A method for preparing Cu-TiB2-Zr by a composite dispersion treatment suspension ball milling method
By using suspension ball milling and spark plasma sintering technology, the problems of poor wettability between the reinforcement and the matrix and the growth and agglomeration of powder particles in traditional methods were solved, and Cu-TiB2-Zr composite materials with superior comprehensive performance were prepared.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- HEFEI UNIV OF TECH
- Filing Date
- 2024-01-17
- Publication Date
- 2026-06-09
AI Technical Summary
When preparing Cu-TiB2 composite materials using traditional methods, the wettability between the reinforcement and the matrix is poor, making alloying difficult. Furthermore, the relatively soft nature of copper easily leads to the growth and agglomeration of powder particles, affecting the overall performance of the material.
The composite dispersion treatment suspension ball milling method and spark plasma sintering technology were adopted. Ammonium polyacrylate was used as a dispersant and mechanical alloying was carried out in the form of suspension. Zr element was added for composite strengthening, and spark plasma sintering technology was used to refine the grains.
The uniform distribution of the second phase was achieved, the aggregation of TiB2 was suppressed, the overall performance of the material was improved, and a Cu-TiB2-Zr composite material with high density and uniform grain structure was prepared.
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Figure CN117845085B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of dispersion copper alloy strengthening technology, specifically relating to a method for preparing Cu-TiB2-Zr by a composite dispersion treatment suspension ball milling method. The method involves co-strengthening a copper matrix with TiB2 and Zr, and preparing the Cu-TiB2-Zr using a composite dispersion treatment suspension ball milling method and a spark plasma sintering method. Background Technology
[0002] Copper-based alloys are widely used in various electronic components due to their excellent electrical properties. However, their relatively poor mechanical properties limit their application in many emerging fields. To meet the high-performance requirements brought about by technological advancements, it is necessary to further improve the comprehensive mechanical properties of copper alloys.
[0003] Strengthening copper matrices with dispersed ceramic particles exhibiting good thermodynamic stability is an excellent method. TiB2 possesses a series of superior properties, including high hardness, high electrical and thermal conductivity. Compared to other ceramic reinforcing phases, it has less impact on the electrical and thermal conductivity of the matrix metal, making it an outstanding reinforcing material.
[0004] Traditional methods for preparing Cu-TiB2 composite materials involve directly adding TiB2 powder to a molten Cu matrix, enabling mass production. However, this method suffers from poor wettability between the reinforcement and the matrix, making alloying difficult. Exploring high-performance, low-cost, and easily mass-producible Cu-TiB2 copper-based composite material preparation processes to fully leverage the design freedom of materials and promote the industrial application of high-strength conductive materials has become an important research topic. Summary of the Invention
[0005] This invention provides a method for preparing Cu-TiB2-Zr using a composite dispersion treatment suspension ball milling method. The suspension ball milling method overcomes the problems caused by the traditional smelting method. The use of ammonium polyacrylate disperses the agglomerated powder in the raw materials, reducing the segregation problem of the reinforcing phase in the composite material caused by raw material agglomeration. Furthermore, the addition of Zr element to Cu-TiB2 achieves composite reinforcement, reduces the agglomeration of TiB2, and improves the overall performance of the composite material. This invention has guiding significance for the preparation process of Cu-TiB2 copper-based composite materials.
[0006] A method for preparing Cu-TiB2-Zr by ball milling of a composite dispersion-treated suspension includes the following steps:
[0007] (1) Powder pretreatment
[0008] Weigh out high-purity Cu powder, TiB2 powder, and Zr powder separately, add them to a 20ml deionized water beaker containing a magnetic rotor, add ammonium polyacrylate, place the beaker in a magnetic stirrer, stir thoroughly, and then place it in an ultrasonic cleaner for ultrasonication at room temperature for 1 hour. After ultrasonication, remove the beaker and place it in a ball milling jar, add cemented carbide balls, and then place the ball milling jar in a vacuum glove box. Under the protection of argon gas, complete the assembly of the ball milling jar. After assembly, fix the ball milling jar in a planetary ball mill for ball milling.
