CN115710683B - A Mo-Cu alloy preparation method based on surface coating technology and flame spraying technology - Google Patents
A Mo-Cu alloy preparation method based on surface coating technology and flame spraying technology Download PDFInfo
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- CN115710683B CN115710683B CN202211472591.3A CN202211472591A CN115710683B CN 115710683 B CN115710683 B CN 115710683B CN 202211472591 A CN202211472591 A CN 202211472591A CN 115710683 B CN115710683 B CN 115710683B
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- 229910017315 Mo—Cu Inorganic materials 0.000 title claims abstract description 78
- 239000000956 alloy Substances 0.000 title claims abstract description 64
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 63
- 238000005516 engineering process Methods 0.000 title claims abstract description 45
- 238000010285 flame spraying Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000011248 coating agent Substances 0.000 title claims abstract description 17
- 238000000576 coating method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 238000002474 experimental method Methods 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 238000005507 spraying Methods 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011247 coating layer Substances 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 230000009467 reduction Effects 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 8
- LNSPFAOULBTYBI-UHFFFAOYSA-N [O].C#C Chemical group [O].C#C LNSPFAOULBTYBI-UHFFFAOYSA-N 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000009825 accumulation Methods 0.000 claims abstract description 3
- 230000008569 process Effects 0.000 claims description 7
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 5
- 238000007731 hot pressing Methods 0.000 claims description 5
- 238000005488 sandblasting Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims 2
- 238000000227 grinding Methods 0.000 claims 1
- 239000010410 layer Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000004663 powder metallurgy Methods 0.000 description 3
- 239000010963 304 stainless steel Substances 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- QFXZANXYUCUTQH-UHFFFAOYSA-N ethynol Chemical group OC#C QFXZANXYUCUTQH-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Coating By Spraying Or Casting (AREA)
Abstract
The invention provides a Mo-Cu alloy preparation method based on a surface coating technology and a flame spraying technology, which comprises the following steps of S1, mixing ammonium tetramolybdate powder and copper nitrate powder according to a mass ratio, adding the mixture of ammonia water and deionized water, continuously stirring and heating, S2, washing a reaction product by adopting deionized water, separating, washing the reaction product by using absolute ethyl alcohol, heating and drying, carrying out a calcination experiment on the dried reaction product powder to prepare Mo-Cu composite powder with a Mo coating layer, S3, spraying the prepared Mo-Cu composite powder with the Mo coating layer on the surface of a substrate by adopting an oxygen-acetylene flame spraying technology, carrying out multilayer spraying accumulation, and S4, carrying out a hydrogen reduction experiment and a vacuum sintering experiment on the prepared Mo-Cu alloy to prepare the high-density Mo-Cu alloy. The Mo-Cu alloy prepared by the method has higher density, can realize the optimal regulation and control of the structure and performance of the technological parameters, and improves the interface bonding strength among particles and the optimal control.
Description
Technical Field
The invention belongs to the field of electrical contact materials, and particularly relates to a preparation method of a high-density Mo-Cu alloy.
Background
Along with the continuous perfect development of the ultra-high voltage transmission network of the national power grid and the gradual increase of the specific gravity of new energy power generation, the high-voltage power transmission gradually becomes a long-distance power transmission main stream mode, so that the service working condition of the high-voltage contact material is more severe, and new requirements are also put forward on the compactness, the uniformity of organization and performance, the mechanical performance and the thermoelectric performance of the Mo-Cu alloy material. The Mo-Cu alloy electrical contact material is used as a heart of a high-voltage transmission device and mainly bears the work of switching on and switching off a high-voltage circuit. At present, the main failure reason of the high-voltage power transmission device is the failure of the high-voltage power contact, once the failure problem of the power contact material occurs, the normal power transmission work of the high-voltage power transmission line is necessarily influenced, and therefore, the preparation of the Mo-Cu power contact material with high compactness and excellent performance has profound significance. The problem of high porosity in the preparation process of the Mo-Cu electrical contact material is always a technical problem to be solved, in order to improve the compactness of the Mo-Cu alloy, the regulation and control of the structure and the performance of the Mo-Cu alloy are realized, the Mo-Cu alloy is prepared by utilizing a surface coating technology and a flame spraying technology, the compactness of the Mo-Cu alloy can be improved, the regulation and control of the structure and the performance of the Mo-Cu alloy can be realized, and the service life of the Mo-Cu alloy is prolonged by controlling the component proportion and the powder particle size of Mo and Cu.
