CN102876949A - Method for manufacturing high-heat-conductivity molybdenum-copper-nickel alloy - Google Patents

Method for manufacturing high-heat-conductivity molybdenum-copper-nickel alloy Download PDF

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Publication number
CN102876949A
CN102876949A CN2012103658964A CN201210365896A CN102876949A CN 102876949 A CN102876949 A CN 102876949A CN 2012103658964 A CN2012103658964 A CN 2012103658964A CN 201210365896 A CN201210365896 A CN 201210365896A CN 102876949 A CN102876949 A CN 102876949A
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powder
copper
molybdenum
blank
cupronickel
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CN102876949B (en
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吴华夏
周秋俊
曹振玲
吴磊
程海
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Anhui East China Institute of Optoelectronic Technology
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Anhui East China Institute of Optoelectronic Technology
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Abstract

The invention discloses a method for manufacturing high-heat-conductivity molybdenum-copper-nickel alloy. The method includes steps of firstly, mixing: weighing mixed powder of Mo (molybdenum) powder, Cu(copper) powder and Ni (nickel) powder to stir on a centrifugal ball mill for 4 hours; secondly, pressing: placing the mixed powder stirred uniformly into a pressing die for blank pressing; thirdly, sintering in vacuum: placing pressed blank into a vacuum furnace to sinter at a high temperature; fourthly, impregnating copper: melting oxygen-free copper in a hydrogen atmosphere furnace, placing the blank sintered in vacuum to impregnate in melted copper liquid; fifthly, turning: turning the impregnated blank according to the requirements, removing surplus copper layers on the surface; and sixthly, scouring: impregnating turned parts into solution to scour, washing the parts by tap water, and dewatering and drying the parts by alcohol. The molybdenum-copper-nickel alloy manufactured by the above method can be used for metal ceramic structures of high-power traveling wave tubes such as energy transmission windows and collector electrodes and key parts having high requirements for heat radiation.