[0009] (2) Calcination and reduction
[0010] The precursor slurry after ball milling was taken out and placed in a tube furnace and dried at 300℃ for 12 h to remove the dispersant (the decomposition temperature of ammonium polyacrylate is 200-300℃). After grinding, the powder was evenly spread on a ceramic firing boat and placed in a high-temperature tube furnace. After setting the program, high-purity hydrogen was introduced for decomposition and reduction treatment to obtain the final Cu-TiB2-Zr composite powder.
[0011] (3) Spark plasma sintering
[0012] After grinding the Cu-TiB2-Zr composite powder that has been reduced in step (2), it is added to a graphite mold and placed in the furnace cavity of a spark plasma sintering furnace for pre-compacting. After setting the pre-compacting program, the furnace cavity is vacuum-treated and then sintered. After sintering, Cu-TiB2-Zr composite material is obtained.
[0013] In step (1), the mass fraction of TiB2 is 1%, the Zr content is 0.1%~0.2%, the remainder is high-purity Cu powder, and the content of ammonium polyacrylate is 0.3%.
[0014] The magnetic stirrer used in step (1) is a DF-101S type heat-collecting magnetic stirrer.
[0015] The ultrasonic cleaner used in step (1) is a JK-5200B ultrasonic cleaner with a power of 200W and a frequency of 40KHz.
[0016] In step (1), the vacuum glove box is model ZKX, the planetary ball mill is Nanjing University Instruments QM-QX4 omnidirectional planetary ball mill, the ball milling speed (rotation speed) is 300 rpm, the ball-to-material ratio is 3:1, and the ball milling time is 30 hours. The ball milling jar is assembled in the vacuum glove box under an argon atmosphere to ensure a pure ball milling environment. The ball jar and the ball milling media balls are both made of hard alloy.
[0017] In step (2), the high-temperature tubular furnace is model GSL-1200X, and the program is set as follows: the temperature is increased from room temperature to 600℃ at 10℃ / min, held for 2 hours, then decreased to 500℃ at 10℃ / min, and then cooled to room temperature with the furnace.
[0018] In step (2), the flow rate of hydrogen gas introduced is 300-500 ml / min.
[0019] In step (3), the diameter of the graphite mold is 20 mm, and carbon paper is used to separate the Cu-TiB2-Zr final treatment composite powder from the graphite mold to facilitate sampling and demolding after sintering.
[0020] In step (3), the pre-compaction pressure is 10 MPa, and the sintering is carried out by thermocouple temperature measurement. The front end of the thermocouple is inserted into the temperature measurement hole of the graphite mold.
[0021] In step (3), the discharge plasma sintering furnace is model LaboxTM-300, and the program is set as follows: the temperature is raised to 600℃ at a rate of 100℃ / min and held for 5min; then the temperature is raised to 900℃ at a rate of 5℃ / min. During this process, the pressure is raised from 10MPa to 50-70MPa, held for 5min and then rapidly cooled.
[0022] The beneficial effects of this invention are as follows: The addition of the second-phase Zr in this invention suppresses the agglomeration and growth of nano-sized TiB2 during sintering, and further improves performance through the co-strengthening mechanism between the two. Traditional smelting methods for preparing Cu-TiB2-based composite materials struggle to achieve elemental alloying. While mechanical alloying with the addition of second-phase particles to the copper matrix effectively overcomes this defect, copper's softness makes it prone to particle growth and agglomeration during ball milling, resulting in a large composite powder particle size. This invention uses a suspension instead of powder for mechanical alloying, introduces deionized water as a process control agent to reduce surface activity, and employs ammonium polyacrylate as a dispersant to weaken the powder's agglomeration ability, accelerating the ball milling process and ensuring the second phase is uniformly and diffusely distributed in the matrix. Spark plasma sintering technology refines the alloy's grain size through the combined effects of plasma activation and sintering densification, ultimately producing a Cu-TiB2-Zr composite material with high density, uniform grain structure, superior mechanical and electrical properties, and a wider range of applications. Attached Figure Description
[0023] Figure 1 This is a surface morphology diagram of the raw material copper powder;
[0024] Figure 2 Fracture morphology of Cu-TiB2-0.1%Zr;
[0025] Figure 3 High-magnification electron microscope image of Cu-TiB2-0.1%Zr monomer powder;
[0026] Figure 4 Energy dispersive spectroscopy (EDS) analysis of Cu-TiB2-0.1%Zr monomer powder. Detailed Implementation
[0027] The present invention will be further described below with reference to the accompanying drawings and specific embodiments.
