Method for calibrating internal temperature field of amorphous alloy prepared by spark plasma sintering

Patent metadata

Field	Value
Publication number	US-11673192-B2
Application number	US-202117616199-A
Country	US
Kind code	B2
Filing date	Apr 6, 2021
Priority date	Jan 31, 2021
Publication date	Jun 13, 2023
Grant date	Jun 13, 2023

Abstract

The invention belongs to the field of amorphous alloys, and more specifically, relates to a method for calibrating the internal temperature field of amorphous alloy prepared by spark plasma sintering. First, the part required for temperature field calibration inside the bulk amorphous alloy sample obtained by spark plasma sintering is cut into a series of small amorphous alloy samples, and the isothermal crystallization treatment is performed to obtain the crystallization time of different parts of the sample. An annealing-isothermal crystallization experiment is performed on the adopted amorphous alloy powder at different annealing temperatures, and the functional relationship between the annealing temperature and the crystallization time is obtained. The crystallization time of different parts inside the amorphous alloy sample is substituted into this functional relationship, the temperature distribution during the temperature holding stage during the sintering of different parts inside the amorphous alloy sample can be obtained.

First claim

What is claimed is:

1. A method for calibrating an internal temperature field of an amorphous alloy prepared by spark plasma sintering (SPS), comprising the following steps:
(1) sintering an amorphous alloy powder by the SPS to obtain a bulk amorphous alloy sample;
(2) cutting a part of the bulk amorphous alloy sample obtained in step (1) into a number of amorphous alloy sub-blocks, and marking a position of each of the amorphous alloy sub-blocks in the bulk amorphous alloy sample, wherein the part of the bulk amorphous alloy sample is where a temperature field needs to be calibrated;
(3) performing a first isothermal crystallization treatment on each of the amorphous alloy sub-blocks obtained in step (2) respectively at a same holding temperature to obtain a crystallization time of each of the amorphous alloy sub-blocks, wherein the holding temperature is in a supercooled liquid region of the amorphous alloy sub-blocks;
(4) performing an annealing treatment and a second isothermal crystallization treatment on an amorphous alloy powder material, which is the same as the amorphous alloy powder used in preparation of the bulk amorphous alloy sample, at different annealing temperatures, so as to obtain a corresponding crystallization time of the amorphous alloy powder material at the different annealing temperatures, and a functional relationship between the annealing temperature and the crystallization time of the amorphous alloy powder material, wherein in step (4), a holding temperature in performing the second isothermal crystallization treatment on the amorphous alloy powder material is the same as the holding temperature in performing the first isothermal crystallization treatment on the amorphous alloy sub-blocks in step (3);
(5) substituting the crystallization times of the amorphous alloy sub-blocks obtained in step (3) into the functional relationship between the annealing temperature and the crystallization time in step (4), thereby obtaining a temperature distribution of the different amorphous alloy sub-blocks corresponding to different positions inside the bulk amorphous alloy sample during the SPS.

2. The calibration method according to claim 1 , wherein step (1) comprises: placing the amorphous alloy powder in a sintering die; pressing the amorphous alloy powder into a green body; then heating to a sintering temperature for performing temperature holding and sintering in a SPS furnace, wherein the sintering temperature is in the supercooled liquid region of the amorphous alloy powder; lowering the temperature to a room temperature after the sintering is completed, and obtaining the bulk amorphous alloy sample.

3. The calibration method according to claim 2 , wherein a heating rate for the heating is 50 to 150 K/min, and a temperature holding time for the temperature holding is 3 to 10 minutes.

4. The calibration method according to claim 1 , wherein step (2) adopts mechanical cutting or wire electrical discharge machining (WEDM), and a three-dimensional size of the amorphous alloy sub-block is no greater than 2 mm×2 mm×2 mm.

5. The calibration method according to claim 1 , wherein in step (3), the amorphous alloy sub-blocks are respectively subjected to the first isothermal crystallization treatment according to a differential scanning calorimeter (DCS) principle to obtain the crystallization time of each of the amorphous alloy sub-blocks.

6. The calibration method according to claim 5 , wherein step (3) comprises: heating the amorphous alloy sub-blocks cut in step (2) to the same holding temperature respectively; keeping the amorphous alloy sub-blocks at the holding temperature until the amorphous alloy sub-blocks are completely crystallized, obtaining a number of isothermal DSC heat flow curves corresponding to the amorphous alloy sub-blocks at the holding temperature; obtaining an initial crystallization time of each of the amorphous alloy sub-blocks as its crystallization time by each of the heat flow curves.

7. The calibration method according to claim 6 , wherein the initial crystallization time is calibrated on the DSC heat flow curve by using a double tangent method, and the double tangent method comprises: making tangents at a smooth baseline on the heat flow curve where crystallization has not occurred yet and at a descending part of a crystallization peak at the beginning of the crystallization respectively; a time corresponding to an intersection of the two tangents being the initial crystallization time; and finally obtaining the initial crystallization time of each of the amorphous alloy sub-blocks at the different positions inside the bulk amorphous alloy sample, wherein the initial crystallization time is taken as its crystallization time.

8. The calibration method according to claim 1 , wherein in step (3), a differential scanning calorimeter is used to perform the first isothermal crystallization treatment on the amorphous alloy sub-blocks.

9. The calibration method according to claim 1 , wherein step (4) comprises the following sub-steps:
(4-1) heating the amorphous alloy powder material to an annealing temperature at a heating rate the same as that of the SPS in step (1) and holding the temperature, wherein a temperature holding time is the same as that of the SPS in step (1); and cooling after the annealing treatment, wherein a cooling rate is the same as that after the SPS in step (1) and the annealing temperature is in the supercooled liquid region of the amorphous alloy powder material;
(4-2) after the temperature is lowered to a value below 100° C. , subjecting the obtained amorphous alloy powder material to the second isothermal crystallization treatment, wherein the holding temperature in performing the second isothermal crystallization treatment is the same as the holding temperature in performing the first isothermal crystallization treatment on the amorphous alloy sub-blocks in step (3); holding the temperature until the amorphous alloy powder material is completely crystallized; and obtaining the corresponding crystallization time at the annealing temperature;
(4-3) changing the annealing temperature within the supercooled liquid region of the amorphous alloy powder material, and repeating steps (4-1) and (4-2) to obtain the corresponding crystallization times at the different annealing temperatures, that is, to obtain the functional relationship between the annealing temperature and the crystallization time of the amorphous alloy powder material.

10. The calibration method according to claim 9 , wherein the crystallization time data corresponding to the different annealing temperatures obtained in step (4-3) is nonlinearly fitted to obtain the functional relationship between the annealing temperature and the crystallization time.

Assignees

• Univ Huazhong Science Tech

Inventors

• Gong Pan
• Ding Huaping
• Wang Xinyun
• Jin Junsong
• Deng Lei
• Zhang Mao
• Tang Xuefeng

Classifications

• B22F3/24 Primary

  After-treatment of workpieces or articles {(B22F3/1146 takes precedence)} · CPC title

• B22F3/105 Primary

  by using electric current {other than for infrared radiant energy}, laser radiation or plasma (B22F3/11 takes precedence){; by ultrasonic bonding (B22F3/115 takes precedence)} · CPC title

• B22F2203/11

  temperature, temperature profile · CPC title

• B22F2998/10

  Processes characterised by the sequence of their steps · CPC title

• Y02P10/25

  Process efficiency · CPC title