WO2022042467A1 - 一种非晶微纳结构的制备方法及热压成型装置 - Google Patents

一种非晶微纳结构的制备方法及热压成型装置 Download PDF

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WO2022042467A1
WO2022042467A1 PCT/CN2021/114019 CN2021114019W WO2022042467A1 WO 2022042467 A1 WO2022042467 A1 WO 2022042467A1 CN 2021114019 W CN2021114019 W CN 2021114019W WO 2022042467 A1 WO2022042467 A1 WO 2022042467A1
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micro
amorphous
hot
amorphous alloy
sleeve
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French (fr)
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马将
闫玉强
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Shenzhen University
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Shenzhen University
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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
    • B21D31/00—Other methods for working sheet metal, metal tubes, metal profiles
    • 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
    • B21D37/10—Die sets; Pillar guides
    • 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
    • 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
    • B21D37/20—Making tools by operations not covered by a single other subclass
    • 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
    • B21D45/00—Ejecting or stripping-off devices arranged in machines or tools dealt with in this subclass

Definitions

  • the application belongs to the technical field of hot-press forming of amorphous alloys, and in particular relates to a preparation method and a hot-press forming device of an amorphous micro-nano structure.
  • amorphous alloys are also known as liquid metals or metallic glasses. They are generally formed by the rapid cooling and solidification of molten alloys, which makes the system too late to crystallize. mechanical and physicochemical properties.
  • Amorphous alloys are thermodynamically metastable materials. When the temperature increases, the material will undergo a glass transition, and the temperature will continue to increase to induce a crystallization reaction. There is generally a temperature range of 20 to 120°C between the glass transition and the onset of crystallization, and this temperature range is called the supercooled liquid phase. It is precisely because of the existence of this interval that the amorphous alloy has properties similar to oxide glass, showing a viscous flow state and excellent superplasticity. Thus, the problems of high strength and high hardness of amorphous alloys at room temperature, which are difficult to process and poor in plasticity, are avoided. Compared with traditional forming processes, amorphous alloy superplastic forming parts have the characteristics of high strength, high precision and high surface finish, and are very suitable for the processing and manufacturing of aerospace, precision machinery, medical equipment, consumer electronics and other products.
  • the basic principle of the superplastic forming of amorphous alloys in the prior art is to use the hot pressing method in the subcooled liquid phase interval.
  • the technical solutions are mostly aimed at processing macroscopic parts.
  • the forming of amorphous alloys with macroscopic structures often requires a small forming pressure and is easy to demold.
  • the amorphous alloy will fill the molding cavity of the mold and squeeze the inner wall of the molding cavity.
  • the post-amorphous alloy will adhere to the inner wall of the molding cavity, resulting in difficulty in demolding, and forced demolding will cause deformation of the product and the mold, and it cannot be demolded in severe cases.
  • One of the purposes of the embodiments of the present application is to provide a method for preparing an amorphous micro-nano structure, which aims to solve the problem of difficulty in demolding an amorphous alloy during hot pressing.
  • a method for preparing an amorphous micro-nano structure for hot pressing the micro-nano structure on an amorphous alloy, and the preparation method of the amorphous micro-nano structure includes the following steps:
  • the hot-pressing mold includes an outer mold with a molding hole and an inner mold sleeve detachably placed in the molding hole;
  • the lower pressure head, the microstructure template and the amorphous alloy are sequentially arranged on the inner mold sleeve from bottom to top, and the microstructure template is provided with a micro-nano structure toward the surface of the amorphous alloy;
  • the hot-pressing mold is placed in a vacuum environment and the amorphous alloy is heated to a subcooled liquid phase region, and one end of the upper indenter is inserted into the molding hole and pressed against the microstructure template. crystalline alloy and hold pressure for a predetermined time;
  • the amorphous alloy is cooled and the amorphous alloy replicated with the micro-nano structure is taken out.
  • the inner mold casing includes a first half casing and a second half casing that is butt-fitted with the first half casing, and both the microstructure template and the amorphous alloy are located in the first half casing between the sleeve and the second sleeve half.
  • the inner mold sleeve is a flexible film sleeve made of temperature resistant material.
  • a plurality of the microstructure templates are stacked and arranged, the amorphous alloy is arranged between any two adjacent microstructure templates, and each of the microstructure templates faces the corresponding amorphous alloy.
  • the surfaces of the crystalline alloys are all provided with micro-nano structures.
  • the micro-nanostructures include nanostructures with a size of nanometers and microstructures with a size of micrometers.
  • the microstructure template is provided with the microstructure and the nanostructure.
  • the thermal expansion coefficients of the upper indenter and the lower indenter are the same.
  • the inner wall of the molded hole is mirror-finished.
  • the temperature range ⁇ T of the subcooled liquid phase region is ⁇ 40°C.
  • the present application also provides a hot-press forming device for hot-press forming an amorphous alloy
  • the hot-press forming device includes an outer mold, an inner mold sleeve, an upper indenter, a lower indenter, a A vacuum hot press of a vacuum heating chamber and a microstructure template
  • the outer mold is provided with a molding hole
  • the inner mold sleeve is detachably arranged in the molding hole
  • the amorphous alloy is sequentially arranged on the inner mold sleeve from bottom to top, and the microstructure template faces the surface of the amorphous alloy with a micro-nano structure
  • the outer mold and the inner mold sleeve are located in the vacuum a heating chamber, the vacuum hot press heats the amorphous alloy to a subcooled liquid phase region, one end of the upper indenter is inserted into the molding hole and compresses the amorphous alloy toward the microstructure template and Hold pressure for
  • the inner mold casing includes a first half casing and a second half casing that is butt-fitted with the first half casing, and both the microstructure template and the amorphous alloy are located in the first half casing between the sleeve and the second sleeve half.
