CN111360146B - Device and method for preparing metal film by area expansion under vacuum environment - Google Patents
Device and method for preparing metal film by area expansion under vacuum environment Download PDFInfo
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D33/00—Special measures in connection with working metal foils, e.g. gold foils
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C51/00—Measuring, gauging, indicating, counting, or marking devices specially adapted for use in the production or manipulation of material in accordance with subclasses B21B - B21F
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D37/00—Tools as parts of machines covered by this subclass
- B21D37/16—Heating or cooling
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physical Vapour Deposition (AREA)
Abstract
A device and a method for preparing a metal film by area expansion under a vacuum environment comprise a vacuum furnace, wherein an experiment table is arranged in the vacuum furnace and is fixed on a manipulator device, a pressurizing device, a reflecting plane mirror and a condensing convex lens are arranged on the experiment table, and a high-melting-point metal ring is arranged on the surface of the experiment table. The method utilizes the characteristic of no air in a vacuum environment, adopts high-melting-point alloy wires to form a circle with controllable area, places a low-melting-point metal block in the middle of a metal ring, gathers sunlight to melt into molten metal, and adheres to the metal wires through surface tension. Because the vacuum environment has no heat conduction and heat convection, the heat exchange can only pass through the heat radiation, so the heat dissipation of the metal liquid is very slow, the metal liquid is not easy to solidify, after the temperature is raised to be slightly higher than the melting point of the low-melting-point metal, the metal liquid is adhered to the alloy wire due to the surface tension, and the metal liquid gradually expands into a film along with the increase of the area of the metal ring. The method combines a heat transfer process without medium in physical change, has the advantages of high material utilization rate, simple and efficient preparation process, environmental protection, energy conservation, high quality of a film forming surface and excellent performance.
Description
The technical field is as follows:
the invention belongs to the technical field of metal film preparation, and particularly relates to a device and a method for preparing a metal film by area expansion in a vacuum environment.
Background art:
the metal film is one of film materials with the best performance after an organic film and a ceramic film because of good plasticity, toughness, strength, high conductivity and adaptability to environment and materials, and is widely applied to various fields such as electronic components, integrated optics, electronic technology, infrared technology, laser technology, aerospace technology, optical instruments and the like, particularly becomes an independent application technology in the application field of light high-strength material films, and becomes an important means for modifying the surfaces of materials and improving certain process levels, so that the preparation of the metal film is widely concerned by researchers at home and abroad. However, how to prepare a high-quality, defect-free, uniform-thickness, and size-controllable metal thin film with high efficiency has been the pursuit of researchers.
At present, the methods for preparing metal thin films mainly include two major types, namely physical methods and chemical methods (including electrochemical methods). The physical method mainly comprises the preparation methods of films such as a vacuum thermal evaporation method, direct current sputtering, a magnetron sputtering method, radio frequency sputtering, pulse laser deposition, a molecular beam epitaxial growth method and the like. The chemical methods mainly include a chemical vapor deposition method (CVD), a liquid phase formation method, an oxidation method, a diffusion method, an electroplating method, and the like. The methods are all used for depositing a film on another object through the transfer of a medium, and no oxide can be generated in the transfer process; because different media can cause the film to be uneven, the quality of the generated metal film is not pure, and defects are easy to generate; in addition, most of the preparation methods have the defects of complicated process, low preparation efficiency, multiple control factors, easy material consumption, easy generation of harmful gas and the like.
The invention content is as follows:
the present invention has been made to overcome the above-mentioned disadvantages of the prior art, and in view of the above problems, it is an object of the present invention to provide a method for preparing a metal thin film in a vacuum, which is highly advantageous. Compared with the traditional metal film preparation method, the metal film is not polluted due to the absence of oxygen in vacuum, and the film is well protected in the vacuum environment, so that the factors influencing the quality of the film are reduced. The adopted heat source is sunlight, and the area expansion method is combined to achieve better energy saving and high efficiency, and meanwhile, the generation of harmful gases is reduced.
However, the area spreading method for preparing a metal thin film depends largely on the surface tension of the metal solution, and when the metal solution comes into contact with a surrounding solid, a surface layer is formed in which the intermolecular distance is larger than the intermolecular distance in the metal solution, and exhibits a large attractive force, so that the surface tension is formed. The surface tension is related to the temperature and pressure, in addition to the different metal solutions themselves. Since there is no oxygen and other impurities in the vacuum, the most important factor for controlling the surface tension in the preparation of the metal film by the area expansion method is the temperature. The molecular bond attraction decreases with increasing temperature, and the surface tension decreases with increasing temperature. Therefore, the metal film with high quality and high purity can be prepared by controlling the temperature to be slightly higher than the melting point of the metal and slowly heating to ensure that the metal solution has larger surface tension. If the method is adopted in the environment of space microgravity, the defects of uneven film, small film forming area and the like caused by gravity can be reduced, so that the method is the first step for preparing the large-area uniform high-quality metal film in the vacuum and gravity-free environment of the space experiment station.