[0028] Example 1:
[0029] In this embodiment, the Cu-TiB2 material is processed by composite dispersion treatment, suspension ball milling, calcination reduction, and spark plasma sintering. The mass fraction of TiB2 is preset to be 1%, the remainder is high-purity Cu powder, and the content of ammonium polyacrylate is 0.3%.
[0030] The preparation method of Cu-TiB2 material in this embodiment is as follows:
[0031] (1) Powder pretreatment
[0032] Weigh 19.8 g of high-purity Cu powder and 0.2 g of TiB2, and add them separately to a 20 ml deionized water beaker containing a magnetic rotor. Add 0.06 g of ammonium polyacrylate and place the mixture in a magnetic stirrer. Stir thoroughly until homogeneous, then place the beaker in an ultrasonic cleaner and sonicate at room temperature for 1 hour. After sonication, remove the beaker and place it in a cemented carbide jar. Add cemented carbide balls at a ball-to-powder ratio of 3:1. Place the grinding jar in a vacuum glove box and assemble it under argon protection. After assembly, fix the grinding jar in a planetary ball mill for ball milling.
[0033] (2) High-temperature decomposition and reduction
[0034] The precursor slurry after ball milling was taken out and dried in a tube furnace at 300℃ for 12 h. After grinding, the powder was evenly spread on a ceramic firing boat and placed in a high-temperature tube furnace. High-purity hydrogen was introduced at a flow rate of 300-500 ml / min to create a reducing atmosphere. The program was set to raise the temperature from room temperature to 600℃ at 10℃ / min, hold for 2 h, and then lower the temperature to 500℃ at 10℃ / min. The furnace was then cooled to room temperature to obtain Cu-TiB2 final-treated composite powder.
[0035] (3) Field-assisted sintering
[0036] The reduced Cu-TiB2 final-treated composite powder was ground and added to a graphite mold covered with carbon paper. The graphite mold was then placed in the furnace cavity of an auxiliary sintering furnace and subjected to a pre-compaction pressure of 10 MPa. The tip of a thermocouple was inserted into the temperature measuring hole of the graphite mold. The furnace cavity was closed and vacuumed. After the furnace cavity reached the vacuum level, the sintering program was set as follows: the temperature was increased to 600℃ at a rate of 100℃ / min and held for 5 min. Then, the temperature was increased to 900℃ at a rate of 5℃ / min. During this process, the pressure was increased from 10 MPa to 50-70 MPa, held for 5 min, and then rapidly cooled. After sintering, the Cu-TiB2 composite material was obtained.
[0037] Example 2:
[0038] In this embodiment, the Cu-TiB2-Zr material is processed by composite dispersion treatment, suspension ball milling, calcination reduction, and spark plasma sintering. The mass fraction of TiB2 is preset to be 1%, the Zr content is 0.1%, the remainder is high-purity Cu powder, and the content of ammonium polyacrylate is 0.3%.
[0039] The preparation method of Cu-TiB2-Zr material in this embodiment is as follows:
[0040] (1) Powder pretreatment
[0041] Weigh 19.78g of high-purity Cu powder, 0.2g of TiB2 powder, and 0.02g of Zr powder, and add them separately to 20ml deionized water beakers containing magnetic rotors. Add 0.06g of ammonium polyacrylate and place the mixture in a magnetic stirrer. Stir thoroughly until homogeneous, then place the mixture in an ultrasonic cleaner and sonicate at room temperature for 1 hour. After sonication, remove the mixture and place it in a cemented carbide jar. Add cemented carbide balls at a ball-to-powder ratio of 3:1. Place the jar in a vacuum glove box and assemble it under argon protection. After assembly, fix the jar in a planetary ball mill for ball milling.
[0042] (2) High-temperature decomposition and reduction
[0043] The precursor slurry after ball milling was taken out and dried in a tube furnace at 300℃ for 12 h. After grinding, the powder was evenly spread on a ceramic firing boat and placed in a high-temperature tube furnace. High-purity hydrogen was introduced at a flow rate of 300-500 ml / min to create a reducing atmosphere. The program was set to raise the temperature from room temperature to 600℃ at 10℃ / min, hold for 2 h, and then lower the temperature to 500℃ at 10℃ / min. The furnace was then cooled to room temperature to obtain Cu-TiB2-Zr final treated composite powder.
