CN-116532630-B - High-flux preparation and characterization method of amorphous composite material

CN116532630BCN 116532630 BCN116532630 BCN 116532630BCN-116532630-B

Abstract

The embodiment of the application provides a high-throughput preparation and characterization method of an amorphous composite material, and relates to the field of amorphous composite materials. The method comprises the steps of enabling alloy melt to enter a conical die cavity of a die through a suction casting method to prepare a solid conical sample, radially sectioning the conical sample, and performing at least one characterization analysis of tissue morphology of the whole section to obtain correlation between the tissue morphology and the diameter size, performing X-ray diffraction on the section to obtain correlation between a phase structure and the diameter size, performing characterization on mechanical properties of the section to obtain correlation between the mechanical properties and the diameter size, and performing characterization on the section to obtain DSC curves of corresponding tissues to obtain correlation between volume fractions of precipitated phases and thermal properties. The method is simple and feasible, can complete the evolution and characterization of the microstructure of a certain component along with the cooling rate at one time, and effectively improves the development efficiency of the optimal component.

Inventors

MA DONG
YANG MING
HUANG YAN
DONG JIE
ZHANG YIBO
LV ZHICHAO
ZHAO JINKUI

Assignees

松山湖材料实验室

Dates

Publication Date: 20260505
Application Date: 20230509

Claims (11)

1. The high-throughput preparation and characterization method of the amorphous composite material is characterized by comprising the following steps of: preparing a solid conical sample by feeding alloy melt into a conical die cavity of a die through a suction casting method, radially cutting the conical sample, and carrying out the following characterization analysis: a. Carrying out characterization analysis on the tissue morphology of the whole section to obtain the correlation between the tissue morphology and the diameter size of the conical sample; b. Performing characterization analysis of X-ray diffraction on different diameter positions of the section to obtain correlation between the phase structure and the diameter size of the conical sample; c. carrying out characterization analysis on mechanical properties of different diameter positions of the section to obtain the correlation between the mechanical properties and the diameter sizes of the conical sample; d. DSC testing is carried out on samples of different diameter positions of the section, and DSC curves of corresponding tissues are obtained, so that the correlation between the volume ratio of precipitated phases of the conical sample and the thermal performance is obtained.
2. The method for high-throughput preparation and characterization of amorphous composites according to claim 1, characterized in that for characterization analysis a, characterization is performed using a light mirror or scanning electron microscope; and analyzing the diameter range corresponding to the all-amorphous structure, the diameter range corresponding to the mixed structure and the diameter range corresponding to the all-precipitated phase structure of the conical sample through the tissue morphology map obtained by characterization, so as to obtain the critical dimension formed by the amorphous composite material.
3. The method for high-throughput preparation and characterization of amorphous composite materials according to claim 1, characterized in that for characterization analysis b, characterization is performed using an X-ray diffractometer; and analyzing the diameter range corresponding to the completely amorphous matrix, the diameter range corresponding to the mixing and the diameter range corresponding to the completely crystalline precipitation of the conical sample by the XRD pattern obtained through characterization, so that the conical sample is axially divided into an amorphous material area, an amorphous composite material area and a crystalline material area.
4. The method for high throughput preparation and characterization of amorphous composites according to claim 1, characterized in that for characterization analysis c, characterization is performed using a durometer; And analyzing the corresponding relation between the hardness distribution state and the diameter of the conical sample through the hardness at the positions with different diameters.
5. The method for high throughput preparation and characterization of amorphous composites according to claim 4, wherein the preparation size of amorphous composites with a target volume percent of precipitated phases is obtained in combination with characterization analysis a.
6. The method for high throughput preparation and characterization of amorphous composites according to claim 4, wherein for characterization analysis d, characterization is performed using a differential scanning calorimeter; And respectively obtaining the temperature field distribution conditions when the solidification volume percentage gradually increases in the cooling process, and combining the characterization analysis c to obtain the mechanical behavior of the amorphous composite material with the target precipitated phase volume percentage.
7. The high-throughput preparation and characterization method of amorphous composite materials according to claim 1, wherein the diameter of the conical sample ranges from 1mm to 15 mm.
8. The high-throughput preparation and characterization method of the amorphous composite material according to claim 1, wherein the die is a water-cooled copper die, the die cavity comprises a molten pool die cavity, a riser die cavity and a conical die cavity which are sequentially communicated from top to bottom, the conical die cavity is vertically arranged, the upper end is a thick end, the lower end is a thin end, and alloy melt enters the conical die cavity from the molten pool die cavity through the riser die cavity under the action of suction casting.
9. The method of claim 8, further comprising a conical spacer disposed in the conical cavity, wherein a gap of 0.05-0.15 mm is provided between the conical spacer and the surface of the conical cavity.
10. The high-throughput preparation and characterization method of amorphous composite materials according to claim 8, wherein the diameter of the riser area mold cavity is 3-5 mm.
11. The high-throughput preparation and characterization method of amorphous composite materials according to claim 1, wherein the master alloy is weighed proportionally, and after the vacuum degree is maintained at 10 -3 ~10 -4 Pa, the alloy melt is obtained by fully smelting under the protection of argon by adopting a non-consumable arc smelting method.

