CN104057088B - A kind of preparation method of ultra-large type carefully brilliant molybdenum flat target - Google Patents
A kind of preparation method of ultra-large type carefully brilliant molybdenum flat target Download PDFInfo
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Abstract
A kind of preparation method of ultra-large type carefully brilliant molybdenum flat target, the molybdenum powder adopting purity > 99.95% prepares, wherein, the length > 450 of molybdenum flat target, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75, preparation method is: takes molybdenum powder and loads in glued membrane, hydrostatic profile, it is placed on intermediate frequency furnace, after sintering slab under hydrogen atmosphere, insert in mould, forge slab mould, after insert tempering furnace, annealing, forms fine grained texture, retrofit, cleaning, dried prepared molybdenum flat target.Instant invention overcomes sintering and the defective workmanship forged, technique is simple, easy industrial production control, reduces and pollutes, and cost is low, Quality advance, and production efficiency greatly improves.
Description
Technical field
The present invention relates to a kind of sputtering target material for photovoltaic element substrate film coating, specifically the preparation method of a kind of ultra-large type made with pure molybdenum powder carefully brilliant molybdenum flat target.
Background technology
At present; flat target is mainly used in the plated film of photovoltaic element substrate; the physical property of this series products itself directly affects the serviceability of plated film; such as: one, in the process of plated film; gas owing to existing in target internal void discharges suddenly; large-sized target granule or microgranule is caused to splash; or the caudacoria material of film forming is subject to the microgranule splashing that secondary electron bombardment causes; the appearance of these microgranules all can reduce film quality; in order to reduce the pore in target solid; improve film performance, generally require that target has higher consistency；Two, due to target atom easily along atom six side most close-packed arrays direction preferential sputtering out, therefore, for reaching the highest sputter rate, sputter rate is increased usually through the method changing target crystalline texture, the thickness evenness of sputtered layer is affected also bigger by the crystallization direction of target, therefore, it is thus achieved that the target material structure of certain crystalline orientation is most important to the sputter procedure of thin film.
At present, the main preparation method of external tungsten flat target is to adopt extrusion forming process to be processed molding, finally thermally treated, machining and backboard combine and are formed, and such method is high to equipment requirements, complex process, relatively costly, and the target compactness difference prepared and grain size is also relatively big, use this product when plated film, uniformity and the cloth line mass of thin film are substantially reduced；
Secondly, current method is only capable of prepares the flat target that area is less, and by the constraint of its preparation method, large-scale flat target molding effect is poor, and percent defective is higher, and the product serviceability prepared is poor；
For change and overcome these defects, it is achieved the highest sputter rate, general way be change target crystalline texture to increase sputter rate, have in order to reduce the pore in target solid, improve film performance, adopt improve target thickness to improve coating quality.
Abroad, for improving flat target at the quality of photovoltaic element substrate film coating and effect, the moulding processs adopting extruding or drawing more.For overcoming the defect of extruding or drawing process, the applicant increases employing oversintering, forges the technique of molding, the steps include: that high temperature sintering-cooling forges-lonneal-polish after processing-heating up.Such as the technical scheme of 201110242640X, when to tungsten material molding, need to adopt cooling water circulation to process after high temperature burns till.And for example 2012100007317 and two technical schemes of 201210000729X in, all have employed when Mo is processed need after high temperature burns till adopt cooling water circulation process technique.Although the processing method of this kind of technique is helpful to the compactness increasing material, but all can not form fine grained texture.
It addition, prior art there is also a significant deficiency, both in forging process, all adopt the surface directly forging pipe, and the deflection of material is uncontrollable in forging, its forging method has had a strong impact on formation and the quality of fine grained texture.
Further, in prior art, the temperature of tempering all adopts lonneal, temperature is all at 450-500 DEG C, owing to temperature is relatively low, and the heavy damage formation of product fine grained texture, have impact on product quality.
Due to the complex process of prior art, causing that quality is on the low side, cost improves, the compactness of flat target is very poor, grain size is bigger, causing when plated film, uniformity and the cloth line mass of thin film are substantially reduced, it is impossible to meet the requirement of the specific impedance to material of the photovoltaic product and membrane stress.
Summary of the invention
The purpose of the present invention aims to solve the problem that the deficiency of above-mentioned technical problem, and flat target adopts Mo to substitute tungsten material and makes, and after changing technique, so that molybdenum powder at sintering and forges formation fine grained texture in technique, improves flat target quality, reduces production cost.Flat target length > 450, width G reatT.GreaT.GT 320, the thickness G reatT.GreaT.GT 75 made, adopts this product to be greatly improved the efficiency of photovoltaic element substrate film coating, it is ensured that the service life of product.