The application provides a device and a method for preparing a metal film by area expansion under a vacuum environment. The method utilizes the adsorption capacity generated by the surface tension of the metal solution to prepare the high-purity and high-quality metal film according to the surface expansion method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a device for preparing a metal film by area expansion under a vacuum environment comprises a vacuum furnace, wherein an experiment table is arranged in the vacuum furnace, a pressurizing device is arranged above the experiment table, the pressurizing device is provided with a reflecting plane mirror and a condensing convex lens, the experiment table is fixed on a manipulator device, a high-melting-point metal ring is arranged on the surface of the experiment table, the high-melting-point metal ring is an area-expandable metal ring, and the high-melting-point metal ring is fixed on the manipulator device; the manipulator device comprises an X axis, a Y axis and a Z axis, wherein the X axis, the Y axis and the Z axis are slidable axes.
The experiment table is a liftable experiment table.
The high melting point metal ring is fixed on the X axis and the Y axis.
The manipulator device is provided with a slide way, so that XYZ-axis sliding can be realized, and the rotary connecting parts at two ends of the X axis are fixedly connected with the vacuum furnace base support.
The mechanical hand device is pushed along the X-axis direction along the Y-axis direction, so that the high-melting-point metal ring is stretched.
The device is internally provided with a temperature tester.
The temperature measuring instrument is a thermocouple.
The device is provided with a light-transmitting observation window and a support.
A method for preparing a metal film by area expansion in a vacuum environment adopts the device, and comprises the following steps:
(1) placing a metal block in the middle of the high-melting-point metal ring on the experiment table, adjusting the temperature of a condensing convex lens, and controlling the heating temperature to be 0.5-100 ℃ above the melting point of the metal block after the metal block is completely melted by a solar light source;
(2) pushing a Y axis of a manipulator device to move along the X axis direction so as to push an extension section of the high-melting-point metal ring, realizing metal ring stretching, enabling the diameter of a metal film to be expanded at a speed of less than 10mm/min, namely the stretching speed of two ends of the metal ring is less than 31.4mm/min, ensuring that molten metal is adhered to the high-melting-point metal wire through moving in the Y axis direction and the Z axis direction in the stretching process, expanding the area enclosed by the metal ring through stretching the high-melting-point metal wire, driving the molten metal to realize area expansion, and gradually reducing the thickness of the center of the molten metal to a target size;
(3) and after the stretching is finished, closing the light source, moving the experiment table away from the light source, and cooling to room temperature to obtain the metal film, wherein the diameter of the metal film is 10-100 m, and the thickness of the metal film is more than or equal to 50 nm.
In the step (1), the high-melting-point metal ring is formed by cross connection of metal wires, the metal wires comprise an extension section after the cross connection, the extension section is fixed on an X shaft and a Y shaft of a manipulator device, specifically, the end part of the extension section at one end is bent and fastened on the Y shaft of the manipulator device, the end part of the extension section at the other end is fastened on the X shaft of the manipulator device, a gap is fixed in the middle of the extension section on the X shaft of the manipulator device, and the gap can enable the high-melting-point metal ring to pass through smoothly.
In the step (1), rectangular coils are arranged at the intersections of the high-melting-point metal rings to ensure that the high-melting-point metal rings are stretched in the horizontal direction completely in the stretching process, so that longitudinal dislocation is avoided.
In the step (1), the size of the metal block and the size of the surrounding high-temperature alloy wires are determined according to the thickness and the size of the prepared metal film. If the diameter span of the manufactured film is 10mm-100m and the thickness is more than 50nm, the size of the required metal block is calculated according to the required thickness and diameter of the film, and then a high-temperature alloy wire larger than the perimeter of the metal film is selected for experiment.
In the step (1), the metal block is made of pure metals of copper, aluminum, tin, bismuth, gallium, magnesium, aluminum, lithium and nickel with low melting point or alloys formed by combination of the pure metals. The alloy comprises aluminum alloy, gallium alloy and lead-tin alloy.
In the step (1), the high-melting-point metal ring is made of nickel-based high-temperature alloy, cobalt-based alloy, tungsten-molybdenum, niobium, tantalum and the like, and the melting point of the metal ring is higher than the experimental heating temperature, so that the metal ring is ensured not to be melted. The diameter range of the metal wire is 0.1-5 mm, more than 0.5mm is preferably selected generally, and the metal wire can be adjusted according to specific implementation conditions.
In the step (1), the high-melting-point metal ring is required to be as flat as possible, and if the bubble blowing principle is adopted, the metal wire cannot be provided with sharp pointed ends, so that the thin film is prevented from being damaged and torn.
In the step (1), the temperature measurement mode is thermocouple temperature measurement or infrared non-contact temperature measurement, and the measurement range of the infrared non-contact temperature measurement is-100 ℃ to 3000 ℃.
In the step (1), thermocouples are attached to the interior of the high-melting-point metal ring, the thermocouples are B-type, K-type, N-type or S-type thermocouples, the temperature measurement range is-100 ℃ to 1800 ℃, and the temperature measurement of the focusing of the condensing convex lens on the metal block is realized.
In the step (1), the metal block is in a vacuum environment, sunlight is focused on the surface of the metal block by using a condensing convex lens, the metal block is heated, heated and melted, and solar energy is mainly consumed in the heating process of the metal material.
In the step (1), resistance wire heating can be adopted to replace the heating of the focusing sunlight by the condensing convex lens.
In the step (1), the calculation process of the temperature control range of controlling the heating temperature to be kept 0.5-100 ℃ above the melting point of the metal block is as follows:
heating temperature T (k) by condensing convex lens and surface tension, namely viscosity mu (Pa s) adsorbed on metal wire
Wherein m (g) is an atomic mass unit, and K is a Boltzmann constant 1.3806505 (24). times.10-23J/k，γ1s(mN/m) is a solid-liquid interfacial tension.
