Background technology
A kind of pseudo-alloy material that molybdenum-copper is made up of molybdenum and copper, because it has low-expansion coefficient and the good characteristic such as conduction and thermal conductivity simultaneously, be widely used in industries such as electric elements, semiconductor packages, electronics, paid attention in high-power LED illumination chip industry again in recent years, there is very large potential market.But, the molybdenum-copper paillon foil part using in semiconductor packages industry, electronics and high-power LED illumination industry, owing to requiring density large, General Requirements is greater than 99.5% of solid density; Thin thickness, is generally 80-200 micron, and thickness deviation requires in 5 micrometer ranges, and Part Surface Roughness requires below Ra0.08.But, adopt current existing process to be difficult to realize these technical requirements.
The major technique of existing molybdenum-copper foil material processing has following two kinds of methods:
(1) to the sintered blank that adopts powder metallurgy process to make, directly cut, then adopt the method for one side mill or two-sided mill to make the molybdenum-copper paillon foil part of desired thickness and surface roughness.
This technology exists stock utilization low, and the output ratio that feeds intake is generally not more than 50%, and adopts the molybdenum copper foil part of this technology production still to have internal void, and part actual density is generally between 92-95%, far below various problems such as solid densities.
(2) in the recrystallization temperature higher than copper, utilize the mechanical means such as forging and stamping, rolling, compacting to exert pressure to molybdenum-copper blank, make it produce plastic deformation, obtain initial blank; Then by cold rolling method, sintering molybdenum-copper is carried out to cold rolling processing, carry out intermediate annealing when compress variation is 30~40%, annealing so repeatedly-cold rolling, is directly processed to desired thickness.
This technology exists the production cycle long, produces the cycle of paillon foil part at least more than 5 days; Energy consumption is high, and the operations such as forge hot, hot rolling, hot pressing, annealing must adopt powerful high-temperature heater; Because processing passage is many, cause finished product rate low, general input-output ratio is not more than 15%; Hold facility kind is more, and mostly is high-power and large-tonnage process equipment, and equipment investment is larger; Product thickness tolerance is difficult to reach 5 microns; Product surface roughness is generally difficult to reach the various problems such as Ra0.08.
The patent No. is the United States Patent (USP) of US5686676, employing sintering in reducibility gas improves the effect of sintering, thereby and the blank that contains oxygen molecule by use discharges oxygen with accelerated reaction in sintering process, and add corrosion inhibitor to reduce the hypergolic reaction of material in blank.Although these means can play certain effect that improves production efficiency,, still there are the problems referred to above of prior art in the framework that it does not depart from prior art in essence.
Application number is the cold rolling process that 201010177490.4 Chinese patent discloses a kind of molybdenum-copper alloy thin plate, the feature of the method is that the whole operation of rolling at room temperature completes, but need to pass through the cold rolling of a few to tens of passages, and pressure rolling speed is lower, between 0.1-1m/s, therefore production efficiency is lower, and the production cycle is longer.In addition, the milled sheet thickness deviation control difficulty that the method obtains is larger, and while reaching 5 microns of tolerances, production efficiency can be lower.
Summary of the invention
The object of this invention is to provide a kind of zerolling method of preparing molybdenum-copper, the method has solved the problem that equipment investment is large, machining accuracy is poor, working (machining) efficiency is low, stock utilization is low existing in existing molybdenum-copper foil production process, improve the machining accuracy of molybdenum-copper foil, and production efficiency, and by adopting the mode of preheating insulation, further reduce rolling pass, improved production efficiency.
In order to reach foregoing invention object, a kind of zerolling method of preparing molybdenum-copper provided by the present invention is achieved through the following technical solutions:
A method of preparing molybdenum-copper foil, comprises the following steps:
(1) adopt conventional method to prepare molybdenum-copper sintering blank;
(2) molybdenum-copper blank is preheated to 40-300 DEG C, and insulation 5-30min is stand-by;
(3) roll of plate mill is preheated to 40-80 DEG C;
(4) preheated molybdenum-copper blank is rolled on milling train, makes molybdenum-copper foil.
Preferably, in described step (1), the percentage by weight of molybdenum-copper sintering blank is copper 5-50%, molybdenum 50-95%.
Preferably, in described step (1), the thickness of molybdenum-copper sintering blank is 0.25-2.5mm.