  • the inner mold sleeve is made of a temperature resistant material.
  • the micro-nanostructures include nanostructures with a size of nanometers and/or microstructures with a size of micrometers.
  • the beneficial effect of the preparation method of the amorphous micro-nano structure provided by the embodiment of the present application is that: the amorphous alloy is placed in the inner mold sleeve, and the upper indenter and the lower indenter are press-fitted, so that the microstructure template is formed.
  • the micro-nano structure is copied to the amorphous alloy by hot pressing, and then the inner mold sleeve is taken out from the molding hole, so as to realize the demoulding of the amorphous alloy and the outer mold, with simple operation and high efficiency.
  • Fig. 1 is the flow chart of the preparation method of the amorphous micro-nano structure provided by the embodiment of this application;
  • FIG. 2 is a schematic structural diagram of a hot-pressing molding device provided in an embodiment of the present application.
  • Fig. 3 is the structural representation of the outer mold of Fig. 2;
  • Fig. 4 is a scanning electron microscope photograph of palladium-based amorphous alloy nanowires of different sizes obtained in an embodiment of the application;
  • FIG. 7 is a scanning electron microscope photograph of platinum-based amorphous alloy nanowires prepared in yet another embodiment of the application.
  • FIG. 8 is the XRD pattern of the palladium-based amorphous alloy before and after hot pressing in an example of the present application.
  • an embodiment of the present application provides a method for preparing an amorphous micro-nano structure, which is used to hot-press a micro-nano structure on an amorphous alloy 30.
  • the micro-nano structure has The texture structure is regular and has certain periodicity. Through different sizes and arrangements, the surface of the material can show different functional properties.
  • the preparation method of amorphous alloy 30 in amorphous micro-nano structure includes the following steps:
  • the hot-pressing mold 20 includes an outer mold 22 having a molding hole 221 and an inner mold sleeve 21 detachably placed in the molding hole 221 .
  • the hole depth direction of the molding hole 221 is vertically arranged, and the inner mold sleeve 21 is detachably placed in the molding hole 221; optionally, the material of the outer mold 22, the upper indenter 50 and the lower indenter 60 can be mold steel.
  • the inner wall of the outer mold 22 is precision machined by slow-moving wire cutting. First, a through hole is roughly drilled, and then through six precision cuttings, a molded hole 221 with a diameter of 8.00 mm and a depth of 20 mm is machined.
  • a 30*30*20mm outer mold 22 is cut with a middle wire, wherein the hole wall of the molded hole 221 is polished with a polishing paste with a particle size of 1 ⁇ m.
  • the upper ram 50 and the lower ram 60 are processed according to the size of the inner die sleeve 21 , and the end surfaces of the upper ram 50 and the lower ram 60 are polished.
  • the height of the lower indenter 60 is 5 mm, and the height of the upper indenter 50 is 21 mm.
  • S2 Arrange the lower indenter 60, the microstructure template 40 and the amorphous alloy 30 on the inner mold sleeve 21 in order from bottom to top, and grind, polish, decontaminate and clean the surface of the amorphous alloy 30.
  • the surface roughness of alloy 30 is Ra ⁇ 0.025.
  • Amorphous alloy 30 was sequentially cleaned in deionized water and ethanol-acetone mixed solution ultrasonically for 5 min.
  • the surface of the microstructure template 40 facing the amorphous alloy 30 is provided with a micro-nano structure
  • S3 Place the hot-pressing die 20 in a vacuum environment and heat the amorphous alloy 30 to the supercooled liquid phase region. It can be understood that the amorphous alloy 30 is heated to the supercooled liquid phase region, thereby making the amorphous alloy 30 To soften, one end of the upper indenter 50 is inserted into the molding hole 221, and the amorphous alloy 30 is pressed against the microstructure template 40 under the driving of external force, and the pressure is maintained for a predetermined time. The dwell time needs to avoid crystallization of the amorphous alloy 30 .
  • the inner mold sleeve 21 can prevent the bonding between the amorphous alloy 30 and the hole wall of the molding hole 221 , and reduce the wear of the hole wall of the molding hole 221 .
  • the hot-pressing mold 20 is placed in a vacuum heating chamber of a vacuum hot-pressing machine, and the vacuum heating chamber adopts resistance heating, induction heating or infrared heating to heat the hot-pressing mold 20 , the heating rate range is 5 ⁇ 150°C/min, the vacuum degree of the vacuum heating chamber is less than 0.01Pa, and nitrogen, argon, etc. can also be introduced into the vacuum heating chamber as protective gas.
  • the pressure range of the upper indenter 50 is 50-600 MPa, and the moving speed of the upper indenter 50 is in the range of 0.01-5 mm/min.
  • the amorphous alloy 30 is placed in the inner mold sleeve 21, and through the press fit of the upper indenter 50 and the lower indenter 60, the micro-nano structure on the microstructure template 40 is hot-pressed and copied to the amorphous alloy 30, and then the The inner mold sleeve 21 is taken out from the molding hole 221, so as to realize the demoulding of the amorphous alloy 30 and the outer mold 22, and the operation is simple and the efficiency is high.
  • the microstructure template 40 is fabricated from anodized aluminum.
  • the inner mold sleeve 21 includes a first half sleeve and a second half sleeve that is butt-fitted with the first half sleeve, and both the microstructure template 40 and the amorphous alloy 30 are located in the first half sleeve. Between the half set and the second half set. Optionally, the abutting surfaces of the first half-sleeve and the second half-sleeve are arranged along the hole depth direction of the embossed hole 221 .
  • the inner mold sleeve 21 can be directly opened to take out the hot-pressed amorphous alloy 30. ,easy to use.