From the formula, it can be seen that when the temperature T is increased, the viscosity mu is reduced, and then the shrinkage rate when the melt is solidified is related to the viscosity:
wherein Δ P (mN/m) is a bath capillary force, R (mm) is a grain radius, W (mol/L) is a liquid phase concentration, and μ (Pa · s) is a liquid viscosity. When the temperature rises and the viscosity decreases, the shrinkage rate increases, which is not beneficial to the preparation of the metal film. But the viscosity can be indirectly controlled according to the relation between the temperature and the viscosity, so that the thickness and the size of the metal film can be controlled. The temperature is controlled to be 0.5-100 ℃ above the melting point, so that the surface tension can be ensured to be sufficiently adsorbed on the metal wire.
In the step (2), the drawing speed of the metal coil wire is related to the material characteristics and the diameter of the prepared metal film, the toughness is better, the drawing speed limit is larger, when the diameter of the prepared metal film is smaller than 50mm, the drawing speed of the metal coil wire is smaller than 10mm/min, when the diameter of the prepared metal film is larger than or equal to 50mm, the influence of gravity is smaller, and the drawing speed limit is larger than or equal to 10 mm/min.
In the step (3), the film with the thickness of 50nm can be prepared on the premise that the equipment space is large enough on the basis of ensuring that the surface tension of the melt is enough to be adsorbed on the metal wire by controlling the heating temperature to be kept 0.5-100 ℃ above the melting point of the metal block.
In the step (3), the experiment table is transversely close to and far from the light source through transverse movement of an X axis and a Y axis, and the experiment table is longitudinally close to and far from the light source through longitudinal movement of a Z axis.
In the step (3), the light source is sunlight.
In the preparation method, molten metal after the metal blocks are melted is adhered to a surrounding high-melting-point metal ring (namely, the melting point of the surrounding wire is higher than that of the raw material metal block), the surrounding area of the metal ring is expanded, and metal films with different areas and different thicknesses are prepared by an area expansion method.
The method of the invention utilizes the adsorption capacity generated by the surface tension of the metal solution to prepare the high-quality metal or alloy film material according to the surface expansion method, and particularly focuses sunlight on the surface of a metal block with a lower melting point by a light-focusing convex lens in a vacuum laboratory to melt the metal block, controls the temperature of the molten metal to be kept in a specific range, generates the adsorption capacity to be adsorbed on a surrounding high-melting-point metal ring (namely, the alloy with the melting point higher than the metal block), and prepares the metal films with different areas and different thicknesses by adjusting the size of the area surrounded by the high-melting-point metal ring.
The invention has the beneficial effects that:
1. the device and the method for preparing the metal film by area expansion under the vacuum environment utilize the characteristics that the condition of weightlessness in vacuum is favorable for spreading metal liquid into the metal film, the impurities in vacuum are less, and no medium is transferred in the preparation process, so that the high-purity pollution-free metal film can be obtained.
2. The heat source utilized by the invention is inexhaustible clean energy, namely solar energy, and the melting and solidification are combined with physical change, so that no harmful substances are generated in the whole metal film preparation process, the material utilization rate is higher, no waste is generated, and the material utilization rate is higher, so that the whole metal film preparation link is simpler, safer, more environment-friendly, more energy-saving and more efficient.
3. The invention controls the temperature by regulating the distance between the condensing convex lens and the object and changing the energy focused on the metal block, the thermocouple collects the temperature information and feeds back the temperature information to the surface tension according to the relational expression of the temperature and the viscosity, and finally controls the expansion speed of the metal wire, and the expansion speed, the thickness and the size of the metal wire can be directly fed back to the film forming speed, the thickness and the size according to the collected temperature information. The method has the characteristics of convenience, simplicity, less controllable variable, high accuracy and automation realization.
Description of the drawings:
fig. 1 is a schematic structural diagram of an apparatus for preparing a metal thin film by area expansion in a vacuum environment in embodiment 1 of the present invention.
FIG. 2 is a partial top view of the vacuum furnace robot apparatus of FIG. 1;
fig. 3 is a detailed view of the change of the melting and stretching process of the metal block in embodiment 1 of the present invention, wherein a is a schematic view of the placement state of the metal block, b is a schematic view of the enlargement of the melting and stretching area, and c is a view of the state that the light source is turned off and the experiment table is moved away from the light source; wherein:
1-pressurizing device, 2-vacuum furnace, 3-manipulator device, 4-light-transmitting observation window, 5-solar beam, 6-rectangular coil, 7-molten metal, 8-sleeve, 9-support, 10-nickel-chromium-nickel-silicon K-type thermocouple, 11-molybdenum wire, 12-temperature measuring instrument, 13-experiment table, 14-condensing convex lens, 15-reflecting flat mirror, 16-sleeve support, 17-manipulator Y axis, 18-manipulator X axis, 19-rotary connecting component and 20-manipulator Z axis.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
A device for preparing a metal film by area expansion under a vacuum environment comprises a vacuum furnace, wherein a liftable experiment table is arranged in the vacuum furnace, a pressurizing device is arranged above the experiment table, the pressurizing device is provided with a reflecting plane mirror and a condensing convex lens, the experiment table is fixed on a manipulator device, the manipulator device comprises a slidable X shaft, a Y shaft and a Z shaft, the manipulator device is provided with a slideway to realize the sliding of the X and Z shafts, rotary connecting parts at two ends of the X shaft are fixedly connected with a base support of the vacuum furnace, a high-melting-point metal ring is arranged on the surface of the experiment table, the high-melting-point metal ring is an area-expandable metal ring, and the high-melting-point metal ring is fixed on; the device is internally provided with a thermocouple for measuring temperature and is provided with a light-transmitting observation window and a support. The X-axis and the Y-axis move transversely to realize that the experiment table is transversely close to and far away from the light source, and the Z-axis moves longitudinally to realize that the experiment table is longitudinally close to and far away from the light source.