At present, the main preparation technology for Mo-Cu alloy is a powder metallurgy method, which mainly comprises the steps of preparing Mo-Cu composite powder through mechanical alloying, performing compression molding by a press machine, and sintering in a vacuum hot-pressing sintering furnace to prepare the Mo-Cu alloy. The Mo-Cu alloy prepared by the powder metallurgy method has higher porosity, poor uniformity of tissue components and easy occurrence of component segregation and agglomeration. Relevant research is carried out by relevant researchers at home and abroad on Mo-Cu alloy and composite powder preparation technology thereof, and the influence of different composite powder preparation technologies on the structure and performance of the Mo-Cu alloy is explored from the composite powder preparation technology, but the problem of low compactness and the like of the Mo-Cu alloy prepared by a powder metallurgy method is common, and the novel Mo-Cu alloy preparation method such as metal powder injection molding is still in a starting stage and cannot realize industrialized batch production.
In view of the technical defects of the Mo-Cu alloy preparation method, the invention provides a Mo-Cu alloy preparation method based on a surface coating technology and a flame spraying technology. The invention prepares the high-density Mo-Cu alloy by optimizing and controlling the solution proportion, the spraying process, the reduction process and the sintering process by a chemical-reduction method, and has important significance for realizing the regulation and control of the structure and the performance of the Mo-Cu alloy and prolonging the service life of the Mo-Cu alloy.
Disclosure of Invention
In order to overcome the defects of the prior Mo-Cu alloy preparation technology, the invention aims to provide the Mo-Cu alloy preparation method based on the surface coating technology and the flame spraying technology, which has the advantages of high compactness, uniform structure and performance, adjustable thermal expansion coefficient and excellent electric and heat conductivity, and the technology improves the compactness of the Mo-Cu alloy, realizes the optimal control of the structure and the performance of the Mo-Cu alloy and ensures that the Mo-Cu alloy is widely applied.
The invention provides a Mo-Cu alloy preparation method based on a surface coating technology and a flame spraying technology, which adopts the technical scheme that the method comprises the following steps:
S1, mixing ammonium tetramolybdate powder and copper nitrate powder according to a mass ratio, adding the mixture into a mixed solution of ammonia water and deionized water, and continuously stirring and heating;
S2, washing and separating a reaction product by deionized water, washing and heating and drying the reaction product by absolute ethyl alcohol to prepare reaction product powder, and performing a calcination experiment on the dried reaction product powder to prepare Mo-Cu composite powder with a Mo coating layer;
S3, polishing the surface of the substrate by adopting sand paper, carrying out sand blasting on the surface of the substrate, spraying the prepared Mo-Cu composite powder with the Mo coating layer on the surface of the substrate by adopting an oxygen-acetylene flame spraying technology, and carrying out multilayer spraying accumulation to prepare Mo-Cu alloy;
and S4, carrying out a hydrogen reduction experiment and a vacuum sintering experiment on the prepared Mo-Cu alloy to prepare the high-density Mo-Cu alloy.
Further, in the step S1, the mass ratio of the ammonium tetramolybdate to the copper nitrate is weighed according to the proportion of 30% -70% of Cu in the Mo-Cu alloy, ammonia water is twice that of deionized water, the water bath heating temperature is 20-80 ℃, the stirring speed is 100-200r/min, and the stirring time is 20-40min.
Further, the drying temperature in the step S2 is 80-120 ℃ and the drying time is 2-4h.
