CN-121976077-A - SPS (SPS) cyclic sintering and extrusion graphene reinforced titanium-based composite material integrated preparation method

CN121976077ACN 121976077 ACN121976077 ACN 121976077ACN-121976077-A

Abstract

The invention discloses an integrated preparation method of an SPS (semi-solid phase sintering) and extruded graphene reinforced titanium-based composite material, which comprises the following steps of S1, SPS (semi-solid phase sintering) circularly sintering, namely, placing mixed powder in a graphite mold for circularly sintering for 1-6 times, under the action of multi-field coupling, raising the temperature, changing the chemical potential of B atoms, and directionally diffusing part of B atoms to a Ti matrix to realize the control of the size of intragranular TiB, the control of the morphology of grain boundaries TiC and GNPs and pinning, and S2, SPS hot extrusion, placing the circularly sintered composite material in the mold, and extruding by utilizing a hydraulic device of SPS equipment after heat preservation at a set temperature to control the distribution of reinforced phases, further refine grains, improve the compactness, and avoid heat loss in the traditional extrusion mode transfer, so that extrusion can be carried out without changing other conditions after heat preservation at the set temperature. The invention can effectively control the morphology and the distribution of the reinforcing phase so as to improve the performance of the composite material.

Inventors

HOU JIABIN
LI ZONGAN
WU SHUO
ZHAN LIQIANG
FU YONGKANG
ZHOU JINGXIN
YANG XIAOHUA

Assignees

山东交通学院

Dates

Publication Date: 20260505
Application Date: 20251225

Claims (7)

1. The integrated preparation method of the SPS cyclic sintering and extrusion graphene reinforced titanium-based composite material is characterized by comprising the following steps of, S1, SPS cyclic sintering, namely placing mixed powder containing three layers of graphene/B/TA 15 in a graphite mold for cyclic sintering for 1-6 times, under the action of discharge heat, joule heat and pressure, raising the temperature, changing the chemical potential of B atoms, and directionally diffusing part of B atoms to a Ti matrix to realize the control of the size of intragranular TiB, the morphology control and pinning of grain boundaries TiC and GNPs, wherein the SPS cyclic sintering accurately regulates the diffusion and reaction of B atoms and C atoms through multiple 'heat-force' cycles, thereby realizing the nanocrystallization of intragranular TiB, the refinement and uniform distribution of grain boundaries TiC/GNPs; S2, SPS hot extrusion, namely placing the composite material after cyclic sintering into a die, preserving heat at a set temperature, extruding by utilizing a hydraulic device of SPS equipment to control the distribution of reinforcing phases, further refining grains and improving compactness, avoiding heat loss during transfer in a traditional extrusion mode through SPS hot extrusion, ensuring that extrusion can be performed without changing other conditions after preserving heat at the set temperature, and finally, utilizing the same equipment to 'forge' a micron-sized dense texture after 'programming' the nano-sized reinforcing phase network by a pulse thermal field, thereby solving the integrated manufacturing problems of shape control, distribution uniformity and matrix densification of the composite material in a one-time synergetic manner in two dimensions of atomic diffusion and macroscopic plastic deformation.
2. The SPS cyclic sintering and extrusion graphene reinforced titanium-based composite material integrated preparation method of claim 1, wherein the step S1 comprises the following specific steps: s11, filling the mixed powder into a hollow mould with the diameter of 30mm, and separating the inner wall of the mould from the pre-dispersed mixed powder by graphite paper with the thickness of 0.2 mm; S12, cold pressing, namely putting the die with the powder into an SPS furnace for cold pressing under the pressure of 1.5T, and then taking out the die for up-down transposition; S13, placing the transposed mold into an SPS furnace, pressurizing to a set pressure, raising the temperature to a sintering temperature for sintering, and preserving heat for a set time to obtain a sintered composite material; S14, naturally cooling the SPS sintered composite material to room temperature in the SPS, and repeatedly sintering for 1-6 times under the same condition.
3. The SPS cyclic sintering and extrusion graphene reinforced titanium-based composite integrated preparation method of claim 2, wherein the method is characterized by: the cycle times of cyclic sintering comprise 1-6 times, wherein the sintering material is not taken out after one sintering, the sintering material is directly cooled in SPS equipment, the sintering is repeated again after the cooling to room temperature, and the diffusion and phase change paths are accurately broken and recombined in atomic scale through the time sequence programming of multiple field pulses, so that the cross-scale cooperative regulation and control of the morphology, distribution and interface structure of the enhanced phase is realized.
4. The SPS cyclic sintering and extrusion graphene reinforced titanium-based composite material integrated preparation method as claimed in claim 1, wherein the step S2 comprises the following steps: S21, removing surface graphite paper from the circularly sintered composite material; S22, placing the sintered composite material with the graphite paper removed into an extrusion die with a set size, heating to a target temperature in an SPS furnace, and directly extruding after heat preservation.
5. The SPS cyclic sintering and extrusion graphene reinforced titanium-based composite material integrated preparation method according to claim 4, wherein in step S22, the hot extrusion process comprises the following steps: Raising the temperature of the SPS furnace to 600 ℃ at a temperature raising rate of 50 ℃ per minute; Raising the temperature of the SPS furnace from 600 ℃ to the extrusion temperature at the temperature raising rate of 50 ℃ per minute; Preserving heat for 30min at a set extrusion temperature; and (3) after heat preservation for 30min, extruding under the pressure of not more than 50 MPa.
6. The method for integrally preparing the SPS cyclic sintered and extruded graphene-reinforced titanium-based composite material according to claim 4, wherein in the step S22, the extrusion temperature is 900-1100 ℃.
7. The SPS cyclic sintering and extrusion graphene reinforced titanium-based composite material integrated preparation method according to claim 4, wherein in the step S32, the extrusion pressure is less than or equal to 50MPa.

