CN117681510A - Anti-perovskite/metal-metal laminated composite material with zero expansion, directional high thermal conductivity and toughness and preparation thereof - Google Patents
Anti-perovskite/metal-metal laminated composite material with zero expansion, directional high thermal conductivity and toughness and preparation thereof Download PDFInfo
- Publication number
- CN117681510A CN117681510A CN202311688102.2A CN202311688102A CN117681510A CN 117681510 A CN117681510 A CN 117681510A CN 202311688102 A CN202311688102 A CN 202311688102A CN 117681510 A CN117681510 A CN 117681510A
- Authority
- CN
- China
- Prior art keywords
- metal
- anmn
- powder
- perovskite
- foil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 98
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 98
- 239000002184 metal Substances 0.000 title claims abstract description 98
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000010410 layer Substances 0.000 claims abstract description 57
- 239000000843 powder Substances 0.000 claims abstract description 54
- 239000000463 material Substances 0.000 claims abstract description 44
- 239000011888 foil Substances 0.000 claims abstract description 34
- 239000006185 dispersion Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002356 single layer Substances 0.000 claims abstract description 6
- 229910018173 Al—Al Inorganic materials 0.000 claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 23
- 239000010439 graphite Substances 0.000 claims description 23
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 9
- 238000004080 punching Methods 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000012459 cleaning agent Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 230000003746 surface roughness Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 4
- 230000000630 rising effect Effects 0.000 claims 2
- 230000003287 optical effect Effects 0.000 abstract description 4
- 238000004100 electronic packaging Methods 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 58
- 238000009792 diffusion process Methods 0.000 description 15
- 238000013001 point bending Methods 0.000 description 12
- 239000011159 matrix material Substances 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 230000002787 reinforcement Effects 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 230000008719 thickening Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000011156 metal matrix composite Substances 0.000 description 2
- 229910001374 Invar Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000000399 optical microscopy Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
Landscapes
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Laminated Bodies (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses an anti-perovskite/metal-metal laminated composite material with zero expansion, directional high thermal conductivity and toughness and a preparation method thereof. The anti-perovskite/metal-metal laminated composite material is formed by alternately distributing a dispersion layer and a metal layer; wherein the single-layer thickness of the dispersion layer is 10 mu m, and the single-layer thickness of the metal layer is 15-105 mu m; the components of the dispersion layer are as follows: inverse perovskite ANMn 3 The volume fraction of the dispersion layer is 30-70%, and the rest is metal powder; the metal layer is made of metal foil material. The laminated composite material prepared by the invention has accurate control of each layer thickness and simple process; the material has high density, and the interface bonding degree between layers is excellent, so that the fracture toughness and the thermal conductivity of the near-zero expansion material are greatly improved. The material with low/zero expansion, high thermal conductivity and high toughness has great application prospect in the fields of electronic packaging, precision optical devices and the like.
Description
Technical Field
The invention belongs to the field of low-zero-expansion high-thermal-conductivity high-toughness metal matrix composite materials, and in particular relates to anti-perovskite ANMn with zero expansion, directional high thermal conductivity and toughness 3 A method for preparing the metal-metal laminated composite material.
Background
Unlike most materials that expand when heated and contract when cooled, zero thermal expansion materials exhibit dimensional stability when temperature changes. The demands for zero thermal expansion materials are great in precision optics and equipment, low temperature, sensors and aerospace fields, because these fields have high thermal stability requirements for the dimensions of critical support components. In addition, the zero thermal expansion material also helps to extend the useful life of the device, reducing unnecessary power consumption (e.g., temperature compensation).
In addition to zero expansion properties, good thermal conductivity and toughness are also necessary to protect the core electronic or optical components from thermal or vibration shocks, thereby ensuring the reliability and durability of the precision instrument. Unfortunately, the single-phase zero-expansion materials described above are either intermetallic or ceramic. Their thermal conductivity is very difficult to exceed 15W/(mK) (e.g., typical invar thermal conductivity 11W/(mK)). Meanwhile, the problems of poor processability, insufficient mechanical properties and the like often exist.
