CN202207799U - Target manufacture device - Google Patents
Target manufacture device Download PDFInfo
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- CN202207799U CN202207799U CN2011202568552U CN201120256855U CN202207799U CN 202207799 U CN202207799 U CN 202207799U CN 2011202568552 U CN2011202568552 U CN 2011202568552U CN 201120256855 U CN201120256855 U CN 201120256855U CN 202207799 U CN202207799 U CN 202207799U
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Abstract
The utility model provides a target manufacture device. The target manufacture device comprises a sintering furnace body, a composite heating mould, a pressurizing device and a heating device, wherein an inner cavity of the sintering furnace body is a vacuum or atmosphere protective cavity; the composite heating mould is arranged inside the inner cavity of the sintering furnace; the composite heating mould is provided with the inner cavity, so that the processed target powder is placed in the inner cavity of the composite heating mould; the pressurizing device and the composite heating mould are connected, and the heating device and the pressurizing device are connected for directly heating the sample, and the composite heating mould can be heated up independently. The target manufacture device can be used for manufacturing alloy targets with large dimension, high melting point, high density, and large melting point difference of components; simultaneously, the target manufacture device has the characteristics of simple device, short sintering time, high energy efficiency, small device and mould loss, and low cost.
Description
Technical field
The utility model relates to the target preparing technical field, and particularly a kind of target preparation facilities can be used for powder sintered preparation large scale, high density, high-melting-point, alloy target material that constituent element fusing point difference is bigger.
Background technology
Sputtering method is a relatively high-efficiency method of preparation film, but the composition proportion of used target, heterogeneous microstructure and uniformity, purity, density, and target size etc. the performance and the plated film efficient of the film of last formation is had very important influence.So institutional framework, high-purity, high density, large-sized target with strict composition proportion, exquisiteness are light, the electrical part manufacturing industry of modern high end, like the basic demand of industries such as display and solar film battery.This has higher requirement also for traditional target technology for producing and equipment.Current, it is powder sintered producing target method commonly used, comprises hot pressed sintering, HIP sintering, microwave sintering, electric current sintering, discharge plasma sintering etc.
Publication number is CN1352375A; Application number is to disclose resistive heating device in 00131150.6 the Chinese invention patent " electric resistor heating type super high temperature vacuum sintering furnace " to utilize two poles to pass through the outer heavy-current bus-bars of stove and the metal water cold electrode gets into the sintering road; The transition electrode of processing via the carbon-graphite material again is connected on the heater grillage, constitutes complete circuit system, and the heater grillage adopts side heater series connection up and down in the resistive heating device; The circuit structure of both sides parallel connection; This structural design can be born 2,000 degree above high temperature and stable work, but utilizes the resistance indirect, certainly will cause a large amount of losses of heat in conductive process.Simultaneously, cause to have thermograde in the sample, when the sintering large-size target, cause the inhomogeneous of target center part and outer portion of tissue structure easily because heat is to rely on the heat conduction to import sample interior into from the outside.This equipment also can't solve the sintering between the big constituent element of fusing point difference in addition.
Publication number is that the United States Patent (USP) of US005234487A discloses through hot isostatic pressing method and prepares the W/Ti target material, and it contains the rich Ti solid solution phase below 15%, and its material density has reached 95%; But its density is difficult to improve again; And the super large pressure of the 200～1000MPa that uses, high to equipment requirements, sintering time needs 2 hours simultaneously; Manufacturing cycle is long, causes growing up of grain structure easily.This method also can't solve the sintering between the big constituent element of fusing point difference in addition.
Publication number is CN1302707A, and application number is 01107084.6 Chinese invention patent " plasma technology for activating sintered material ", discloses plasma technology for activating sintered material; Publication number is CN1676251A, and application number is the method that 200510052092.9 Chinese invention patent application discloses a kind of nano aluminium oxide plasma sintering.More than two kinds of methods all be when being employed in pressurization; Apply pulse voltage and produce plasma, particle surface is carried out activation, the more logical direct current of constant voltage; Heat the material to temperature required method and carry out sintering; Because sintering time is short, has suppressed the activation of grain growth and particle surface, makes the performance of agglomerated material obtain raising in essence.But since the plasma that produces along with the difference of composition, electric property, mechanical property, powder shape and the size etc. of powder difference; Cause the resistance heating efficient of heterogeneity powder different; Finally cause the inhomogeneous of institutional framework and composition, so the general sintering that only is fit to single constituent element powder or has same alloy composition powder of plasma agglomeration method; Nor the sintering of suitable large scale sample.If the prolongation sintering time then causes grain growth easily; When the sintering large-size target, because big cross section, required electric current is big simultaneously, and power-supply device and grid power are required height, and this method also can't solve the sintering between the big constituent element of fusing point difference in addition.
Publication number is that the U.S. Patent application of US005896553A discloses with pressure sintering and prepares single phase through controlling its temperature, pressure and time parameter; The relative density of its target reaches more than 95%; But its sintering temperature reaches 1600 ℃～1650 ℃ high temperature, and the time also needs 3 hours, and energy consumption is very big; High temperature sintering also makes grain structure grow up easily for a long time simultaneously, and this method also can't solve the sintering between the big constituent element of fusing point difference in addition.
Publication number is CN1911599A, and application number is that 200510017879.1 Chinese invention patent discloses metal bonding agent extra hard material grinding wheel centrifuge hot press sintering method and device, is utilized under the heating condition; Compound in the mold high speed revolution, mould self with centrifugal medium action of centrifugal force under realize hot pressed sintering, heater adopts eddy-current heating or resistance heated; This patent utilization centrifugal force is realized radially evenly hot pressed sintering, has improved the uniformity of the axial density of high thickness metal bonding agent extra hard material grinding wheel, has realized the hot pressed sintering of the axial complex profile metal bonding agent extra hard material grinding wheel of cylindrical; But only utilize resistance heated; Just exist heat time heating time long, the cost problem of higher is only utilized current flow heats; Just there is perpendicular to radial direction the uneven problem of being heated.This method also only is suitable for the parts sintering with axial symmetric shape.This method does not solve the sintering problem between the big constituent element of fusing point difference simultaneously.