The technical solution adopted in the present invention is: the preparation method of a kind of ultra-large type carefully brilliant molybdenum flat target, the molybdenum powder adopting purity > 99.95% prepares, wherein, the length > 450 of molybdenum flat target, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75
Step one, take the molybdenum powder of granularity 2.8-3.8 μm, load in the rubber die sleeve made in advance, adopt 160-200MPa hydrostatic profile, be placed on intermediate frequency furnace, under the atmosphere of hydrogen, keeps temperature 1900-2000 DEG C of sintering 55-65 hour, after burning till slab, standby；
Step 2, the slab burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, control temperature 1350-1400 DEG C of slab, forge slab mould, the deflection < 50% of panel base when forging, forge into the tabular component of length > 450, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75；
Step 3, lay down mould, take out the tabular component forging molding, insert in the tempering furnace of 1000-1200 DEG C, keep 1-3 hour, stablize fine grained texture；
Step 4, tabular component being carried out machining, by cleaning, dry, prepared ultra-large type is brilliant molybdenum flat target carefully.
Described sintering, can sinter under vacuo, and during vacuum-sintering, temperature progressively heats up from zero degree to 2000 DEG C.
In described step one in sintering process, temperature 2000 DEG C in intermediate frequency furnace, is kept to sinter 60 hours.
In described step 2, the temperature of the front control plate base forged 1350 DEG C.
In described step 3, take out in the tempering furnace that the tabular component forging molding inserts 1200 DEG C, keep 2 hours, stablize fine grained texture.
The present invention, adopts Mo to make, and owing to the character of molybdenum Yu tungsten is very close, its floating-point and electric conductivity highlight, and coefficient of linear thermal expansion is little, and relatively tungsten is easily worked., in the best collocation, its fusing point: 2620 DEG C, intensity and density are more than tungsten, and molybdenum still has high intensity at 1200 DEG C, and molybdenum has the ability doubling tungsten for the thermal conductivity of molybdenum [135 watts/(rice is opened)] and specific heat [0.276 kilojoule (kilogram open)].
Molybdenum, under the temperature and pressure that vacuum drying oven works, has extremely low vapour pressure, and therefore, molybdenum is to working in stove or the pollution of operation material is minimum, and evaporation loss will not restrict the service life of the molybdenum matter hot parts such as heating element heater and heat insulation encapsulating.
The present invention; molybdenum flat target is in the process of sputter coating; owing to flat target is fine grained texture; compactness is good; when sputtering target is bombarded, overcome and generally adopt tungsten target to discharge suddenly due to the gas existed in target internal void, cause large-sized target granule or microgranule to splash; or the caudacoria material of film forming is subject to the microgranule splashing that secondary electron bombardment causes, cause the phenomenon reducing film quality.
Tests prove that, during sputtering, target atom is easily along atom six side most close-packed arrays direction preferential sputtering out.For reaching the highest sputter rate, people generally adopt raising sputter rate method to realize effect.One of means that the present invention takes are that coarse structure is changed into aplitic texture, to increase sputter rate (thickness evenness of sputtered layer is affected also bigger by the crystallization direction of target).For this, it is thus achieved that the target material structure of certain crystalline orientation is most important to the sputter procedure of thin film.It addition, flat target length > 450, width G reatT.GreaT.GT 320, the thickness G reatT.GreaT.GT 75 made, this product is adopted to be greatly improved the efficiency of photovoltaic element substrate film coating, it is ensured that the service life of product.
The present invention, not only meet the requirement of the specific impedance to material of the photovoltaic product and membrane stress, add, in forging, the grain formation fine grained texture making molybdenum man-hour simultaneously, the uniformity of film and the cloth line mass that make LED industry glass substrate are obviously improved, and extend the service life of LCD element.
The present invention, when the base of molding sinters, eliminates cooling process (particularly cooling water circulation operation).It has been investigated that, temperature-fall period can destroy the formation of the fine grained texture of material.Adopt after high temperature sintering and directly forge, the formation of fine grained texture can be kept, the effect that this technique produces be prior it is not expected that.
The present invention, changes and forges technique, and conventional forges the surface all directly forging workpiece, and it has the drawback that: forge uneven, it is impossible to controlling deflection, poor product quality, qualification rate is low, is also highly vulnerable to breakage the crystallization of flat target.The present invention adopts and inserts in mould by slab, directly forges mould, effectively controls the deflection (control of deflection of the present invention is for less than 50%) of slab, neither destroys fine grained texture, and properties of product are greatly improved, and qualification rate can realize 100%.
