CN112779532A - Method for preparing zirconium-based amorphous/nanocrystalline composite coating on surface of zirconium alloy - Google Patents
Method for preparing zirconium-based amorphous/nanocrystalline composite coating on surface of zirconium alloy Download PDFInfo
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- CN112779532A CN112779532A CN202110024343.1A CN202110024343A CN112779532A CN 112779532 A CN112779532 A CN 112779532A CN 202110024343 A CN202110024343 A CN 202110024343A CN 112779532 A CN112779532 A CN 112779532A
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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
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/106—Coating with metal alloys or metal elements only
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C16/00—Alloys based on zirconium
Abstract
The invention discloses a method for preparing a zirconium-based amorphous/nanocrystalline composite coating on the surface of a zirconium alloy, which comprises the following steps: (1) firstly, preprocessing a substrate, including polishing the surface to remove an oxide layer and impurities on the surface, and cleaning and drying the substrate by using alcohol or acetone; (2) carrying out cladding by adopting a preset powder method, wherein the laser power is as follows: 1200-: 4mm, scanning speed: 4-6mm/s, and the cladding time is as follows: 3-5 s; (3) carrying out laser remelting treatment on the clad coating: laser power: 800-: 4mm, scanning speed: 8-12mm/s, and the cladding time is as follows: 1-2 s. The preparation method has advanced process and accurate technical parameters, and is an advanced preparation method of the zirconium-based amorphous coating.
Description
Technical Field
The invention relates to an amorphous/nanocrystalline coating material, in particular to an amorphous/nanocrystalline composite coating material for strengthening the surface wear resistance of a zirconium alloy by laser cladding, and belongs to the technical field of composite coating materials.
Background
Zirconium alloys are solid solutions of zirconium or other metals. Zirconium has a very low thermal neutron absorption cross section, high hardness, ductility and corrosion resistance, and is mainly used in the field of nuclear technology, such as fuel rods in nuclear reactors and the like. Pure zirconium does not meet the requirements of nuclear fuel cladding and pressure pipe in terms of strength, wear resistance and corrosion resistance.
In recent years, researchers at home and abroad make use of the characteristics of laser rapid heating and rapid cooling to obtain some achievements and progresses in the aspect of preparing amorphous coatings with excellent performance on the surfaces of metal materials. The laser cladding process parameters have a large relationship with the amorphous coating structure, especially the amorphous content in the coating. Firstly, the non-uniform components in the coating are caused by the excessively low laser power, so that the amorphous formation is not facilitated, but the excessively high laser power causes the excessively high dilution rate of the coating and the crystallization is easy to occur, so that the amorphous content is reduced, and the amorphous content in the coating tends to decrease after the amorphous content in the coating increases to reach the peak value along with the increase of the laser power. Second, higher scan rates result in faster cooling of the bath and easier access to higher amorphous content. However, for an alloy system with stronger amorphous forming capability, a higher amorphous content can be obtained at a lower scanning speed, but the higher scanning speed leads to too short solidification time of a molten pool, so that alloy elements cannot be fully diffused to cause local component nonuniformity and deviate from the amorphous forming component range, thereby reducing amorphous components.
The laser remelting technology can improve the bonding performance of the coating, effectively eliminate the defects of cracks, air holes and the like, improve the defects of the air holes, the cracks and the like caused by laser cladding, and increase the amorphous content of the coating because the coating is rapidly cooled for the second time.
The Zr-based amorphous alloy has become one of the research hotspots in the amorphous field due to the high glass forming capability and excellent physical and chemical properties.
TIG Cladding + Laser Replacing of ZrAlNiCu Amorphous Coating discloses a preparation technology of a zirconium-based Amorphous Coating by TIG welding and Laser Remelting. The coating is an amorphous coating preparation technology combining the advantages of TIG electric arc and laser beam. Cladding Zr on carbon steel surface by TIG electric arc63.8Ni17.2Al11.4Cu7.6After the powder layer is formed, CO is used2And (4) laser remelting. TIG arcs facilitate good bonding and uniform solidification of the coating to the substrate. While the laser beam helps to cool rapidly to form an amorphous structure. The coating has a complex microstructure consisting of crystalline and amorphous states. XRD showed that TIG welding + laser remelting had a higher amorphous volume fraction than traditional laser cladding. Compared with the traditional laser cladding, the microhardness of the coating is improved by 1330MPa, the corrosion potential is improved by 0.07v, and the corrosion current is reduced by more than 10 times. However, because the solidification rate of the melt is extremely fast, the melt does not have sufficient time to homogenize, leaving voids and cracks in the coating, which can significantly degrade the performance of the laser cladding.
