CN113322393A - Preparation method of copper-cuprous phosphide eutectic mixture - Google Patents
Preparation method of copper-cuprous phosphide eutectic mixture Download PDFInfo
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- CN113322393A CN113322393A CN202110593651.6A CN202110593651A CN113322393A CN 113322393 A CN113322393 A CN 113322393A CN 202110593651 A CN202110593651 A CN 202110593651A CN 113322393 A CN113322393 A CN 113322393A
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- copper
- cuprous phosphide
- eutectic mixture
- copper foil
- cuprous
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- 239000000374 eutectic mixture Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011889 copper foil Substances 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 9
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 48
- 239000010431 corundum Substances 0.000 claims description 48
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 239000010949 copper Substances 0.000 abstract description 8
- 229910052802 copper Inorganic materials 0.000 abstract description 7
- 239000000463 material Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1047—Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/60—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes
- C23C8/62—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes only one element being applied
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adornments (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a preparation method of a copper-cuprous phosphide eutectic mixture, which adopts sodium hypophosphite and copper foil as precursors, and cuprous phosphide crystals grow on the surface of the copper foil by heating in an inert atmosphere; then heating the copper foil with cuprous phosphide on the surface at high temperature to form liquid melt; and then cooling the liquid melt to obtain the copper-cuprous phosphide eutectic mixture composite material. The invention has the characteristics different from the common cuprous phosphide-copper composite material, such as high strength and electric conductivity.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a copper-cuprous phosphide eutectic mixture.
Background
Cuprous phosphide (Cu)3P) is attracting attention in the application research of the fields of catalysis, fluorescence and sensitive devices. The cuprous phosphide is compounded with copper, so that the mechanical strength and the conductivity can be improved, and the application range is expandedSuch as anode materials for lithium ion batteries, electrostatic shielding materials, catalysts, solders, and the like.
Disclosure of Invention
The invention provides a preparation method of a copper-cuprous phosphide eutectic mixture aiming at the defects of the prior art.
The method adopts sodium hypophosphite and copper foil as precursors, and cuprous phosphide crystals grow on the surface of the copper foil by heating in an inert atmosphere; then heating the copper foil with cuprous phosphide on the surface at high temperature to form liquid melt; and then cooling the liquid melt to obtain the copper-cuprous phosphide eutectic mixture composite material.
Preferably, the cuprous phosphide crystal is obtained by growing on the surface of the copper foil, and the method specifically comprises the following steps:
step (1), sodium hypophosphite is placed into a corundum boat, and then copper foil with the thickness of 250-;
step (2), putting the product obtained in the step (1) into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (3), heating the product in the step (2) to 280 ℃ and 300 ℃ by a tubular furnace, wherein the heating rate is 10 ℃/min; the temperature is increased to 280-300 ℃, and then the temperature is preserved for 30-60 min; and naturally cooling to room temperature, vacuumizing the corundum tube to remove residual gas in the corundum tube, and taking out the copper foil with cuprous phosphide growing on the surface of the product.
Preferably, the copper foil with cuprous phosphide grown on the surface is heated at high temperature to form a liquid melt; then cooling the liquid melt to obtain a copper-cuprous phosphide eutectic mixture composite material; the method specifically comprises the following steps:
putting a copper foil with cuprous phosphide growing on the surface into a corundum boat, then transferring into a corundum tube, vacuumizing, filling argon gas at 1 atmosphere, and then sealing two ends of the corundum tube;
step (2), heating the product in the step (1) to 800-; the temperature is raised to 800-; then naturally cooling to room temperature, and then taking out the product to obtain the copper-cuprous phosphide eutectic mixture.
Preferably, the corundum tube vacuumizing device is provided with tail gas purifying equipment.
Preferably, the corundum boat has dimensions of 0.8 cm × 0.6 cm × 6 cm.
The invention has the advantages that: the cuprous phosphide growing on the surface of the copper foil is melted at high temperature, and the composite material grows by cooling, wherein the cuprous phosphide is obtained by growing on the surface of the copper foil, the cuprous phosphide and the copper foil are tightly combined, the interface is easy to diffuse among high-temperature atoms, and a liquid phase is generated. After the two are melted into liquid state at high temperature, the eutectic mixture is formed by cooling and crystallization. And 4, melting and cooling the cuprous phosphide to grow crystal again, wherein the microstructure appearance of the precipitated crystal cuprous phosphide is different from that before melting. Before melting, most of cuprous phosphide and crystalline copper are in a mutually separated state, and different from the state before melting, the periphery of cuprous phosphide microcrystals in the copper-cuprous phosphide eutectic mixture is wrapped by copper, the appearance of a crystal boundary is changed, the crystallization quality of the cuprous phosphide is reduced, and more defects are generated. The copper penetrates through the composite material and plays a role of mechanical support for the material. The special structure of the copper-cuprous phosphide eutectic mixture leads to the material having different characteristics such as high strength and electric conductivity from the common cuprous phosphide-copper composite material.