Description

A kind of method of making high heat conductance molybdenum cupronickel
Technical field
The present invention relates to the microwave vacuum devices field, especially relate to a kind of method of making high heat conductance molybdenum cupronickel.
Background technology
Some key parts of high power travelling wave tube are in the condition of high temperature when work, such as delivery of energy window, collector etc., therefore the thermal conductivity of material there is high requirement, only has the material of high heat conductance its heat in time could be transferred out, thereby guarantee the homogeneous tube working reliability.And these parts all are the sintering metal structures, to the metallic substance that uses require must the coefficient of expansion close to pottery, so that soldering.
Conventional alloys with controlled expansion can satisfy for the requirement of the coefficient of expansion, but heat-sinking capability is poor as cutting down, can't be in these applications; And as molybdenum-copper, tungsten-copper alloy etc., since undesirable to the wetting property of scolder, to some extent restriction used at parts such as the demanding delivery of energy windows of soldering reliability.Therefore, study a kind of high heat conductance that namely has, the coefficient of expansion with pottery approaches again, but also the good material of the wetting property of scolder is had great significance to high power travelling wave tube.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of making high heat conductance molybdenum cupronickel for problems of the prior art, its objective is that the molybdenum cupronickel by the manufacturing of this kind method can be used in the sintering metal structures such as the delivery of energy window of high power travelling wave tube, collector and on the demanding key part that dispels the heat.
Technical scheme of the present invention is that the method for this kind manufacturing high heat conductance molybdenum cupronickel comprises:
1) compounding process: taking by weighing mass ratio is the Mo powder: the Cu powder: the mixed powder of Ni powder=80:10:10, stirred 4 hours at ball-bearing mill;
2) suppression process: the mixed powder after will stirring is put into compacting tool set, at hydropress pressure 10~50t is set, and carries out the blank compacting;
3) vacuum sintering operation: the blank after the punching press is put into the vacuum oven high temperature sintering;
4) soak copper process: in the nitrogen atmosphere middle fusing of sitting around a fire, the copper liquid of the blank after the vacuum sintering being put into fusing floods with oxygen free copper, and dipping time is 0.5~1h;
5) Vehicle Processing operation: the blank that will soak behind the copper machines as requested, removes simultaneously the unnecessary copper layer in surface;
6) pickling process: the part after the Vehicle Processing is immersed solution carry out pickling, hold-time 10~15s washed part at least 30 seconds with tap water afterwards, dried with dehydration of alcohol again.
In the described vacuum sintering operation, the temperature curve of high temperature sintering is:
Be warmed up to (800 ± 50) ° C in 1 hour, be incubated 0.5-1.5 hour;
Be warmed up to again (1250 ± 10) ° C in 1 hour, be incubated 0.5-1.5 hour;
Cool to room temperature in 2 hours subsequently.
The granularity of described Mo powder, Cu powder, Ni powder all is the powders less than 10 microns.
The composition of described Acidwash solution is: sulfuric acid: (1000 ± 20) mL, nitric acid: (1000 ± 20) mL, sodium-chlor: (2~5) g/L.
As a kind of more preferred condition of above-mentioned manufacture method, in the described vacuum sintering operation, the temperature curve of high temperature sintering is preferably:
Be warmed up to (800 ± 10) ° C in 40 minutes, be incubated 1 hour;
Be warmed up to again (1250 ± 10) ° C in 40 minutes, be incubated 1 hour;
60 minutes subsequently cool to room temperature.
The granularity of described Mo powder, Cu powder, Ni powder is preferably the powder less than 5 microns.
Method with this kind manufacturing high heat conductance molybdenum cupronickel of said structure has the following advantages:
1. the high thermal conductance molybdenum alloy of the method manufacturing of this kind manufacturing high heat conductance molybdenum cupronickel is except thermal conductivity height, the coefficient of expansion and pottery approach, also very good to the wetting property of scolder, its coefficient of expansion is because the rational proportion between powder simultaneously, can be more approaching with 95 alumina ceramics in 1000 ℃, therefore be highly suitable for using on the parts such as heat radiation, the demanding high power travelling wave tube delivery of energy of soldering reliability window, thus the working reliability of assurance homogeneous tube.
2. this kind made in the method for high heat conductance molybdenum cupronickel and soaked the technique of copper so that material is finer and close and even, and the assurance of its vacuum-tightness is highly profitable.
Description of drawings
The invention will be further described below in conjunction with accompanying drawing:
Fig. 1 is the structural representation of the compacting tool set used in the suppression process of the present invention.
Embodiment
The method that this kind made high heat conductance molybdenum cupronickel comprises:
1) compounding process: taking by weighing mass ratio is the Mo powder: the Cu powder: the mixed powder of Ni powder=80:10:10, stirred 4 hours at ball-bearing mill;
2) suppression process: the mixed powder after will stirring is put into compacting tool set, at hydropress pressure 10~50t is set, and carries out the blank compacting;
3) vacuum sintering operation: the blank after the punching press is put into the vacuum oven high temperature sintering, and the temperature curve of high temperature sintering is:
Be warmed up to (800 ± 50) ° C in 1 hour, be incubated 0.5-1.5 hour;
Be warmed up to again (1250 ± 10) ° C in 1 hour, be incubated 0.5-1.5 hour;
Cool to room temperature in 2 hours subsequently;
4) soak copper process: in the nitrogen atmosphere middle fusing of sitting around a fire, the copper liquid of the blank after the vacuum sintering being put into fusing floods with oxygen free copper, and dipping time is 0.5~1h;
5) Vehicle Processing operation: the blank that will soak behind the copper machines as requested, removes simultaneously the unnecessary copper layer in surface;
6) pickling process: the composition of Acidwash solution is: sulfuric acid: (1000 ± 20) mL, nitric acid: (1000 ± 20) mL, sodium-chlor: (2~5) g/L; Part after the Vehicle Processing is immersed solution carry out pickling, hold-time 10~15s washed part at least 30 seconds with tap water afterwards, dried with dehydration of alcohol again.
Wherein, the granularity of Mo powder, Cu powder, Ni powder all is the powders less than 10 microns, is preferably granularity less than 5 microns powder.
As of the present invention a kind of more preferred embodiment, the temperature curve of high temperature sintering is preferably in the vacuum sintering operation:
Be warmed up to (800 ± 10) ° C in 40 minutes, be incubated 1 hour;
Be warmed up to again (1250 ± 10) ° C in 40 minutes, be incubated 1 hour;
60 minutes subsequently cool to room temperature.
The high thermal conductance molybdenum alloy that the method for this kind manufacturing high heat conductance molybdenum cupronickel is made is except thermal conductivity height, the coefficient of expansion and pottery approach, also very good to the wetting property of scolder, its coefficient of expansion is because the rational proportion between powder, can be more approaching with 95 alumina ceramics in 1000 ℃, therefore be highly suitable for using on the parts such as heat radiation, the demanding high power travelling wave tube delivery of energy of soldering reliability window, thus the working reliability of assurance homogeneous tube.
Simultaneously, soak the technique of copper so that material is finer and close and even, the assurance of its vacuum-tightness is highly profitable.Require the sintering metal structure devices high, that soldering reliability is high all can be applicable for other heat radiation in addition.