  • the inner mold sleeve 21 is a flexible film sleeve made of temperature resistant material.
  • the inner mold sleeve 21 is a flexible film sleeve made of red copper, the thickness of the inner mold sleeve 21 is 0.25 mm, and the outer diameter is 8.00 mm.
  • the inner mold sleeve 21 is cut into small pieces with a length of 20 mm and the burrs are removed, and the inner and outer surfaces are cleaned.
  • the inner mold sleeve 21 can also be made of copper alloy, aluminum or alloy stainless steel.
  • the hot-pressed amorphous alloy 30 and the microstructure template 40 can be obtained by peeling off the soft inner mold sleeve 21, and then the microstructure template 40 can be removed to obtain the amorphous alloy 30 with a micro-nano structure. , by directly tearing the flexible inner mold sleeve 21 by hand, it is convenient to take out the amorphous alloy 30, and the operation is simple.
  • the microstructure templates 40 are plate-shaped and arranged in multiple layers, the amorphous alloy 30 is disposed between any two adjacent microstructure templates 40, and each microstructure template 40 faces the corresponding amorphous alloy.
  • the surfaces of 30 are all provided with micro-nano structures.
  • the dimensional micro-nano structures can be hot-pressed on the two surfaces of the amorphous alloy 30, and a plurality of amorphous alloys 30 can also be processed at one time, which improves the hot pressing. effectiveness.
  • the micro-nano structures include nano-structures with a size of nano-scale and micro-structures with a size of micro-scale.
  • the microstructure template 40 can also be provided with microstructures and nanostructures at the same time. It can be understood that, the nano-structure and the micro-structure can be simultaneously hot-pressed on the amorphous alloy 30 by one hot pressing.
  • the nanostructures are 10 nanometers, 80 nanometers, 100 nanometers or 200 nanometers in size.
  • the micro-nano structure can be prepared by hot pressing of the amorphous alloy 30, especially the replication of the nano-structure has an accurate replication effect, and an amorphous nano-structure of about 10 nanometers can be replicated at the highest.
  • the thermal expansion coefficients of the upper ram 50 and the lower ram 60 are the same.
  • the upper indenter 50 and the lower indenter 60 are made of the same material, which may be metal, ceramic and other composite materials. The upper indenter 50 and the lower indenter 60 maintain the same thermal expansion during the hot-pressing process, thereby facilitating the stability and reliability of the hot-pressing.
  • the hole wall of the molded hole 221 is mirror-finished. Through the mirror surface processing, the mold release of the inner mold sleeve 21 and the outer mold 22 can be improved.
  • the temperature range ⁇ T of the subcooled liquid phase region is greater than or equal to 40°C.
  • the hot-press forming device 100 is used for hot-press forming the amorphous alloy 30 .
  • the hot-press forming device 100 includes an outer mold 22 , an inner mold The mold sleeve 21 , the upper indenter 50 , the lower indenter 60 , the vacuum hot press with a vacuum heating chamber, and the microstructure template 40 , the outer mold 22 is provided with a molding hole 221 , and the inner mold sleeve 21 is detachably arranged in the molding hole 221 ;
  • the lower indenter 60, the microstructure template 40 and the amorphous alloy 30 are sequentially arranged in the inner mold sleeve 21 from bottom to top, and the microstructure template 40 is provided with a micro-nano structure on the surface of the amorphous alloy 30; the outer mold 22 and the inner mold
  • the sleeve 21 is located in the vacuum heating chamber.
  • the vacuum hot press heats the amorphous alloy 30 to the subcooled liquid phase region.
  • One end of the upper indenter 50 is inserted into the molding hole 221 and presses the amorphous alloy 30 toward the microstructure template 40 and maintains a predetermined pressure. time.
  • the hot pressing forming apparatus 100 further includes a temperature sensor for measuring the temperature of the amorphous alloy 30, the outer mold 22 is provided with a temperature measuring hole 50, and the temperature measuring end of the temperature sensor is disposed in the temperature measuring hole 50, wherein, The diameter of the temperature measuring hole 50 is 1 mm, the distance from the bottom of the outer mold is 6 mm, and the distance from the inner wall of the molding hole 221 is 2.5 mm.
  • a 7mm diameter Pd 40 Ni 10 Cu 30 P 20 palladium-based amorphous alloy 30 rod is prepared by copper mold suction casting method, and a 0.5mm thick slice is cut out, and one side of the slice is ground and polished , and then polished with 1 ⁇ m polishing solution for 30 min, and ultrasonically cleaned the whole sample, and then confirmed the amorphous state by XRD detection.
  • the microstructure template 40 is a dual-channel anodized aluminum template, with an external diameter of 7.4 mm, a micro-nano structure pore depth of 50,000 nanometers, and pore diameters of 20 nanometers, 40 nanometers, 80 nanometers, 110 nanometers, and 300 nanometers, respectively.
  • Figure 4 is a scanning electron microscope photo of palladium-based nanowires:
  • Figure 4(a) is a nanostructure with a size of 300 nm
  • Figure 4(b) shows the palladium-based nanowire length of 300 nm
  • Figure 4(c) is a nanostructured palladium-based amorphous nanowire with a size of 80 nm;
  • Figure 4(d) is a nanowire with a nanostructure of 40 nm in size.
  • palladium-based amorphous nanostructures of different sizes can be prepared by the above method, and the length of the nanowires can be adjusted by a hot pressing process, and the surface of the prepared nanostructures is smooth and defect-free.
  • the palladium-based amorphous 81 after hot pressing has no crystallization phenomenon compared with the palladium-based amorphous 82 before hot pressing.