Preferably, in described step (2), optimum Preheating Temperature raises with the increase of molybdenum content in molybdenum-copper blank, and best temperature retention time extends with the increase of the thickness of molybdenum-copper blank.
Preferably, described method also comprises step (5): after the passage processing capacity of rolling first reaches, rapidly molybdenum-copper blank is again incubated at the temperature of 40-300 DEG C to 5-30min, and then rolling, so, through the rolling of 2-8 passage, can make thickness is the molybdenum-copper foil of 0.05-0.5mm.
Preferably, the percentage by weight of molybdenum-copper sintering blank is copper 15-25%, molybdenum 75-85%, and preheat temperature is 40-100 DEG C.
Preferably, the passage processing capacity of described mill milling is less than or equal to 50%, and mill speed is less than or equal to 15m/s.
Preferably, described milling train is two rollers, four rollers, 12 rollers or mill.
The present invention adopts the cold-rolling process of infusibility molybdenum molybdenum processing, compared with traditional hot rolling cogging, annealing, cold rolling production technology, has that production efficiency is high, Product Precision good, stock utilization high.Adopt the present invention, only need a conventional baking oven, a platen mill, equipment investment is few; General only through the rolling of no more than 8 passages, every time rolling time is generally no more than 30min, and production efficiency improves greatly; Can process the foil part being as thin as within the scope of 0.05-0.5mm; Can directly make thickness deviation, surface roughness meets the requirements of molybdenum-copper part; And stock utilization improves greatly, the output ratio that feeds intake generally can be lower than 70%.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail.
As shown in Figure 1, a kind of method of preparing molybdenum-copper foil, comprises the following steps:
(1) adopt conventional method to prepare molybdenum-copper sintering blank;
Raw material adopts commercially available molybdenum-copper sintering blank, or the molybdenum-copper sintering blank that adopts other powder metallurgy process to be prepared from as mold pressing, rolling, isostatic pressing moulding etc.;
Preferably, the percentage by weight of molybdenum-copper sintering blank is copper 5-50%, molybdenum 50-95%, and thickness is 0.2
(2) molybdenum-copper blank is preheated to 40-300 DEG C, and insulation 5-30min is stand-by;
The selection that it is pointed out that preheating optimum temperature raises with the increase of molybdenum content in molybdenum-copper blank, and the length of best temperature retention time extends with the increase of the thickness of molybdenum-copper blank.
Preferably, the percentage by weight of molybdenum-copper sintering blank is copper 15-25%, molybdenum 75-85%, be preheated to 40-100 DEG C, and it is stand-by to be incubated 5-30min.
(3) roll of milling train is preheated to 40-80 DEG C;
(4) preheated molybdenum-copper blank is rolled on milling train, can make thickness is the molybdenum-copper foil of 0.05-0.5mm.
Can use two rollers, four rollers, 12 rollers, mill to be directly rolled preheated molybdenum-copper blank, wherein, passage processing capacity is less than or equal to 50%, and mill speed is less than or equal to 15m/s.
According to actual needs, often need rolling repeatedly just can obtain the molybdenum-copper foil of ideal thickness.Therefore described method, further comprise step (5): after the passage processing capacity of rolling first reaches, rapidly molybdenum-copper blank is again incubated at the temperature of 40-300 DEG C to 5-30min, and then rolling, so general through 2-5 passage rolling (maximum is not more than 8 times), make the molybdenum-copper foil of ideal thickness.
Rolling is the same with rolling first again, can use two rollers, four rollers, 12 rollers, mill to be rolled, and passage processing capacity is less than or equal to 50%, and mill speed is less than or equal to 15m/s.
Be specific embodiment below:
Embodiment 1
Adopt powder rolling process to make the molybdenum-copper sintering blank that percentage by weight is copper 20%, molybdenum 80%, its thickness is 0.5mm; The roll of 20 roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 40-100 DEG C in baking oven, 5-8min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on 20 roller plate mills through preheating, passage processing capacity is less than or equal to 45%, and mill speed is 8m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 5-8min at the temperature of 40-100 DEG C rapidly, and then rolling; So, through 3 passage rollings, can make thickness is the molybdenum-copper foil of 0.25mm.Through measuring, the density reachable to 99.95% of this molybdenum-copper foil, thickness deviation is 3 microns, and surface roughness is Ra0.05, and input-output ratio reaches 89%.