[0044] (3) Field-assisted sintering
[0045] The reduced Cu-TiB2-Zr final-treated composite powder was ground and added to a graphite mold covered with carbon paper. The graphite mold was then placed in the furnace cavity of an auxiliary sintering furnace and subjected to a pre-compaction pressure of 10 MPa. The tip of a thermocouple was inserted into the temperature measuring hole of the graphite mold. The furnace cavity was closed and vacuumed. After the furnace cavity reached the vacuum level, the sintering program was set as follows: the temperature was increased to 600℃ at a rate of 100℃ / min and held for 5 min. Then, the temperature was increased to 900℃ at a rate of 5℃ / min. During this process, the pressure was increased from 10 MPa to 50-70 MPa, held for 5 min, and then rapidly cooled. After sintering, the Cu-TiB2-Zr composite material was obtained.
[0046] Example 3:
[0047] In this embodiment, the Cu-TiB2-Zr material is processed by composite dispersion treatment, suspension ball milling, calcination reduction, and spark plasma sintering. The mass fraction of TiB2 is preset to be 1%, the Zr content is 0.2%, the remainder is high-purity Cu powder, and the content of ammonium polyacrylate is 0.3%.
[0048] The preparation method of Cu-TiB2-Zr material in this embodiment is as follows:
[0049] (1) Powder pretreatment
[0050] Weigh 19.76g of high-purity Cu powder, 0.2g of TiB2 powder, and 0.04g of Zr powder, and add them separately to 20ml deionized water beakers containing magnetic rotors. Add 0.06g of ammonium polyacrylate and place the mixture in a magnetic stirrer. Stir thoroughly until homogeneous, then place the mixture in an ultrasonic cleaner and sonicate at room temperature for 1 hour. After sonication, remove the mixture and place it in a cemented carbide jar. Add cemented carbide balls at a ball-to-powder ratio of 3:1. Place the jar in a vacuum glove box and assemble it under argon protection. After assembly, fix the jar in a planetary ball mill for ball milling.
[0051] (2) High-temperature decomposition and reduction
[0052] The precursor slurry after ball milling was taken out and dried in a tube furnace at 300℃ for 12 h. After grinding, the powder was evenly spread on a ceramic firing boat and placed in a high-temperature tube furnace. High-purity hydrogen was introduced at a flow rate of 300-500 ml / min to create a reducing atmosphere. The program was set to raise the temperature from room temperature to 600℃ at 10℃ / min, hold for 2 h, and then lower the temperature to 500℃ at 10℃ / min. The furnace was then cooled to room temperature to obtain Cu-TiB2-Zr final treated composite powder.
[0053] (3) Field-assisted sintering
[0054] The reduced Cu-TiB2-Zr final-treated composite powder was ground and added to a graphite mold covered with carbon paper. The graphite mold was then placed in the furnace cavity of an auxiliary sintering furnace and subjected to a pre-compaction pressure of 10 MPa. The tip of a thermocouple was inserted into the temperature measuring hole of the graphite mold. The furnace cavity was closed and vacuumed. After the furnace cavity reached the vacuum level, the sintering program was set as follows: the temperature was increased to 600℃ at a rate of 100℃ / min and held for 5 min. Then, the temperature was increased to 900℃ at a rate of 5℃ / min. During this process, the pressure was increased from 10 MPa to 50-70 MPa, held for 5 min, and then rapidly cooled. After sintering, the Cu-TiB2-Zr composite material was obtained.
[0055] Example 4:
[0056] In this embodiment, the Cu-TiB2-Zr material is processed by powder ball milling, calcination reduction, and spark plasma sintering. The mass fraction of TiB2 is preset to be 1%, the Zr content is 0.1%, and the remainder is high-purity Cu powder.
[0057] The preparation method of Cu-TiB2-Zr material in this embodiment is as follows:
[0058] (1) Powder pretreatment
[0059] Weigh 19.78g of high-purity Cu powder, 0.2g of TiB2 powder, and 0.02g of Zr powder and place them in a cemented carbide jar. Add cemented carbide balls at a ball-to-powder ratio of 3:1. Place the jar in a vacuum glove box and assemble it under argon protection. After assembly, fix the jar in a planetary ball mill for ball milling.