  • a 5mm diameter La 55 Al 25 Ni 5 Cu 10 Co 5 amorphous alloy 30 rod was prepared by copper mold suction casting method, and a 1.5mm thick slice was cut, and one side of the slice was ground and polished, and finally polished with 1 ⁇ m Liquid polishing for 30 min, and ultrasonic cleaning of the entire sample, and then confirmed by XRD to be amorphous.
  • the microstructure template 40 is an anodized aluminum template, and the appearance diameter of the microstructure template 40 is 7.4 mm.
  • the pore size of the micro-nano structure is 110 nanometers, 200 nanometers, 300 nanometers, and 390 nanometers.
  • the hot-pressing mold 20 is fixedly placed into the high-vacuum hot-pressing machine, the temperature sensor is inserted into the hot-pressing mold 20, the vacuum is made to be lower than 0.01 Pa by means of a molecular pump, and is heated at a heating rate of 30° C./min by means of infrared heating.
  • the temperature of the hot-pressing mold 20 reaches 210-250°C, the heating is stopped, and a pressure of 50-500 MPa is slowly applied to the upper indenter 50, and after maintaining the pressure for 1 minute, the nitrogen purge is turned on to cool down, and when the temperature is lower than 150°C, the hot-pressing mold 20 is taken out. Cool in cold water.
  • the amorphous alloy 30 sample was then taken out, and the anodic aluminum template was removed by etching in a 15% NaOH aqueous solution to obtain a characteristic black structure.
  • the samples were characterized by XRD and SEM.
  • Figure 5(b) shows the lanthanum-based nanowire length of 300 nm.
  • lanthanum-based amorphous nanowires with easily oxidized surfaces can also be prepared by this method, and the length of the nanowires can be adjusted by hot pressing process.
  • the surface of the prepared nanostructures is smooth and defect-free, and characterized by XRD , the lanthanum-based amorphous alloy 30 has no crystallization before and after hot pressing.
  • a Zr 35 Ti 30 Cu 8.25 Be 26.75 amorphous alloy 30 rod with a diameter of 7mm was prepared by copper mold suction casting, and a 0.5mm thick slice was cut, and one side of the slice was ground and polished, and finally polished with a 1 ⁇ m polishing solution 30min, and ultrasonically cleaned the whole sample, and then confirmed the amorphous state by XRD.
  • the microstructure template 40 is an anodized aluminum template with an appearance diameter of 7.4 mm and a pore diameter of 300 nanometers.
  • the hot-pressing mold 20 is fixedly placed into the high-vacuum hot-pressing machine, the temperature sensor is inserted into the hot-pressing mold 20, the vacuum is made to be lower than 0.01 Pa by means of a molecular pump, and heated at a heating rate of 100° C./min by means of infrared heating.
  • the temperature of the hot-pressing mold 20 reaches 350°C, the heating is stopped, and a pressure of 300 MPa is slowly applied to the upper indenter 50, and after maintaining the pressure for 1 minute, the nitrogen purge is turned on to cool down, and when the temperature is lower than 250°C, the hot-pressing mold 20 is taken out and placed in cold water. Cool down.
  • the amorphous alloy 30 sample was then taken out, and the anodic aluminum template was removed by etching in a 15% NaOH aqueous solution to obtain a characteristic black structure.
  • the samples were characterized by XRD and SEM.
  • the scanning electron microscope photo of the zirconium-based nanowires, with a size of 300 nanometers, is characterized by XRD, and the zirconium-based amorphous alloy 30 has no crystallization before and after hot pressing.
  • the microstructure template 40 is an anodized aluminum template with an appearance diameter of 7.4 mm and a pore size of 10 nanometers, 20 nanometers, 40 nanometers, 80 nanometers, 110 nanometers, and 300 nanometers.
  • the hot-pressing mold 20 is fixedly placed into the high-vacuum hot-pressing machine, the temperature sensor is inserted into the hot-pressing mold 20, the vacuum is made to be lower than 0.01 Pa by means of a molecular pump, and is heated at a heating rate of 30° C./min by means of infrared heating.
  • the temperature of the hot-pressing mold 20 reaches 280°C, the heating is stopped, and a pressure of 50-500 MPa is slowly applied to the upper indenter 50, and after maintaining the pressure for 1 min, the nitrogen purge is turned on to cool down, and when the temperature is lower than 250°C, the hot-pressing mold 20 is taken out and placed in Cool in cold water.
  • the amorphous alloy 30 sample was then taken out, and the anodic aluminum template was removed by etching in a 15% NaOH aqueous solution to obtain a characteristic black structure.
  • the samples were characterized by XRD and SEM.
  • Figure 7 is a scanning electron microscope photo of platinum-based nanowires:
  • Figure 7(a) is a nanostructure with a size of 110 nm
  • Figure 7(b) is a magnified image of 110 nm platinum-based nanowires.