Further, the calcining temperature of the calcining experiment in the step S2 is 240-600 ℃, the heat preservation time is 1-2h, the heating rate is 2-5 ℃ per minute, and the cooling rate is 5-10 ℃ per minute.
Further, in the step S3, the acetylene flow rate of oxygen-acetylene flame spraying is 200-400L/h, the oxygen flow rate is 100-200L/h, the spraying distance is 20-50mm, the spraying speed is 50-150mm/S, the acetylene pressure is 0.1-0.2MPa, the oxygen pressure is 0.4-0.8MPa, the powder feeding amount of Mo-Cu composite powder is 10g/min, and the preheating temperature of a substrate is 600-700 ℃.
Further, the hydrogen reduction temperature of the hydrogen reduction experiment in the step S4 is 1050-1200 ℃, the heat preservation time is 2-6h, the hydrogen flow is 0.5-1.5L/min, the heating rate is 5-10 ℃/min, and the cooling rate is 5-10 ℃/min.
Further, the Mo-Cu alloy vacuum sintering experiment process in the step S4 comprises the steps that the vacuum degree required by a vacuum hot-pressing sintering furnace is 10 -2-10-6 Pa, the sintering temperature is 1150-1350 ℃, the heat preservation time is 2-4h, the heating rate is 2-5 ℃ per minute, and the furnace is cooled.
Further, the density of the Mo-Cu alloy is more than 98%.
Further, the substrate is 304 stainless steel.
The invention has the beneficial effects that:
(1) The composite powder with the Mo coating layer can be used for preparing Mo-Cu composite powder with different proportions by adjusting the proportion of powder raw materials, can inhibit the growth of a Cu phase in the preparation process of Mo-Cu alloy, and ensures that two phases are uniformly distributed without agglomeration segregation phenomenon.
(2) According to the invention, the Mo-Cu alloy is prepared by an oxygen-acetylene flame spraying technology, the preparation of the high-density Mo-Cu alloy can be realized by adjusting various technological parameters, the high-density Mo-Cu alloy with uniform microstructure can be obtained after spraying by the flame spraying technology, and the interface bonding between particles has higher strength.
(3) According to the invention, the structure and the performance of the composite powder with the Mo coating layer and the Mo-Cu alloy are regulated through low-temperature calcination, hydrogen reduction and vacuum sintering experiments, so that the obtained composite powder with the Mo coating layer has better powder flowability, eliminates the powder agglomeration phenomenon, and regulates interface bonding among Mo-Cu alloy particles and regulation of the structure and the performance.
Drawings
FIG. 1 is a schematic diagram of the operation flow of a Mo-Cu alloy preparation method based on the surface coating technology and the flame spraying technology.
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1:
as shown in fig. 1, in this example, a composite powder with a Mo coating layer was prepared by a surface coating technique, and a high-density mo—cu alloy was prepared on the surface of a stainless steel substrate by an oxy-acetylene flame spraying technique.
In this embodiment, the substrate is made of 304 stainless steel.
In this example, the prepared mo—cu composite powder having a Mo coating layer was prepared by a chemical method.
In this example, the prepared high-density Mo-Cu alloy was prepared by oxy-acetylene flame spraying, which has excellent interfacial bonding strength.