[0060] (2) High-temperature decomposition and reduction
[0061] The ball-milled precursor slurry was removed and dried in a tube furnace at 300 °C for 12 h. After grinding, the powder was evenly spread on a ceramic firing boat and placed in a high-temperature tube furnace. High-purity hydrogen was introduced at a flow rate of 300–500 ml / min to create a reducing atmosphere. The program was set to raise the temperature from room temperature to 600 °C at 10 °C / min, hold for 2 h, and then lower the temperature to 500 °C at 10 °C / min. The furnace was then cooled to room temperature to obtain Cu-TiB2-Zr final-treated composite powder.
[0062] (3) Field-assisted sintering
[0063] The reduced Cu-TiB2-Zr final-treated composite powder was ground and added to a graphite mold covered with carbon paper. The graphite mold was then placed in the furnace cavity of an auxiliary sintering furnace and subjected to a pre-compaction pressure of 10 MPa. The tip of a thermocouple was inserted into the temperature measuring hole of the graphite mold. The furnace cavity was closed and vacuumed. After the furnace cavity reached the vacuum level, the sintering program was set as follows: the temperature was increased to 600℃ at a rate of 100℃ / min and held for 5 min. Then, the temperature was increased to 900℃ at a rate of 5℃ / min. During this process, the pressure was increased from 10 MPa to 50-70 MPa, held for 5 min, and then rapidly cooled. After sintering, the Cu-TiB2-Zr composite material was obtained.
[0064] Table 1 below shows the bulk mechanical properties of Cu, Cu-TiB2, Cu-TiB2-(0.1%, 0.2%)Zr, and powder ball-milled Cu-TiB2-0.1%Zr alloy. Formed by spark plasma sintering, compared to pure copper and Cu-TiB2, the strength and hardness are effectively improved while maintaining almost the same conductivity. Table 1. Performance of the Sample Block
[0065]
[0066] Depend on Figure 1 As can be seen, the copper powder is spherical with a particle size of about 1 μm. The powder agglomerates into grape-like clusters and has a smooth surface.
[0067] Depend on Figure 2 It can be seen that the Cu-TiB2-0.1%Zr fracture surface exhibits an overall morphology of equiaxed dimple aggregation, with a relatively uniform dimple distribution. Simultaneously, tearing ridges and some steps characteristic of cleavage fracture were observed. This suggests a mixed fracture primarily characterized by ductile fracture. The embedding of second-phase particles within the dimples confirms the strengthening effect of the second phase.
[0068] Depend on Figure 3 and Figure 4 It can be seen from the energy dispersive spectroscopy analysis that various elemental additives can be found, and the reinforcing phase is uniformly distributed on the surface of the Cu matrix and has good bonding with the Cu matrix interface.
[0069] This invention incorporates a second-phase Zr to suppress the agglomeration and growth of nano-sized TiB2 during sintering, and further enhances performance through a co-strengthening mechanism between the two. Traditional smelting methods for preparing Cu-TiB2-based composites struggle to achieve elemental alloying. While mechanical alloying with second-phase particles into the copper matrix effectively overcomes this defect, copper's softness makes it prone to particle growth and agglomeration during ball milling, resulting in large composite powder particle sizes. This invention uses a suspension instead of powder for mechanical alloying, introducing deionized water as a process control agent to reduce surface activity, and employing ammonium polyacrylate as a dispersant to weaken powder agglomeration, accelerating the ball milling process and ensuring a uniform and dispersed second-phase distribution within the matrix. Spark plasma sintering technology refines the alloy's grain size through the combined effects of plasma activation and sintering densification, ultimately producing a Cu-TiB2-Zr composite material with high density, uniform grain structure, superior mechanical and electrical properties, and a wider range of applications.
[0070] The above embodiments are merely illustrative of specific implementations of this disclosure, but the implementations of this disclosure are not limited to the above content. Any changes, modifications, substitutions, combinations, or simplifications made without substantially departing from the spirit and principle of the inventive concept of this disclosure shall be considered equivalent substitutions and included within the scope of protection defined by the claims.
