CN101979191A - Method for preparing molybdenum copper part with complex shape - Google Patents
Method for preparing molybdenum copper part with complex shape Download PDFInfo
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- CN101979191A CN101979191A CN 201010555941 CN201010555941A CN101979191A CN 101979191 A CN101979191 A CN 101979191A CN 201010555941 CN201010555941 CN 201010555941 CN 201010555941 A CN201010555941 A CN 201010555941A CN 101979191 A CN101979191 A CN 101979191A
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Abstract
The invention discloses a method for preparing a molybdenum copper part with complex shape. The method comprises the following steps of: mixing an organic monomer and a cross-linking agent according to a certain volumetric ratio and adding into water to prepare 10 to 35 weight percent premixed solution; adding a certain proportion of molybdenum powder and a small amount of dispersing agent to prepare uniform and stable paste in which the volumetric ratio of the powder is 42 to 52 percent; adding a proper amount of initiator and catalyst and performing injection molding to obtain a billet with the shape of a required product; drying the billet and removing the adhesive; sintering at the temperature of between 1,200 and 1,450 DEG C to obtain a near-net-shape molybdenum frame, and infiltrating copper to obtain high-compactness molybdenum copper. The method has the advantages of simple process, high utilization ratio of material, low cost and high mechanical property and thermal property of product, is easy to realize large-batch direct preparation of the molybdenum copper part with complex shape and can be conveniently applied to the fields such as electronics, instruments, aviation and the like.
Description
Technical field
The present invention relates to a kind of method for preparing molybdenum-copper component, particularly relate to the method that a kind of direct preparation complicated shape contains the molybdenum-copper component of 70～90wt%Mo.
Background technology
Molybdenum copper (Mo-Cu) alloy is the pseudo-alloy that is made of high-melting-point, high rigidity molybdenum and high conduction, high heat-conducting copper, have characteristics such as high-strength, high hard, high heat conduction, low bulk, as electrical contact material, electrode material, electrothermal alloy, heat sink or electronic package material, be widely used in fields such as machinery, electrotechnical, electronic, Aero-Space, instrument and meter, information and military project, also be considered to the new structure function integration material that the utmost point has development potentiality and application prospect.
The Mo-Cu alloy is existing preparation method mainly contain: hot rolling is compound, skeleton-infiltration of copper, powder method.But these methods all exist certain limitation or deficiency.As the preparation of, hot rolling composite algorithm be composite material of molybdenum and copper but not alloy, the alloy density of powder technique method preparation is general≤95%, so product mechanics and thermal property are lower.Molybdenum skeleton-infiltration of copper method is molybdenum-copper preparation method commonly used, but because the molybdenum skeleton of methods such as traditional powder compaction, hot pressing preparation is simple shape, has limited the freedom of product design.
Along with the development of modern science and technology, particularly microelectric technique, the demand of Mo-Cu alloy is increased day by day, its performance and shape of product complexity are all had higher requirement, to satisfy the requirement of current designs " compactedness " principle.But complex-shaped product can not directly be obtained by traditional press forming technology, need carry out machined toward contact, higher and unmanageable Mo-Cu alloy has increased production cost undoubtedly greatly, has wasted resource for the prices of raw and semifnished materials for this, both do not met the development trend of materials processing technology " short flow process, nearly end form ", also do not meet the policy that the world today builds a resource-conserving society, thereby it is just especially important to explore the low-cost method that prepare complicated shape molybdenum copper part.
Summary of the invention
Technical problem to be solved by this invention provides the method for preparing large scale, high accuracy complicated shape molybdenum-copper component that a kind of technology is simple, cost is low, stock utilization is high, be easy to produce in enormous quantities.