The present invention, changes tempering process, and conventional tempering all adopts low temperature (450-500 DEG C) tempering, it have been investigated that, lonneal is very big to fine grained texture's destructiveness of molybdenum, it is impossible to ensure product quality.Temperature of the present invention adopts 1000-1200 DEG C, substantially increases formation and the stability of fine grained texture, greatly improves quality and the life-span of product, and it is unexpected in advance that this technique is told on.
The molybdenum flat target of the present invention, has higher intensity and density than tungsten target, uses this product when LED plated film, and uniformity and the cloth line mass of thin film can improve more than twice.
Beneficial effects of the present invention:
First, instant invention overcomes the defect (in existing technology many employing metal alloy molybdenums or metal synthesis Mo) that pure Mo cannot be adopted to prepare flat target, great change has been made on material selects, flat target adopts Mo to substitute tungsten material and makes, the change of combined process, make to be formed the molybdenum flat target of a kind of fine grained texture, improve flat target quality.
They are two years old, instant invention overcomes and can only produce the area defect compared with facet target in the past, by length > 450, the width G reatT.GreaT.GT 320 of flat target, thickness G reatT.GreaT.GT 75, adopts this product to be greatly improved the efficiency of photovoltaic element substrate film coating.
Its three, instant invention overcomes the defect of sintering difficulty, after changing conventional sintering, need to adopt a difficult problem for cooling water circulation.The present invention eliminates temperature reduction technology in high-sintering process, directly forges after adopting high temperature sintering, and this process advan, in the compactness increasing material, forms fine grained texture.
They are four years old, instant invention overcomes and forge that technique compactness is poor, forge uneven defect, the surface directly forging slab in process will be forged in the past, change into and slab is loaded the technique forging mould in mould, effectively control the deflection < 50% forged, effectively accelerate formation and the Quality advance of fine grained texture.
They are five years old, instant invention overcomes the defect of the STRESS VARIATION that tempering after forging molding is uneven and lonneal causes, change conventional lonneal (450-500 DEG C) into high tempering (1000-1300 DEG C), greatly ensure that material performance under tempered condition, effective stabilizing material still has high intensity and density at 1200 DEG C, after fine grained texture is formed, guarantee that molybdenum has extremely low vapour pressure under the temperature and pressure that vacuum drying oven works, make it to working in stove or the pollution of operation material is minimum, and evaporation loss will not restrict the service life of the molybdenum matter hot parts such as heating element heater and heat insulation encapsulating.
Its six, present invention process is simple, and easy industrial production control reduces pollution.
Its seven, present invention reduces production cost, improve quality, production efficiency greatly improves.
Detailed description of the invention
The preparation method of a kind of ultra-large type carefully brilliant molybdenum flat target, adopts the molybdenum powder of purity > 99.95% to prepare, wherein, the length > 450 of molybdenum flat target, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75
Step one, take the molybdenum powder of granularity 2.8-3.8 μm, load in the rubber die sleeve made in advance, adopt 160-200MPa hydrostatic profile, be placed on intermediate frequency furnace, under the atmosphere of hydrogen, keeps temperature 1900-2000 DEG C of sintering 55-65 hour, after burning till slab, standby；
Step 2, the slab burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, control temperature 1350-1400 DEG C of slab, forge slab mould, the deflection < 50% of panel base when forging, forge into the tabular component of length > 450, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75；
Step 3, lay down mould, take out the tabular component forging molding, insert in the tempering furnace of 1000-1200 DEG C, keep 1-3 hour, stablize fine grained texture；
Step 4, tabular component being carried out machining, by cleaning, dry, prepared ultra-large type is brilliant molybdenum flat target carefully.
Described sintering, can sinter under vacuo, and during vacuum-sintering, temperature progressively heats up from zero degree to 2000 DEG C.
Embodiment one
The preparation method of a kind of ultra-large type carefully brilliant molybdenum flat target, adopts the molybdenum powder of purity > 99.95% to prepare, wherein, the length > 450 of molybdenum flat target, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75
Step one, take the molybdenum powder of granularity 2.8 μm, load in the rubber die sleeve made in advance, adopt 160MPa hydrostatic profile, be placed on intermediate frequency furnace, sinter 55 hours at 1900 DEG C under hydrogen atmosphere, after burning till slab, keep temperature, standby；
Step 2, the slab burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, control the temperature 1350 DEG C of slab, forge slab mould, the deflection < 50% of panel base when forging, forge into the tabular component of length > 450, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75；
Step 3, lay down mould, take out the tabular component forging molding, insert in the tempering furnace of 1000 DEG C, keep 1 hour, stablize fine grained texture；
Step 4, tabular component being carried out machining, by cleaning, dry, prepared ultra-large type is brilliant molybdenum flat target carefully.