A method for preparing a metal film by area expansion in a vacuum environment adopts the device, and comprises the following steps:
(1) putting a metal block into the high-melting-point metal ring on the experiment table, adjusting the temperature of the condensing convex lens to control the temperature, and controlling the heating temperature to be 0.5-100 ℃ above the melting point of the metal block after the metal block is completely melted; wherein:
the high-melting-point metal ring is formed by cross connection of metal wires, the metal wires comprise extension sections after the cross connection, the extension sections are fixed on an X shaft and a Y shaft of a manipulator device, specifically, the end part of one extension section is bent and fastened on the Y shaft of the manipulator device, the end part of the other extension section is fastened with the X shaft of the manipulator device, a gap is fixed in the middle of the extension section and can be used for enabling the high-melting-point metal ring to pass through smoothly; rectangular coils are arranged at the intersections of the high-melting-point metal rings to ensure that the high-melting-point metal rings are stretched in the completely horizontal direction in the stretching process, so that longitudinal dislocation is avoided;
the size of the metal block and the size of the surrounding high-temperature alloy wires are determined according to the thickness and the size of the prepared metal film. If the diameter span of the manufactured film is 10mm-100m and the thickness is more than 50nm, calculating the size of the required metal block according to the required thickness and diameter of the film, and selecting a high-temperature alloy wire with the circumference larger than that of the metal film for experiment;
the metal block is made of pure metals of copper, aluminum, tin, bismuth, gallium, magnesium, aluminum, lithium and nickel with low melting points or alloy formed by combination of the pure metals. The alloy includes aluminum alloy, gallium alloy, lead-tin alloy;
the high-melting-point metal ring is made of nickel-based high-temperature alloy, cobalt-based alloy, tungsten-molybdenum, niobium, tantalum and the like, the melting point of the metal ring is higher than the experimental heating temperature, and the metal ring is guaranteed not to be melted. The diameter range of the metal wire is 0.1-5 mm, more than 0.5mm is preferably selected generally, and the metal wire can be adjusted according to specific implementation conditions;
the high melting point metal ring is required to be as flat as possible, and as for the bubble blowing principle, the metal wire cannot be provided with sharp pointed ends, so that the thin film is prevented from being damaged and torn;
the temperature measurement mode is thermocouple temperature measurement or infrared non-contact temperature measurement, and the measurement range of the infrared non-contact temperature measurement is-100 ℃ to 3000 ℃;
the thermocouple is attached inside the high-melting-point metal ring, is a B-type, K-type, N-type or S-type thermocouple, and has a temperature measuring range of-100-1800 ℃ so as to realize the temperature measurement of the focusing of the condensing convex lens on the metal block.
The metal block is in a vacuum environment, sunlight is focused on the surface of the metal block by utilizing a condensing convex lens, so that the metal block is heated, heated and melted, and the solar energy is mainly consumed in the heating process of the metal material; resistance wire heating can be adopted to replace the heating of the focusing sunlight by the condensing convex lens.
The calculation process of the temperature control range for controlling the heating temperature to be kept 0.5-100 ℃ above the melting point of the metal block is as follows:
heating temperature T (k) by condensing convex lens and surface tension, namely viscosity mu (Pa s) adsorbed on metal wire
Wherein m (g) is an atomic mass unit, and K is a Boltzmann constant 1.3806505 (24). times.10-23J/k，γ1s(mN/m) is a solid-liquid interfacial tension.
From the formula, it can be seen that when the temperature T is increased, the viscosity mu is reduced, and then the shrinkage rate when the melt is solidified is related to the viscosity:
wherein Δ P (mN/m) is a bath capillary force, R (mm) is a grain radius, W (mol/L) is a liquid phase concentration, and μ (Pa · s) is a liquid viscosity. When the temperature rises and the viscosity decreases, the shrinkage rate increases, which is not beneficial to the preparation of the metal film. But the viscosity can be indirectly controlled according to the relation between the temperature and the viscosity, so that the thickness and the size of the metal film can be controlled. The temperature is controlled to be 0.5-100 ℃ above the melting point, so that the surface tension can be ensured to be sufficiently adsorbed on the metal wire.
(2) Pushing a Y axis of a manipulator device to move along the X axis direction so as to push an extension section of the high-melting-point metal ring to stretch the metal ring, so that the diameter of a metal film is expanded at a speed of less than 10mm/min, namely the wire stretching speed of the metal ring is less than 31.4mm/min, and in the stretching process, moving along the Y axis direction and the Z axis direction to ensure that molten metal is adhered to the high-melting-point metal wire, expanding the area surrounded by the metal ring by stretching the high-melting-point metal wire, driving the molten metal to realize area expansion, and gradually reducing the thickness of the center of the molten metal to a target size; specifically, the drawing speed of the metal coil wire is related to the material characteristics and the diameter of the prepared metal film, the toughness is better, the drawing speed limit is larger, when the diameter of the prepared metal film is smaller than 50mm, the drawing speed of the metal coil wire is smaller than 10mm/min, when the diameter of the prepared metal film is larger than or equal to 50mm, the influence of gravity is smaller, and the drawing speed limit is larger than or equal to 10 mm/min;
(3) and after the stretching is finished, closing the light source, moving the experiment table away from the light source, and cooling to room temperature to obtain the metal film, wherein the diameter of the metal film is 10mm-100m, and the thickness of the metal film is more than or equal to 50 nm.