In order to solve the problems of the technologies described above, the present invention realizes by following steps:
(1), premixed liquid preparation:
With organic monomer and crosslinking agent (20～100) by volume: 1 mixes mutually, and adds deionized water and be mixed with the premixed liquid that concentration is 10～35wt%;
(2), high-volume fractional pulp preparation:
In premixed liquid, add purity 〉=99%, granularity is the molybdenum powder of 2～10 μ m and the ammonium citrate dispersant that mass ratio is 0.2～3wt% thereof, and add ammoniacal liquor and regulate pH value to 8～10, through mechanical ball milling prepare the molybdenum powder volume ratio be 42～55% evenly, stable slurry;
(3), casting and curing:
The ammonium persulfate (AP S) initator and the N that in the slurry for preparing, add 0.1～4wt%, N, N, N-tetramethylethylenediamine (TEMED) catalyst, 0.1 the n-octyl alcohol defoamer of～0.3wt%, and mix fast in a vacuum, rubber, plastics, metal or the glass mold of required product shape are slowly injected in and degasification then, and under 50～80 ℃ of temperature, leave standstill 2～30min, make it to solidify fully, obtain solidifying base, this moment, base substrate had higher intensity;
(4), molybdenum skeleton preparation:
Solidify base and be warming up to dry 60～180min under 90～110 ℃ of temperature in the speed with 3～6 ℃/min under vacuum or the hydrogen atmosphere earlier, get rid of to solidify in the base behind the moisture, speed with 8～15 ℃/min is warming up to 400～550 ℃ subsequently, and be incubated 15～45min, with organic matter in the abundant eliminating base substrate, be rapidly heated subsequently to 1200～1450 ℃, and be incubated 60～150min, obtain the molybdenum skeleton of complicated shape;
(5), the infiltration of copper:
The anaerobic copper sheet is placed molybdenum skeleton bottom or top, subsequently at sintering furnace in vacuum, hydrogen or argon gas, handling 60～120min under 1150～1325 ℃ of temperature does not press or pressuring method infiltration copper to have, and obtain 70～90wt%Mo-Cu alloy fine and close, even tissue, alloy density 〉=99.8%.
Wherein, adopting acrylamide (AM) or Methacrylamide (MAM) is organic monomer, N, and N ,-methylene-bisacrylamide (MBAM) or diallyl tartaric acid diamides (DATDA) are made crosslinking agent.
Wherein, after will solidifying the base taking-up, also can reprocess to modify in case of necessity and handle its shape.
Molybdenum-copper density 〉=99.8% according to method for preparing.
The invention has the advantages that:
Existing relatively molybdenum-copper preparation method, it belongs to a kind of method of near-net-shape, can direct forming and prepare high-performance 70～90wt%Mo-Cu alloy product of large scale, complicated shape, its technology is simple, cost is low, stock utilization is high, be easy to production in enormous quantities, molybdenum-copper poor in processability, the difficult problem of complex parts preparation have been solved, and the mould therefor material source is extensive, is easy to make.
Description of drawings
Fig. 1 is a process chart of the present invention.
Fig. 2 is the molybdenum skeleton microscopic structure of the present invention's preparation.
Fig. 3 is the 85Mo-Cu alloy microscopic structure of the present invention's preparation.
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1:
Referring to Fig. 1, Fig. 2 and Fig. 3, acrylamide (AM) and N, N ,-methylene-bisacrylamide (MBAM) mixed in 20: 1 by volume mutually, and the adding deionized water is mixed with the premixed liquid that concentration is 20wt%; Adding purity 〉=99%, particle mean size are that molybdenum powder and the mass ratio thereof of 6 μ m is the ammonium citrate of 1wt%, and add ammoniacal liquor adjusting pH value to 9, prepare powder volume than even, the stable slurry that is 48% through mechanical ball milling; The ammonium persulfate (APS) and the N that add 1.2wt% subsequently, N, N, N-tetramethylethylenediamine (TEMED), the n-octyl alcohol defoamer of 0.2wt%, and mix fast in a vacuum, with degasification, the rubber mold die cavity of the complicated shape that slow then injection has designed and made, and, obtain solidifying base at 60 ℃ of temperature-curable 25min; To solidify base and place hydrogen sintering furnace, and be warming up to 110 ℃ of temperature at a slow speed with 4 ℃/min earlier, 90min is with drying in insulation, speed with 10 ℃/min is warming up to 550 ℃ subsequently, and insulation 30min is with binder removal, be rapidly heated then to 1380 ℃, and insulation 90min, the molybdenum skeleton obtained; The anaerobic copper sheet is placed molybdenum skeleton bottom, last in hydrogen furnace 1300 ℃ of infiltration copper that carry out 90min handle, obtain Tissue distribution evenly, density is 99.99% 85Mo-Cu alloy parts.