Embodiment 2
Adopt stamping of powder technique to make the molybdenum-copper sintering blank that percentage by weight is copper 25%, molybdenum 75%, its thickness is 1.5mm; The roll of two roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 40-90 DEG C in baking oven, 10-15min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on two roller plate mills through preheating, passage processing capacity is less than or equal to 45%, and mill speed is 15m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 10-15min at the temperature of 40-90 DEG C rapidly, and then rolling; So, through 5 passage rollings, can make thickness is the molybdenum-copper foil of 0.05mm.Through measuring, the density reachable to 99.95% of this molybdenum-copper foil, thickness deviation is 3 microns, and surface roughness is Ra0.05, and input-output ratio reaches 85%.
Embodiment 3
Adopt powder rolling process to make the molybdenum-copper sintering blank that percentage by weight is copper 20%, molybdenum 80%, its thickness is 0.5mm; The roll of 20 roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 40-100 DEG C in baking oven, 5-8min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on 20 roller plate mills through preheating, passage processing capacity is less than or equal to 55%, and mill speed is 8m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 5-8min at the temperature of 150-260 DEG C rapidly, and then rolling; So, through 2 passage rollings, can make thickness is the molybdenum-copper foil of 0.05mm.Through measuring, the density reachable to 99.5% of this molybdenum-copper foil, thickness deviation is 3 microns, and surface roughness is Ra0.05, and input-output ratio reaches 85%.
Embodiment 4
Adopt stamping of powder technique to make the molybdenum-copper sintering blank that percentage by weight is copper 15%, molybdenum 85%, its thickness is 2.5mm; The roll of four roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 40-100 DEG C in baking oven, 15-20min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on four roller plate mills through preheating, passage processing capacity is less than or equal to 35%, and mill speed is 10m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 15-20min at the temperature of 50-120 DEG C rapidly, and then rolling; So, through 5 passage rollings, can make thickness is the molybdenum-copper foil of 0.5mm.Through measuring, the density reachable to 99.95% of this molybdenum-copper foil, thickness deviation is 4 microns, and surface roughness is Ra0.05, and input-output ratio reaches 85%.
Embodiment 5
Adopt powder isostatic pressing process to make the molybdenum-copper sintering blank that percentage by weight is copper 10%, molybdenum 90%, its thickness is 2.0mm; The roll of four roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 60-150 DEG C in baking oven, 20-30min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on four roller plate mills through preheating, passage processing capacity is less than or equal to 25%, and mill speed is 6m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 20-30min at the temperature of 60-150 DEG C rapidly, and then rolling; So, through 5 passage rollings, can make thickness is the molybdenum-copper foil of 0.5mm.Through measuring, the density reachable to 99.95% of this molybdenum-copper foil, thickness deviation is 4 microns, and surface roughness is Ra0.05, and input-output ratio reaches 86%.
Embodiment 6
Adopt powder rolling process to make the molybdenum-copper sintering blank that percentage by weight is copper 15%, molybdenum 85%, its thickness is 1.0mm; The roll of four roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 150-250 DEG C in baking oven, 10-15min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on four roller plate mills through preheating, passage processing capacity is less than or equal to 35%, and mill speed is 8m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 10-15min at the temperature of 150-250 DEG C rapidly, and then rolling; So, through 4 passage rollings, can make thickness is the molybdenum-copper foil of 0.08mm.Through measuring, the density reachable to 99.95% of this molybdenum-copper foil, thickness deviation is 4 microns, and surface roughness is Ra0.05, and input-output ratio reaches 82%.
Embodiment 7
Adopt stamping of powder technique to make the molybdenum-copper sintering blank that percentage by weight is copper 15%, molybdenum 85%, its thickness is 2.5mm; The roll of four roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 200-300 DEG C in baking oven, 10-20min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on four roller plate mills through preheating, passage processing capacity is less than or equal to 35%, and mill speed is 10m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 15-20min at the temperature of 200-300 DEG C rapidly, and then rolling; So, through 5 passage rollings, can make thickness is the molybdenum-copper foil of 0.5mm.Through measuring, the density reachable to 99.5% of this molybdenum-copper foil, thickness deviation is 4 microns, and surface roughness is Ra0.05, and input-output ratio reaches 88%.