Publication number is CN101050121A; Application number is that 200710051776.6 Chinese invention patent discloses the dual heating mode flash sintering method that a kind of current flow heats combines radiation heating; In agglomerating plant by current flow heats power and radiation heating power than 30: 1-5: 1 disposes radiant heating device; At the sintering diameter during greater than the sample of 30mm; Adopt Fast Sintering under current flow heats and the radiation heating dual heating mode, utilize this method can prepare the sample of the diameter of material internal even structure, and sintering time is short, energy-conservation greater than 30mm.But this sintering method is main with direct current flow heats still; During for sintering multicomponent target; Because the electric property of each component, mechanical strength, granular size and shape are different, will there be bigger difference in the heating-up temperature of each component, be prone to cause the volatilization of the inhomogeneous and low-melting component of structure.
Publication number is CN1454736A; Application number is that 03128621.6 Chinese invention patent application discloses casting device and deposite metal feedway; This metal material of heated and the generation that are utilized in the metal material in the accepting container make the interior deposite metal of prevention accepting container use coil from the eddy-current heating that the masterpiece that spills between opening and the lid is used in the magnetic field on this deposite metal; But this mode of heating only is suitable for single metal molten; When carrying out the metal molten of two or more different melting points, cause vaporing away earlier of low melting point constituent element easily, cause the change of final target composition.
People such as Chen Jianjun disclose the big and more crisp preparation that has the target of preparation difficulty of material self owing to component fusing point difference such as ITO target, Tb-Fe-Co/Ti complex gradient magneto-optic target in " Hunan non-ferrous metal " article " kind of sputtering target material, application, preparation and development trend " that 04 phase delivered in 2006; Prepared target intensity and toughness are better; But heat time heating time is longer, preparation process more complicated.
From existing document and report, can find out, in the target sintering method, the target of pressure sintering, hot isostatic pressing method preparation; Compactness is better relatively; But they tend to receive the restriction that target requires size, microscopic appearance and low cost etc., and to the activation degree of sample, promptly dynamic process remains further to be improved in the while hot pressed sintering process; And apparatus expensive, the process-cycle is long; Discharge plasma sintering technique has the characteristics that realize the Fast Sintering dense material at a lower temperature; Can effectively suppress the volatilization with constituent element of growing up of dusty material particle; Energy efficiency is high; But the sintering of the small size target of the general only suitable single component powder of this method, the inhomogeneities owing to electric current when the sintering large-size target causes the inconsistent of target different parts institutional framework easily; Microwave sintering has special requirement to powder property, and its process causes the inefficacy effect easily, and powder is produced inhomogeneous heating, thereby has influenced the various performances of sintered products; During spark plasma sintering, along with reaching certain density, the particle hole diminishes and is unfavorable for discharge sintering, especially is unfavorable for the sintering of large scale product, causes the center inconsistent with peripheral density.The direct current sintering produces fuel factor by electric current, can be adapted to the large scale sintering, but when sintering heterogeneity target powder, can cause the inhomogeneous and grain growth of phase constituent equally.So, also do not have at present a kind of efficient, low-cost preparation method that high density, high-purity, fusing point fusing point high, constituent differ bigger large-size target that can be used in.
The utility model content
The main purpose of the utility model is to overcome the shortcoming of above-mentioned prior art with not enough, provides a kind of simple and reasonable for structure, can be used for the target preparation facilities of the bigger alloy target material of the fusing point difference of large scale, high-melting-point, high density and constituent.
For reaching above-mentioned purpose, the utility model adopts following technical scheme:
A kind of target preparation facilities comprises sintering body of heater, compound heating mould, pressue device and heater, and the inner chamber of said sintering body of heater is vacuum or atmosphere protection cavity, and compound heating mould places in the inner chamber of sintering body of heater; Said compound heating mould is provided with inner chamber, and processed target powder places in the inner chamber of compound heating mould; Said pressue device is connected with compound heating mould, and heater is connected with compound heating mould, pressue device respectively.
Said compound heating mould is that the skin that is employed in the insulation mould adds a conductive die, earlier with DC current or pulse current or alternating current through conductive die, the target material powder to pre-compacted preheats sintering in certain atmosphere or under the vacuum condition; And control at a certain temperature; Preferential control temperature is lower than the boiling point of the minimum fusing point constituent element in all constituent elements, under this temperature, makes full and uniformization of low melting point composition, and this mold heated mode has the energy efficiency height; Heat temperature raising speed is fast; Controllable Temperature, device structure is simple simultaneously, and cost is low.Be specially: said compound heating mould comprises the conductive die that overlaps in the mould and be socketed in cover periphery in the mould, and cover is the insulation mould in the said mould; The inner chamber of said compound heating mould is the inner chamber of insulation mould; Said pressue device is connected with the insulation mould, and said conductive die is connected with heater.
Said pressue device is meant the device that can adopt continuity supercharging mode, continuity pressure reducing mode or alternation formula transformation mode, and the pressure of continuity supercharging mode, continuity pressure reducing mode or alternation formula transformation mode can be provided; The pressure limit of said transformation is 5MPa～700Mpa; The pressure amplitude scope of said alternation formula transformation mode is 0～40% of a pressure of foundation, and frequency range is 0.01Hz～200Hz.As on the basis of 50MPa pressure, carrying out range value is 30%, i.e. the cyclically-varying of 15MPa, and its frequency is 100Hz.Be specially: said pressue device comprises pressure control device, transformation electrode, pressure head electrode and pressure head; Said pressure control device is connected through lead with the transformation electrode; Be connected through non-conductive plate between transformation electrode and the pressure head electrode, the pressure head electrode is connected with the pressure head one; The lower end of said pressure head stretch into the insulation mould inner chamber and with the insulation mould inner chamber be connected, to contact said processed target powder; Said pressure head electrode is connected with heater.