Drawings
FIG. 1 is a comparative XRD diagram of cuprous phosphide and copper-cuprous phosphide eutectic mixture grown on the surface of copper foil.
Detailed Description
The first embodiment is as follows:
step (1), 6g of sodium hypophosphite is put into a corundum boat, and a copper foil which is 5 square centimeters in thickness and 1000 microns is covered on the surface of the corundum boat;
step (2), putting the product obtained in the step (1) into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (3), heating the product of the step (2) to 300 ℃ through a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature for 60min after the temperature is raised to 300 ℃; then naturally cooling to room temperature, vacuumizing the corundum tube (with tail gas purification equipment) to remove residual gas in the corundum tube, and then taking out a product: copper foil with cuprous phosphide grows on the surface;
step (4), putting the product prepared in the step (3) into a new corundum boat, then transferring into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (5), heating the product of the step (4) to 1000 ℃ through a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature for 60min after the temperature is raised to 1000 ℃; then naturally cooling to room temperature, and then taking out the product to obtain a copper-cuprous phosphide eutectic mixture;
example two:
step (1), 3g of sodium hypophosphite is put into a corundum boat, the area of the corundum boat is 0.8 cm multiplied by 0.6 cm multiplied by 6 cm, and a copper foil with the thickness of 250 microns and the square cm is covered on the surface of the corundum boat;
step (2), putting the product obtained in the step (1) into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (3), heating the product of the step (2) to 280 ℃ by a tubular furnace, wherein the heating rate is 10 ℃/min; keeping the temperature for 30min after the temperature is raised to 280 ℃; then naturally cooling to room temperature, vacuumizing the corundum tube (with tail gas purification equipment) to remove residual gas in the corundum tube, and then taking out a product: copper foil with cuprous phosphide grows on the surface;
step (4), putting the product prepared in the step (3) into a new corundum boat, then transferring into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (5), heating the product of the step (4) to 800 ℃ through a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature for 30min after the temperature is raised to 800 ℃; then naturally cooling to room temperature, and then taking out the product to obtain a copper-cuprous phosphide eutectic mixture;
example three:
step (1), putting 5g of sodium hypophosphite into a corundum boat, and covering a copper foil with the thickness of 800 microns, wherein the surface of the corundum boat is 3 square centimeters;
step (2), putting the product obtained in the step (1) into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (3), heating the product of the step (2) to 290 ℃ by a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature after the temperature is increased to 290 ℃, wherein the heat preservation time is 40 min; then naturally cooling to room temperature, vacuumizing the corundum tube (with tail gas purification equipment) to remove residual gas in the corundum tube, and then taking out a product: copper foil with cuprous phosphide grows on the surface;
step (4), putting the product prepared in the step (3) into a new corundum boat, then transferring into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (5), heating the product of the step (4) to 900 ℃ by a tube furnace, wherein the heating rate is 10 ℃/min; keeping the temperature for 40min after the temperature is increased to 900 ℃; then naturally cooling to room temperature, and then taking out the product to obtain a copper-cuprous phosphide eutectic mixture;
as shown in FIG. 1, the XRD pattern of cuprous phosphide (curve 1) grown on the surface of copper foil and the XRD pattern of copper-cuprous phosphide eutectic mixture (curve 2) were observed. As can be seen from the figure, XRD is different before and after the cuprous phosphide is melted and cooled, and the crystalline form and structure of the cuprous phosphide are changed; in the XRD pattern, diffraction peaks of copper crystals are at 43 degrees, 50.4 degrees and 74 degrees, and diffraction peaks at other positions are from cuprous phosphide.
Claims (5)
1. The preparation method of the copper-cuprous phosphide eutectic mixture is characterized by comprising the following steps of: adopting sodium hypophosphite and copper foil as precursors, and heating in an inert atmosphere to grow cuprous phosphide crystals on the surface of the copper foil; then heating the copper foil with cuprous phosphide on the surface at high temperature to form liquid melt; and then cooling the liquid melt to obtain the copper-cuprous phosphide eutectic mixture composite material.