As an alternative, zero expansion is easier to achieve in a composite consisting of a negative thermal expansion filler and a positive thermal expansion matrix (e.g., metallic aluminum and copper). However, in the reported zero expansion metal matrix composites, a large number of negative thermal expansion particles (typically exceeding 30 vol.%) are randomly distributed in the metal matrix. In addition, similar to single-phase zero-expansion materials, negative thermal expansion materials are brittle and have poor thermal conductivity. These characteristics are inherited to the associated zero expansion composite material, thereby greatly reducing the inherent thermal and mechanical properties of the metal matrix. Thus, despite efforts to build up connected copper networks, the thermal conductivity of the zero expansion composites reported previously is very difficult to exceed 60W/(m·k). Furthermore, the toughness and associated damage tolerance of zero expansion composites are severely reduced compared to metal matrices. Therefore, it has been a challenge to design zero expansion materials with metal-like properties (such as relatively high thermal conductivity and good toughness).
Disclosure of Invention
The invention aims at the problems existing in the prior art and provides the anti-perovskite ANMn with zero expansion, directional high thermal conductivity and toughness 3 A method for preparing the metal-metal laminated composite material.
The invention utilizes the negative expansion material as the reinforcement for the first time, synthesizes a series of Al-based (ANMn) materials through discharge plasma sintering 3 Al-Al) and Cu-based (ANMn 3 Cu-Cu) laminated composite material, low/zero thermal expansion is obtained, and the cooperative optimization of thermal conductivity and mechanical property is realized. The low/zero expansion material has great application prospect in the fields of electronic packaging, aerospace and precision electronic devices.
The invention has zero expansion, directional high thermal conductivity and toughness of anti-perovskite ANMn 3 The metal-metal laminated composite material consists of alternately distributed dispersion layers and metal layers; wherein the thickness of the single layer of the dispersion layer is 10 mu m, and the thickness of the single layer of the metal layer is 15-105 mu m. The components of the dispersion layer are as follows: inverse perovskite ANMn 3 The volume fraction of the dispersion layer is 30-70%, and the rest is metal powder. The metal layer is made of metal foil material.
The anti-perovskite ANMn 3 The particle size of the metal powder is 2-30 μm and the particle size of the metal powder is 1-5 μm.
The invention has zero expansion, directional high thermal conductivity and toughness of anti-perovskite ANMn 3 A method for preparing a metal-metal laminate composite comprising the steps of:
step 1: ANMn as negative thermal expansion material 3 Grinding with mortar, ball milling in a ball milling tank machine at 400r/min for 2 hr, sieving to obtain ANMn with particle diameter of 2-30 μm 3 Powder;
step 2: ANMn obtained in step 1 3 Mixing the powder with metal powder, and mixing in a tank mill at 200r/min for 1 hr to obtain ANMn 3 Metal mixed powder;
step 3: removing greasy dirt on the surface of the metal foil by using a greasy dirt cleaning agent, soaking the metal foil by using a metal polishing agent to remove an oxide layer on the surface of the metal foil, and punching the metal foil into a wafer with uniform size by using a sheet punching machine;
step 4: placing a graphite pressing head at one end into a cylindrical graphite mold, placing a metal disc into the graphite mold (the diameter of the inner cavity of the graphite mold is consistent with the diameter of the metal disc at the moment), and quantitatively weighing ANMn according to the designed components 3 Pouring the metal mixed powder into a graphite mold, placing the graphite mold cavity by using a metal pressure head with the surface roughness less than 1 mu m, and rotating the metal pressure head to obtain ANMn 3 After the metal mixed powder is paved, cold pressing is carried out, and the operation is repeated for a plurality of times to obtain the anti-perovskite ANMn 3 A layered preform of metal-metal foil.
Step 5: graphite mould and anti-perovskite ANMn obtained in the step 4 are subjected to 3 Placing the layered preform of metal-metal foil into discharge plasma sintering equipment, and sintering under vacuum environment to obtain anti-perovskite ANMn 3 Metal-metal laminate composite; the material is processed into proper size by a cutting machine and is used for physical property tests such as thermal expansion coefficient, sample microcosmic appearance, mechanical property, thermal conductivity and the like.
In the step 2, the metal powder is Al powder or Cu powder. The Al powder is aluminum alloy powder, such as one of 2-7 aluminum alloy powder, or pure aluminum; the copper powder is pure copper powder, and copper alloy powder can also be used.
When Al powder is used, ANMn 3 The mixing volume ratio of the powder to the Al powder is 39vol%:61vol% to 23vol%:77vol%.
Further, when Al and an alloy thereof are used as a matrix, ANMn 3 39% of the total composite volume, ANMn at an Al layer thickness of 15, 45, 75, 105 μm 3 ANMn in Al diffusion layer 3 The volume fractions were 44%,55%,66%,77%, respectively.