Embodiment 8
Adopt powder rolling process to make the molybdenum-copper sintering blank that percentage by weight is copper 20%, molybdenum 80%, its thickness is 0.5mm; The roll of 20 roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 150-260 DEG C in baking oven, 5-8min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on 20 roller plate mills through preheating, passage processing capacity is less than or equal to 55%, and mill speed is 8m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 5-8min at the temperature of 150-260 DEG C rapidly, and then rolling; So, through 2 passage rollings, can make thickness is the molybdenum-copper foil of 0.05mm.Through measuring, the density reachable to 99.5% of this molybdenum-copper foil, thickness deviation is 3 microns, and surface roughness is Ra0.05, and input-output ratio reaches 82%.
Embodiment 9
Adopt powder isostatic pressing process to make the molybdenum-copper sintering blank that percentage by weight is copper 10%, molybdenum 90%, its thickness is 2.0mm; The roll of four roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 200-300 DEG C in baking oven, 20-30min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on four roller plate mills through preheating, passage processing capacity is less than or equal to 45%, and mill speed is 6m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 20-30min at the temperature of 200-300 DEG C rapidly, and then rolling; So, through 3 passage rollings, can make thickness is the molybdenum-copper foil of 0.5mm.Through measuring, the density reachable to 99.5% of this molybdenum-copper foil, thickness deviation is 4 microns, and surface roughness is Ra0.05, and input-output ratio reaches 82%.
Embodiment 10
Adopt stamping of powder technique to make the molybdenum-copper sintering blank that percentage by weight is copper 30%, molybdenum 70%, its thickness is 1.5mm; The roll of four roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 150-250 DEG C in baking oven, 10-15min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on four roller plate mills through preheating, passage processing capacity is less than or equal to 55%, and mill speed is 15m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 10-15min at the temperature of 150-250 DEG C rapidly, and then rolling; So, through 3 passage rollings, can make thickness is the molybdenum-copper foil of 0.15mm.Through measuring, the density reachable to 99.5% of this molybdenum-copper foil, thickness deviation is 4 microns, and surface roughness is Ra0.05, and input-output ratio reaches 83%.
Embodiment 11
Adopt powder rolling process to make the molybdenum-copper sintering blank that percentage by weight is copper 15%, molybdenum 85%, its thickness is 1.0mm; The roll of four roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 100-200 DEG C in baking oven, 10-15min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on four roller plate mills through preheating, passage processing capacity is less than or equal to 45%, and mill speed is 8m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 10-15min at the temperature of 100-200 DEG C rapidly, and then rolling; So, through 3 passage rollings, can make thickness is the molybdenum-copper foil of 0.08mm.Through measuring, the density reachable to 99.5% of this molybdenum-copper foil, thickness deviation is 4 microns, and surface roughness is Ra0.05, and input-output ratio reaches 85%.
Embodiment 12
Adopt powder rolling process to make the molybdenum-copper sintering blank that percentage by weight is copper 15%, molybdenum 85%, its thickness is 0.25mm; The roll of four roller plate mills is preheated to 40-80 DEG C; This molybdenum-copper blank is preheated to 100-150 DEG C in baking oven, 10-15min when insulation; Then rapidly by the molybdenum-copper blank Direct Rolling on four roller plate mills through preheating, passage processing capacity is less than or equal to 35%, and mill speed is 2m/s; After passage processing capacity reaches, then molybdenum-copper blank is put into baking oven is again incubated 10-15min at the temperature of 100-150 DEG C rapidly, and then rolling; So, through 3 passage rollings, can make thickness is the molybdenum-copper foil of 0.08mm.Through measuring, the density reachable to 99.5% of this molybdenum-copper foil, thickness deviation is 4 microns, and surface roughness is Ra0.05, and input-output ratio reaches 82%.
The present invention is used in the production process of the molybdenum-copper foil product of the multi-field application such as electronics, communication, semiconductor, illumination, safety, medical treatment, military project, space flight, aviation, ocean.
One of ordinary skill in the art of the present invention are appreciated that; the above embodiment of the present invention is only one of the preferred embodiments of the present invention; for length restriction; here can not all embodiments of particularize; any enforcement that can embody the claims in the present invention technical scheme, all in protection scope of the present invention.
It should be noted that; above content is in conjunction with concrete embodiment further description made for the present invention; can not assert that the specific embodiment of the present invention only limits to this; under above-mentioned guidance of the present invention; those skilled in the art can carry out various improvement and distortion on the basis of above-described embodiment, and these improvement or distortion drop in protection scope of the present invention.