Said insulation mould, conductive die are rectangular mould; Said non-conductive plate, pressure head electrode all place in the inner chamber of sintering body of heater, and said sintering body of heater, insulation mould be equipped with the punching press mouth that is communicated with its inner chamber, and the punching press mouth of the punching press mouth of sintering body of heater and the mould that insulate is on same straight line; The punching press mouth that said transformation electrode passes the sintering body of heater is connected with non-conductive plate, and said pressure head is stretched in the inner chamber of insulation mould by the punching press mouth of sintering body of heater.
The effect of said heater is to adopt heat conducting mode that the target powder is heated earlier; Through the pressure head electrodes use current flow heats mode that is added on the target powder target powder of presintering is carried out Fast Sintering again, obtain the target of desired density and institutional framework.Be specially: said heater comprises mold heated power supply and target heating power supply, and said mold heated power supply is connected with conductive die through lead, and said target heating power supply is connected with the pressure head electrode through lead.
Said mold heated power supply is dc source, AC power or the pulse power, and said target heating power supply is dc source, AC power or the pulse power.The electrically heated current density size of said direct current is 0.0003～40A/mm
2, its voltage swing is 1～700V, concrete electric current and voltage swing are according to the resistivity of target, than performance synthesis considerations such as thermal parameter, heat conduction, powder size size and mechanical characteristics; It can be high frequency, intermediate frequency or low frequency that said alternating current heats used electric current; The peak value of the pulse current density of said pulse current heating is 0.003～40A/mm
2, base value is 0～20A/mm
2, frequency is 55～500Hz, dutycycle is 57%～89%.
Said insulation mould is the good and resistant to elevated temperatures insulating materials of thermal conductivity, is preferably by a kind of or some kinds of moulds that material is processed in aluminium oxide, Mo Laishi, quartz, titanium oxide, titanium nitride or the aluminium nitride.
Said conductive die is good conductivity, resistant to elevated temperatures high-strength material, is preferably the mould of being processed by graphite, molybdenum, molybdenum alloy, tungsten, tungsten alloy, nichrome or stainless steel.
Target process by above-mentioned target preparation facilities is realized comprises the steps:
(1) preliminary treatment: under the protection of vacuum or inert gas, adopt ball mill that processed target powder is carried out ball milling, treat that said target powder mixes evenly after, it is positioned in the inner chamber of the mould that insulate;
(2) pre-compacted: pressue device is exerted pressure through pressure head target powder in said mould, so that the target powder is by pre-compacted; Extract vacuum or logical protective atmosphere in the sintering body of heater simultaneously, and make the pressure in the sintering body of heater reach the pressure values that preheats sintering;
(3) preheat sintering: start the mold heated power supply, mold heated power connection conductive die, and conductive mould input current; Under the effect of electric current, conductive die, insulation mould, processed target powder are realized the heat conduction successively, and then realize the sintering that preheats of target powder;
(4) current flow heats target sintering: when the temperature of target powder reaches the pre-sintering temperature value; Start the target heating power supply, the target heating power supply is connected pressure head electrode and pressure head, and to pressure head electrode, pressure head input current; Make electric current flow through the target powder; Thereby to target powder heat processed, simultaneously, pressue device applies transformation power to the target powder;
(5) when the temperature of target powder reaches the sintering temperature value, then accomplish the current flow heats sintering, close the target heating power supply, stop the current flow heats sintering,, accomplish the processing of target cooling of target powder and pressure release.
In the said step (2), elder generation is to the inner chamber extracting vacuum of sintering body of heater, so that its internal pressure is 3.2 * 10
-4Pa～5 * 10
-4Behind the Pa, feed gas (preferred helium, argon gas) again,, make the sintering furnace intracoelomic cavity reach the pressure values that preheats sintering so that its pressure becomes 1～10 atmospheric pressure;
In the said step (4), when then the temperature of the target powder after step (3) preheats reached the pre-sintering temperature value, the target powder is insulation 0～10h earlier, restarts the target heating power supply and carries out the current flow heats sintering;
In the said step (4), if adopt DC current heat-agglomerating, then said galvanic current density size is 0.0003～40A/mm
2, its voltage swing is 1～700V, concrete electric current and voltage swing can be according to the resistivity of target, than performance synthesis considerations such as thermal parameter, heat conduction, powder size size and mechanical characteristics; When carrying out DC current heat-agglomerating; Pressue device applies the transformation power that increases progressively to the target powder; When said transformation power reaches 5MPa～700Mpa; Pressue device applies the transformation power that size fluctuates with 0～40% amplitude to the target powder on the basis of 5MPa～700Mpa, frequency range is 0.01Hz～200Hz;
In the said step (4), if adopt pulse current heat-agglomerating, then the pressure in the sintering body of heater keeps original pressure values, and the peak value of the pulse current density of said pulse current heating is 0.003～40A/mm
2, base value is 0～20A/mm
2, frequency is 55～500Hz, dutycycle is 57%～89%; When carrying out pulse current heat-agglomerating; Pressue device applies the transformation power that increases progressively to the target powder; After transformation power reaches 5MPa～700MPa; Pressue device applies the transformation power that size fluctuates with 15%～20% amplitude to the target powder on the basis of 5MPa～700Mpa, frequency is 0.01Hz～200Hz;
Pre-sintering temperature value in the said step (4) is to hang down 10～2000 ℃ temperature value than the boiling point of minimum fusing point composition in the target powder, and the sintering temperature value in the step (5) is to hang down 10～1000 ℃ temperature value than the fusing point of peak melting point composition in the target powder;
In the said step (5), close the target heating power supply after, treat that the target powder drops to 200～100 ℃, begins pressure release again; After pressure release is accomplished, treat that temperature reduces to 20 ℃～80 ℃ dischargings again.
The average grain diameter of the main component powder of said target is 1～5 μ m, and maximum particle diameter is less than 15um.
The density of the target of the said preparation of employing the utility model device can be greater than 99%TD.