When Cu powder is used, ANMn 3 The mixing volume ratio of the powder to the Cu powder is 31vol%:69vol% to 62vol%:38vol%.
Further, when Cu and its alloy are used as the matrix, ANMn 3 The total volume of the composite material is 31.5%, and when the thickness of the Al layer is 20, 40, 60, 80, 100 mu m, the ANMn is as follows 3 ANMn in Cu diffusion layer 3 The volume fractions were 37%,43%,50%,63%, respectively.
In the step 3, the metal foil is an Al foil or a Cu foil; the Al foil is pure aluminum foil or one of 2-7 aluminum alloy foils; the Cu foil is pure copper foil or one of copper alloy foils. The thickness of the Al foil is 15-105 mu m; the thickness of the Cu foil is 20-100 mu m.
In step 5, sintering under vacuum environment means that the controlled air pressure is less than 1.0X10 -2 MPa。
Further, when using negative expansion material ANMn 3 When the layered prefabricated body is obtained by mixing the Al powder and the Al foil, in the step 5, 50MPa pressure is applied by a discharge plasma sintering device; heating to 200deg.C at 50deg.C/min, heating to 300deg.C at 40deg.C/min, heating to 420-470 deg.C at 25deg.C/min, maintaining for 6-7min, and cooling to room temperature with furnace to obtain ANMn 3 Al-Al laminate composite.
Further, when using negative expansion material ANMn 3 When the layered preform is obtained by mixing the powder with Cu foil, in step 5, a pressure of 50MPa is applied by a discharge plasma sintering apparatusForce; heating to 200deg.C at 50deg.C/min, heating to 300deg.C at 40deg.C/min, heating to 600-650deg.C at 25deg.C/min, maintaining for 6-7min, and cooling to room temperature with furnace to obtain ANMn 3 Cu-Cu laminate composite.
For the prepared aluminum-based composite material, no obvious third phase diffraction peak is found from the X-ray diffraction (figure 1) result, which means that the reaction between the reinforcement and the aluminum matrix is controllable, which is beneficial to obtaining a good composite interface, thereby realizing excellent mechanical and thermal properties. Series of ANMn pairs using an optical microscope 3 The section of the Al-Al laminated composite material sample is subjected to microscopic morphology characterization (figure 2), so that the combination of each phase is well known, the thickness of a diffusion layer and the thickness of a metal layer are consistent with the design, the thickness of the metal layer is gradually increased, and ANMn in the diffusion layer is clearly seen 3 The ratio of the (A) to the (B) is continuously increased, and the ANMn of the whole system is maintained 3 The duty ratio is unchanged. The results of the linear expansion coefficient test (fig. 3) show that the expansion coefficient of the aluminum-based composite material remains unchanged with the thickening of the metal layer. In the 300-330K range, the linear thermal expansion coefficient alpha of the material in three directions of XYZ L Between 280 and 335K, the linear thermal expansion coefficient α of the material in three directions XYZ is =0-1 ppm/K L <5ppm/K. FIG. 4 shows the ANMn series 3 Thermal conductivity test results of/Al-Al laminate composite samples in the 220-360K temperature region, thermal conductivity k=96-120W/(m·k) parallel to the layup direction, thermal conductivity k=84-14W/(m·k) perpendicular to the layup direction, ANMn 3 Compared with the dispersed Al-based composite material, the thermal conductivity of the Al-Al laminated composite material is improved by 30 percent. FIG. 5 shows the ANMn series 3 Three-point bending test results of Al-Al laminated composite material, anti-perovskite ANMn 3 The elongation of the Al-Al laminated composite material is improved by 500 percent compared with that of the Al-based composite material in dispersion distribution. FIG. 6 shows the ANMn series 3 Scanning electron microscope images of the Al-Al laminate composite after three-point bending fracture, it can be seen that the (ANMn 3 Al-105 μmAl), crack deflection between layers, ANMn combined with diffusion 3 Comparison of Al composite (39 vol% ANMn) 3 /Al) to achieve a large dissipation of energy, breaking of materialThe toughness is greatly improved. In the prepared anti-perovskite ANMn 3 In the laminated Al-Al composite material, the fracture toughness in the direction perpendicular to the layering direction is 5-15 (10 3 J·m -2 )。