The vacuum furnace used in the following examples is a JSCJ-I type vacuum furnace; the vacuum degree is adjusted to 10-4Pa；
The thermocouple is a nickel-chromium-nickel-silicon K-type thermocouple, the diameter of the thermocouple is 0.3mm, and the measurement range is 0-1000 ℃;
example 1
A device for preparing a metal film by area expansion under a vacuum environment is shown in a schematic structural diagram of fig. 1 and comprises a vacuum furnace 2, a liftable experiment table 13 is arranged in the vacuum furnace 2, a pressurizing device 1 is arranged above the experiment table 13, the pressurizing device 1 is provided with a reflecting plane mirror 15 and a light-gathering convex lens 14, the experiment table 13 is fixed on a manipulator device 3, a partial top view of the manipulator device is shown in fig. 2, a molybdenum wire ring is arranged on the surface of the experiment table 13 and fixed on an X axis 18 and a Y axis 17, the molybdenum wire ring is an area-expandable metal ring, and the molybdenum wire ring is fixed on the manipulator device 3; the manipulator device 3 comprises an X shaft 18, a Y shaft 17 and a Z shaft 20, the manipulator device 3 is provided with a slideway, the sliding of XYZ shafts 20 can be realized, rotary connecting parts 19 at two ends of the X shaft 18 are fixedly connected with a base support of the vacuum furnace 2, the Y shaft 17 of the manipulator device 3 is pushed towards the X shaft 18 direction, the stretching of a molybdenum wire ring is realized, the X shaft 18 and the Y shaft 17 move transversely, the experiment table 13 is transversely close to and far away from a light source, the experiment table 13 is longitudinally close to and far away from the light source through the longitudinal movement of the Z shaft 20, a nickel-chromium-nickel-silicon K type thermocouple 10 is arranged in the device, the thermocouple is connected with a temperature measuring instrument 12, and the device.
By adopting the device, the preparation of the metal film by area expansion under the vacuum environment is carried out: the JSCJ-I type vacuum furnace 2 with a manipulator device 3, a light-transmitting observation window 4 and a support 9 in the figure 1 is used as an experimental device for simulating a vacuum environment, and the vacuum degree of the smelting furnace is 10-4Pa, thus ensuring that the prepared metal film has no oxide impurities and has higher purity.
A laboratory table 13 with the center of the furnace capable of lifting is placed with a size of 5 multiplied by 5mm3The 6061-T651 aluminum alloy with the weight of 0.34g is selected to be connected with a molybdenum wire 11 (the melting point of the high-temperature alloy wire is 2623 ℃, the melting point is far higher than the melting point of the aluminum alloy (580 ℃), and the diameter is 0.5mm) of a thermocouple 10 to form a circle, sleeves 8 made of the same high-temperature alloy wire material are fixed on a mechanical device 3, two sleeves 8 in the middle are in clearance fit with an X shaft 18 of a manipulator, the distance is 0.4mm, the molybdenum wire 11 can pass through the sleeves smoothly when being stretched, the two ends are in transition fit to prevent sliding, the sleeve 8 at the rightmost end enables the molybdenum wire 11 to be fixed on a Y shaft 17 of the manipulator, the molybdenum wire can be stretched along with the change of displacement in the horizontal direction, and the area surrounded by.
The same molybdenum wire is adopted to be made into a rectangular coil 6 which is pricked at the cross position of the molybdenum wire, so that the molybdenum wire 11 can be stretched without staggering up and down to damage the film. Two ends of the molybdenum wire 11 are connected with a thermocouple 10 and connected to a temperature measuring instrument 12 for measuring the temperature in the experimental process.
A pressurizing device 1 and a sleeve support 16 are arranged in the vertical direction and used for fixing a reflecting plane mirror 15 and a condensing convex lens 14 which form an angle of 45 degrees with the light rays 5 which are emitted in the horizontal direction. When the parallel solar beams 5 irradiate the reflecting plane mirror 15 through the light-transmitting observation window 4, the parallel solar beams are vertically reflected downwards to the lower condensing convex lens 14 and are converged on an aluminum alloy block on the test bed, so that the aluminum alloy block is melted into molten metal 7 to cover the area of a metal ring surrounded by the molybdenum wires 11.
The distance between the experiment table 13 and the condensing convex lens 14 is adjusted by a mechanical device such as a mechanical arm Z shaft 20 shown in figure 2, so that the superheat degree is adjusted, the temperature of the metal liquid 7 is 3-5 ℃ higher than the melting point (580 ℃) of the aluminum alloy, namely the temperature of the thermocouple 10 connected with the molybdenum wire is 583-585 ℃ through a temperature measuring instrument 12, at the moment, the metal liquid of the aluminum alloy has enough surface tension to adhere to the molybdenum wire 11, and the relationship between the temperature and the viscosity is controlled to be 2-5 ℃ higher than the melting point of the aluminum alloy, at the moment, the viscosity is enough to adhere to the molybdenum wire 11, and through an area expansion method, the area surrounded by the molybdenum wire 11 is expanded to expand the metal liquid 7 to carry out area expansion, and the expansion is developed to a film, and is like the metal liquid adhered.