The principle of the utility model: under certain atmosphere or vacuum condition; Adopt the technology of first heating mould; Can effectively control powder temperature, make its boiling point that is lower than low-melting component, when preventing low-melting component volatilization, can make powder organization obtain to a certain degree homogenising and densified; It is too fast to heat up when preventing the direct heated sample of electric current, causes the volatilization of low melting point, and atmosphere protection can play certain effect that prevents to the volatilization of low melting point simultaneously.Directly during electric current sintering,, can make the size of current at each position in the whole sintered powder more consistent at subsequently sample (target powder), guarantee large-size target powder each several part sintering uniformity because presintering powder has had good structural homogeneity; Simultaneously owing to adopted powder directly through the mode of current flow heats, heat time heating time is very short, has effectively avoided the volatilization of low melting point composition, can not bring also that significantly grain growth and phase constituent are inhomogeneous; Adopt first mould resistance heated to the basis of uniform temperature again to the sintered powder current flow heats; It is slower to overcome when adopting the mould resistance heated all the time heating; The low melting point composition is volatile in the target; The problem of growing up easily with crystal grain also helps carrying out the constituent fusing point simultaneously and differs the sintering of bigger target and the sintering of high-melting-point target; Added the control of transformation power, be adapted to the characteristics of various different powder particle sizes and material character, increased the exposure level between the powder particle, can effectively increase density and shorten sintering time, and can reduce wearing and tearing mould; Whole sintering process energy consumption is lower, and the time is short, has suppressed the grain growth problem effectively, and the sample crystallite dimension of preparation is tiny, even size distribution, and density is bigger.In a word, the utility model promptly kept plasma agglomeration or electric current direct sintering method fast, characteristics that efficiency is high, avoided being not suitable for the shortcoming of sintering large-size target again, also effectively solved the powder sintered problem between the constituent element of fusing point difference simultaneously.
Compared with prior art, the utlity model has following advantage and beneficial effect:
1, the utility model can prepare the higher large-size target of institutional framework homogeneous and controllable, purity and density, is particularly suitable for preparing containing big powder sintered of multiple composition and fusing point difference, reaches high-performance and large scale that existing sintering technology can't be realized.
2, the utlity model has that sintering time is short, energy efficiency is high, to equipment and little, the lower-cost characteristics of mould loss.
Description of drawings
Fig. 1 is the structural representation of the utility model device.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing the utility model is described in further detail, but the embodiment of the utility model is not limited thereto.
Embodiment 1
As shown in Figure 1, this target preparation facilities comprises sintering body of heater 1, compound heating mould, pressue device and heater, and the inner chamber 2 of said sintering body of heater 1 is a vacuum cavity, and compound heating mould places in the inner chamber 2 of sintering body of heater 1; Said compound heating mould is provided with inner chamber 9, and processed target powder places in the inner chamber 9 of compound heating mould; Said pressue device is connected with compound heating mould, and heater is connected with compound heating mould, pressue device respectively.
Said compound heating mould comprises interior cover 7 of mould and the conductive die 6 that is socketed in cover 7 peripheries in the mould, overlaps in the said mould to be the insulation mould; The inner chamber 9 of said compound heating mould is the inner chamber of insulation mould 7; Said pressue device is connected with insulation mould 7, and said conductive die 6 is connected with heater.
Said pressue device comprises pressure control device 5, transformation electrode 12, pressure head electrode 10 and pressure head 8; Said pressure control device 5 and transformation electrode 12 are connected through lead; Be connected through non-conductive plate 11 between transformation electrode 12 and the pressure head electrode 10, pressure head electrode 10 is connected with pressure head 8 one; The lower end of said pressure head 8 stretch into the insulation mould 7 inner chamber 9 and with the insulation mould 7 inner chamber 9 be connected, to contact said processed target powder; Said pressure head electrode 10 is connected with heater.
Said insulation mould 7, conductive die 6 are rectangular mould; Said non-conductive plate 11, pressure head electrode 10 all place in the inner chamber 2 of sintering body of heater 1, and said sintering body of heater 1, insulation mould 7 be equipped with the punching press mouth that is communicated with its inner chamber, and the punching press mouth of the punching press mouth of sintering body of heater 1 and the mould 7 that insulate is on same straight line; The punching press mouth that said transformation electrode 12 passes sintering body of heater 1 is connected with non-conductive plate 11, and said pressure head 8 is stretched in the inner chamber 9 of insulation mould 7 by the punching press mouth of sintering body of heater 1.
The effect of said heater is to adopt heat conducting mode that the target powder is heated earlier; Adopt the current flow heats modes that the target powder of presintering is carried out Fast Sintering through being added in pressure head electrode 10 on the target powder again, obtain the target of desired density and institutional framework.Be specially: said heater comprises mold heated power supply 3 and target heating power supply 4, and said mold heated power supply 3 is connected with conductive die 6 through lead, and said target heating power supply 4 is connected with pressure head electrode 10 through lead.
Said mold heated power supply is a dc source; Said target heating power supply is a dc source.
Said insulation mould 7 is the good and resistant to elevated temperatures insulating materials of thermal conductivity, is the mould of being processed by aluminium oxide.
Said conductive die 6 is good conductivity, resistant to elevated temperatures high-strength material, is the mould of being processed by graphite.