2. The method for preparing the copper-cuprous phosphide eutectic mixture according to claim 1, characterized in that: growing a cuprous phosphide crystal on the surface of the copper foil, and specifically comprising the following steps:
step (1), sodium hypophosphite is placed into a corundum boat, and then copper foil with the thickness of 250-;
step (2), putting the product obtained in the step (1) into a corundum tube, vacuumizing, filling argon gas with 1 atmosphere, and then sealing two ends of the corundum tube;
step (3), heating the product in the step (2) to 280 ℃ and 300 ℃ by a tubular furnace, wherein the heating rate is 10 ℃/min; the temperature is increased to 280-300 ℃, and then the temperature is preserved for 30-60 min; and naturally cooling to room temperature, vacuumizing the corundum tube to remove residual gas in the corundum tube, and taking out the copper foil with cuprous phosphide growing on the surface of the product.
3. The method for preparing the copper-cuprous phosphide eutectic mixture according to claim 1, characterized in that: heating the copper foil with cuprous phosphide on the surface at high temperature to form liquid melt; then cooling the liquid melt to obtain a copper-cuprous phosphide eutectic mixture composite material; the method specifically comprises the following steps:
putting a copper foil with cuprous phosphide growing on the surface into a corundum boat, then transferring into a corundum tube, vacuumizing, filling argon gas at 1 atmosphere, and then sealing two ends of the corundum tube;
step (2), heating the product in the step (1) to 800-; the temperature is raised to 800-; then naturally cooling to room temperature, and then taking out the product to obtain the copper-cuprous phosphide eutectic mixture.
4. The method for preparing the copper-cuprous phosphide eutectic mixture according to claim 2, characterized in that: the corundum tube vacuumizing device is provided with tail gas purifying equipment.
5. A method for preparing a copper-cuprous phosphide eutectic mixture, according to claim 2 or 3, characterized in that: the corundum boat has the size of 0.8 cm multiplied by 0.6 cm multiplied by 6 cm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114284384A (en) * | 2021-12-27 | 2022-04-05 | 杭州电子科技大学 | Preparation method of photoelectric detector based on zinc oxide-cuprous phosphide |
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|---|---|---|---|---|
| JP2000307217A (en) * | 1999-04-26 | 2000-11-02 | Shinko Electric Ind Co Ltd | Forming method of wiring pattern and semiconductor device |
| CN1653016A (en) * | 2002-05-15 | 2005-08-10 | 于尔根·舒尔策-哈德 | Method for producing a ceramic-copper composite substrate |
| CN101574663A (en) * | 2009-06-11 | 2009-11-11 | 南开大学 | Preparation method of copper phosphide (Cu3P) catalyst with hypophosphite by prosoma pyrolytic process |
| CN105845932A (en) * | 2016-05-05 | 2016-08-10 | 苏州大学 | Preparation method of Cu3P nanowire negative electrode, Cu3P nanowire negative electrode prepared by method and application of Cu3P nanowire negative electrode |
| CN109225286A (en) * | 2018-10-08 | 2019-01-18 | 兰州理工大学 | A kind of Cu-NiPO nano-fiber material and the preparation method and application thereof |
-
2021
- 2021-05-28 CN CN202110593651.6A patent/CN113322393B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000307217A (en) * | 1999-04-26 | 2000-11-02 | Shinko Electric Ind Co Ltd | Forming method of wiring pattern and semiconductor device |
| CN1653016A (en) * | 2002-05-15 | 2005-08-10 | 于尔根·舒尔策-哈德 | Method for producing a ceramic-copper composite substrate |
| CN101574663A (en) * | 2009-06-11 | 2009-11-11 | 南开大学 | Preparation method of copper phosphide (Cu3P) catalyst with hypophosphite by prosoma pyrolytic process |
| CN105845932A (en) * | 2016-05-05 | 2016-08-10 | 苏州大学 | Preparation method of Cu3P nanowire negative electrode, Cu3P nanowire negative electrode prepared by method and application of Cu3P nanowire negative electrode |
| CN109225286A (en) * | 2018-10-08 | 2019-01-18 | 兰州理工大学 | A kind of Cu-NiPO nano-fiber material and the preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114284384A (en) * | 2021-12-27 | 2022-04-05 | 杭州电子科技大学 | Preparation method of photoelectric detector based on zinc oxide-cuprous phosphide |
| CN114284384B (en) * | 2021-12-27 | 2024-01-30 | 杭州电子科技大学 | Preparation method based on zinc oxide-cuprous phosphide photoelectric detector |
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