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Abstract

一种非晶微纳结构的制备方法及热压成型装置，包括准备热压模具（20）、上压头（50）、下压头（60）以及微结构模板（40），热压模具（20）包括开设有模压孔的外模具（22）以及可拆卸地放置于模压孔的内模套（21）；将下压头（60）、微结构模板（40）以及非晶合金（30）从下往上依次设置于内模套（21）；将热压模具（20）置于真空环境中并将非晶合金加热至过冷液相区，上压头（50）的一端插入模压孔并朝微结构模板压紧非晶合金且保压预定时间；将非晶合金（30）进行冷却并取出复制有微纳结构的非晶合金。该制备方法及热压成型装置可以降低非晶合金与外模具的脱模难度。

Description

一种非晶微纳结构的制备方法及热压成型装置
本申请要求于2020年08月31日在中国专利局提交的、申请号为202010893909.X、发明名称为“一种非晶微纳结构的制备方法及热压成型装置”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本申请属于非晶合金热压成型技术领域，尤其涉及一种非晶微纳结构的制备方法及热压成型装置。
 背景技术
这里的陈述仅提供与本申请有关的背景信息，而不必然构成现有技术。
目前，非晶合金也称液态金属或金属玻璃，其一般是熔融态合金急冷凝固使得体系来不及结晶所形成，原子排列继承液态具有的长程无序、短程有序点的结构特点，从而具有很多优异的力学与物化性能。
非晶合金在热力学上属于亚稳态材料，当温度升高时，材料会发生玻璃化转变，继续升高温度进而诱发晶化反应。在玻璃化转变与晶化开始温度之间一般存在20~120℃的温度区间，这个温度区间被称为过冷液相区。正是由于这一区间的存在，赋予了非晶合金具有和氧化物玻璃及其相似的性质，呈现粘流性状态，表现出优良的超塑性。从而避免了室温条件下非晶合金高强度、高硬度、引起的加工困难、可塑性差的问题。与传统成形工艺相比，非晶合金超塑性成形零件具有高强度、高精度、高表面光洁度的特点，非常适用于航空航天、精密机械、医疗器械、电子消费等产品的加工制造。
现有技术中的非晶合金超塑性成形，其基本原理都是利用过冷液相区间的热压法。技术方案多以加工解决宏观零件为目的，宏观结构的非晶合金成型往往需要较小的成形压力，脱模也容易。但是对于微纳结构尤其纳米结构的制备，由于结构尺寸小填充阻力大，为了成型充分往往需要施加极大的压力，非晶合金会向四周填充模具的模压腔并挤压模压腔的内壁，冷却后非晶合金会粘接模压腔的内壁，从而造成脱模困难，而强制脱模会造成产品和模具变形，严重时无法脱模。
 技术问题
本申请实施例的目的之一在于：提供一种非晶微纳结构的制备方法，旨在解决非晶合金在热压过程中脱模困难的问题。
 技术解决方案
为解决上述技术问题，本申请实施例采用的技术方案是：
第一方面，提供了一种非晶微纳结构的制备方法，用于在非晶合金上热压出微纳结构，所述非晶微纳结构的制备方法包括以下步骤：
准备热压模具、上压头、下压头以及微结构模板，所述热压模具包括开设有模压孔的外模具以及可拆卸地放置于所述模压孔的内模套；
将所述下压头、所述微结构模板以及所述非晶合金从下往上依次设置于所述内模套，所述微结构模板朝向所述非晶合金的表面开设有微纳结构；
将所述热压模具置于真空环境中并将所述非晶合金加热至过冷液相区，所述上压头的一端插入所述模压孔并朝所述微结构模板压紧所述非晶合金且保压预定时间；
将所述非晶合金进行冷却并取出复制有所述微纳结构的非晶合金。
在一个实施例中，所述内模套包括第一半套和与所述第一半套对接配合的第二半套，所述微结构模板和所述非晶合金均位于所述第一半套和所述第二半套之间。
在一个实施例中，所述内模套是由耐温材料制成的柔性薄膜套。
在一个实施例中，所述微结构模板层叠设置有多个，任意相邻的两所述微结构模板之间均设置有所述非晶合金，各所述微结构模板朝向对应的所述非晶合金的表面均开设有微纳结构。
在一个实施例中，所述微纳结构包括尺寸为纳米级的纳米结构和尺寸为微米级的微米结构。
在一个实施例中，所述微结构模板开设有所述微米结构和所述纳米结构。
在一个实施例中，所述上压头和所述下压头的热膨胀系数相同。
在一个实施例中，所述模压孔的内壁镜面加工处理。
在一个实施例中，所述过冷液相区的温度区间ΔT≥40℃。
第二方面，本申请还提供了一种热压成型装置，用于对非晶合金进行热压成型，所述热压成型装置包括外模具、内模套、上压头、下压头、具有真空加热室的真空热压机以及微结构模板，所述外模具开设有模压孔，所述内模套可拆卸地设置于所述模压孔；所述下压头、所述微结构模板以及所述非晶合金从下往上依次设置于所述内模套，所述微结构模板朝向所述非晶合金的表面开设有微纳结构；所述外模具和所述内模套位于所述真空加热室，所述真空热压机将所述非晶合金加热至过冷液相区，所述上压头的一端插入所述模压孔并朝所述微结构模板压紧所述非晶合金且保压预定时间。
在一个实施例中，所述内模套包括第一半套和与所述第一半套对接配合的第二半套，所述微结构模板和所述非晶合金均位于所述第一半套和所述第二半套之间。
在一个实施例中，所述内模套是由耐温材料所制成。
在一个实施例中，所述微纳结构包括尺寸为纳米级的纳米结构和/或尺寸为微米级的微米结构。
 有益效果
本申请实施例提供的非晶微纳结构的制备方法的有益效果在于：将非晶合金放置在内模套，并通过上压头和下压头的压紧配合，从而将微结构模板上的微纳结构热压复制至非晶合金，再将内模套从模压孔内取出来，从而实现非晶合金和外模具的脱模，操作简单，效率高。
 附图说明