Embodiment two
The preparation method of a kind of ultra-large type carefully brilliant molybdenum flat target, adopts the molybdenum powder of purity > 99.95% to prepare, wherein, the length > 450 of molybdenum flat target, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75
Step one, take the molybdenum powder of granularity 3 μm, load in the rubber die sleeve made in advance, adopt 180MPa hydrostatic profile, be placed on intermediate frequency furnace, sinter 60 hours at 1950 DEG C under hydrogen atmosphere, after burning till slab, keep temperature, standby；
Step 2, the slab burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, control the temperature 1375 DEG C of slab, forge slab mould, the deflection < 50% of panel base when forging, forge into the tabular component of length > 450, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75；
Step 3, lay down mould, take out the tabular component forging molding, insert in the tempering furnace of 1100 DEG C, keep 2 hours, stablize fine grained texture；
Step 4, tabular component being carried out machining, by cleaning, dry, prepared ultra-large type is brilliant molybdenum flat target carefully.
Embodiment three
The preparation method of a kind of ultra-large type carefully brilliant molybdenum flat target, adopts the molybdenum powder of purity > 99.95% to prepare, wherein, the length > 450 of molybdenum flat target, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75
Step one, take the molybdenum powder of granularity 3.8 μm, load in the rubber die sleeve made in advance, adopt 200MPa hydrostatic profile, be placed on intermediate frequency furnace, sinter 65 hours at 2000 DEG C under hydrogen atmosphere, after burning till slab, keep temperature, standby；
Step 2, the slab burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, control the temperature 1400 DEG C of slab, forge slab mould, the deflection < 50% of panel base when forging, forge into the tabular component of length > 450, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75；
Step 3, lay down mould, take out the tabular component forging molding, insert in the tempering furnace of 1200 DEG C, keep 3 hours, stablize fine grained texture；
Step 4, tabular component being carried out machining, by cleaning, dry, prepared ultra-large type is brilliant molybdenum flat target carefully.
Claims (4)
1. the preparation method of a ultra-large type carefully brilliant molybdenum flat target, the molybdenum powder adopting purity > 99.95% prepares, wherein, the length > 450 of molybdenum flat target, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75, it is characterised in that:
Step one, take the molybdenum powder of granularity 2.8-3.8 μm, load in the rubber die sleeve made in advance, adopt 160-200MPa hydrostatic profile, be placed on intermediate frequency furnace, under the atmosphere of hydrogen, keep temperature 1900 DEG C to sinter 55-65 hour, after burning till slab, standby；
Step 2, the slab burnt till from intermediate frequency furnace taking-up, insert in the mould made in advance, control the temperature 1350 DEG C of slab, forge slab mould, the deflection < 50% of panel base when forging, forge into the tabular component of length > 450, width G reatT.GreaT.GT 320, thickness G reatT.GreaT.GT 75；
Step 3, lay down mould, take out the tabular component forging molding, insert in the tempering furnace of 1000-1200 DEG C, keep 1-3 hour, stablize fine grained texture；
Step 4, tabular component being carried out machining, by cleaning, dry, prepared ultra-large type is brilliant molybdenum flat target carefully.
2. the preparation method of a kind of ultra-large type according to claim 1 carefully brilliant molybdenum flat target, it is characterised in that: described sintering, sinter under vacuo, during vacuum-sintering, temperature progressively heats up from zero degree to 2000 DEG C.
3. the preparation method of a kind of ultra-large type according to claim 1 carefully brilliant molybdenum flat target, it is characterised in that: in described step one in sintering process, in intermediate frequency furnace, keep temperature 2000 DEG C to sinter 60 hours.
4. the preparation method of a kind of ultra-large type according to claim 1 carefully brilliant molybdenum flat target, it is characterised in that: in described step 3, take out in the tempering furnace that the tabular component forging molding inserts 1200 DEG C, keep 2 hours, stablize fine grained texture.
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| CN101259584A (en) * | 2008-04-25 | 2008-09-10 | 胡延槽 | Method for preparing high-density molybdenum tube |
| CN102277558A (en) * | 2011-08-23 | 2011-12-14 | 洛阳科威钨钼有限公司 | Process for manufacturing tungsten spin-coated sputtering tube target |
| CN102699329A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Process for manufacturing large-sized molybdenum rods |
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| JP2014034684A (en) * | 2012-08-07 | 2014-02-24 | Hitachi Metals Ltd | Molybdenum based sputtering target material and method for manufacturing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101259584A (en) * | 2008-04-25 | 2008-09-10 | 胡延槽 | Method for preparing high-density molybdenum tube |
| CN102277558A (en) * | 2011-08-23 | 2011-12-14 | 洛阳科威钨钼有限公司 | Process for manufacturing tungsten spin-coated sputtering tube target |
| CN102699329A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Process for manufacturing large-sized molybdenum rods |
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