For the prepared Cu-based composite material, no obvious third phase diffraction peak is found from the X-ray diffraction (figure 7) result, which means that the reaction between the reinforcement and the Cu matrix is controllable, which is beneficial to obtaining a good composite interface, thereby realizing excellent mechanical and thermal properties. Using scanning electron microscope to scan the series ANMn 3 The section of the Cu-Cu laminated composite material sample is subjected to microscopic morphology characterization (figure 8), so that the combination of each phase is well known, the thickness of a diffusion layer and the thickness of a metal layer are consistent with the design, the thickness of the metal layer is gradually increased, and ANMn in the diffusion layer is clearly seen 3 The ratio of the (A) to the (B) is continuously increased, and the ANMn of the whole system is maintained 3 The duty ratio is unchanged. The results of the linear expansion coefficient test (fig. 9) show that the expansion coefficient of the Cu-based composite material remains unchanged with the thickening of the Cu layer. In the 278-308K interval, the linear thermal expansion coefficient alpha of the material in three directions of XYZ L Between 265 and 315K, the linear thermal expansion coefficient α of the material in three directions XYZ is =0-1 ppm/K L <6ppm/K. FIG. 10 shows the ANMn series 3 Thermal conductivity test results of the Cu-Cu laminated composite sample in the 220-360K temperature zone, thermal conductivity k=95-200W/(m·k) in the direction parallel to the layup and thermal conductivity k=47-16W/(m·k) in the direction perpendicular to the layup; ANMn (ANMn) 3 Compared with a Cu-based composite material in dispersion distribution, the thermal conductivity of the Cu-Cu laminated composite material is improved by 230%. FIG. 11 shows the ANMn series 3 Three-point bending test results of Cu-Cu laminated composite material, anti-perovskite ANMn 3 The elongation of the Cu-Cu laminated composite material is improved by 300 percent compared with that of a Cu-based composite material in dispersion distribution. FIG. 12 shows the ANMn series 3 Scanning electron microscopy images after three-point bending fracture of the Cu-Cu laminate composite, it can be seen that upon fracture of the laminate sample (ANMn 3 Cu-100 mu mCu) to generate a large number of tunnel cracks, and ANMn compounded with diffusion 3 Cu composite Compare (31 vol% ANMn) 3 Cu), a great dissipation of energy is achieved, and the fracture toughness of the material is greatly improved. In the prepared anti-perovskite ANMn 3 In the Cu-Cu laminate composite, the fracture toughness in the direction perpendicular to the layering direction is 14-54 (10 3 J·m -2 )。
Drawings
FIG. 1 shows ANMn as the present invention 3 XRD pattern of Al-Al laminate composite.
FIG. 2 shows ANMn as the present invention 3 Scanning electron microscope pictures of the Al-Al laminated composite material.
FIG. 3 shows ANMn as the present invention 3 Thermal expansion coefficient test results of the Al-Al laminate composite.
FIG. 4 shows ANMn as the present invention 3 Thermal conductivity test results of Al-Al laminate composite.
FIG. 5 shows ANMn as the present invention 3 Three-point bending test results of the Al-Al laminated composite material.
FIG. 6 shows ANMn as the present invention 3 Three-point bending test section scanning electron microscope pictures of the Al-Al laminated composite material.
FIG. 7 shows ANMn as the present invention 3 XRD pattern of Cu-Cu laminate composite.
FIG. 8 shows ANMn as the present invention 3 Optical microscopy of Cu-Cu laminated composite.
FIG. 9 shows ANMn as the present invention 3 Thermal expansion coefficient test results of Cu-Cu laminated composite materials.
FIG. 10 shows ANMn as the present invention 3 Thermal conductivity test results of Cu-Cu laminate composite.
FIG. 11 shows ANMn as the present invention 3 Three-point bending test results of Cu-Cu laminated composite materials.
FIG. 12 shows ANMn as the present invention 3 Three-point bending test section scanning electron microscope image of the Cu-Cu laminated composite material.
Detailed Description
Embodiments of the present invention are described below by way of specific examples.
Example 1: low/zero expansion ANMn 3 Al-Al laminated composite material
The embodiment has zero expansion, directional high thermal conductivity and toughnessPerovskite ANMn 3 The composite material of Al-Al lamination is made of negative expansion material ANMn 3 ANMn prepared by sintering with discharge plasma as diffusion layer and Al foil as metal layer 3 Al-Al laminated composite material, abbreviated as ANMn 3 /Al-Al。
The Al powder used in this example was a 2-series aluminum alloy powder.
The Al foil used in this example was a pure Al foil having a thickness of 15-105. Mu.m.