Structure and Properties of Zr-Based Metallic Glasses in As-case State and After Laser Welding disclose a technique for preparing a zirconium-Based amorphous coating by casting and Laser Welding. The coating has an amorphous phase in the fusion zone and an amorphous phase in the heat affected zone. Laser welding was demonstrated to have higher nano-hardness and lower Young's modulus values with higher pulse energy (2.78J) and pulse peak power (1000W). However, the constituent elements of zirconium-based alloys are characterized by a high affinity for oxygen, resulting in more impurities in the alloy, easier pore formation and increased crystalline phases, which ultimately leads to a reduction in the glass forming ability and a poorer wear resistance of the coating.
Disclosure of Invention
The invention aims to provide a preparation method of a laser cladding and laser remelting zirconium-based amorphous/nanocrystalline composite coating material, which improves the hardness of the surface of a zirconium alloy, obtains a coating without holes and cracks and with fine grains, and further improves the wear resistance of the coating.
The laser remelting can improve the bonding performance of the coating, effectively eliminate the defects of cracks, air holes and the like, and eliminateThe defects of air holes, cracks and the like caused in the laser cladding process, and simultaneously, the amorphous content of the coating can be increased because the coating is rapidly cooled for the second time. The invention utilizes laser cladding and laser remelting to improve the amorphous content of the zirconium-based amorphous composite coating, thereby greatly improving the hardness and the wear resistance of the coating. In the laser cladding process, intermetallic compound Al is generated in situ through the interaction between elements in the powder2Zr3，CuZr2And Zr2A Ni reinforcing phase, and a Zr-Ni-Al-Cu system has larger chaos and long-range disorder, so that an amorphous/nanocrystalline composite coating is obtained; the coating is divided into 3 layers, an amorphous layer on the outermost layer, an amorphous-nanocrystalline composite layer in the middle layer and a crystal phase layer at the bottom. The formation of the composite coating structure means the complexity of solidification behavior in laser cladding, which is controlled not only by the melting and mass transfer characteristics of the coating material and the substrate, but also has a great relationship with the crystallographic characteristics thereof. In the cooling and solidification process of a molten pool, each element has no time to perform long-range diffusion and component redistribution, so that only short-range diffusion and combination can be performed, and thus, the amorphous which is difficult to form by the conventional process is formed at the optimal amorphous forming component point (surface layer); when the melted coating material makes the surface of the substrate micro-melted through heat conduction, the instability of the crystal boundary structure of the metal of the substrate causes the actual melting point to change microscopically, so that the liquid/solid interface generates uneven fluctuation on the micro scale, and the melted edge crystal grains are in a semi-melting state; during the subsequent solidification process, these semi-molten grains will become the core of new grain growth; the crystal has a great nucleation speed due to the favorable positions of a plurality of nucleation on the same substrate crystal grain, and the crystal extends and grows to the inside of a molten pool in a columnar crystal form along the direction of maximum heat dissipation; in the process of growing the columnar crystal, because the enhancement of the convection disturbance effect of the alloy melt and the reduction of the dilution degree, the growth of the columnar crystal is inhibited, and the size of the crystal grain is reduced; instead, an amorphous-nanocrystalline composite layer with a near crystalline structure and solid solution formation forms the middle layer and the bottom crystalline phase layer.
The invention provides a method for preparing a zirconium-based amorphous/nanocrystalline composite coating on the surface of a zirconium alloy, which comprises the following steps:
(1) firstly, preprocessing a substrate, including polishing the surface to remove an oxide layer and impurities on the surface, and cleaning and drying the substrate by using alcohol or acetone;
(2) adopting preset powder to clad, wherein the laser power is as follows: 1200-: 4mm, scanning speed: 4-6mm/s, and the cladding time is as follows: 3-5 s;
(3) carrying out laser remelting treatment on the clad coating: laser power: 800-: 4mm, scanning speed: 8-12mm/s, and the cladding time is as follows: 1-2 s.