Target process by above-mentioned target preparation facilities is realized comprises the steps:
(1) preliminary treatment: with fusing point is that 1084 ℃ copper powder (purity >=99.5%), fusing point is that 29.8 ℃, boiling point are that 2403 ℃ Ga (gallium) powder (purity >=99.5%) is a raw material powder;
With average grain diameter is Cu (copper) powder, the Ga powder of 0.5～30 μ m; In required ratio weighing; In inert gas (Ar gas, i.e. argon gas) protection after ball milling mixed in 4 hours down, it is positioned in 800mm * 580mm rectangle high strength, the high temperature resistant and insulation mould 7;
Adopt earlier DC current is passed through conductive die 6, the target material powder to pre-compacted under certain atmosphere preheats sintering, carries out the DC current sintering again, promptly carries out step (2)～(5):
(2) pre-compacted: pre-compacted also is evacuated to 5 * 10
-4Pa feeds helium, and pressure becomes five atmospheric pressure;
(3) preheat sintering: begin to preheat, be warming up to 403 ℃ through the powder of die coat heating power supply device output direct current to compacting, insulation 10min, pressure is pressurized to 30MPa continuously from 10MPa therebetween;
(4) current flow heats sintering: when the temperature of target powder reaches the pre-sintering temperature value (temperature value of low 2000 ℃ of the boiling point of minimum fusing point composition in than target powder; Promptly 403 ℃) time, keep original vacuum, start the target heating power supply; The target heating power supply is connected pressure head electrode and pressure head; And, make electric current flow through the target powder, thereby to target powder heat processed to pressure head electrode, pressure head input dc power stream; Wherein DC current density size is 1.5A/mm
2; In current flow heats, pressue device applies transformation power to the target powder, and transformation power is pressurized to 50MPa continuously from 30MPa; When transformation power size reaches 50MPa; Transformation power is on the 50MPa basis, and the amplitude of carrying out is 10% cyclically-varying (fluctuating), i.e. 5MPa; Frequency is 200Hz, and circulation transformation scope is in 45MPa～55MPa;
(5) when the temperature of target powder reaches sintering temperature value (fusing point of peak melting point composition hangs down 10 ℃ temperature value, promptly 1074 ℃ in than target powder), insulation 8min; Then close DC heating subsequently, temperature drops to 200 ℃, the beginning pressure release; Temperature is reduced to 80 ℃, and processing is accomplished in discharging.
The density of target is 6.657g/cm
3, relative density is greater than 99%, and the main particle average dimension of copper gallium target is no more than 5 μ m.
Embodiment 2
Present embodiment except that following characteristics other architectural features with embodiment 1: the mould of said insulation mould 7 for processing by titanium nitride.The mould of said conductive die 6 for processing by tungsten and tungsten alloy.
Said mold heated power supply is a dc source; Said target heating power supply is the pulse power.
Target process by above-mentioned target preparation facilities is realized comprises the steps:
(1) preliminary treatment: with fusing point is that 1660 ℃ titanium valve (purity >=99.5%), fusing point is that 660 ℃, boiling point are that 2467 ℃ aluminium powder (purity >=99.5%) is a raw material powder;
With average grain diameter is titanium valve, the aluminium powder of 0.5～30 μ m, at inert gas (Ar gas) protection ball milling 6 hours down, after mixing under inert gas (He gas) protection, it is positioned in 800mm * 580mm rectangle high strength, the high temperature resistant and mould 7 that insulate;
Adopt earlier DC current through conductive die 6, the target material powder to pre-compacted under certain atmosphere preheats sintering, carries out pulse electric current sintering again, like step (2)～(5):
(2) pre-compacted: pre-compacted also is evacuated to 3.2 * 10
-4Pa feeds helium, and pressure becomes four atmospheric pressure;
(3) preheat sintering: begin to preheat, be warming up to 1000 ℃ through the powder of die coat heating power supply device output DC stream to compacting;
(4) carry out pulse current heat-agglomerating then: when the temperature of target powder reaches the pre-sintering temperature value (temperature value of low 1467 ℃ of the boiling point of minimum fusing point composition in than target powder; Promptly 1000 ℃) time, keep original vacuum, start the target heating power supply; The target heating power supply is connected pressure head electrode and pressure head; And, make pulse current flow through the target powder, thereby to target powder heat processed to pressure head electrode, pressure head input pulse electric current; The pulse current density amplitude is from 1A/mm
2Be increased to 1.2A/mm
2, and frequency falls fewly to 68Hz from 89Hz, and the dutycycle perseverance is 57%; In current flow heats, pressue device applies transformation power to the target powder, and transformation power is pressurized to 50MPa continuously from 10MPa therebetween; When transformation power reached 50MPa, the size of said transformation power was on the basis of 50MPa, and the amplitude of carrying out is 20% cyclically-varying (fluctuating), i.e. 10MPa, and frequency is 100Hz, circulation transformation scope is closed sintering in 40MPa～60MPa;
(5) when the temperature of target powder reaches sintering temperature value (fusing point of peak melting point composition hangs down 140 ℃ temperature value, promptly 1520 ℃ in than target powder), then be incubated 10min, temperature drops to 200 ℃ subsequently, the beginning pressure release, and temperature is reduced to 80 ℃, and processing is accomplished in discharging.The density of target is 3.6g/cm3, and relative density is greater than 99%, and the main particle size of titanium aluminium target is no more than 5 μ m.
Embodiment 3
Present embodiment except that following characteristics other architectural features with embodiment 2: pressure becomes 10 atmospheric pressure after feeding gas in the said step (3); In the said step (4); When then the temperature of the target powder after step (3) preheats reaches the pre-sintering temperature value; The target powder is insulation 10h earlier, directly starts the target heating power supply and carries out the current flow heats sintering;
The peak value of pulse current density is 40A/mm
2, base value is 20A/mm
2, frequency is 500Hz, dutycycle is 89%; When carrying out pulse current heat-agglomerating, pressue device applies the transformation power that increases progressively to the target powder, and after transformation power reached 700MPa, the size of said transformation power amplitude with 20% on the basis of 700Mpa fluctuated, and frequency is 200Hz;
In the said step (5), close the target heating power supply after, treat that the target powder drops to 100 ℃, begins pressure release again; After pressure release is accomplished, treat that temperature reduces to 50 ℃ of dischargings again.