Anti-perovskite ANMn with zero expansion, directional high thermal conductivity and toughness in this embodiment 3 The preparation method of the Al-Al laminated composite material comprises the following steps:
step 1: ANMn as negative thermal expansion material 3 Grinding with mortar, ball milling in a ball milling tank machine at 400r/min for 2 hr, sieving to obtain ANMn with particle diameter of 2-30 μm 3 And (3) powder.
Step 2: ANMn as negative thermal expansion material 3 Mixing with Al powder, and placing into a pot mill to mix for 1h at a speed of 200r/min to obtain mixed powder. Negative thermal expansion material ANMn 3 The mixing volume ratio with Al powder is 39vol%:61vol% to 23vol%:77vol%.
Step 3: removing greasy dirt on the surface of the Al foil by using a greasy dirt cleaning agent, soaking the metal foil by using a metal polishing agent to remove an oxide layer on the surface of the metal foil, and punching the Al foil into a wafer with uniform size by using a sheet punching machine.
Step 4: placing a graphite pressing head at one end into a cylindrical graphite mold, placing a metal disc into the graphite mold (the diameter of the inner cavity of the graphite mold is consistent with the diameter of the metal disc at the moment), and quantitatively weighing ANMn according to the designed components 3 Pouring the/Al mixed powder into a graphite mold, placing the graphite mold cavity by using a metal pressure head with the surface roughness less than 1 mu m, and rotating the metal pressure head to obtain ANMn 3 After the Al mixed powder is paved, cold pressing is carried out, and the above operation is repeated for a plurality of times to obtain the anti-perovskite ANMn 3 Laminar preform of Al-Al foil. Placing the preform into a discharge plasma sintering device for sintering; sintering pressure is 50MPa; heating to 200deg.C at 50deg.C/min, and heating to 300deg.C at 40deg.C/min, and heating to 420-470 deg.C at 25deg.C/minAnd preserving heat for 7min, and cooling to room temperature along with the furnace to obtain ANMn 3 Al-Al laminate composite. The material is processed into proper size by a cutting machine and is used for physical property tests such as thermal expansion coefficient, sample microcosmic appearance, mechanical property, thermal conductivity and the like.
For the prepared obtained ANMn 3 The fact that no distinct third phase diffraction peak is found in the X-ray diffraction (figure 1) results for the al—al laminate composite material means that the reaction between the reinforcement and the aluminum matrix is controllable, which is advantageous for obtaining a good composite interface, thus achieving excellent mechanical and thermal properties. Series of ANMn pairs using an optical microscope 3 The section of the Al-Al laminated composite material sample is subjected to microscopic morphology characterization (figure 2), so that the combination of each phase is well known, the thickness of a diffusion layer and the thickness of a metal layer are consistent with the design, the thickness of the metal layer is gradually increased, and ANMn in the diffusion layer is clearly seen 3 The ratio of the (A) to the (B) is continuously increased, and the ANMn of the whole system is maintained 3 The duty ratio is unchanged. The results of the linear expansion coefficient test (fig. 3) show that the expansion coefficient of the aluminum-based composite material remains unchanged with the thickening of the metal layer. In the 300-330K range, the linear thermal expansion coefficient alpha of the material in three directions of XYZ L Between 280 and 335K, the linear thermal expansion coefficient α of the material in three directions XYZ is =0-1 ppm/K L <5ppm/K. FIG. 4 shows the ANMn series 3 Thermal conductivity test results of/Al-Al laminate composite samples in the 220-360K temperature region, thermal conductivity k=96-120W/(m·k) parallel to the layup direction, thermal conductivity k=84-14W/(m·k) perpendicular to the layup direction, ANMn 3 Compared with the dispersed Al-based composite material, the thermal conductivity of the Al-Al laminated composite material is improved by 30%; FIG. 5 shows the ANMn series 3 Three-point bending test results of Al-Al laminated composite material, anti-perovskite ANMn 3 The elongation of the Al-Al laminated composite material is improved by 500 percent compared with that of the Al-based composite material in dispersion distribution. FIG. 6 shows the ANMn series 3 Scanning electron microscope images of the Al-Al laminate composite after three-point bending fracture, it can be seen that the (ANMn 3 Al-105 μmAl), crack deflection between layers, ANMn combined with diffusion 3 Comparison of Al composite (39 vol% ANMn) 3 /Al) to achieve a large dissipation of energy, a materialThe fracture toughness of the material is greatly improved.