Description

SPS (SPS) cyclic sintering and extrusion graphene reinforced titanium-based composite material integrated preparation method Technical Field The invention relates to the technical field of powder metallurgy SPS (sintering process) circulating sintering and graphene extrusion reinforced titanium-based composite materials, in particular to an integrated preparation method of the SPS circulating sintering and graphene extrusion reinforced titanium-based composite materials. Background Titanium and titanium alloy have excellent characteristics of high specific strength, good corrosion resistance, high temperature resistance and the like, so that the titanium and titanium alloy rapidly become key materials in the fields of aerospace, deep sea and the like, and particularly are used for parts requiring high strength and higher temperature resistance in aircraft and engines, so that good weight reduction benefits can be obtained. With the continuous development of the fields of aviation equipment and the like, the requirements on the strength, high temperature resistance, corrosion resistance and the like of materials are continuously improved, and single titanium or titanium alloy cannot meet the requirements on the mechanical properties of materials at key parts in the high-end field. Numerous researchers began to introduce graphene as a reinforcing phase into a titanium matrix to increase the tensile strength and improve the plasticity of the composite. The graphene is used as a reinforcing phase, so that more problems still exist, and the size and morphology of GNPs (Graphene Nanoplatelets, graphene), tiC and TiB are difficult to control. Part of B atoms can be directionally diffused to the Ti matrix through SPS cyclic sintering, so that the control of the size of the intragranular TiB, the morphology control and pinning of grain boundaries TiC and GNPs are realized, the distribution of reinforcing phases can be controlled through hot extrusion, grains are further refined, and the compactness is improved. Meanwhile, in the traditional extrusion mode, the presintered blank is heated and kept at a high temperature in a high-temperature furnace, then the blank is transferred to a hydraulic press for extrusion, and the temperature of the blank is reduced due to contact with air in the transfer process, so that errors exist between the blank and the set temperature during extrusion. Therefore, how to control morphology and distribution of the reinforcing phase and control variation of extrusion temperature by adopting a proper process becomes one of the urgent problems in the field. Disclosure of Invention The invention aims to provide an integrated preparation method of SPS cyclic sintering and extrusion graphene reinforced titanium-based composite material, which solves the defects in the prior art, and the invention utilizes SPS (SPARK PLASMA SINTERING ) can lead part of B atoms to directionally diffuse to the Ti matrix, thereby realizing the control of the size of the intragranular TiB, the control of the morphology of the grain boundary TiC and GNPs and the pinning. By utilizing the characteristic that SPS equipment can apply pressure when heating, a corresponding extrusion die is designed to extrude in the SPS equipment, and after the blank sintered by SPS circulation is put into the die, the blank is heated in the SPS equipment for a certain time and then extruded in the SPS equipment directly. The distribution of the reinforcing phase can be controlled through SPS hot extrusion, the density is improved, meanwhile, the heat loss during transfer can be avoided, and the extrusion can be directly carried out after the heat preservation at the set temperature. The invention provides an SPS cyclic sintering and extrusion graphene reinforced titanium matrix composite integrated preparation method, which comprises the following steps, S1, SPS cyclic sintering, namely placing mixed powder containing GNPs/B/TA15 in a graphite die to carry out cyclic sintering for 1-6 times, increasing the temperature under the action of discharge heat, joule heat and pressure, changing the chemical potential of B atoms, and directionally diffusing part of B atoms to a Ti matrix to realize the control of the size of the TiB in a crystal, the control of the morphology of the TiC and the GNPs in a crystal boundary and pinning; s2, SPS hot extrusion, namely placing the composite material after cyclic sintering into a die, and after heat preservation at a set temperature, extruding by utilizing a hydraulic device of SPS equipment to control the distribution of reinforcing phases, further refining grains and improving compactness. Heat loss during transfer in the traditional extrusion mode can be avoided through SPS hot extrusion, and extrusion can be performed without changing other conditions after heat preservation at a set temperature. According to the SPS cyclic sintering and extrusion graphene reinforced titanium-based composite mate