sample by using a metallographic microscope (OM), and finding that the number of surface melting pits is reduced and the size of the melting pits is obviously reduced after the sample is irradiated by HCPEB for 20 times, the average size is about 2 mu m, and a shrinkage cavity exists in the center of the melting pit. Further, the surface of the sample was observed, and it was found that the surface of the sample was covered with a large amount of dispersed gray particles. The surface of the material tends to be flattened, and the surface state is better than that of a 10-irradiation sample.
The surface microhardness values of the sample before and after irradiation are tested by using a Vickers microhardness tester, and the test result shows that the hardness value of the surface of the sample after irradiation alloying is improved to some extent and is about 1.92 times of that of the original sample. The friction wear resistance of the samples before and after alloying is tested by a friction wear instrument, and the friction coefficient of the 20 times of radiation alloying samples is reduced from 0.95 of the original sample to 0.15, and the wear rate is changed from 9.6210-3mm3the/Nm is reduced to 3.94 multiplied by 10-3mm3The reduction of/Nm is more obvious than that of the sample which is not irradiated for 10 times. The size of the friction coefficient and the wear rate reflect the difficulty of the material in friction and wear, and the smaller the friction coefficient is, the lower the wear rate is, and the less the material is prone to wear. Therefore, the HCPEB surface alloying treatment improves the frictional wear performance of the Pb/Al alloy surface.
Example 3
(1) Preparing an alloy layer:
firstly, after cutting, pre-grinding, cleaning and polishing treatment are carried out on bulk pure aluminum of a substrate 1060, a pure Pb coating is deposited on the surface of the substrate 1060 by utilizing a mechanical coating technology, and the thickness of the Pb coating is 10 microns; selecting the ball material mass ratio as 10 according to the technical requirements of mechanical coating equipment: 1, the rotating speed is 250r/min, the time is 1h, and the coating thickness is 10 mu m.
Fixing the sample to be irradiated on an objective table, and vertically irradiating the surface of the preset coating by using a HOPE-1 type high-current pulse electron beam device so as to obtain a Pb/Al alloy layer on the surface of the Al matrix sample. Wherein, the irradiation technical parameters of the high current pulse electron beam are as follows: the electron beam energy was 23.4KeV and the energy density was 3.5J/cm2Target source distance 15cm, pulse width 1.5 mus, vacuum degree 5X 10-3Pa, and the irradiation times are 30 times.
(2) Alloy layer microstructure characterization and performance testing
And observing the surface appearance of the treated sample by adopting a metallographic microscope (OM), and finding that the surface of the sample is smooth after the sample is irradiated by HCPEB for 30 times. The surface appearance of the sample is observed by adopting a Scanning Electron Microscope (SEM), and a large number of dispersed nano gray particles appear on the surface of the sample, and the nano gray particles contain 81.11% of Al and 18.89% of Pb through energy spectrum verification. Cross-sectional SEM pictures and EDS spectra of the bonded samples revealed that Pb was successfully metallurgically bonded to Al with an Al-Pb alloy layer thickness of about 12 μm.
The surface microhardness values of the sample before and after irradiation are tested by using a Vickers microhardness tester, and the test result shows that the hardness value of the surface of the sample after irradiation alloying is improved to some extent and is about 1.91 times of that of the original sample. Wear resistance of samples before and after alloying by using friction and wear instrumentThe test shows that the friction coefficient of 30 times of irradiation alloying samples is reduced to 0.13 from 0.95 of the original sample, and the wear rate is reduced to 9.62X 10-3mm3the/Nm is reduced to 1.34 multiplied by 10-3mm3the/Nm is obviously reduced compared with the original sample and the sample irradiated for 10 times and 20 times. The size of the friction coefficient and the wear rate reflect the difficulty of the material in friction and wear, and the smaller the friction coefficient is, the lower the wear rate is, and the less the material is prone to wear. Therefore, the HCPEB surface alloying treatment improves the frictional wear performance of the Pb/Al alloy surface. The significant improvement in frictional wear performance is caused by a number of factors. Firstly, the addition of Pb element on the surface of the sample after HCPEB irradiation plays an important role, and secondly, the increase of the surface hardness of the sample after irradiation is also beneficial to the improvement of frictional wear performance.
Claims (6)
1. A preparation method of a high-performance Pb/Al coating is characterized in that an Al block and pure lead powder are placed into a ball mill together for mixed ball milling, the Pb powder is embedded into the surface of an Al block matrix in advance to form a Pb film layer under the action of high-pressure impact force, and then the surface tissue structure of the alloy layer is adjusted through electron beam treatment, so that metallurgical bonding of Al and Pb is realized, residual stress generated in the ball milling process is eliminated, and the hardness and the wear resistance of the material are improved.
2. The method for preparing a high-performance Pb/Al coating according to claim 1, comprising the following steps:
(1) pretreatment of the surface of a substrate:
selecting 1060 block pure aluminum as a base material, cutting into aluminum block samples, mechanically polishing all the aluminum block samples by using sand paper, polishing by using diamond gypsum, ultrasonically cleaning in acetone, and drying the aluminum block samples by using a blower;
(2) pre-setting a Pb coating:
the powder raw material for preparing the coating is Pb powder, and the aluminum block sample prepared in the step (1) and the Pb powder are uniformly mixed and ball-milled under the protection of high-purity argon gas, so that the Pb powder is adhered to the surface of the aluminum block sample serving as the substrate to prepare a pure Pb coating;
(3) irradiation treatment by a high-current pulse electron beam:
fixing an aluminum block sample with a pure Pb coating prepared on the surface on an objective table, and vertically irradiating the surface of the Pb coating by using a HOPE-1 type high-current pulse electron beam device to obtain a Pb/Al alloy layer on the surface of an Al matrix sample.
3. The method for preparing a high-performance Pb/Al coating as claimed in claim 2, wherein in the step (1), SiC sand paper with specification of 150 and 3000 meshes is sequentially adopted for mechanical grinding, and diamond gypsum grinding agent with particle size of 0.5 μm is selected as the grinding agent; the size of the aluminum block is 10 multiplied by 5 mm.
4. The method for preparing a high-performance Pb/Al coating according to claim 2, wherein in the step (2), the ball milling process comprises: quenching steel balls and a stainless steel tank are adopted, the mass ratio of the ball materials is 10: 1-1.5, the rotating speed is 250r/min, and the ball milling time is 1 h; the purity of the Pb powder is 99.9 wt%, and the granularity is 200 meshes; the thickness of the prepared pure Pb coating is 10 mu m; the ball milling is carried out for 20min every time, and then the interval is 10min so as to prevent the temperature in the ball milling tank from being overhigh.
5. The method for preparing a high-performance Pb/Al coating according to claim 2, wherein in the step (3), the parameters of the high-current pulsed electron beam irradiation technology are as follows: the electron beam acceleration voltage is 23.4kV, and the energy density is 3-4J/cm2The distance between the target source and the target source is 12-15cm, the pulse width is 0.5-5 mu s, and the vacuum degree is 3.5 multiplied by 10-3-5×10-3Pa, the irradiation times are 10-30 times.
6. The method for preparing a high performance Pb/Al coating according to claim 2, wherein in the step (3), the electron beam energy is 23.4KeV and the energy density is 3.5J/cm2Target source distance 15cm, pulse width 1.5 mus, vacuum degree 5X 10-3Pa, and the irradiation times are 30 times.
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Application publication date: 20200605 |