Example 2: low/zero expansion ANMn 3 Cu-Cu laminated composite material
Anti-perovskite ANMn with zero expansion, directional high thermal conductivity and toughness in this embodiment 3 The Cu-Cu laminated composite material is made of negative expansion material ANMn 3 ANMn prepared by spark plasma sintering with Cu foil as metal layer and Cu mixed powder as dispersion layer 3 Cu-Cu laminated composite material, abbreviated as ANMn 3 /Cu-Cu。
The Cu powder used in this example is pure Cu powder.
The Cu foil used in this example was a pure Cu foil with a Cu foil thickness of 20-100 μm.
Anti-perovskite ANMn with zero expansion, directional high thermal conductivity and toughness in this embodiment 3 The preparation method of the Cu-Cu laminated composite material comprises the following steps:
step 1: ANMn as negative thermal expansion material 3 Grinding with mortar, ball milling in a ball milling tank machine at 400r/min for 2 hr, sieving to obtain ANMn with particle diameter of 2-30 μm 3 And (3) powder.
Step 2: ANMn as negative thermal expansion material 3 Mixing with Cu powder, and placing into a pot mill to mix for 1h at a speed of 200r/min to obtain mixed powder. Negative thermal expansion material ANMn 3 The mixing volume ratio with Cu powder is 31vol%:69vol% to 62vol%:38vol%.
Step 3: removing greasy dirt on the surface of the Cu foil by using a greasy dirt cleaning agent, soaking the Cu foil by using a metal polishing agent to remove an oxide layer on the surface of the Cu foil, and punching the Cu foil into a wafer with uniform size by using a sheet punching machine.
Step 4: placing a graphite pressing head at one end into a cylindrical graphite mold, placing a metal disc into the graphite mold (the diameter of the inner cavity of the graphite mold is consistent with the diameter of the metal disc at the moment), and quantitatively weighing ANMn according to the designed components 3 Pouring the Cu mixed powder into a graphite mold, placing the graphite mold cavity by using a metal pressure head with the surface roughness less than 1 mu m, and rotating the metal pressure head to obtain ANMn 3 After the Cu mixed powder is paved, cold pressing is carried out, and the operation is repeated for a plurality of times to obtain the anti-perovskite ANMn 3 /Cu-CuIs a layered preform of (a). Placing the preform into a discharge plasma sintering device for sintering, wherein the sintering pressure is 50MPa; heating to 200deg.C at 50deg.C/min, heating to 300deg.C at 40deg.C/min, heating to 600-650deg.C at 25deg.C/min, maintaining for 7min, and cooling to room temperature to obtain ANMn 3 Cu-Cu laminate composite; the material is processed into proper size by a cutting machine and is used for physical property tests such as thermal expansion coefficient, sample microcosmic appearance, mechanical property, thermal conductivity and the like.
For the prepared Cu-based composite material, no obvious third phase diffraction peak is found from the X-ray diffraction (figure 7) result, which means that the reaction between the reinforcement and the Cu matrix is controllable, which is beneficial to obtaining a good composite interface, thereby realizing excellent mechanical and thermal properties. Using scanning electron microscope to scan the series ANMn 3 The section of the Cu-Cu laminated composite material sample is subjected to microscopic morphology characterization (figure 8), so that the combination of each phase is well known, the thickness of a diffusion layer and the thickness of a metal layer are consistent with the design, the thickness of the metal layer is gradually increased, and ANMn in the diffusion layer is clearly seen 3 The ratio of the (A) to the (B) is continuously increased, and the ANMn of the whole system is maintained 3 The duty ratio is unchanged. The results of the linear expansion coefficient test (fig. 9) show that the expansion coefficient of the Cu-based composite material remains unchanged with the thickening of the Cu layer. In the 278-308K interval, the linear thermal expansion coefficient alpha of the material in three directions of XYZ L Between 265 and 315K, the linear thermal expansion coefficient α of the material in three directions XYZ is =0-1 ppm/K L <6ppm/K. FIG. 10 shows the ANMn series 3 Thermal conductivity test results of the Cu-Cu laminated composite sample in the 220-360K temperature zone, thermal conductivity k=95-200W/(m·k) in the direction parallel to the layup and thermal conductivity k=47-16W/(m·k) in the direction perpendicular to the layup; ANMn (ANMn) 3 Compared with a Cu-based composite material in dispersion distribution, the thermal conductivity of the Cu-Cu laminated composite material is improved by 230%; FIG. 11 shows the ANMn series 3 Three-point bending test results of Cu-Cu laminated composite material, anti-perovskite ANMn 3 The elongation of the Cu-Cu laminated composite material is improved by 300 percent compared with that of a Cu-based composite material in dispersion distribution. FIG. 12 shows the ANMn series 3 Scanning electron microscope images of the Cu-Cu laminated composite material after three-point bending fracture can be seen in the laminated sampleAt break (ANMn) 3 Cu-100 mu mCu) to generate a large number of tunnel cracks, and ANMn compounded with diffusion 3 Cu composite Compare (31 vol% ANMn) 3 Cu), a great dissipation of energy is achieved, and the fracture toughness of the material is greatly improved.