Embodiment 2:
Referring to Fig. 1, obtain solidifying base by embodiment 1 described method.To solidify base and place hydrogen sintering furnace, and be warming up to 110 ℃ of temperature at a slow speed with 4 ℃/min earlier, 90min is with drying in insulation, speed with 10 ℃/min is warming up to 550 ℃ subsequently, and insulation 30min is with binder removal, be rapidly heated then to 1200 ℃, and insulation 120min, the molybdenum skeleton obtained; The anaerobic copper sheet is placed molybdenum skeleton bottom, and last 1180 ℃ of infiltration copper processing of carrying out 120min in hydrogen furnace obtain the uniform 70Mo-Cu alloy of full densification and Tissue distribution parts.
Embodiment 3:
Methacrylamide (MAM) and diallyl tartaric acid diamides (DATDA) were mixed in 50: 1 by volume mutually, and the adding deionized water is mixed with the premixed liquid that concentration is 30wt%; The adding particle mean size is that molybdenum powder and the mass ratio thereof of 4 μ m is the ammonium citrate of 1.5wt%, and adds ammoniacal liquor adjusting pH value to 9.5, prepares powder volume than even, the stable slurry that is 52% through mechanical ball milling; The ammonium persulfate (APS) and the N that add 2wt% subsequently, N, N, N-tetramethylethylenediamine (TEMED), the n-octyl alcohol defoamer of 0.2wt%, and mix fast in a vacuum, with degasification, the metal die die cavity of the complicated shape that slow then injection has designed and made, and, obtain solidifying base at 80 ℃ of temperature-curable 20min; To solidify base and place vacuum sintering furnace, and be warming up to 110 ℃ of temperature at a slow speed with 4 ℃/min earlier, 90min is with drying in insulation, speed with 10 ℃/min is warming up to 550 ℃ subsequently, and insulation 30min is with binder removal, be rapidly heated then to 1450 ℃, and insulation 120min, the molybdenum skeleton obtained; The anaerobic copper sheet is placed molybdenum skeleton top, last in the 10-2Pa vacuum atmosphere, handles in 1300 ℃ of infiltration copper that carry out 90min, obtain Tissue distribution evenly, density is 99.86% 90Mo-Cu alloy parts.
Embodiment 4:
Methacrylamide (MAM) and diallyl tartaric acid diamides (DATDA) were mixed in 80: 1 by volume mutually, and the adding deionized water is mixed with the premixed liquid that concentration is 10wt%; The adding particle mean size is that molybdenum powder and the mass ratio thereof of 8 μ m is the ammonium citrate of 0.2wt%, and adds ammoniacal liquor adjusting pH value to 9.5, prepares powder volume than even, the stable slurry that is 42% through mechanical ball milling; The ammonium persulfate (AP S) and the N that add 4wt% subsequently, N, N, N-tetramethylethylenediamine (TEMED), the n-octyl alcohol defoamer of 0.2wt%, and mix fast in a vacuum, with degasification, the mould of plastics die cavity of the complicated shape that slow then injection has designed and made, and, obtain solidifying base at 50 ℃ of temperature-curable 30min; To solidify base and place hydrogen sintering furnace, and be warming up to 100 ℃ of temperature at a slow speed with 3 ℃/min earlier, 120min is with drying in insulation, speed with 8 ℃/min is warming up to 500 ℃ subsequently, and insulation 30min is with binder removal, be rapidly heated then to 1400 ℃, and insulation 100min, the molybdenum skeleton obtained; The anaerobic copper sheet is placed molybdenum skeleton top, last in argon gas atmosphere, handles in 1150 ℃ of infiltration copper that carry out 120min, obtain Tissue distribution evenly, density is 99.98% 85Mo-Cu alloy parts.