为了更清楚地说明本申请实施例中的技术方案，下面将对实施例或示范性技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本申请的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其它的附图。
图1为本申请实施例提供的非晶微纳结构的制备方法的流程图；
图2是本申请实施例提供的热压成型装置的结构示意图；
图3是图2的外模具的结构示意图；
图4为本申请一个实施例中制得的不同尺寸钯基非晶合金纳米线扫描电镜照片图；
图5为本申请另一实施例中制得的不同尺寸镧基非晶合金纳米线扫描电镜照片图；
图6为本申请又一实施例中制得锆基非晶合金纳米线扫描电镜照片图；
图7为本申请再一实施例中制得的铂基非晶合金纳米线扫描电镜照片图；
图8是本申请一个实施例中热压前后钯基非晶合金的XRD图谱。
 本发明的实施方式
为了使本申请的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本申请进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本申请。
需说明的是，当部件被称为“固定于”或“设置于”另一个部件，它可以直接在另一个部件上或者间接在该另一个部件上。当一个部件被称为是“连接于”另一个部件，它可以是直接或者间接连接至该另一个部件上。术语“上”、“下”、“左”、“右”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本申请的限制，对于本领域的普通技术人员而言，可以根据具体情况理解上述术语的具体含义。术语“第一”、“第二”仅用于便于描述目的，而不能理解为指示或暗示相对重要性或者隐含指明技术特征的数量。“多个”的含义是两个或两个以上，除非另有明确具体的限定。
为了说明本申请所述的技术方案，以下结合具体附图及实施例进行详细说明。
请参阅图1及图3，本申请实施例提供了一种非晶微纳结构的制备方法，其用于在非晶合金30上热压出微纳结构，可选地，微纳结构是具有纹理结构规则、并有一定的周期性等特点，通过不同的尺寸和排列组合，可使材料表面表现出不同的功能特性。非晶合金30在非晶微纳结构的制备方法包括以下步骤：
S1：准备热压模具20、上压头50、下压头60、微结构模板40；
热压模具20包括开设有模压孔221的外模具22以及可拆卸地放置于模压孔221内的内模套21。模压孔221的孔深方向竖直设置，将内模套21可拆卸地放置于模压孔221；可选地，外模具22、上压头50和下压头60的材料均可以为模具钢。外模具22的内壁利用慢走丝线切割进行精密加工，首先粗钻出穿丝通孔，然后经过六次精密切割，加工出直径为8.00mm，且深度为20mm的模压孔221。然后用中走丝线切割出30*30*20mm的外模具22，其中模压孔221的孔壁用颗粒尺寸为1μm的抛光膏进行抛光。上压头50和下压头60根据内模套21的尺寸而加工，并对上压头50和下压头60的端面进行抛光。其中，下压头60的高度为5mm，上压头50的高度为21mm。
S2：将下压头60、微结构模板40以及非晶合金30从下往上依次设置于内模套21，并对非晶合金30的表面研磨抛光、去污清洗，可选地，非晶合金30的表面粗糙度Ra≤0.025。非晶合金30依次在去离子水、乙醇-丙酮混合液超声中清洗5min。
微结构模板40朝向非晶合金30的表面开设有微纳结构；
S3：将热压模具20置于真空环境中并将非晶合金30加热至过冷液相区，可以理解的是，将非晶合金30加热至过冷液相区，从而使非晶合金30软化，上压头50的一端插入模压孔221并在外力的驱动下朝微结构模板40压紧非晶合金30且保压预定时间，可选地，保压时间的范围为0~5min，同时保压时间需避免非晶合金30发生晶化。在热压成型过程中，内模套21可以避免非晶合金30与模压孔221的孔壁之间发生粘接，并降低了模压孔221孔壁的磨损。
请参阅图1及图3，可选地，将热压模具20放置于真空热压机的真空加热室，真空加热室采用电阻加热、感应加热或红外加热的方式，对热压模具20进行加热，升温速率的范围为5~150℃/min，真空加热室的真空度小于0.01Pa，并还可在真空加热室内通入氮气、氩气等作为保护气体。可选地，上压头50的压力范围为50~600MPa，且上压头50的移动速率的范围为0.01~5mm/min。
S4：将非晶合金30进行冷却并取出复制有微纳结构的非晶合金30。可选地，可以通过液氮对非晶合金30进行冷却，也可直接将模具取出并迅速放入冷却溶液中。
将非晶合金30放置在内模套21，并通过上压头50和下压头60的压紧配合，从而将微结构模板40上的微纳结构热压复制至非晶合金30，再将内模套21从模压孔221内取出来，从而实现非晶合金30和外模具22的脱模，操作简单，效率高。
可选地，微结构模板40由阳极氧化铝制作而成。
请参阅图1及图3，在一个实施例中，内模套21包括第一半套和与第一半套对接配合的第二半套，微结构模板40和非晶合金30均位于第一半套和第二半套之间。可选地，第一半套和第二半套的对接面沿模压孔221的孔深方向设置。可以理解的是，通过将内模套21设置成两个半套，从而在非晶合金30与外模具22完成脱模后，可以直接打开内模套21而取出热压成形的非晶合金30，操作简单。
在一个实施例中，内模套21是由耐温材料制成的柔性薄膜套。可选地，内模套21是由紫铜制成的柔性薄膜套，内模套21的厚度为0.25mm，外径为8.00mm。内模套21切割成长度为20mm的小段并去除毛边，清洗内外表面。在其它实施例中，内模套21也可以由铜合金、铝或合金不锈钢制成。可以理解的是，通过剥离柔软的内模套21即可得热压成型后的非晶合金30和微结构模板40，再去除微结构模板40，便可得到具有微纳结构的非晶合金30，通过直接用手撕开柔性的内模套21，方便取出非晶合金30，操作简单。