Claims (10)
1. An inverse perovskite/metal-metal laminate composite material with zero expansion, directional high thermal conductivity and toughness, characterized by:
the anti-perovskite/metal-metal laminated composite material is formed by alternately distributing a dispersion layer and a metal layer; wherein the single-layer thickness of the dispersion layer is 10 mu m, and the single-layer thickness of the metal layer is 15-105 mu m;
the components of the dispersion layer are as follows: inverse perovskite ANMn 3 The volume fraction of the dispersion layer is 30-70%, and the rest is metal powder; the metal layer is made of metal foil material.
2. The anti-perovskite/metal-metal laminate composite material of claim 1, wherein:
the anti-perovskite ANMn 3 The particle size of the metal powder is 2-30 μm and the particle size of the metal powder is 1-5 μm.
3. A method of preparing an inverse perovskite/metal-metal laminate composite material as claimed in claim 1, comprising the steps of:
step 1: ANMn as negative thermal expansion material 3 Grinding with mortar, ball milling, sieving to obtain ANMn with particle diameter of 2-30 μm 3 Powder;
step 2: ANMn obtained in step 1 3 Mixing the powder with metal powder, and mixing in a tank mill to obtain ANMn 3 Metal mixed powder;
step 3: removing greasy dirt on the surface of the metal foil by using a greasy dirt cleaning agent, soaking the metal foil by using a metal polishing agent to remove an oxide layer on the surface of the metal foil, and punching the metal foil into a wafer with uniform size by using a sheet punching machine;
step 4: putting the metal wafer obtained in the step 3 into a graphite die, and assembling according to designWeighing ANMn 3 Pouring the metal mixed powder into a graphite mold, placing the graphite mold cavity by using a metal pressure head with the surface roughness less than 1 mu m, and rotating the metal pressure head to obtain ANMn 3 Paving the metal mixed powder and then cold pressing; repeating the above operation to obtain anti-perovskite ANMn 3 A layered preform of a metal-metal foil;
step 5: graphite mould and anti-perovskite ANMn obtained in the step 4 are subjected to 3 Placing the layered preform of metal-metal foil into discharge plasma sintering equipment, and sintering under vacuum environment to obtain anti-perovskite ANMn 3 Metal-metal laminate composite.
4. A method of preparation according to claim 3, characterized in that:
in the step 2, the metal powder is Al powder or Cu powder;
when the metal powder is Al powder, ANMn 3 The mixing volume ratio of the powder to the Al powder is 39vol%:61vol% to 23vol%:77vol%;
when the metal powder is Cu powder, ANMn 3 The mixing volume ratio of the powder to the Cu powder is 31vol%:69vol% to 62vol%:38vol%.
5. A method of preparation according to claim 3, characterized in that:
in the step 3, the metal foil is an Al foil or a Cu foil; the thickness of the Al foil is 15-105 mu m; the thickness of the Cu foil is 20-100 mu m.
6. A method of preparation according to claim 3, characterized in that:
in step 5, sintering under vacuum environment means that the controlled air pressure is less than 1.0X10 -2 MPa。
7. The method of manufacturing according to claim 4, wherein:
when the metal powder is Al powder to prepare a layered preform, in the step 5, 50MPa pressure is applied by a discharge plasma sintering device, the temperature is raised to 420-470 ℃ and kept for 6-7min, and the layered preform is cooled along with a furnaceTo room temperature, ANMn is obtained 3 Al-Al laminate composite.
8. The method of manufacturing according to claim 7, wherein:
the temperature rising rate is controlled as follows: firstly heating to 200 ℃ at a speed of 50 ℃/min, then heating to 300 ℃ at a speed of 40 ℃/min, finally heating to 420-470 ℃ at a speed of 25 ℃/min, preserving heat for 6-7min, and cooling to room temperature along with a furnace.