Description

High-flux preparation and characterization method of amorphous composite material Technical Field The application relates to the field of amorphous composite materials, in particular to a high-flux preparation and characterization method of an amorphous composite material. Background In order to solve the problems of room temperature brittleness and strain softening of amorphous alloys, amorphous composite materials taking an austenitic B2-CuZr phase as an in-situ primary crystal phase have been successfully developed in CuZr-based alloy systems. In the tensile deformation process, the B2 phase of the ordered cubic structure of the amorphous composite material can generate martensitic phase with a monoclinic structure (B19') through martensitic phase Transformation, so that good macroscopic uniform tensile plasticity and remarkable work hardening capacity are generated, and the amorphous composite material is called as a Transformation-induced plasticity (TRIP) effect. At present, the phase-change induced plasticity toughened amorphous composite material is mainly intensively researched in Zr-based, ti-based, mg-based and other materials, and along with the progress of technology, research work for developing a new-component phase-change toughened amorphous composite material is paid attention to. The traditional method is to prepare samples one by one according to different sizes so as to obtain critical size ranges from amorphous alloy to amorphous composite material and from amorphous composite material to full crystal material. Conventional methods of obtaining critical dimensions of amorphous composites on a size-by-size basis have therefore limited the rate of development and research of the materials. How to prepare and study the solidification behavior of the phase change toughened amorphous composite material by a high-throughput method, for example, it is very important to determine the critical size range in which the B2-CuZr phase is dispersed in an amorphous matrix and no other brittle phase is formed. Disclosure of Invention The embodiment of the application aims to provide a high-flux preparation and characterization method of an amorphous composite material, which is simple and feasible, can finish the evolution and characterization of a microstructure of a certain component along with the cooling rate in a short time, effectively improves the development efficiency of the optimal component, and is convenient for the deep study of the solidification behavior and the phase change toughening mechanism. In a first aspect, embodiments of the present application provide a high throughput preparation and characterization method of an amorphous composite material, comprising the steps of: preparing a solid conical sample by feeding alloy melt into a conical die cavity of a die through a suction casting method, radially cutting the conical sample, and performing at least one characterization analysis of the conical sample: a. Carrying out characterization analysis on the tissue morphology of the whole section to obtain the correlation between the tissue morphology and the diameter size of the conical sample; b. performing characterization analysis of X-ray diffraction on different diameter positions of the section to obtain correlation between the phase structure and the diameter size of the conical sample; c. carrying out characterization analysis on mechanical properties of different diameter positions of the section to obtain the correlation between the mechanical properties and the diameter sizes of the conical sample; d. DSC testing is carried out on samples at different diameter positions of the section to obtain DSC (differential scanning calorimetry) curves of corresponding tissues so as to obtain the correlation between the volume ratio of the precipitated phases and the thermal performance of the conical sample. In the technical scheme, the method fully combines the theories of alloy melt flow, heat transfer in the solidification process and the like, and conical samples (amorphous alloy or amorphous composite material) with different lengths can be obtained by adjusting the conical die cavity, and each conical sample has different diameters and solidification temperature gradients and radial uniformity. The radial direction of any diameter position of the conical sample is uniform and the uniformity, the tissue uniformity of any diameter cylindrical sample can be accurately represented and the high-flux preparation characteristic is represented, while the traditional wedge-shaped sample has various differential cooling speeds, and the tissue formed by two-dimensional heat transfer can not represent the critical forming size of the cylindrical sample. The sample is axially split, and as different diameter positions of the conical sample correspond to different cooling rates, high-throughput rapid characterization of microstructure morphology, phase structure and macroscopic performance obt