1. A preparation method of a high-strength plastic amorphous composite material is characterized by comprising the following steps:

(1) preparation of an as-cast sample: removing oxide skin from amorphous material, weighing according to weight ratio of components, ultrasonically cleaning, placing into vacuum arc furnace, vacuumizing until the pressure in furnace is 1.5 × 10^-3When Pa is needed, closing the molecular pump, opening the mechanical pump, introducing protective gas argon to 0.05Pa, repeatedly smelting until the components of the amorphous material are homogenized, wherein the smelting current is less than or equal to 400mA, and then carrying out suction casting;

(2) pre-deformation: cutting an amorphous material rod to a proper height, polishing to ensure that the upper surface and the lower surface are horizontal, and performing pre-deformation after the height of a sample is measured, wherein the pre-deformation amount is less than or equal to 6% after the yield point;

(3) and (3) heat treatment: taking out after reaching the preset deformation, ultrasonically cleaning the sample again, vacuum packaging by using a quartz tube, preheating a resistance furnace at 900 ℃, putting the sample into the quartz tube after reaching the preset temperature of 900 ℃, preserving the temperature for 8-16min, taking out and rapidly water-quenching.

Background

Since the 21 st century, more and more scholars are invested in the field of amorphous research, on one hand, amorphous alloys show excellent mechanical properties such as high strength, high hardness, high elastic limit and wear resistance; on the other hand, a large amount of amorphous alloy is researched and designed, the mechanical property and the process property of the amorphous alloy are improved unprecedentedly, but the most critical room temperature brittleness of the amorphous alloy is not effectively solved, and the amorphous alloy becomes the biggest obstacle to the application of the bulk amorphous alloy. The material performance is closely related to the structure, so the room temperature brittleness of the material can be improved by regulating and controlling the structure change of the amorphous composite material. The existing amorphous composite material treatment process comprises a semi-solid processing technology, cryogenic treatment, shot blasting, rolling, annealing treatment and the like, but the mechanical property of the finally obtained material is poor. Therefore, it is very necessary to invent a heat treatment process capable of effectively improving the texture of the material and enhancing the mechanical properties of the material.

Disclosure of Invention

The invention aims to provide a preparation method of a high-strength plastic amorphous composite material.

The invention is realized by the following technical scheme.

The preparation method of the high-strength plastic amorphous composite material comprises the following steps.

(1) Preparation of as-cast samples.

Removing oxide skin from amorphous material, weighing according to weight ratio of components, ultrasonically cleaning, placing into vacuum arc furnace, vacuumizing until the pressure in furnace is 1.5 × 10^-3And when Pa is needed, closing the molecular pump, opening the mechanical pump, introducing protective gas argon to 0.05Pa, repeatedly smelting until the components of the amorphous material are homogenized, wherein the smelting current is less than or equal to 400mA, and then carrying out suction casting.

(2) And (4) pre-deforming.

Cutting an amorphous material rod to a proper height, polishing to ensure that the upper surface and the lower surface are horizontal, and performing pre-deformation after the height of a sample is measured, wherein the pre-deformation amount is 3-15% behind the yield point;

(3) and (4) performing a heat treatment process.

Taking out the sample after reaching the preset deformation, ultrasonically cleaning the sample again, then carrying out vacuum packaging by using a quartz tube, preheating a resistance furnace, taking the sample to 900 ℃, putting the sample into the quartz tube after reaching the preset temperature of 900 ℃, keeping the temperature for 8-16min, and then taking out the sample and rapidly carrying out water quenching.

The amorphous composite material prepared by the method has the advantages of fine crystal grains, uniform distribution and high roundness. Meanwhile, the heat treatment process has the advantages of short flow, high efficiency, low equipment requirement, simple operation and less pollution.

Drawings

FIG. 1 is a structure diagram after heat treatment. The graphs a, b and c correspond to the structure graphs after the heat treatment in examples 1, 2 and 3, respectively.

FIG. 2 is a shear band diagram after heat treatment. Wherein, the graphs a, b and c respectively correspond to the shear band graphs after the heat treatment of the examples 1, 2 and 3, and the strips indicated by the arrows are shear bands (shear bands).

Detailed Description

The invention is further described below with reference to the accompanying drawings.

Example 1.

The preparation method of the high-strength plastic amorphous composite material comprises the following steps.

(1) Preparation of as-cast samples.

Adding Zr_60.0Ti_14.7Nb_5.3Cu_5.6Ni_4.4Be_10.0Weighing amorphous material components in proportion by weight, cleaning in an ultrasonic cleaner for 30 mm, air drying, placing in a copper crucible, placing low-melting-point material at the bottom, high-melting-point material at the top, placing the copper crucible in a vacuum arc furnace, vacuumizing with a molecular pump, and keeping the pressure in the furnace to 1.5 × 10^-3And when Pa is needed, closing the molecular pump, opening the mechanical pump, and introducing protective gas argon to 0.05 Pa.