9. The method of manufacturing according to claim 4, wherein:
when the metal powder is Cu powder to prepare a layered preform, in the step 5, 50MPa pressure is applied through a discharge plasma sintering device, the temperature is raised to 600-650 ℃ and kept for 6-7min, and the metal powder is cooled to room temperature along with a furnace to obtain ANMn 3 Cu-Cu laminate composite.
10. The method of manufacturing according to claim 9, wherein:
the temperature rising rate is controlled as follows: firstly heating to 200 ℃ at a speed of 50 ℃/min, then heating to 300 ℃ at a speed of 40 ℃/min, finally heating to 600-650 ℃ at a speed of 25 ℃/min, preserving heat for 6-7min, and cooling to room temperature along with a furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311688102.2A CN117681510A (en) | 2023-12-11 | 2023-12-11 | Anti-perovskite/metal-metal laminated composite material with zero expansion, directional high thermal conductivity and toughness and preparation thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311688102.2A CN117681510A (en) | 2023-12-11 | 2023-12-11 | Anti-perovskite/metal-metal laminated composite material with zero expansion, directional high thermal conductivity and toughness and preparation thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117681510A true CN117681510A (en) | 2024-03-12 |
Family
ID=90129520
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311688102.2A Pending CN117681510A (en) | 2023-12-11 | 2023-12-11 | Anti-perovskite/metal-metal laminated composite material with zero expansion, directional high thermal conductivity and toughness and preparation thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117681510A (en) |
-
2023
- 2023-12-11 CN CN202311688102.2A patent/CN117681510A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR100836150B1 (en) | Sintered silicon nitride, method of manufacturing the same and sintered silicon nitride substrate | |
| WO2017065139A1 (en) | Aluminum-diamond composite and method for producing same | |
| CN111992708A (en) | Method for preparing high-performance diamond/copper composite material | |
| EP2485257A1 (en) | Heat sink for electronic device, and process for production thereof | |
| JP2005330583A (en) | Cu-Cr ALLOY AND Cu-Cr ALLOY PRODUCTION METHOD | |
| CN109759596B (en) | Heterogeneous gradient composite material and preparation method thereof | |
| JP6908248B2 (en) | SiC ceramics using coated SiC nanoparticles and their manufacturing method | |
| JP7165341B2 (en) | Graphite-copper composite material, heat sink member using the same, and method for producing graphite-copper composite material | |
| CN114315359A (en) | Method for preparing high-strength and high-toughness complex-phase high-entropy ceramic by using solid solution coupling method and application | |
| CN108774699A (en) | Aluminium silicon/aluminium gold hard rock gradient composites and preparation method thereof | |
| Dong et al. | W–Cu system: synthesis, modification, and applications | |
| CN110453126A (en) | A kind of diamond-metal-based compound Heat Conduction Material and preparation method thereof | |
| JP3775335B2 (en) | Silicon nitride sintered body, method for producing silicon nitride sintered body, and circuit board using the same | |
| KR20190032966A (en) | Tape casting slurry composition for manufacturing silicon nitride sintered body | |
| CN117681510A (en) | Anti-perovskite/metal-metal laminated composite material with zero expansion, directional high thermal conductivity and toughness and preparation thereof | |
| CN114951656B (en) | Preparation method of high-entropy alloy-ceramic coating composite material | |
| CN113403493B (en) | High-toughness medium-entropy CrCoNi particle reinforced Cu-based composite material and preparation method thereof | |
| JP2004262756A (en) | Silicon nitride powder, silicon nitride sintered compact, and circuit board for electronic component using the sintered compact | |
| CN113957294A (en) | CrCoNi intermediate entropy alloy reinforced Al-based composite material and preparation method thereof | |
| Wei et al. | Microstructure and properties of Al–Si functionally graded materials for electronic packaging | |
| JP5457992B2 (en) | Method for producing aluminum-ceramic composite structural part | |
| CN111825463A (en) | LaB6-CrB2Composite cathode material and preparation method thereof | |
| Jiang et al. | Properties of WCu, MoCu, and Cu/MoCu/Cu high-performance heat sink materials and manufacturing technologies | |
| CN115488345A (en) | Powder hot-extrusion heat-resistant aluminum alloy and preparation method thereof | |
| CN108486397A (en) | A kind of discharge plasma sintering preparation method of beryllium alumin(i)um alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |