A method for preparing diamond / W-Cu composite material by combining adhesive spraying 3D printing technology

Abstract

This invention discloses a method for preparing diamond / W-Cu composite materials using binder jet 3D printing technology. The preparation method includes the following steps: (1) adding diamond / W-Cu mixed powder into a printing device and printing a diamond / W-Cu green blank using a binder jet 3D printing device; (2) placing the diamond / W-Cu green blank into a tube furnace, placing a Cu block for melting and infiltration below the green blank, and performing melting and infiltration under an argon atmosphere to obtain the diamond / W-Cu composite material. This invention adds diamond to the W-Cu composite material, utilizing the high thermal conductivity of diamond to improve the thermal conductivity of the W-Cu composite material. Simultaneously, the prepared diamond / W-Cu composite material exhibits low shrinkage and high dimensional accuracy, making it particularly suitable for near-net-shape forming of complex shapes. This improves the designability and processability of the diamond / W-Cu composite material, and the preparation process is simple with low production costs.

Description

Technical Field

[0001] This invention relates to the field of metal matrix composite material preparation, and specifically to a method for preparing diamond / W-Cu composite materials using adhesive jetting 3D printing technology. Background Technology

[0002] The development of society, economy, and science and technology is accompanied by massive energy consumption, and energy shortage has become an urgent problem to be solved. Compared with other energy sources, thermonuclear fusion energy is considered an infinitely abundant resource that can meet future energy needs. The Tokamak device is currently the most promising device for successful controlled thermonuclear fusion. However, in fusion devices, especially the plasma-facing material (PFM), it is subjected to high heat generated by the discharge of plasma and the thermal effects of high particle flux and neutron load. Excessive heat load will lead to high-temperature failure of the PFM. In order to further accelerate the heat transfer rate and ensure the safety and stability of the plasma-facing components, it is necessary to develop advanced heat sink materials to improve thermal conductivity. W has the characteristics of high melting point, high hardness, high strength and low coefficient of thermal expansion, while Cu has good thermal and electrical conductivity. W-Cu composite materials combine a series of excellent properties of W and Cu, such as high thermal conductivity, high hardness and adjustable coefficient of thermal expansion, making them ideal heat sink materials for use in thermonuclear fusion devices. However, the thermal conductivity of W-Cu composite materials is still not high, and further improving the thermal conductivity of composite materials has become one of the urgent problems to be solved.

[0003] Diamond has a thermal conductivity of up to 2200 W·m -1 ·K -1 It also has a low coefficient of thermal expansion (0.86×10⁻⁶). -6 / ℃). Currently, the main methods for preparing diamond / W-Cu composite materials are powder metallurgy, melt infiltration, and high-temperature and high-pressure methods. However, diamond / W-Cu composite materials prepared by these methods all suffer from shape limitations and inconvenient subsequent processing. Summary of the Invention

[0004] The purpose of this invention is to provide a method for preparing diamond / W-Cu composite materials using binder jet 3D printing technology. This method involves mixing diamond powder with W powder and Cu powder, preparing diamond / W-Cu green blanks using binder jet 3D printing technology, and then using pressureless melting infiltration technology to infiltrate Cu. This produces diamond / W-Cu composite materials with high thermal conductivity, complex shapes, low shrinkage, and high dimensional accuracy. The preparation process is simple and the production cost is low.

[0005] In one aspect of the invention, a method for preparing diamond / W-Cu composite materials using binder jetting 3D printing technology is provided. According to an embodiment of the invention, the method includes the following steps:

[0006] (1) Add diamond / W-Cu mixed powder to the printing equipment and print diamond / W-Cu green blank by spraying the adhesive through the 3D printing equipment.

[0007] (2) Place the diamond / W-Cu green blank into a tube furnace, place the Cu block used for melting and infiltration below the green blank, and carry out melting and infiltration under an argon atmosphere to obtain the diamond / W-Cu composite material.

[0008] In addition, the method for preparing diamond / W-Cu composite materials using adhesive jetting 3D printing technology according to the above embodiments of the present invention may also have the following additional technical features:

[0009] In some embodiments of the present invention, in step (1), the diamond / W-Cu mixed powder is prepared as follows: diamond powder, W powder and Cu powder are mixed in a powder mixer to obtain the diamond / W-Cu mixed powder.

[0010] In some embodiments of the present invention, the diamond powder is prepared by mechanical crushing and has a particle size of 15-30 μm, and the W powder and Cu powder are prepared by plasma spheroidization and have a spherical shape with a particle size of 10-90 μm and a sphericity of more than 95%.

[0011] In some embodiments of the present invention, the loose packing density of the diamond powder is 1-2 g / cm³. 3 The bulk density of W powder is 11.5-15.5 g / cm³. 3 The loose density of Cu powder is 4.5-6.5 g / cm³. 3 .

[0012] In some embodiments of the present invention, in step (1), the mass percentage of diamond powder in the diamond / W-Cu mixed powder is 1%-15%, the mass percentage of Cu powder is 1%-15%, and the remainder is W powder.

[0013] In some embodiments of the present invention, in step (1), diamond / W-Cu mixed powder is added to the printing equipment. Based on the particle size distribution and powder flowability of the mixed powder, the binder saturation, printing layer thickness, recoating speed, oscillator speed and roller transverse speed are set to print diamond / W-Cu green blanks. After printing, the diamond / W-Cu green blanks are placed in a curing chamber for curing to remove moisture from the binder.

[0014] In some embodiments of the present invention, the adhesive saturation is 50%-150%, the printed layer thickness is 50-150μm, the recoating speed is 80-120mm / s, the oscillator speed is 1500-2500rpm, and the roller lateral speed is 8-12mm / s.

[0015] In some embodiments of the present invention, after printing, the diamond / W-Cu green blank is placed in a curing chamber for curing to remove moisture from the binder. The curing temperature is 120-200℃ and the curing time is 2-8h.

[0016] In some embodiments of the present invention, in step (2), the melting temperature is 1200-1500℃, the holding time is 2-5h, the argon flow rate is 500-1500mL / min, the argon purity is greater than 99.99%, and the mass percentage of Cu in the diamond / W-Cu composite material is 15%-30%.

[0017] In another aspect of the present invention, the present invention proposes a method for preparing diamond / W-Cu composite materials according to the aforementioned adhesive jetting 3D printing technology.

[0018] Compared with the prior art, the beneficial effects of the present invention are:

[0019] (1) This invention improves the thermal conductivity of W-Cu composite material by adding diamond to it and utilizing the high thermal conductivity of diamond.

[0020] (2) This invention combines binder jet 3D printing with pressureless melting infiltration technology to prepare diamond / W-Cu composite materials. First, a diamond / W-Cu green blank is prepared by binder jet 3D printing, and then Cu is infiltrated into the green blank using pressureless melting infiltration technology. During the melting infiltration process, the Cu powder inside the green blank melts and promotes the rearrangement of W particles. At the same time, the external Cu liquid penetrates into the green blank under the action of capillary force and fills the pores inside the green blank, thus obtaining a composite material with uniform structure and dense structure. In addition, during the melting infiltration process, the pores inside the green blank are filled by the external Cu liquid, resulting in a composite material with small shrinkage and high dimensional accuracy. This avoids the problem of large shrinkage and low dimensional accuracy of the sample when the green blank is sintered due to the low density of the "green blank" prepared by binder jet 3D printing.

[0021] (3) This invention is particularly suitable for near-net-shape forming of complex shapes, improves the designability and processability of diamond / W-Cu composite materials, and has a simple preparation process and low production cost. Attached Figure Description

[0022] Figure 1 The process flow diagrams are for embodiments 1-3 of the present invention;

[0023] Figure 2 In the figure, (a), (b), and (c) are SEM images, PSD images, and XRD patterns of W powder used in Example 1 of the present invention, respectively; (d), (e), and (f) are SEM images, PSD images, and XRD patterns of Cu powder used in Example 1 of the present invention, respectively; and (g), (h), and (i) are SEM images, PSD images, and XRD patterns of diamond powder used in Example 1 of the present invention, respectively.

[0024] Figure 3 Here is a SEM image of the diamond / W-Cu composite material prepared in Example 1 of this invention;

[0025] Figure 4 The image shows the XRD pattern of the diamond / W-Cu composite material prepared in Example 1 of this invention. Detailed Implementation

[0026] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0027] Example 1

[0028] A method for preparing diamond / W-Cu composite materials using adhesive jetting 3D printing technology, the specific steps of which are as follows:

[0029] (1) Diamond powder, W powder, and Cu powder are mixed in a powder mixer to obtain a diamond / W-Cu mixed powder, wherein the diamond powder is prepared by mechanical crushing and has an average particle size of 19.6 μm and a loose packing density of 1.38 g / cm³. 3 W powder and Cu powder were prepared by plasma spheroidization and were spherical in shape, with average particle sizes of 38.2 μm and 33.5 μm, respectively, and loose bulk densities of 11.92 g / cm³. 3 and 4.73 g / cm 3 The diamond / W-Cu mixed powder contains 3% diamond powder by mass, 10% Cu powder by mass, and the remainder is W powder.

[0030] (2) The diamond / W-Cu mixed powder prepared in step (1) was added to the printing equipment. The binder saturation was set to 60%, the printing layer thickness to 50 μm, the recoating speed to 90 mm / s, the oscillator speed to 2000 rpm, and the roller lateral speed to 10 mm / s. A diamond / W-Cu green blank with dimensions of 1.2 × 1.2 × 0.3 cm was printed using the binder jet 3D printing equipment. After printing, the green blank was placed in a curing chamber for curing to remove moisture from the binder. The curing temperature was 120℃, and the curing time was 8 h. After curing, the mass and volume of the green blank were measured to be 4.12 g and 0.438 cm³, respectively. 3 The calculated density of the green body was 61.03%.

[0031] (3) Place the diamond / W-Cu green blank obtained in step (2) into a tube furnace, place the 1.18g Cu block used for melting and infiltration under the green blank, and carry out melting and infiltration under an argon atmosphere. The argon flow rate is 1000mL / min, the argon purity is greater than 99.99%, the melting and infiltration temperature is 1300℃, the holding time is 4h, and after the holding time is completed, cool to room temperature to obtain the diamond / W-Cu composite material. The diamond / W-Cu composite material contains 3% diamond by mass and 30% Cu by mass.

[0032] Figure 2 In the figures, (a) and (b) are SEM and PSD images of the W powder used in this embodiment, respectively, and (d) and (e) are SEM and PSD images of the Cu powder used in this embodiment, respectively. As can be seen from the figures, the W powder and Cu powder have high sphericity and wide particle size distribution. During the printing process, small particles fill the gaps between large particles, which is beneficial to improving the density of the composite material.

[0033] Figure 3 The image shows a SEM image of the diamond / W-Cu composite material prepared in this embodiment. As can be seen from the image, the sample surface is dense and there are no obvious pores. Diamond is uniformly distributed in the W-Cu composite material, and Cu forms a continuous network structure, which is conducive to heat transfer and improves the thermal conductivity of the composite material.

[0034] Figure 4 The image shows the XRD pattern of the diamond / W-Cu composite material prepared in this embodiment. As can be seen from the image, there is a diffraction peak of WC, indicating that the C atoms on the diamond surface have diffused and reacted with the W atoms to form WC. This reaction is beneficial to improving the interfacial bonding between diamond and W and Cu, reducing the interfacial thermal resistance, and improving the thermal conductivity of the composite material.

[0035] The density of the diamond / W-Cu composite material obtained in this embodiment was 96.21%, and the thermal conductivity was 242 W·m. -1·K -1 It has a linear shrinkage rate of less than 2%, a dense structure, high dimensional accuracy, and good thermal conductivity.