And (3) turning on a smelting power supply, smelting the titanium block, and detecting whether oxygen remains in the furnace at a smelting current of 400 mA. And melting and cooling the amorphous material, turning the ingot by using a mechanical arm, melting again, and repeating the step for 5 times to ensure the homogenization of the material components. And (3) putting the ingot with uniform components into a crucible of a mold by using a mechanical arm, melting the amorphous material by the same operation, and pressing a suction casting valve to obtain the amorphous composite material bar with the length of 70 mm.

(2) And (4) pre-deforming.

Cutting the amorphous rod to obtain an amorphous rod with the height of 8-10mm, polishing the amorphous rod by 2000# abrasive paper, measuring the height of the amorphous rod again, placing a compression test platform of an MTS universal tester horizontally, and performing room-temperature quasi-static compression and pre-deformation at the compression rate of 1 multiplied by 10⁻⁴S⁻¹. Firstly, performing as-cast press-breaking to determine the yield strength and plastic strain of the material, wherein the plastic deformation starting point in the subsequent pre-deformation process is based on the condition that the stress reaches the yield strength, and the pre-deformation amount is 6 percent behind the yield deformation point, namely the plastic deformation is 6 percent;

(3) and (4) performing a heat treatment process.

And (3) putting the pre-deformed cast sample into an ultrasonic cleaner, cleaning and drying, then packaging by using a quartz tube with the diameter of about 6mm, and vacuumizing the quartz tube during packaging to ensure that the material is not interfered by oxygen in the heating process. The resistance furnace is preheated for 8 minutes before the experiment, so that the temperature of the resistance furnace is ensured not to be suddenly changed in the heat treatment process. The heating temperature is 900 ℃, and the heat preservation time is 10 minutes. And (3) after the quartz tube is placed into the resistance furnace, timing is started after the instrument is stabilized, the water quenching is quickly taken out after the set heat preservation time is reached, and the quartz tube is smashed by using a clamp. And finally, taking out the quartz tube and the oxide skin adhered to the surface. And cutting the sample again, grinding, polishing and corroding a part of the sample after being embedded, and then photographing the sample by using a microscope, and grinding the upper surface and the lower surface of the other part of the sample, and then performing the compression experiment again.

Example 2.

The preparation method of the high-strength amorphous composite material in this embodiment is basically the same as that in embodiment 1, except that: the pre-deformation amount is 0%.

Example 3.

The preparation method of the high-strength amorphous composite material in this embodiment is basically the same as that in embodiment 1, except that: the incubation time was 15 minutes.

Example 4.

The preparation method of the high-strength amorphous composite material in this embodiment is basically the same as that in embodiment 1, except thatIn the following steps: the material component is Ti₄₈Zr₁₈V₁₂Cu₅Be₁₇。

Example 5.

The preparation method of the high-strength amorphous composite material in this embodiment is basically the same as that in embodiment 2, except that: the material component is Ti₄₈Zr₁₈V₁₂Cu₅Be₁₇。

Example 6.

The preparation method of the high-strength amorphous composite material in this embodiment is basically the same as that in embodiment 4, except that: the pre-deformation amount is 3%.

The results of the tissue and mechanical property tests of examples 1, 2 and 3 are shown in the following table.

In FIG. 1, a, b and c correspond to those of examples 1, 2 and 3 Zr_60.0Ti_14.7Nb_5.3Cu_5.6Ni_4.4Be_10.0Texture maps of the materials after heat treatment, examples 4, 5 and 6 corresponding to Ti₄₈Zr₁₈V₁₂Cu₅Be₁₇And (4) carrying out heat treatment after different pre-deformation amounts. It can be known that with the increase of the pre-deformation amount, the volume fraction of the crystal phase of the material is reduced, the shape factor, namely the crystal grain roundness is increased, and the equivalent diameter, namely the crystal grain size is reduced; with the increase of the holding time, the volume fraction of the crystal phase of the material is reduced, the shape factor is reduced, and the equivalent diameter is increased. Compared with the embodiment 2, the plastic deformation and the compressive strength of the embodiment 1 and the embodiment 3 are greatly improved, the plasticity is improved by 106.22% after the pre-deformation is improved, and the plasticity is improved by 85.34% after the pre-deformation is improved and the heat preservation temperature is improved, and compared with the embodiment 5, the plasticity is respectively improved by 28.78% and 8.53% after the pre-deformation is improved in the embodiment 4 and the embodiment 6; both example 1 and example 3 had compressive strengths far exceeding those of example 2, and example 4 and example 6 also had compressive strengths exceeding those of example 5. In FIG. 2 a, b and c correspond to examples 1, 2 and 3 Zr after heat treatment_60.0Ti_14.7Nb_5.3Cu_5.6Ni_4.4Be_10.0The material shear band diagram. The arrows indicate the shear bands and it was found that the better the plasticity, the higher the shear band density, the more pronounced the multiple shear band crossing and proliferation phenomena. The material mechanical property can be effectively improved and the tissue distribution and the shape can be improved by indicating the proper pre-deformation amount and the heat preservation time.

The above examples and illustrations are not intended to limit the technical aspects of the present invention, and those skilled in the art can modify the present invention without departing from the spirit and scope of the present invention.