Claims
1. A method for preparing Cu-TiB2-Zr by ball milling of a composite dispersion-treated suspension, characterized in that: Includes the following steps: (1) Powder pretreatment High-purity Cu powder, TiB2 powder, and Zr powder were weighed separately and added to a 20ml deionized water beaker containing a magnetic rotor. Ammonium polyacrylate was added, and the mixture was placed in a magnetic stirrer and thoroughly stirred. The mixture was then placed in an ultrasonic cleaner and ultrasonicated at room temperature for 1 hour. After ultrasonication, the mixture was removed and placed in a ball mill jar. Hard alloy balls were added, and the jar was then placed in a vacuum glove box. Assembly of the ball mill jar was completed under argon protection. After assembly, the jar was fixed in a planetary ball mill for ball milling. The mass fraction of TiB2 was 1%, the Zr content was 0.1%~0.2%, the remainder was high-purity Cu powder, and the ammonium polyacrylate content was 0.3%. (2) Calcination and reduction The ball-milled precursor slurry was taken out and placed in a tube furnace, where it was dried at 300°C for 12 hours to remove the dispersant. After grinding, the powder was evenly spread on a ceramic firing boat and placed in a high-temperature tube furnace. After setting the program, high-purity hydrogen was introduced for decomposition and reduction treatment to obtain the final Cu-TiB2-Zr composite powder. The program was as follows: the temperature was increased from room temperature to 600°C at 10°C / min, held for 2 hours, and then decreased to 500°C at 10°C / min. The temperature was then cooled to room temperature with the furnace. (3) Spark plasma sintering The Cu-TiB2-Zr composite powder reduced in step (2) was ground and added to a graphite mold. The graphite mold was then placed in the furnace cavity of a spark plasma sintering furnace for pre-compaction. After pre-compaction, the furnace cavity was vacuum-treated and then sintered. After sintering, Cu-TiB2-Zr composite material was obtained. The set program was as follows: the temperature was increased to 600℃ at a rate of 100℃ / min and held for 5min; then the temperature was increased to 900℃ at a rate of 5℃ / min. During this process, the pressure was increased from 10MPa to 50-70MPa, held for 5min, and then rapidly cooled.
2. The method for preparing Cu-TiB2-Zr by ball milling of a composite dispersion-treated suspension as described in claim 1, characterized in that: The magnetic stirrer used in step (1) is a DF-101S type heat-collecting magnetic stirrer.
3. The method for preparing Cu-TiB2-Zr by ball milling of a composite dispersion-treated suspension as described in claim 1, characterized in that: In step (1), the ultrasonic cleaner is a JK-5200B ultrasonic cleaner with a power of 200W and a frequency of 40KHz.
4. The method for preparing Cu-TiB2-Zr by ball milling of a composite dispersion-treated suspension as described in claim 1, characterized in that: In step (1), the vacuum glove box is model ZKX, the planetary ball mill is Nanjing University Instruments QM-QX4 omnidirectional planetary ball mill, the ball milling speed is 300 rpm, the ball-to-material ratio is 3:1, and the ball milling time is 30 hours. The ball milling jar is assembled in the vacuum glove box under an argon atmosphere to ensure a pure ball milling environment. The ball jar and the ball milling media balls are both made of hard alloy.
5. The method for preparing Cu-TiB2-Zr by ball milling of a composite dispersion-treated suspension as described in claim 1, characterized in that: The high-temperature tubular furnace in step (2) is model GSL-1200X.
6. The method for preparing Cu-TiB2-Zr by ball milling of a composite dispersion-treated suspension as described in claim 1, characterized in that: In step (2), the flow rate of hydrogen gas introduced is 300-500 ml / min.
7. The method for preparing Cu-TiB2-Zr by ball milling of a composite dispersion-treated suspension as described in claim 1, characterized in that: In step (3), the diameter of the graphite mold is 20 mm, and carbon paper is used to separate the Cu-TiB2-Zr final treatment composite powder from the graphite mold to facilitate sampling and demolding after sintering.
8. The method for preparing Cu-TiB2-Zr by ball milling of a composite dispersion-treated suspension as described in claim 1, characterized in that: In step (3), the pre-compaction pressure is 10 MPa, and the sintering is carried out by thermocouple temperature measurement. The front end of the thermocouple is inserted into the temperature measurement hole of the graphite mold.
9. The method for preparing Cu-TiB2-Zr by ball milling of a composite dispersion-treated suspension as described in claim 1, characterized in that: The discharge plasma sintering furnace in step (3) is model LaboxTM-300.