在一个实施例中，微结构模板40呈板状且层叠设置有多个，任意相邻的两微结构模板40之间均设置有非晶合金30，各微结构模板40朝向对应的非晶合金30的表面均开设有微纳结构。可选地，通过层叠设置多个微结构模板40，从而可以在非晶合金30的两个表面热压出维微纳结构，且还可以一次性加工多个非晶合金30，提高了热压效率。
请参阅图1及图2，在一个实施例中，所述微纳结构包括尺寸为纳米级的纳米结构和尺寸为微米级的微米结构。
在一个实施例中，微结构模板40也可同时开设有微米结构和纳米结构。可以理解的是，通过一次热压可以在非晶合金30上同时热压出纳米结构和微米结构。
在一个实施例中，纳米结构的尺寸为10纳米、80纳米、100纳米或200纳米。本实施例可以对非晶合金30热压制备微纳结构尤其对纳米结构的复制具有精确的复制效果，最高可复制得到10纳米左右的非晶纳米结构。
在一个实施例中，上压头50和下压头60的热膨胀系数相同。可选地，上压头50和下压头60由相同材料制成，材料可以是金属、陶瓷及其它复合材料。上压头50和下压头60在热压过程中保持相同的热膨胀，从而有利于热压的稳定和可靠。
在一个实施例中，模压孔221的孔壁镜面加工处理。通过镜面加工处理，可以提高内模套21和外模具22的脱模。
在一个实施例中，过冷液相区的温度区间ΔT≥40℃。
请参阅图1及图2，本申请还提出了一种热压成型装置100，该热压成型装置100用于对非晶合金30进行热压成型，热压成型装置100包括外模具22、内模套21、上压头50、下压头60、具有真空加热室的真空热压机以及微结构模板40，外模具22开设有模压孔221，内模套21可拆卸地设置于模压孔221；下压头60、微结构模板40以及非晶合金30从下往上依次设置于内模套21，微结构模板40朝向非晶合金30的表面开设有微纳结构；外模具22和内模套21位于真空加热室，真空热压机将非晶合金30加热至过冷液相区，上压头50的一端插入模压孔221并朝微结构模板40压紧非晶合金30且保压预定时间。
在一个实施例中，热压成型装置100还包括用于测量非晶合金30温度的温度传感器，外模具22开设有测温孔50，温度传感器的测温端设置于测温孔50，其中，测温孔50的直径为1mm，距离外模的底部6mm，距离模压孔221的内壁2.5mm。
请参阅图4和图8，利用铜模吸铸法制备7mm直径的 Pd 40Ni 10Cu 30P 20钯基非晶合金30棒材，并切割出0.5mm厚的薄片，将薄片的一面研磨抛光，再用1μm的抛光液抛光30min，并超声清洗整个样品，然后通过XRD检测确保为非晶态。
微结构模板40选择双通道阳极氧化铝模板，外观直径为7.4mm，微纳结构的孔深为50000纳米，孔径分别为20纳米、40纳米、80纳米、110纳米、300纳米。
将热压模具20固定放入高真空热压机，将温度传感器插入外模具22的测温孔50，利用分子泵抽至真空度低于0.01Pa，利用红外加热的方式，以50℃/min的升温速率加热，待热压模具20温度达到330℃时停止加热，对上压头50缓慢施加400MPa的压力，并保压1min后开启氮气吹扫降温，当温度低于250℃取出热压模具20置于冷水中降温，再取出样品，在15%的NaOH水溶液中腐蚀去掉阳极氧化铝模板，得到表观黑色结构。并将热压后的非晶合金30样品的表征通过XRD、SEM扫描。
如图4，是钯基纳米线的扫描电子显微镜照片：
其中，图4（a）是尺寸为300纳米的纳米结构；
图4（b）为300纳米的钯基纳米线长度；
图4（c）是尺寸为80纳米的纳米结构的钯基非晶纳米线；
图4（d）是尺寸为40纳米的纳米结构的纳米线。
从图4中可以看出利用上述方法可以制备出不同尺寸的钯基非晶纳米结构，并且纳米线长度可通过热压工艺进行调节，制备的纳米结构表面光滑无缺陷。
如图8通过XRD表征，热压后的钯基非晶81相比热压前的钯基非晶82并无晶化现象。
请参阅图5，利用铜模吸铸法制备5mm直径的La 55 Al 25Ni 5Cu 10Co 5非晶合金30棒材，切割出1.5mm厚的薄片，将薄片的一面研磨抛光最后用1μm抛光液抛光30min，并超声清洗整个样品，然后通过XRD检测确保为非晶态。
微结构模板40选择阳极氧化铝模板，微结构模板40的外观直径为7.4mm。微纳结构的孔径为110纳米、200纳米、300纳米、390纳米。
将热压模具20固定放入高真空热压机，将温度传感器插入热压模具20，利用分子泵抽制真空低于0.01Pa，利用红外加热的方式以30℃/min的升温速率加热，待热压模具20的温度达到210~250℃时停止加热，对上压头50缓慢施加50-500MPa的压力，并保压1min后开启氮气吹扫降温，当温度低于150℃取出热压模具20置于冷水中降温。再取出非晶合金30样品，在15%的NaOH水溶液中腐蚀去掉阳极氧化铝模板，得到表征黑色结构。
样品的表征通过XRD、SEM。
如图5，镧基纳米线的扫描电子显微镜照片：
其中，图5（a）尺寸为200纳米的纳米结构；
图5（b）为300纳米的镧基纳米线长度。
从图5中可以看出，利用此方法同样可以制备出表面易氧化的镧基非晶纳米线，并且纳米线长度可通过热压工艺调节，制备的纳米结构表面光滑无缺陷，且通过XRD表征，热压前后镧基非晶合金30并无晶化现象。
请参阅图6，利用铜模吸铸法制备7mm直径的Zr 35 Ti 30Cu 8.25Be 26.75非晶合金30棒材，切割出0.5mm厚的薄片，将薄片的一面研磨抛光最后用1μm抛光液抛光30min，并超声清洗整个样品，然后通过XRD检测确保为非晶态。