Referring to fig. 1, a method for preparing Mo-Cu alloy based on surface cladding technology and flame spraying technology includes the following steps:
firstly, weighing and mixing ammonium tetramolybdate and copper nitrate according to the mass ratio of 30% -70% of Cu in the Mo-Cu alloy, adding the mixture into a mixed solution (2:1) of ammonia water and deionized water, continuously stirring and heating, wherein the water bath heating temperature is 20-80 ℃, the stirring speed is 100-200r/min, and the stirring time is 20-40min;
Step two, washing and separating a reaction product by deionized water, washing the reaction product by absolute ethyl alcohol, and heating and drying the reaction product at the drying temperature of 80-120 ℃ for 2-4 hours;
Step three, performing a calcination experiment on the reaction product powder, wherein the calcination temperature is 240-600 ℃, the heat preservation time is 1-2h, the heating rate is 2-5 ℃ per minute, and the cooling rate is 5-10 ℃ per minute, so as to prepare Mo-Cu composite powder with a Mo coating layer;
step four, polishing the surface of the substrate by adopting sand paper, and carrying out sand blasting treatment on the surface of the substrate;
Preparing Mo-Cu alloy by adopting an oxygen-acetylene flame spraying technology, wherein the acetylene flow is 200-400L/h, the oxygen flow is 100-200L/h, the spraying distance is 20-50mm, the spraying speed is 50-150mm/s, the acetylene pressure is 0.1-0.2MPa, the oxygen pressure is 0.4-0.8MPa, the powder feeding amount of Mo-Cu composite powder is 10g/min, and the preheating temperature of a substrate is 600-700 ℃;
step six, adopting a tubular atmosphere furnace to perform a hydrogen reduction experiment, wherein the heating temperature is 1050-1200 ℃, the heat preservation time is 2-6h, the hydrogen flow is 0.5-1.5L/min, the heating rate is 5-10 ℃/min, and the cooling rate is 5-10 ℃/min;
And step seven, performing a high-temperature sintering experiment by adopting a vacuum hot-pressing sintering furnace, wherein the vacuum degree required by the vacuum hot-pressing sintering furnace is 10 -2-10-6 Pa, the sintering temperature is 1150-1350 ℃, the heat preservation time is 2-4h, the heating rate is 2-5 ℃ per minute, and the furnace is cooled.
The invention is described more clearly and completely by way of example, but the invention is not limited thereto. It is within the scope of the claims to those skilled in the art to adjust the parameters designed (e.g., by changing the calcination process, flame spraying process, hydrogen reduction and high temperature sintering process) and to change the proportioning preparation method of the mo—cu composite powder.
Claims (8)
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1226152A (en) * | 1984-01-23 | 1987-09-01 | Alloy Metals, Inc. | Corrosion resistant thermal spray alloy and coating method |
| CN106119760A (en) * | 2016-07-28 | 2016-11-16 | 西安石油大学 | A kind of thermal barrier coating with double-layer bonding layer and preparation method thereof |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3254970A (en) * | 1960-11-22 | 1966-06-07 | Metco Inc | Flame spray clad powder composed of a refractory material and nickel or cobalt |
| JP2004124130A (en) * | 2002-09-30 | 2004-04-22 | Fujimi Inc | Powder for thermal spraying, method for manufacturing the same, and thermal spraying method using the powder for thermal spraying |
| JP4394993B2 (en) * | 2004-03-29 | 2010-01-06 | トヨタ自動車株式会社 | Method for producing thermal spraying powder |
| RU2327548C1 (en) * | 2006-09-14 | 2008-06-27 | Федеральное Государственное Унитарное Предприятие "Центральный научно-исследовательский институт черной металлургии им. И.П. Бардина" (ФГУП "ЦНИИчермет им. И.П. Бардина") | Method of producing iron base powder (its variants) |
| JP5626947B2 (en) * | 2008-09-22 | 2014-11-19 | 独立行政法人物質・材料研究機構 | Alloy particles and wires used for atmospheric plasma spraying and hot wire arc spraying |
| CN109980107B (en) * | 2017-12-28 | 2020-12-01 | Tcl科技集团股份有限公司 | CuMO2Preparation method thereof and light-emitting device |
| CN113913721B (en) * | 2021-09-14 | 2023-01-24 | 河海大学 | Composite powder for supersonic flame spraying, preparation and application |
| CN114086023B (en) * | 2021-11-10 | 2022-08-05 | 浙江福达合金材料科技有限公司 | Method for preparing copper-based electric contact material based on foaming infiltration process and product thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1226152A (en) * | 1984-01-23 | 1987-09-01 | Alloy Metals, Inc. | Corrosion resistant thermal spray alloy and coating method |
| CN106119760A (en) * | 2016-07-28 | 2016-11-16 | 西安石油大学 | A kind of thermal barrier coating with double-layer bonding layer and preparation method thereof |
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