[0036] Example 2

[0037] A method for preparing diamond / W-Cu composite materials using adhesive jetting 3D printing technology, the specific steps of which are as follows:

[0038] (1) Diamond powder, W powder, and Cu powder are mixed in a powder mixer to obtain a diamond / W-Cu mixed powder, wherein the diamond powder is prepared by mechanical crushing and has an average particle size of 19.6 μm and a loose packing density of 1.38 g / cm³. 3 W powder and Cu powder were prepared by plasma spheroidization and were spherical in shape, with average particle sizes of 38.2 μm and 33.5 μm, respectively, and loose bulk densities of 11.92 g / cm³. 3 and 4.73 g / cm 3 The diamond / W-Cu mixed powder contains 5% diamond powder by mass, 10% Cu powder by mass, and the remainder is W powder.

[0039] (2) The diamond / W-Cu mixed powder prepared in step (1) was added to the printing equipment. The binder saturation was set to 60%, the printing layer thickness to 50 μm, the recoating speed to 90 mm / s, the oscillator speed to 2000 rpm, and the roller lateral speed to 10 mm / s. A diamond / W-Cu green blank with dimensions of 1.2 × 1.2 × 0.3 cm was printed using the binder jet 3D printing equipment. After printing, the green blank was placed in a curing chamber for curing to remove moisture from the binder. The curing temperature was 120℃, and the curing time was 8 h. After curing, the mass and volume of the green blank were measured to be 3.70 g and 0.443 cm³, respectively. 3 The calculated density of the green body was 58.10%.

[0040] (3) Place the diamond / W-Cu green blank obtained in step (2) into a tube furnace, place the 1.06g Cu block used for melting and infiltration under the green blank, and carry out melting and infiltration under an argon atmosphere. The argon flow rate is 1000mL / min, the argon purity is greater than 99.99%, the melting and infiltration temperature is 1300℃, the holding time is 4h, and after the holding time is completed, cool to room temperature to obtain the diamond / W-Cu composite material. The diamond / W-Cu composite material contains 5% diamond by mass and 30% Cu by mass.

[0041] The density of the diamond / W-Cu composite material obtained in this embodiment was 93.62%, and the thermal conductivity was 229 W·m. -1 ·K -1It has a linear shrinkage rate of less than 3.5%, high dimensional accuracy, and good thermal conductivity.

[0042] Example 3

[0043] A method for preparing diamond / W-Cu composite materials using adhesive jetting 3D printing technology, the specific steps of which are as follows:

[0044] (1) Diamond powder, W powder, and Cu powder are mixed in a powder mixer to obtain a diamond / W-Cu mixed powder, wherein the diamond powder is prepared by mechanical crushing and has an average particle size of 19.6 μm and a loose packing density of 1.38 g / cm³. 3 W powder and Cu powder were prepared by plasma spheroidization and were spherical in shape, with average particle sizes of 38.2 μm and 33.5 μm, respectively, and loose bulk densities of 11.92 g / cm³. 3 and 4.73 g / cm 3 The diamond / W-Cu mixed powder contains 5% diamond powder by mass, 10% Cu powder by mass, and the remainder is W powder.

[0045] (2) The diamond / W-Cu mixed powder prepared in step (1) was added to the printing equipment. The binder saturation was set to 60%, the printing layer thickness to 50 μm, the recoating speed to 90 mm / s, the oscillator speed to 2000 rpm, and the roller lateral speed to 10 mm / s. A diamond / W-Cu green blank with dimensions of 1.2 × 1.2 × 0.3 cm was printed using the binder jet 3D printing equipment. After printing, the green blank was placed in a curing chamber for curing to remove moisture from the binder. The curing temperature was 120℃, and the curing time was 8 h. After curing, the mass and volume of the green blank were measured to be 3.70 g and 0.443 cm³, respectively. 3 The calculated density of the green body was 58.10%.

[0046] (3) Place the diamond / W-Cu green blank obtained in step (2) into a tube furnace, place the 1.06g Cu block used for melting and infiltration under the green blank, and carry out melting and infiltration under an argon atmosphere. The argon flow rate is 1000mL / min, the argon purity is greater than 99.99%, the melting and infiltration temperature is 1400℃, the holding time is 4h, and after the holding time is completed, cool to room temperature to obtain the diamond / W-Cu composite material. The diamond / W-Cu composite material contains 5% diamond by mass and 30% Cu by mass.

[0047] The diamond / W-Cu composite material obtained in this embodiment has a density of 95.02% and a thermal conductivity of 235 W·m, according to testing. -1 ·K -1It has a linear shrinkage rate of less than 3.5%, a dense structure, high dimensional accuracy, and good thermal conductivity.

[0048] The above description is merely an example and illustration of the structure of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the structure of the present invention or exceed the scope defined in the claims, all of which should fall within the protection scope of the present invention.

Claims

1. A method for preparing diamond / W-Cu composite material by combining adhesive jetting 3D printing technology, characterized in that, Includes the following steps: (1) Diamond / W-Cu mixed powder is added to a printing device, and a diamond / W-Cu green body is printed using a 3D printing device with adhesive jetting. The preparation method of the diamond / W-Cu mixed powder is as follows: diamond powder, W powder and Cu powder are mixed in a powder mixer to obtain the diamond / W-Cu mixed powder. The diamond powder is prepared by mechanical crushing and has a particle size of 15-30 μm. The loose packing density of the diamond powder is 1-2 g / cm³. 3 The diamond / W-Cu mixed powder contains 1%-15% diamond powder by mass, 1%-15% Cu powder by mass, and the remainder is W powder. (2) Place the diamond / W-Cu green blank into a tube furnace, place the Cu block used for melting and infiltration below the green blank, and carry out melting and infiltration under an argon atmosphere to obtain the diamond / W-Cu composite material. The diamond is uniformly distributed in the W-Cu composite material, and the Cu forms a continuous network structure. The melting and infiltration temperature is 1200-1500℃, the holding time is 2-5h, the argon flow rate is 500-1500mL / min, and the argon purity is greater than 99.99%.

2. The method for preparing diamond / W-Cu composite material by combining adhesive bonding agent jetting 3D printing technology according to claim 1, characterized in that: In step (1), the W powder and Cu powder are prepared by plasma spheroidization and are spherical in shape, with a powder particle size of 10-90 μm and a powder sphericity of more than 95%.

3. The method of claim 1, wherein the method is characterized by: In step (1), the W powder has a loose density of 11.5-15.5 g / cm 3 , and the Cu powder has a loose density of 4.5-6.5 g / cm 3 .

4. The method of claim 1, wherein the method is characterized by: In step (1), diamond / W-Cu mixed powder is added to the printing equipment. Based on the particle size distribution and powder flowability of the mixed powder, the binder saturation, printing layer thickness, recoating speed, oscillator speed and roller transverse speed are set to print diamond / W-Cu green blanks. After printing, the diamond / W-Cu green blanks are placed in a curing chamber for curing to remove moisture from the binder.

5. The method of claim 1, wherein the method is characterized by: The adhesive saturation is 50%-150%, the printing layer thickness is 50-150μm, the recoating speed is 80-120mm / s, the oscillator speed is 1500-2500rpm, and the roller lateral speed is 8-12mm / s.

6. The method of claim 1, wherein the method is characterized by: After printing, the diamond / W-Cu green blank is placed in a curing chamber for curing to remove moisture from the adhesive. The curing temperature is 120-200℃ and the curing time is 2-8 hours.

7. The method of claim 1, wherein the method is characterized by: In step (2), the mass percentage of Cu in the diamond / W-Cu composite material is 15%-30%.

8. A diamond / W-Cu composite material prepared by a method for preparing diamond / W-Cu composite material using adhesive jet 3D printing technology according to any one of claims 1-7.

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