In the laser cladding process, intermetallic compound Al is generated in situ through the interaction between elements in the powder2Zr3，CuZr2And Zr2The Ni reinforcing phase has larger size difference of Zr and Ni atoms, smaller size difference of Ni and Cu atoms, and larger disorder degree and long-range disorder of a Zr-Ni-Al-Cu system, so that the amorphous/nanocrystalline composite coating is obtained. The coating is divided into 3 layers, an amorphous layer on the outermost layer, an amorphous-nanocrystalline composite layer in the middle layer and a crystal phase layer at the bottom.
In the preset powder method, the cladding powder is prepared by mixing the following raw materials in atomic number percentage:
60-65% of Zr powder (purity 99.5%), 15-20% of Ni powder (purity 99.5%), 10-15% of Cu powder (purity 99.5%) and 10-15% of Al powder (purity 99.5%).
The preferable cladding powder proportion is as follows: zr powder 63.5%, Ni powder 15.1%, Al powder 10.7%, Cu powder 10.7% to obtain Zr63.5Ni15.1Al10.7Cu10.7And (3) alloying powder.
Specifically, the granularity of Zr powder, Al powder, Ni powder and Cu powder in the cladding powder is preferably 100-200 meshes.
Zr according to the invention63.5Ni15.1Al10.7Cu10.7The alloy powder is obtained by fully mixing the various powder materials in a QM-3SP4 planetary ball mill, wherein the ball milling speed is 500r/min, the ball milling time is 2 hours, the vacuum drying is carried out for 1-2 hours, the temperature is 50 ℃, and the alloy powder is naturally cooled.
The invention has the beneficial effects that:
(1) compared with the prior art, the invention has obvious advancement of 702 zirconium plate hardness (178 HV)0.2) Under the conditions of low content, poor wear resistance and short service life, the zirconium-based amorphous composite coating is laser-cladded on the surface of the 702 zirconium plate so as to improve the surface hardness, wear resistance and amorphous content of the stainless steel plate, and the hardness reaches 850.7HV0.2The wear resistance is improved by more than 4 times;
(2) the laser remelting can repair cracks, holes and unmelted solid particles on the surface of the coating, reduce the dilution rate of the coating, improve the quality of the coating and improve the amorphous proportion;
(3) the preparation method has advanced process and accurate technical parameters, and is an advanced preparation method of the zirconium-based amorphous coating.
Drawings
FIG. 1 is a graph comparing hardness of various examples and comparative examples;
FIG. 2 is a graph comparing the wear rates of various examples, comparative examples, and substrates;
FIG. 3 is a sectional SEM image of a cladding layer in example 1;
FIG. 4 is a sectional scanning electron micrograph of a cladding layer of comparative example 1.
Detailed Description
In order that the objects, features and effects of the invention may be more fully realized and more readily understood, the invention will now be further described with reference to the following specific examples. The examples are not intended to limit the invention in any way. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Example 1
Firstly, drying zirconium powder with the granularity of 200 meshes for 12 hours at the temperature of 50 ℃ in a vacuum environment, then weighing 75.87gZr powder, 11.37gNi powder, 3.79gAl powder and 8.94gCu powder with the granularity of 200 meshes, fully mixing various powder materials in a QM-3SP4 planetary ball mill at the ball milling speed of 500r/min for 2 hours, drying in vacuum for 2 hours at the temperature of 50 ℃, and naturally cooling to obtain the mixed powder for laser cladding. In the cladding powder, the granularity of the Zr powder, the Al powder, the Ni powder and the Cu powder is 100-200 meshes, and the purity is 99.5%.
A702 zirconium block sample with the specification of 20 multiplied by 10mm is taken, the surface of the sample is subjected to coarse grinding treatment by 180-mesh metallographic abrasive paper, then the sample is cleaned by acetone to remove oil stains, wiped clean, wiped by alcohol and dried by blowing, and the pretreated zirconium alloy base material is obtained.
And placing the zirconium alloy sample subjected to surface treatment on a laser cladding workbench for later use, and using argon as a protective gas.
Adopting a laser cladding method of pre-laying powder, pre-laying the mixed alloy powder on the surface of a substrate, and adjusting laser cladding technological parameters as follows: laser power is 1800W, the diameter of a light spot is 4mm, the scanning speed is 5mm/s, and the cladding time is 4 s; and generating a coating which is metallurgically bonded with the substrate on the surface of the zirconium alloy under the irradiation of laser energy.
Carrying out laser remelting treatment on the clad coating: the laser power is 1300W, the diameter of a light spot is 4mm, the scanning speed is 10mm/s, and the cladding time is 2 s.
The Vickers hardness was measured with a JMHVS-1000AT precision automatic turret digital display microhardness tester. The indenter material is diamond and is in a regular pyramid shape, the loading load is 500g, the load retention time is 10s, the hardness is sequentially dotted from the coating to the substrate direction, and the relationship between the measured hardness value and the distance from the surface of the coating is drawn into a curve, wherein the curve is shown in figure 1. Hardness of the matrix is 178HV0.2。
The friction and wear test of the test specimens was carried out on a MG-2000 model testing machine. In the test, YG6 hard alloy with the hardness of 63-64 HRC is selected as a grinding wheel, the rotating speed is 500r/min, the abrasion time is 20min, and the test load is 20N. After the experiment is finished, the MT-500 type probe material surface wear mark measuring instrument is used for measuring the wear rate, the smaller the wear rate is, the better the high-temperature wear resistance of the coating cladding layer is, and the wear rate result is shown in figure 2.
Comparative example 1
And taking the matrix and the powder in the first embodiment, and cladding by using the laser cladding process parameters of the first embodiment 1. And generating a coating which is metallurgically bonded with the substrate on the surface of the zirconium alloy under the irradiation of laser energy. Laser remelting treatment is not carried out.
The hardness and wear resistance of the cladding layer were measured according to the test method of example 1. The hardness profile is shown in figure 1 and the wear rate results are shown in figure 2.
Example 2
Taking the matrix and the powder in the embodiment 1, and adjusting the laser cladding process parameters as follows: laser power 1600W, spot diameter 4mm, scanning speed 5 mm/s. And generating a coating which is metallurgically bonded with the substrate on the surface of the zirconium alloy under the irradiation of laser energy.
And (3) carrying out laser remelting treatment on the coating after cladding, wherein the laser remelting process parameters are the same as those of the embodiment 1.
The hardness and wear resistance of the cladding layer were measured according to the test method of example 1. The hardness profile is shown in figure 1 and the wear rate results are shown in figure 2.
Comparative example 2
Taking the matrix and the powder in the first embodiment, and adjusting the laser cladding process parameters as follows: the laser power is 2500W, the spot diameter is 4mm, and the scanning speed is 5 mm/s. And generating a coating which is metallurgically bonded with the substrate on the surface of the zirconium alloy under the irradiation of laser energy.
And (3) carrying out laser remelting treatment on the coating after cladding, wherein the laser remelting process parameters are the same as those of the embodiment 1.
The hardness and wear resistance of the cladding layer were measured according to the test method of example 1. The hardness profile is shown in figure 1 and the wear rate results are shown in figure 2.
Experimental example 3
And taking the matrix and the powder in the example 1, and cladding by using the laser cladding process parameters of the example 1. And generating a coating which is metallurgically bonded with the substrate on the surface of the zirconium alloy under the irradiation of laser energy.
Carrying out laser remelting treatment on the clad coating: the laser power is 1500W, the spot diameter is 4mm, and the scanning speed is 12 mm/s.
Comparative example 3
Weighing 80gZr powder, 11gNi powder, 3gAl powder and 6gCu powder with the granularity of 200 meshes, adding the materials into a ball mill, and mixing for 2 hours to obtain the mixed powder for laser cladding.
The substrate was pretreated in the same manner as in example 1.
And placing the zirconium alloy sample subjected to surface treatment on a laser cladding workbench for later use, and using argon as a protective gas.
According to the same laser cladding process parameters of the embodiment 1, under the irradiation of laser energy, a coating which is metallurgically bonded with the substrate is generated on the surface of the zirconium alloy.
And (3) carrying out laser remelting treatment on the coating after cladding, wherein the laser remelting process parameters are the same as those of the embodiment 1.
The hardness and wear resistance of the cladding layer were measured according to the test method of example 1. The hardness profile is shown in figure 1 and the wear rate results are shown in figure 2.
Fig. 1 shows the hardness of each of the examples and the comparative examples. As can be seen from the graph, the hardness (850.7 HV) of example 10.2) Hardness of the substrate (178 HV)0.2) The improvement is more than 4 times, and the improvement is great.