The device for drawing molybdenum wire is shown in fig. 2, and a robot device having a slide is capable of drawing the molybdenum wire 11 while moving the robot Y-axis 17 in the horizontal direction. The stretching speed is mechanically adjusted to be 1.57mm/s, namely the diameter speed of the expanded area is 0.5mm/s, in the process, the distance between the condensing convex lens and the experiment table is adjusted through the temperature range displayed on a thermodetector in the metal film forming process, and the experiment table 13 is lifted and descended through the Z axis 20 of the manipulator shown in the figure 2. According to the viscosity and temperature formula and the shrinkage and viscosity calculation formula, in combination with the good ductility of 6061 aluminum alloy, in this example, the detail change of the metal block melting and stretching process is shown in fig. 3, the schematic diagram of the metal block placing state is shown in a, and the heating temperature t (k) ranges from 583 ℃ to 585 ℃ (the melting point of 6061 aluminum alloy is 580 ℃) from 3 ℃ to 5 ℃ to melt the 6061 aluminum alloy. With the enlargement of the area, the thickness of the center of the molten metal is smaller and smaller, the schematic drawing of the melting and stretching area is shown as b, the molten metal is drawn into a silvery white 6061 aluminum alloy film with the diameter of 28mm and the average thickness of 0.2mm (error of 5%) and a catenary surface through 47s, a light source is turned off, a state diagram of moving an experiment table away from the light source is shown as c, and the film mechanical property data are shown in the following table 1 and can be applied to electronic elements such as a radiator and the like.
TABLE 1
Example 2
The structure of the device for preparing a metal film by area expansion under a vacuum environment in this example is the same as that of example 1.
The process of preparing the metal thin film was the same as that of example 1 except that the gallium thin film was prepared by replacing the 6061 aluminum alloy block with pure gallium metal and replacing the molybdenum wire with the GH4169 high temperature alloy wire.
In the same experimental environment as in example 1, a lead-tin alloy of 0.74g in the weight of a 5X 5mm cube was placed in the center of the furnace, and the position of the condensing convex lens was adjusted by a robot. According to the formula of viscosity and temperature and the formula of shrinkage and viscosity calculation, gallium metal is combined with a solidification point lower than 0 ℃, in the example, the heating temperature T (k) ranges from 30 ℃ to 32 ℃ (the melting point of gallium metal is 29.8 ℃), the gallium metal is melted into silvery white molten metal, the molten metal is adhered to a surrounding GH4169 high-temperature alloy wire, the drawing speed is automatically adjusted to be 1.57mm/s by a manipulator (the drawing speed can also be changed by automation, the drawing speed is the same as that of example 1 in the experiment), and the molten metal is drawn into a film with the diameter of 15mm after 20 s. The volume of the solidified gallium metal is increased by about 3.2%, so that the average thickness of the finally generated gallium thin film is 0.2mm, the error is 5%, and the gallium thin film is a light blue gallium alloy thin film with a catenary surface. The gallium metal film prepared by the embodiment can be used for manufacturing semiconductors and heat exchange media, and the hardness can reach 2.5HV。
Example 3
The structure of the device for preparing a metal film by area expansion under a vacuum environment in this example is the same as that of example 1.
The metal thin film preparation process was carried out in the same environment as in example 1 except that a 6061 aluminum alloy block was replaced with a lead-tin alloy containing 60% of tin and 40% of lead, and a molybdenum wire was replaced with a GH4169 high temperature alloy wire (having good overall properties at 650 c).
In the experimental environment the same as example 1, a 5 × 5 × 5mm cube of 0.55g lead-tin alloy with a weight is placed in the center of the furnace, the position of the condenser convex lens is adjusted by the manipulator, the lead-tin alloy is melted according to the viscosity and temperature formula and the shrinkage and viscosity calculation formula, in this example, the heating temperature t (k) ranges from 190 ℃ to 203 ℃ (the melting point of the lead-tin alloy is 183 ℃), the lead-tin alloy is adhered to the surrounding GH4169 high temperature alloy wire, the stretching speed is automatically adjusted by the manipulator device Y axis 17 to 1.57mm/s (the stretching speed can also be changed automatically, the same stretching speed as in example 1 is adopted in this experiment), and the molten metal is stretched into a light gray lead-tin alloy film with a diameter of 28mm, an average thickness of 0.1mm and an error of 5% and a catenary surface after 46 s. The lead-tin alloy film prepared by the embodiment can be mainly used for electric heating elements, and the measured heat flux density reaches 95%.
Example 4
The structure of the device for preparing a metal film by area expansion under a vacuum environment in this example is the same as that of example 1.
The metal thin film preparation process environment was the same as that of example 1 except that 6061 aluminum alloy block was replaced with copper and molybdenum wire, and a type B thermocouple was used instead of a type K thermocouple to perform a copper thin film preparation experiment.
The experimental environment was the same as in example 1, a 10X 10mm square of 8.96g of a copper alloy was placed in the center of the furnace, and the position of the condensing convex lens was adjusted by a robot. According to the formula of viscosity and temperature and the formula of calculation of shrinkage rate and viscosity, the copper has good ductility, in this example, the heating temperature T (k) is 1085 ℃ -1100 ℃ (the melting point of copper is 1083.4 ℃), the molten metal is melted, the molten metal is ensured to be adhered to the surrounding molybdenum wires, the drawing speed is automatically adjusted to be 30mm/s (the drawing speed can be properly reduced, the drawing speed is less than or equal to 30mm/s based on the film forming quality in the experimental process), and the molten metal is drawn into a claret-colored metal film with the diameter of 100mm, the average thickness of 0.05mm and the error of 5% and a catenary surface after 10 s. The mechanical property data of the copper film prepared by the embodiment are shown in the following table 2, and the copper film can also be applied to the fields of electronic components, industrial machines and equipment, medicine and the like.
TABLE 2
Example 5
The structure of the device for preparing a metal film by area expansion under a vacuum environment in this example is the same as that of example 1.
The metal thin film preparation process was conducted in the same environment as in example 1 except that a preparation experiment of a pure nickel metal thin film was conducted by replacing a 6061 aluminum alloy block with a pure nickel metal and a molybdenum wire, and a type B thermocouple was used instead of a type K thermocouple, and the measurement range was 0 to 1800 ℃.
In the same experimental environment as in example 1, a nickel metal block having a square weight of 1.92g and a size of 6X 6mm was placed in the center of the furnace, and the position of the condensing convex lens was adjusted by a robot. According to the formula of viscosity and temperature and the formula of calculation of shrinkage rate and viscosity, in combination with the good ductility of nickel metal, in this example, the heating temperature t (k) is 1460 ℃ -1553 ℃ (nickel metal melting point 1453 ℃), metal nickel is melted and adhered to the surrounding molybdenum wires, the drawing speed is automatically adjusted to 10mm/s by a manipulator (the drawing speed can also be automatically changed), and molten metal is drawn into a silver white pure nickel metal film with the diameter of 50mm, the average thickness of 0.1mm and the error of 5% and a catenary surface through 47 s. The mechanical property data of the pure nickel metal film prepared by the embodiment are shown in the following table 3, and the pure nickel metal film is widely applied to the field of corrosion resistance industry.
TABLE 3
Comparative example 1
The difference from embodiment 1 is that in this embodiment, six high temperature alloy rods with thermocouples connected to the sliding ways are used to drive the metal extension area to prepare the metal thin film. The specific scheme is as follows:
the same material as that of example 1 was used, six high temperature alloy rods with slides were used to form a regular hexagon, the metal block was placed in the middle, and after melting the metal block by the condenser convex lens, the high temperature alloy lead screw was extended outward perpendicular to the rod face. The principle is the same as that of example 1, but the hexagonal corners reduce the limit of surface tension, and because the existence of six corners interferes with the surface tension signal fed back by the thermocouple, the mechanical motion signal fed back to the superalloy rod is delayed, and the tearing is generated for a plurality of times. Finally, the 6061 aluminum alloy film is obtained at the drawing speed of 1.05mm/s for 60s, cracks are formed at the sharp corner, the metal film is not complete enough, cracks are expanded, and the performance index is low. This comparison shows that the less edges are favorable for the area expansion of the molten metal, and the higher the quality and success rate of the obtained metal film.
Comparative example 2
The difference from embodiment 1 is that the present embodiment uses a heat source heated by a resistance method, i.e., two electrodes are added to control the temperature.
The specific scheme is as follows:
using a high temperature alloy wire of the same material and shape as in example 1, a metal block was placed in the middle, except that the heat source was changed to two electrode plates having a sliding varistor voltage of 3000 ohms and a voltage of 7V, the sliding varistor was adjusted to 1100 ohms, and then 6061 metal block having a specific heat capacity of 896 ℃/(kg. k) was heated. When molten metal is tightly adsorbed on the alloy wire, the two ends of the high-temperature alloy wire stretch horizontally, the area of the metal liquid is expanded due to the tension of the liquid level, the power supply is turned off after 47 seconds, and the metal film with high purity is obtained after cooling. Similar to embodiment 1, it can be seen that the solar light source of the present application can completely realize the heat source supply that the resistance wire heating method can realize, and simultaneously, the solar energy is fully utilized to clean energy, thereby avoiding resource waste.
Comparative example 3
The difference from example 1 is that the present example prepares a metal thin film in an air environment. The specific scheme is as follows:
moving the experimental element into the air, taking a telescopic bracket to replace a manipulator in a vacuum furnace, adjusting the position of a light-gathering convex lens, controlling the temperature focused on a metal block to be 600 ℃, melting aluminum alloy, adhering the aluminum alloy to a surrounding molybdenum wire to fix a ring at the cross position of the molybdenum wire, and drawing two ends of the molybdenum wire at the speed of 10mm/s by using two speed-adjustable toy cars according to the same principle as the embodiment 1, and drawing molten metal into a 6061 aluminum alloy film which has the diameter of 28mm, the average thickness of 0.2mm and the error of 5 percent and is in a catenary surface after 10 s. Different from embodiment 1, oxide is generated in the prepared metal film, the quality of the metal film is poor, and due to the existence of air, impurities are more, the color of the film is uneven, the performance index can not reach the technical effect of the technical scheme, the control factors are more, the embodiment 1 is simple and efficient, and the rule is not easy to summarize due to the complex environment.