微结构模板40选择阳极氧化铝模板，外观直径为7.4mm，孔径300纳米。
将热压模具20固定放入高真空热压机，将温度传感器插入热压模具20，利用分子泵抽制真空低于0.01Pa，利用红外加热的方式以100℃/min的升温速率加热，待热压模具20的温度达到350℃时停止加热，对上压头50缓慢施加300MPa的压力，并保压1min后开启氮气吹扫降温，当温度低于250℃取出热压模具20置于冷水中降温。再取出非晶合金30样品，在15%的NaOH水溶液中腐蚀去掉阳极氧化铝模板，得到表征黑色结构。
样品的表征通过XRD、SEM。
如图6，锆基纳米线的扫描电子显微镜照片，尺寸为300纳米结构，通过XRD表征，热压前后锆基非晶合金30并无晶化现象。
请参阅图7，利用铜模吸铸法制备5mm直径的Pt 57.5Cu 14.7Ni 5.3P 22.5非晶合金30棒材，切割出1.5mm厚的薄片，将薄片的一面研磨抛光最后用1μm抛光液抛光30min，并超声清洗整个样品，然后通过XRD检测确保为非晶态。
微结构模板40选择阳极氧化铝模板，外观直径为7.4mm，孔径为10纳米、20纳米、40纳米、80纳米、110纳米、300纳米。
将热压模具20固定放入高真空热压机，将温度传感器插入热压模具20，利用分子泵抽制真空低于0.01Pa，利用红外加热的方式以30℃/min的升温速率加热，待热压模具20的温度达到280℃时停止加热，对上压头50缓慢施加50~500MPa的压力，并保压1min后开启氮气吹扫降温，当温度低于250℃取出热压模具20置于冷水中降温。再取出非晶合金30样品，在15%的NaOH水溶液中腐蚀去掉阳极氧化铝模板，得到表征黑色结构。
样品的表征通过XRD、SEM。
如图7，是铂基纳米线的扫描电子显微镜照片：
图7（a）为尺寸为110纳米的纳米结构，
图7（b）为110纳米的铂基纳米线放大图像。
从图7中可以看出利用此方法可以大面积制备出铂基非晶纳米结构，并且纳米线长度可通过热压工艺调节，制备的纳米结构表面光滑无缺陷，通过XRD表征，热压前后铂基非晶合金30并无晶化现象。
以上仅为本申请的可选实施例而已，并不用于限制本申请。对于本领域的技术人员来说，本申请可以有各种更改和变化。凡在本申请的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本申请的权利要求范围之内。

Claims (13)

  1. 一种非晶微纳结构的制备方法，用于在非晶合金上热压出微纳结构，其特征在于，所述非晶微纳结构的制备方法包括以下步骤：
    准备热压模具、上压头、下压头以及微结构模板，所述热压模具包括开设有模压孔的外模具以及可拆卸地放置于所述模压孔的内模套；
    将所述下压头、所述微结构模板以及所述非晶合金从下往上依次设置于所述内模套，所述微结构模板朝向所述非晶合金的表面开设有微纳结构；
    将所述热压模具置于真空环境中并将所述非晶合金加热至过冷液相区，所述上压头的一端插入所述模压孔并朝所述微结构模板压紧所述非晶合金且保压预定时间；
    将所述非晶合金进行冷却并取出复制有所述微纳结构的非晶合金。
  2. 如权利要求1所述的非晶微纳结构的制备方法，其特征在于：所述内模套包括第一半套和与所述第一半套对接配合的第二半套，所述微结构模板和所述非晶合金均位于所述第一半套和所述第二半套之间。
  3. 如权利要求1所述的非晶微纳结构的制备方法，其特征在于：所述内模套是由耐温材料制成的柔性薄膜套。
  4. 如权利要求1所述的非晶微纳结构的制备方法，其特征在于：所述微结构模板层叠设置有多个，任意相邻的两所述微结构模板之间均设置有所述非晶合金，各所述微结构模板朝向对应的所述非晶合金的表面均开设有微纳结构。
  5. 如权利要求1所述的非晶微纳结构的制备方法，其特征在于：所述微纳结构包括尺寸为纳米级的纳米结构和尺寸为微米级的微米结构。
  6. 如权利要求5所述的非晶微纳结构的制备方法，其特征在于：所述微结构模板开设有所述微米结构和所述纳米结构。
  7. 如权利要求1所述的非晶微纳结构的制备方法，其特征在于：所述上压头和所述下压头的热膨胀系数相同。
  8. 如权利要求1所述的非晶微纳结构的制备方法，其特征在于：所述模压孔的内壁镜面加工处理。
  9. 如权利要求1所述的非晶微纳结构的制备方法，其特征在于：所述过冷液相区的温度区间ΔT≥40℃。
  10. 一种热压成型装置，用于对非晶合金进行热压成型，其特征在于，所述热压成型装置包括外模具、内模套、上压头、下压头、具有真空加热室的真空热压机以及微结构模板，所述外模具开设有模压孔，所述内模套可拆卸地设置于所述模压孔；所述下压头、所述微结构模板以及所述非晶合金从下往上依次设置于所述内模套，所述微结构模板朝向所述非晶合金的表面开设有微纳结构；所述外模具和所述内模套位于所述真空加热室，所述真空热压机将所述非晶合金加热至过冷液相区，所述上压头的一端插入所述模压孔并朝所述微结构模板压紧所述非晶合金且保压预定时间。
  11. 如权利要求10所述的热压成型装置，其特征在于：所述内模套包括第一半套和与所述第一半套对接配合的第二半套，所述微结构模板和所述非晶合金均位于所述第一半套和所述第二半套之间。
  12. 如权利要求10所述的热压成型装置，其特征在于：所述内模套是由耐温材料所制成。
  13. 如权利要求10所述的热压成型装置，其特征在于：所述微纳结构包括尺寸为纳米级的纳米结构和/或尺寸为微米级的微米结构。
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