Embodiment 5:
Acrylamide (AM) and N, N ,-methylene-bisacrylamide (MBAM) mixed in 30: 1 by volume mutually, and the adding deionized water is mixed with the premixed liquid that concentration is 35wt%; The adding particle mean size is that molybdenum powder and the mass ratio thereof of 2 μ m is the ammonium citrate of 2.0wt%, and adds ammoniacal liquor adjusting pH value to 8, prepares powder volume than even, the stable slurry that is 50% through mechanical ball milling; The ammonium persulfate (APS) and the N that add 3wt% subsequently, N, N, N-tetramethylethylenediamine (TEMED), the n-octyl alcohol defoamer of 0.3wt%, and mix fast in a vacuum, with degasification, the metal die die cavity of the complicated shape that slow then injection has designed and made, and, obtain solidifying base at 80 ℃ of temperature-curable 2min; To solidify base and place vacuum sintering furnace, and be warming up to 110 ℃ of temperature at a slow speed with 5 ℃/min earlier, 60min is with drying in insulation, speed with 10 ℃/min is warming up to 400 ℃ subsequently, and insulation 45min is with binder removal, be rapidly heated then to 1300 ℃, and insulation 150min, the molybdenum skeleton obtained; The anaerobic copper sheet is placed molybdenum skeleton top, at last 10
-2Handle in 1325 ℃ of infiltration copper that carry out 60min in the Pa vacuum atmosphere, obtain Tissue distribution evenly, density is 100% 80Mo-Cu alloy parts.
Embodiment 6:
Methacrylamide (MAM) and diallyl tartaric acid diamides (DATDA) were mixed in 100: 1 by volume mutually, and the adding deionized water is mixed with the premixed liquid that concentration is 30wt%; The adding particle mean size is that molybdenum powder and the mass ratio thereof of 10 μ m is the ammonium citrate of 3.0wt%, and adds ammoniacal liquor adjusting pH value to 10, prepares powder volume than even, the stable slurry that is 55% through mechanical ball milling; The ammonium persulfate (APS) and the N that add 0.1wt% subsequently, N, N, N-tetramethylethylenediamine (TEMED), the n-octyl alcohol of 0.1wt%, and mix fast in a vacuum, with degasification, the glass mold die cavity of the complicated shape that slow then injection has designed and made, and, obtain solidifying base at 70 ℃ of temperature-curable 10min; To solidify base and place hydrogen sintering furnace, and be warming up to 90 ℃ of temperature at a slow speed with 6 ℃/min earlier, 180min is with drying in insulation, speed with 15 ℃/min is warming up to 550 ℃ subsequently, and insulation 15min is with binder removal, be rapidly heated then to 1450 ℃, and insulation 60min, the molybdenum skeleton obtained; The anaerobic copper sheet is placed molybdenum skeleton top, last in argon gas atmosphere, handles in 1200 ℃ of infiltration copper that carry out 100min, obtain Tissue distribution evenly, density is 99.8% 90Mo-Cu alloy parts.
Claims (3)
1. method for preparing the complicated shape molybdenum-copper component, it is characterized in that: its preparation technology is:
(1), premixed liquid preparation:
Organic monomer is pressed (20～100) by volume with crosslinking agent: 1 mixes mutually, and the adding deionized water is mixed with the premixed liquid that concentration is 10～35wt%;
(2), high-volume fractional pulp preparation:
In premixed liquid, add purity 〉=99%, granularity is the molybdenum powder of 2～10 μ m and the ammonium citrate dispersant that mass ratio is 0.2～3wt% thereof, and add ammoniacal liquor and regulate pH value to 8～10, preparing the molybdenum powder volume ratio through mechanical ball milling is 42～55% even, stable slurry;
(3), casting and curing:
The ammonium persulfate initiator and the N that in slurry, add 0.1～4wt%, N, N, N-tetramethylethylenediamine catalyst, 0.1 the n-octyl alcohol defoamer of～0.3wt%, and stir fast in a vacuum and degasification, the mould of complicated shape slowly injected then, and under 50～80 ℃ of temperature, solidify 2～30min, obtain solidifying base;
(4), molybdenum skeleton preparation:
Described curing base is warming up to dry 60～180min under 90～110 ℃ of temperature in the speed with 3～6 ℃/min under vacuum or the hydrogen atmosphere earlier, speed with 8～15 ℃/min is warming up to 400～550 ℃ subsequently, and be incubated 15～45min, be rapidly heated then to 1200～1450 ℃, insulation 60～150min obtains the molybdenum skeleton;
(5), the infiltration of copper:
The anaerobic copper sheet is placed described molybdenum skeleton bottom or top, and in vacuum, hydrogen or argon gas atmosphere, 1150～1325 ℃ of temperature infiltration copper 60～120min obtain molybdenum-copper component.
2. the method for preparing the complicated shape molybdenum-copper component according to claim 1, it is characterized in that: described organic monomer is acrylamide or Methacrylamide, described crosslinking agent is N, N ,-methylene-bisacrylamide or diallyl tartaric acid diamides.
3. the method for preparing the complicated shape molybdenum-copper component according to claim 1 and 2 is characterized in that: described mould is rubber, plastics, metal or glass mold.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451222A (en) * | 2014-12-30 | 2015-03-25 | 中南大学 | Preparation method of nano W-Cu composite block material |
| CN109202086A (en) * | 2018-09-06 | 2019-01-15 | 河源职业技术学院 | A kind of preparation method of nut |
| CN113102756A (en) * | 2021-04-12 | 2021-07-13 | 哈尔滨理工大学 | Method for improving quality of molybdenum-copper alloy |
| CN116618647A (en) * | 2023-07-21 | 2023-08-22 | 安徽诺星航空科技有限公司 | Molybdenum-copper alloy composite material and preparation process thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698909A (en) * | 2009-10-30 | 2010-04-28 | 北京工业大学 | Method for preparing molybdenum-copper alloy |
| CN101774020A (en) * | 2010-01-20 | 2010-07-14 | 中南大学 | Method for preparing molybdenum-copper component |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698909A (en) * | 2009-10-30 | 2010-04-28 | 北京工业大学 | Method for preparing molybdenum-copper alloy |
| CN101774020A (en) * | 2010-01-20 | 2010-07-14 | 中南大学 | Method for preparing molybdenum-copper component |
Non-Patent Citations (1)
| Title |
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| 《中北大学学报> 20091231 刘斌等 钼铜复合材料快速成型制备工艺研究 全文 1-3 第30卷, 第1期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104451222A (en) * | 2014-12-30 | 2015-03-25 | 中南大学 | Preparation method of nano W-Cu composite block material |
| CN109202086A (en) * | 2018-09-06 | 2019-01-15 | 河源职业技术学院 | A kind of preparation method of nut |
| CN113102756A (en) * | 2021-04-12 | 2021-07-13 | 哈尔滨理工大学 | Method for improving quality of molybdenum-copper alloy |
| CN116618647A (en) * | 2023-07-21 | 2023-08-22 | 安徽诺星航空科技有限公司 | Molybdenum-copper alloy composite material and preparation process thereof |
| CN116618647B (en) * | 2023-07-21 | 2023-10-13 | 安徽诺星航空科技有限公司 | Molybdenum-copper alloy composite material and preparation process thereof |
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Application publication date: 20110223 Assignee: Jiangsu Star Limited company of tungsten and molybdenum Assignor: Central South University Contract record no.: 2013320000434 Denomination of invention: Method for preparing molybdenum copper part with complex shape Granted publication date: 20111214 License type: Exclusive License Record date: 20130520 |
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