Comparative example 4
The difference from example 1 is that the atmosphere for forming the metal thin film in this example is not a vacuum atmosphere, but an argon atmosphere.
The specific scheme is as follows:
argon gas is flushed into a JSCJ-I type vacuum furnace, a high-temperature alloy wire with the same material and shape as those of the embodiment 1 is used, a metal block is placed in the middle, after the metal block is melted through a condensing convex lens, when molten metal is tightly adsorbed on the alloy wire, two ends of the high-temperature alloy wire are horizontally stretched, and the molten metal is pulled into a 6061 aluminum alloy film with the diameter of 28mm, the average thickness of 0.2mm and the error of 5 percent under the action of surface tension for 40s, wherein the 6061 aluminum alloy film is in a catenary surface. Tests show that a small amount of oxides still exist in the prepared metal film, the surface quality is not as good as that of the metal film prepared in the embodiment 1, the prepared metal film has uneven color due to defects generated in the preparation process, and the performance index completely fails to achieve the technical effect of the embodiment 1.
Claims (10)
1. The device for preparing the metal film by area expansion under the vacuum environment is characterized by comprising a vacuum furnace, wherein an experiment table is arranged in the vacuum furnace, a pressurizing device is arranged above the experiment table, the pressurizing device is provided with a reflecting plane mirror and a condensing convex lens, the experiment table is fixed on a manipulator device, a high-melting-point metal ring is arranged on the surface of the experiment table, the high-melting-point metal ring is an area-expandable metal ring, and the high-melting-point metal ring is fixed on the manipulator device; the manipulator device comprises an X axis, a Y axis and a Z axis, wherein the X axis, the Y axis and the Z axis are slidable axes.
2. The apparatus for area expansion preparation of metal thin film according to claim 1, wherein the experimental table is a liftable experimental table, and the refractory metal rings are fixed on the X-axis and the Y-axis.
3. The apparatus for area expansion preparation of metal films under vacuum environment as claimed in claim 1, wherein the robot device is provided with a slide rail capable of sliding along XYZ axes, and the two ends of the X axis are connected with the rotary connecting components and the vacuum furnace base frame.
4. The apparatus for area expansion preparation of metal thin film according to claim 1, wherein said apparatus is provided with a temperature measuring device, and said apparatus is provided with a transparent viewing window and a support.
5. The method for preparing the metal film by adopting the device for preparing the metal film by area expansion under the vacuum environment as claimed in claim 1, which is characterized by comprising the following steps:
(1) putting a metal block into the high-melting-point metal ring on the experiment table, adjusting the temperature of the condensing convex lens to control the temperature, and controlling the heating temperature to be 0.5-100 ℃ above the melting point of the metal block after the metal block is completely melted;
(2) pushing a Y axis of a manipulator device to move along the X axis direction so as to push an extension section of the high-melting-point metal ring to stretch the high-melting-point metal ring, so that the diameter of a metal film is expanded at a speed of less than 10mm/min, the linear stretching speed of the high-melting-point metal ring is less than 31.4mm/min, and in the stretching process, through the movement of the Y axis and the Z axis direction, the molten metal is ensured to be adhered to the high-melting-point metal ring, through stretching the high-melting-point metal ring, the area surrounded by the high-melting-point metal ring is enlarged, the molten metal is driven to realize area expansion, and the thickness of the center of the molten;
(3) and after the stretching is finished, closing the light source, moving the experiment table away from the light source, and cooling to room temperature to obtain the metal film, wherein the diameter of the metal film is 10mm-100m, and the thickness of the metal film is more than or equal to 50 nm.
6. The method for area expansion preparation of a metal film under a vacuum environment as claimed in claim 5, wherein in the step (1), the refractory metal rings are formed by cross-connecting metal wires, the cross-connected metal wires comprise extension sections, the extension sections are fixed to an X axis and a Y axis of a manipulator device, specifically, one end of the extension section is bent and fastened to the Y axis of the manipulator device, the other end of the extension section is fastened to the X axis of the manipulator device, a gap is fixed to the X axis of the manipulator device in the middle of the extension section, and the gap is used for enabling the refractory metal rings to pass through smoothly.
7. The method for preparing a metal film by area expansion under a vacuum environment according to claim 5, wherein in the step (1), rectangular coils are arranged at the intersections of the high-melting-point metal rings so as to ensure that the high-melting-point metal rings are stretched in a complete horizontal direction in the stretching process and avoid longitudinal dislocation.
8. The method for area expansion preparation of a metal thin film under a vacuum environment as claimed in claim 5, wherein in the step (1), the metal block is made of pure metals of low melting point copper, aluminum, tin, bismuth, gallium, magnesium, lithium, nickel, or alloys formed by combination thereof.
9. The method for preparing a metal film by area expansion under a vacuum environment as claimed in claim 5, wherein in the step (1), the high melting point metal ring is made of nickel-based superalloy, cobalt-based alloy, tungsten-molybdenum, niobium or tantalum material, the melting point of the high melting point metal ring is higher than the experimental heating temperature, and the diameter range of the metal wire of the high melting point metal ring is 0.1-5 mm.
10. The method for area expansion preparation of metal films under vacuum environment as claimed in claim 5, wherein in step (3), the lateral approach and the distance of the experiment table to the light source are realized by the lateral movement of X-axis and Y-axis, and the longitudinal approach and the distance of the experiment table to the light source are realized by the longitudinal movement of Z-axis.
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