Embodiment 4
Present embodiment except that following characteristics other architectural features with embodiment 2: in the said step (4); When then the temperature of the target powder after step (3) preheats reaches the pre-sintering temperature value; The target powder is insulation 10h earlier, directly starts the target heating power supply and carries out the current flow heats sintering;
The peak value of pulse current density is 0.003A/mm
2, base value is 0mA/mm
2, frequency is 55Hz, dutycycle is 57%; When carrying out pulse current heat-agglomerating, pressue device applies the transformation power that increases progressively to the target powder, and after transformation power reached 5MPa, the size of said transformation power amplitude with 15% on the basis of 5Mpa fluctuated, and frequency is 0.01Hz;
In the said step (5), close the target heating power supply after, treat that the target powder drops to 150 ℃, begins pressure release again; After pressure release is accomplished, treat that temperature reduces to 50 ℃ of dischargings again.
Embodiment 5
Present embodiment except that following characteristics other architectural features with embodiment 1: the mould of said insulation mould 7 for processing by aluminium nitride.The mould of said conductive die 6 for processing by nichrome.
Target process by above-mentioned target preparation facilities is realized comprises the steps:
(1) preliminary treatment: with fusing point is that 660 ℃, boiling point are that 2467 ℃ aluminium powder (purity >=99.5%), the nickel powder (purity >=99.5%) that fusing point is 1455 ℃ are raw material powder;
With average grain diameter is Ni powder, the Al powder of 10～30 μ m, in required ratio weighing, in inert gas (Ar gas) protection down, after ball milling mixed in 6 hours, it is positioned in 800mm * 580mm rectangle high strength, the high temperature resistant and mould 7 that insulate;
Adopt earlier DC current through conductive die 6, the target material powder to pre-compacted under certain atmosphere preheats sintering, carries out the DC current sintering again, like step (2)～(5):
(2) pre-compacted: pre-compacted also is evacuated to 3.5 * 10
-4Pa feeds argon gas, and pressure becomes three atmospheric pressure;
(3) preheat sintering: begin to preheat, be warming up to 800 ℃ through the powder of die coat heating power supply device output DC stream to compacting;
(4) current flow heats sintering: when the temperature of target powder reached pre-sintering temperature value (boiling point of minimum fusing point composition hangs down 1667 ℃ temperature value, promptly 800 ℃ in than target powder), the target powder is insulation 10min earlier; Restart the target heating power supply and carry out DC current heat-agglomerating; Keep original vacuum, the target heating power supply is connected pressure head electrode and pressure head, and to pressure head electrode, pressure head input current; Make electric current flow through the target powder, thereby to target powder heat processed; Wherein, DC current density size is 1.7A/mm
2When carrying out DC current heat-agglomerating, pressue device applies the transformation power that increases progressively to the target powder again, and transformation power is pressurized to 60MPa continuously from 40MPa therebetween; When transformation power reached 60MPa, the size of transformation power was on the 60MPa basis, and the amplitude of carrying out is 15% cyclically-varying (fluctuating); Be 9MPa, frequency is 200Hz, and circulation transformation scope is in 51MPa～69MPa; Frequency is 200Hz, closes DC heating subsequently;
(5) when the temperature of target powder reaches sintering temperature value (fusing point of peak melting point composition hangs down 145 ℃ temperature value, promptly 1310 ℃ in than target powder), insulation 8min; Then close the target heating power supply; Stop the current flow heats sintering, temperature drops to 200 ℃ subsequently, the beginning pressure release; Temperature is reduced to 80 ℃, discharging processing.The density of target is 5.11g/cm
3, relative density is greater than 99%, and the main particle average dimension of nickel aluminium target is no more than 5 μ m.
Embodiment 6
Present embodiment except that following characteristics other architectural features with embodiment 1: the serve as reasons mould of Mo Lai one-tenth made of stones of said insulation mould 7.The mould of said conductive die 6 for processing by stainless steel.Said mold heated power supply is an AC power.
Embodiment 7
Present embodiment except that following characteristics other architectural features with embodiment 1: said insulation mould 7 mould that quartz is processed of serving as reasons.
In the said step (4), when then the temperature of the target powder after step (3) preheats reached the pre-sintering temperature value, the target powder is insulation 10h earlier, restarts the target heating power supply and carries out the current flow heats sintering;
Said galvanic current density size is 40A/mm
2When carrying out DC current heat-agglomerating, pressue device applies the transformation power that increases progressively to the target powder again, and when transformation power reached 700Mpa, the size of said transformation power amplitude with 0～40% on the basis of 700Mpa fluctuated, and frequency is 200Hz.
Embodiment 8
Present embodiment except that following characteristics other architectural features with embodiment 1: the mould of said insulation mould 7 for processing by titanium oxide.
In the said step (4), when then the temperature of the target powder after step (3) preheats reached the pre-sintering temperature value, the target powder need not be incubated, and directly started the target heating power supply and carried out the current flow heats sintering;
Said galvanic current density size is 0.0003A/mm
2, its voltage swing is 1V; When carrying out DC current heat-agglomerating, pressue device applies the transformation power that increases progressively to the target powder again, and when transformation power reached 5Mpa, the size of said transformation power amplitude with 1% on the basis of 5Mpa fluctuated, and frequency is 0.01Hz;
Said pre-sintering temperature value is to hang down 10 ℃ temperature value than the boiling point of minimum fusing point composition in the target powder, and said sintering temperature value is to hang down 10 ℃ temperature value than the fusing point of peak melting point composition in the target powder;
In the said step (5), close the target heating power supply after, treat that the target powder drops to 200 ℃, begins pressure release again; After pressure release is accomplished, treat that temperature reduces to 20 ℃ of dischargings again.
Embodiment 9
With fusing point is that 1565 ℃ indium sesquioxide powder (purity >=99.5%), fusing point is that 1127 ℃, boiling point are that 1800 ℃ putty powder (purity >=99.5%) is a raw material powder, preparation ITO target.