Claims (6)

1. method of making high heat conductance molybdenum cupronickel is characterized in that: the method for described manufacturing high heat conductance molybdenum cupronickel comprises,
1) compounding process: taking by weighing mass ratio is the Mo powder: the Cu powder: the mixed powder of Ni powder=80:10:10, stirred 4 hours at ball-bearing mill;
2) suppression process: the mixed powder after will stirring is put into compacting tool set, at hydropress pressure 10~50t is set, and carries out the blank compacting;
3) vacuum sintering operation: the blank after the punching press is put into the vacuum oven high temperature sintering;
4) soak copper process: in the nitrogen atmosphere middle fusing of sitting around a fire, the copper liquid of the blank after the vacuum sintering being put into fusing floods with oxygen free copper, and dipping time is 0.5~1h;
5) Vehicle Processing operation: the blank that will soak behind the copper machines as requested, removes simultaneously the unnecessary copper layer in surface;
6) pickling process: the part after the Vehicle Processing is immersed solution carry out pickling, hold-time 10~15s washed part at least 30 seconds with tap water afterwards, dried with dehydration of alcohol again.
2. a kind of method of making high heat conductance molybdenum cupronickel according to claim 1, it is characterized in that: in the described vacuum sintering operation, the temperature curve of high temperature sintering is:
Be warmed up to (800 ± 50) ° C in 1 hour, be incubated 0.5-1.5 hour;
Be warmed up to again (1250 ± 10) ° C in 1 hour, be incubated 0.5-1.5 hour;
Cool to room temperature in 2 hours subsequently.
3. a kind of method of making high heat conductance molybdenum cupronickel according to claim 2, it is characterized in that: the granularity of described Mo powder, Cu powder, Ni powder all is the powders less than 10 microns.
4. a kind of method of making high heat conductance molybdenum cupronickel according to claim 3, it is characterized in that: the composition of described Acidwash solution is: sulfuric acid: (1000 ± 20) mL, nitric acid: (1000 ± 20) mL, sodium-chlor: (2~5) g/L.
5. the described a kind of method of making high heat conductance molybdenum cupronickel of each claim according to claim 2-4, it is characterized in that: in the described vacuum sintering operation, the temperature curve of high temperature sintering is preferably:
Be warmed up to (800 ± 10) ° C in 40 minutes, be incubated 1 hour;
Be warmed up to again (1250 ± 10) ° C in 40 minutes, be incubated 1 hour;
60 minutes subsequently cool to room temperature.
6. a kind of method of making high heat conductance molybdenum cupronickel according to claim 5, it is characterized in that: the granularity of described Mo powder, Cu powder, Ni powder is preferably the powder less than 5 microns.
CN201210365896.4A 2012-09-27 2012-09-27 Method for manufacturing high-heat-conductivity molybdenum-copper-nickel alloy Active CN102876949B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106683959A (en) * 2017-01-25 2017-05-17 中国科学院电子学研究所 Collector electrode, preparation method thereof, space traveling wave tube and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101121972A (en) * 2007-09-11 2008-02-13 中北大学 Method for preparing Mo-Cu composite material
JP2009001882A (en) * 2007-06-22 2009-01-08 Kobe Steel Ltd Powder mixture for powder metallurgy, and iron powder sintered body
CN101942592A (en) * 2010-08-04 2011-01-12 湖南科技大学 Method for preparing molybdenum copper alloy by activated sintering

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009001882A (en) * 2007-06-22 2009-01-08 Kobe Steel Ltd Powder mixture for powder metallurgy, and iron powder sintered body
CN101121972A (en) * 2007-09-11 2008-02-13 中北大学 Method for preparing Mo-Cu composite material
CN101942592A (en) * 2010-08-04 2011-01-12 湖南科技大学 Method for preparing molybdenum copper alloy by activated sintering

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106683959A (en) * 2017-01-25 2017-05-17 中国科学院电子学研究所 Collector electrode, preparation method thereof, space traveling wave tube and preparation method thereof
CN106683959B (en) * 2017-01-25 2018-10-02 中国科学院电子学研究所 Collector and preparation method thereof, space travelling wave tube and preparation method thereof

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