Fig. 2 shows wear rates of the respective examples and comparative examples. It can be seen from the graph that the wear rate of example 1 was the lowest (0.21), and was greatly improved compared to the other cases and the base body.
Fig. 3 shows the scanning electron microscope image of example 1, and it can be seen that there are a lot of amorphous parts in the image, which indicates that there is a lot of amorphous phase, because each element has no time to diffuse and redistribute the components in the cooling and solidification process of the molten pool, and thus diffusion and combination can be performed only in a short distance, thereby forming amorphous. FIG. 4 shows a scanning electron micrograph of comparative example 1, in which a small amount of amorphous portions are present and thus an amorphous phase is small, and only a small amount of amorphous phase is generated as compared with FIG. 3.
Claims (6)
1. A method for preparing a zirconium-based amorphous/nanocrystalline composite coating on the surface of a zirconium alloy is characterized by comprising the following steps:
(1) firstly, preprocessing a substrate, including polishing the surface to remove an oxide layer and impurities on the surface, and cleaning and drying the substrate by using alcohol or acetone;
(2) carrying out cladding by adopting a preset powder method, wherein the laser power is as follows: 1200-: 4mm, scanning speed: 4-6mm/s, and the cladding time is as follows: 3-5 s;
(3) carrying out laser remelting treatment on the clad coating: laser power: 800-: 4mm, scanning speed: 8-12mm/s, and the cladding time is as follows: 1-2 s.
2. The method for preparing the zirconium-based amorphous/nanocrystalline composite coating on the surface of the zirconium alloy according to claim 1, characterized in that: in the laser cladding process, intermetallic compound Al is generated in situ through the interaction between elements in the powder2Zr3，CuZr2And Zr2A Ni reinforcing phase, and a Zr-Ni-Al-Cu system has larger chaos and long-range disorder, so that an amorphous/nanocrystalline composite coating is obtained; the coating is divided into 3 layers, an amorphous layer on the outermost layer, an amorphous-nanocrystalline composite layer in the middle layer and a crystal phase layer at the bottom.
3. The method for preparing the zirconium-based amorphous/nanocrystalline composite coating on the surface of the zirconium alloy according to claim 1, characterized in that: in the preset powder method, the cladding powder is prepared by mixing the following raw materials in atomic number percentage:
60-65% of Zr powder, 15-20% of Ni powder, 10-15% of Cu powder and 10-15% of Al powder.
4. The method for preparing the zirconium-based amorphous/nanocrystalline composite coating on the surface of the zirconium alloy according to claim 3, characterized in that: the cladding powder comprises the following components in percentage by weight: 63.5% of Zr powder, 15.1% of Ni powder, 10.7% of Al powder and 10.7% of Cu powder.
5. The method for preparing the zirconium-based amorphous/nanocrystalline composite coating on the surface of the zirconium alloy according to claim 3 or 4, characterized in that: in the cladding powder, the granularity of the Zr powder, the Al powder, the Ni powder and the Cu powder is 100-200 meshes, and the purity is 99.5%.
6. The method for preparing the zirconium-based amorphous/nanocrystalline composite coating on the surface of the zirconium alloy according to claim 3 or 4, characterized in that: the material is obtained by fully mixing various powder materials in a ball mill, wherein the ball milling speed is 500r/min, the ball milling time is 2 hours, the vacuum drying is carried out for 1-2 hours, the temperature is 50 ℃, and the natural cooling is carried out.
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| CN113265614A (en) * | 2021-05-14 | 2021-08-17 | 安徽智模新材料科技有限公司 | Manufacturing method of long-life hot forging steel piston die |
| CN113351372A (en) * | 2021-06-07 | 2021-09-07 | 珠海格力电器股份有限公司 | Zr-based amorphous coating, preparation process thereof and application thereof in electric purification |
| CN115478193A (en) * | 2022-09-16 | 2022-12-16 | 中南大学 | Amorphous-crystal dual-phase structure degradable ZnZr alloy and preparation method thereof |
| CN116770301A (en) * | 2023-08-23 | 2023-09-19 | 南京工业大学 | Zirconium-based amorphous alloy-aluminum alloy composite material coating and preparation method thereof |
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| CN116770301B (en) * | 2023-08-23 | 2023-10-27 | 南京工业大学 | Zirconium-based amorphous alloy-aluminum alloy composite material coating and preparation method thereof |
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Application publication date: 20210511 |