With average grain diameter is the In of 10～30 μ m
2O
3Powder, SnO
2Powder in required ratio weighing, in inert gas (Ar gas) protection down, after ball milling mixed in 6 hours, is positioned over it in 800mm * 580mm rectangle high strength, the high temperature resistant and mould that insulate.Adopt earlier DC current is passed through conductive die, the target material powder to pre-compacted under certain atmosphere preheats sintering, and carry out the DC current sintering again: pre-compacted also is evacuated to 3.5 * 10
-4Pa feeds helium, and pressure becomes two atmospheric pressure; Begin to preheat through the powder of die coat heating power supply device (being the mold heated power supply) output DC stream to compacting; Be warming up to 1200 degree, insulation 10min, pressure is pressurized to 30MPa continuously from 10MPa therebetween; Keep original vacuum, carry out the heating of sample DC current again, wherein DC current density size is 0.9A/mm
2, be warming up to 1500 ℃, insulation 8min, pressure is pressurized to 60MPa continuously from 40MPa therebetween; Be on the 60MPa basis at pressure simultaneously, the amplitude of carrying out is 15% cyclically-varying, i.e. 9MPa, and frequency is 200Hz; Circulation transformation scope is in 51MPa～69MPa, and frequency is 200Hz, closes DC heating subsequently, and temperature drops to 200 ℃; The beginning pressure release, temperature is reduced to 80 ℃, discharging processing.The density of target is 7.02g/cm
3, relative density is greater than 99%, and the main particle average dimension of ITO target is no more than 5 μ m.
Embodiment 10
With fusing point is that 1336 ℃, boiling point are that 3023 ℃ terbium powder (purity >=99.5%), fusing point is that 1535 ℃, boiling point are that 2750 ℃ iron powder (purity >=99.5%) fusing point is that 1495 ℃, boiling point are that 2870 ℃ cobalt powder, fusing point is that 1660 ℃, boiling point are that 3287 ℃ titanium valve is a raw material powder; Preparation Tb-Fe-Co/Ti complex gradient magneto-optic target is Tb powder, Fe powder, the Co powder of 10～30 μ m with average grain diameter; In required ratio weighing; In inert gas (Ar gas) protection after ball milling mixed in 6 hours down, it is positioned in 800mm * 580mm rectangle high strength, the high temperature resistant and mould that insulate.Adopt earlier DC current is passed through conductive die, the target material powder to pre-compacted under certain atmosphere preheats sintering, and carry out the DC current sintering again: pre-compacted also is evacuated to 3.5 * 10
-4Pa feeds helium, and pressure becomes two atmospheric pressure; Begin to preheat through the powder of die coat heating power supply device (being the mold heated power supply) output DC stream to compacting; Be warming up to 1500 degree, insulation 10min, pressure is pressurized to 30MPa continuously from 10MPa therebetween; Keep original vacuum, carry out the heating of sample DC current again, wherein DC current density size is 0.8A/mm
2, be warming up to 1520 ℃, insulation 8min, pressure is pressurized to 60MPa continuously from 40MPa therebetween; Be on the 60MPa basis at pressure simultaneously, the amplitude of carrying out is 15% cyclically-varying, i.e. 9MPa, and frequency is 200Hz; Circulation transformation scope is in 51MPa～69MPa, and frequency is 200Hz, closes DC heating subsequently, and temperature drops to 200 ℃; The beginning pressure release, temperature is reduced to 80 ℃, after the discharging processing, fragmentation; And cross 400 mesh sieves (aperture is 38 μ m), and obtain needed magneto-optic target material powder, after this target powder and titanium valve are mixed, be positioned in 800mm * 580mm rectangle high strength, the high temperature resistant and mould that insulate; Adopt earlier DC current is passed through conductive die, the target material powder to pre-compacted under certain atmosphere preheats sintering, carries out the DC current sintering again, and pre-compacted also is evacuated to 3.5 * 10
-4Pa feeds helium, and pressure becomes an atmospheric pressure, begins to preheat through the powder of die coat heating power supply device output DC stream to compacting, is warming up to 1000 degree, insulation 10min, and pressure is pressurized to 30MPa continuously from 10MPa therebetween; Keep original vacuum, carry out the heating of sample DC current again, wherein DC current density size is 1.1A/mm
2, be warming up to 1600 ℃, insulation 8min, pressure is pressurized to 60MPa continuously from 40MPa therebetween; Be on the 60MPa basis at pressure simultaneously, the amplitude of carrying out is 15% cyclically-varying, i.e. 9MPa, and frequency is 200Hz; Circulation transformation scope is in 51MPa～69MPa, and frequency is 200Hz, closes DC heating subsequently, and temperature drops to 200 ℃; The beginning pressure release, temperature is reduced to 80 ℃, discharging processing.The density of target is for being 7.298g/cm
3, relative density is greater than 99%, and the main particle average dimension of Tb-Fe-Co/Ti target is no more than 5 μ m.
Embodiment 11
Target process by the target preparation facilities is realized comprises the steps:
(1) preliminary treatment: under the protection of inert gas, adopt ball mill that processed target powder is carried out ball milling, treat that said target powder mixes evenly after, it is positioned in the inner chamber of the mould that insulate;
(2) pre-compacted: pressue device is exerted pressure to the target powder through pressure head, so that the target powder is by pre-compacted; Then, extract the vacuum in the sintering body of heater, so that the pressure in the sintering body of heater reaches the pressure values that preheats sintering through pressue device;
(3) preheat sintering: start the mold heated power supply, mold heated power connection conductive die, and conductive mould input current signal; Under the effect of current signal, conductive die, insulation mould, processed target powder are realized the heat conduction successively, and then realize the sintering that preheats of target powder;
(4) current flow heats sintering: when the temperature of target powder reaches the pre-sintering temperature value; Start the target heating power supply, the target heating power supply is connected pressure head electrode and pressure head, and to pressure head electrode, pressure head input current; Make electric current flow through the target powder, thereby to target powder heat processed; In current flow heats, pressue device applies transformation power to the target powder;
(5) when the temperature of target powder reaches the sintering temperature value, then close the target heating power supply, stop the current flow heats sintering,, accomplish the processing of target cooling of target powder and pressure release.
Said pre-sintering temperature value is to hang down 2000 ℃ temperature value than the boiling point of minimum fusing point composition in the target powder, and said sintering temperature value is to hang down 1000 ℃ temperature value than the fusing point of peak melting point composition in the target powder;
In the said step (5), close the target heating power supply after, treat that the target powder drops to 200 ℃, begins pressure release again; After pressure release is accomplished, treat that temperature reduces to 50 ℃ of dischargings again.
Embodiment 12
Present embodiment except that following characteristics other characteristics with embodiment 11: said pre-sintering temperature value is the temperature value than low 10 ℃ of the boiling point of minimum fusing point composition in the target powder, and said sintering temperature value be that the fusing point than peak melting point composition in the target powder hangs down 10 ℃ of temperature values;
In the said step (5), close the target heating power supply after, treat that the target powder drops to 100 ℃, begins pressure release again; After pressure release is accomplished, treat that temperature reduces to 20 ℃ of dischargings again.
Embodiment 13
Present embodiment except that following characteristics other characteristics with embodiment 1: said mold heated power supply is an AC power, and said target heating power supply is a dc source.
Embodiment 14
Present embodiment except that following characteristics other characteristics with embodiment 1: said mold heated power supply is the pulse power, and said target heating power supply is the pulse power.
The foregoing description is the utility model preferred implementation; But the embodiment of the utility model is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit and the principle of the utility model, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within the protection domain of the utility model.
Claims (8)
1. target preparation facilities, it is characterized in that: comprise sintering body of heater, compound heating mould, pressue device and heater, the inner chamber of said sintering body of heater is vacuum or atmosphere protection cavity, and compound heating mould places in the inner chamber of sintering body of heater; Said compound heating mould is provided with inner chamber, and processed target powder places in the inner chamber of compound heating mould; Said pressue device is connected with compound heating mould, and heater is connected with compound heating mould, pressue device respectively.
2. target preparation facilities according to claim 1 is characterized in that: said compound heating mould comprises the conductive die that overlaps in the mould and be socketed in cover periphery in the mould, and cover is the insulation mould in the said mould; The inner chamber of said compound heating mould is the inner chamber of insulation mould; Said pressue device is connected with the insulation mould, and said conductive die is connected with heater.
3. target preparation facilities according to claim 2; It is characterized in that: said pressue device comprises pressure control device, transformation electrode, pressure head electrode and pressure head; Said pressure control device is connected through lead with the transformation electrode; Be connected through non-conductive plate between transformation electrode and the pressure head electrode, the pressure head electrode is connected with the pressure head one; The lower end of said pressure head stretch into the insulation mould inner chamber and with the insulation mould inner chamber be connected, to contact said processed target powder; Said pressure head electrode is connected with heater.
4. target preparation facilities according to claim 3; It is characterized in that: said non-conductive plate, pressure head electrode all place in the inner chamber of sintering body of heater; And said sintering body of heater, insulation mould are equipped with the punching press mouth that is communicated with its inner chamber, and the punching press mouth of the punching press mouth of sintering body of heater and insulation mould is on same straight line; The punching press mouth that said transformation electrode passes the sintering body of heater is connected with non-conductive plate, and said pressure head is stretched in the inner chamber of insulation mould by the punching press mouth of sintering body of heater.
5. target preparation facilities according to claim 3; It is characterized in that: said heater comprises mold heated power supply and target heating power supply; Said mold heated power supply is connected with conductive die through lead, and said target heating power supply is connected with the pressure head electrode through lead.
6. target preparation facilities according to claim 5 is characterized in that: said mold heated power supply is dc source, AC power or the pulse power; Said target heating power supply is dc source, AC power or the pulse power.
7. target preparation facilities according to claim 2 is characterized in that: said insulation mould is by a kind of mould of processing in aluminium oxide, Mo Laishi, quartz, titanium oxide, titanium nitride or the aluminium nitride.
8. target preparation facilities according to claim 2 is characterized in that: the mould of said conductive die for being processed by graphite, molybdenum, molybdenum alloy, tungsten, tungsten alloy, nichrome or stainless steel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202568552U CN202207799U (en) | 2011-07-20 | 2011-07-20 | Target manufacture device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202568552U CN202207799U (en) | 2011-07-20 | 2011-07-20 | Target manufacture device |
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| CN202207799U true CN202207799U (en) | 2012-05-02 |
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| CN2011202568552U Withdrawn - After Issue CN202207799U (en) | 2011-07-20 | 2011-07-20 | Target manufacture device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260802A (en) * | 2011-07-20 | 2011-11-30 | 佛山市钜仕泰粉末冶金有限公司 | Target preparation device and target processing method thereof |
| CN103542715A (en) * | 2013-09-27 | 2014-01-29 | 合肥高歌热处理应用技术有限公司 | Composite sintering furnace for target material |
| CN105135873A (en) * | 2015-08-05 | 2015-12-09 | 清华大学 | Dynamic pressure electric pulse double-field control sintering furnace and sintering method |
| CN106513678A (en) * | 2016-11-29 | 2017-03-22 | 河南科技大学 | Powder sintering molding method and mold |
-
2011
- 2011-07-20 CN CN2011202568552U patent/CN202207799U/en not_active Withdrawn - After Issue
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260802A (en) * | 2011-07-20 | 2011-11-30 | 佛山市钜仕泰粉末冶金有限公司 | Target preparation device and target processing method thereof |
| CN102260802B (en) * | 2011-07-20 | 2013-06-12 | 佛山市钜仕泰粉末冶金有限公司 | Target preparation device and target processing method thereof |
| CN103542715A (en) * | 2013-09-27 | 2014-01-29 | 合肥高歌热处理应用技术有限公司 | Composite sintering furnace for target material |
| CN105135873A (en) * | 2015-08-05 | 2015-12-09 | 清华大学 | Dynamic pressure electric pulse double-field control sintering furnace and sintering method |
| CN106513678A (en) * | 2016-11-29 | 2017-03-22 | 河南科技大学 | Powder sintering molding method and mold |
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