CN102260802A - Target preparation device and target processing method thereof - Google Patents
Target preparation device and target processing method thereof Download PDFInfo
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- CN102260802A CN102260802A CN2011102032484A CN201110203248A CN102260802A CN 102260802 A CN102260802 A CN 102260802A CN 2011102032484 A CN2011102032484 A CN 2011102032484A CN 201110203248 A CN201110203248 A CN 201110203248A CN 102260802 A CN102260802 A CN 102260802A
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Abstract
The invention provides a target preparation device which comprises a sintering furnace body, a composite heating mould, a pressurizing device and a heating device, wherein the inner cavity of the sintering furnace body is a vacuum or atmosphere protection cavity; the composite heating mould is placed in the inner cavity of the sintering furnace body and provided with an inner cavity, and target powder to be processed is placed to the inner cavity of the composite heating mould; and the pressurizing device is connected with the composite heating mould, the heating device is connected with the pressurizing device and directly heats a sample, and the composite heating mould can be singly used for heating. The invention also provides a target processing method achieved by the target preparation device. The target preparation device and target processing method can be used for manufacturing an alloy target with large size, high melting point, high density and components large in melting point differences; and simultaneously, the target preparation device and target processing method have the characteristics of simple equipment, short sintering time, high energy efficiency, small equipment and mould losses and low cost.
Description
Technical field
The present invention relates to the target preparing technical field, particularly a kind of target preparation facilities and target working method thereof can be used for powder sintered preparation large size, 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 homogeneity, 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 weave construction, high purity, high-density, large-sized target with strict composition proportion, exquisiteness are light, the electrical part production of modern high end, as the basic demand of industries such as indicating meter 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 enter the sintering road by outer heavy-current bus-bars of stove and metal water cold electrode, the transition electrode of making via the carbon-graphite material is connected on the heating element grillage again, constitute complete circuit system, the heating element grillage adopts side heating element series connection up and down in the resistive heating device, the circuit structure of both sides parallel connection, this structure design can be born 2,000 degree above high temperature and stable work, but utilize the resistance indirect heating, 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 thermal 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 be US005234487A U.S. Patent Publication prepare the W/Ti target material by hot isostatic pressing method, 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, to the equipment requirements height, sintering time needs 2 hours simultaneously, preparation 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 that 200510052092.9 Chinese invention patent application discloses a kind of nano aluminium oxide plasma agglomerating method.More than two kinds of methods all be to adopt in pressurization, apply pulsed voltage and produce plasma body, particle surface is activated, constant voltage is led to direct current again, 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, make the performance of agglomerated material obtain in essence raising.But since the plasma body that produces along with the difference of composition, electric property, mechanical property, powder shape and the size etc. of powder difference, the resistance heating efficient difference that causes the heterogeneity powder, finally cause the inhomogeneous of weave construction 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 size sample.If the prolongation sintering time then causes grain growth easily; When the sintering large-size target, because big square section, required electric current is big simultaneously, and power unit 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 be US005896553A U.S. Patent Application Publication prepare single phase with pressure sintering by 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, time also needs 3 hours, 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, 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, utilization is under heating condition, the mold high speed revolution, compound in the mould is realized hot pressed sintering under self and centrifugal medium action of centrifugal force, heating unit adopts induction heating or resistive heating, this patent utilization centrifugal force is realized radially evenly hot pressed sintering, improved the homogeneity of the axial density of high thickness metal bonding agent extra hard material grinding wheel, realized the hot pressed sintering of the axial complex profile metal bonding agent extra hard material grinding wheel of cylindrical, but only utilize resistive heating, just exist heat-up 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 of a kind of current flow heats in conjunction with 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 still based on direct current flow heats, during for sintering polycomponent target, because electric property, mechanical strength, granular size and the shape difference of each component, will there be bigger difference in the Heating temperature of each component, easily 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, the induced current of the metallic substance of utilization in accepting container heat this metallic substance and generation make stop deposite metal in the accepting container from opening with cover between the masterpiece that spills be used in the induction heating coil in the magnetic field on this deposite metal, but this type of heating only is suitable for single melting of metal, when carrying out the melting of metal 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-up time is longer, the preparation process more complicated.
From existing document and report as can be seen, in the target sintering method, the target of pressure sintering, hot isostatic pressing method preparation, compactness is better relatively, but they tend to be subjected to 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 suppress effectively that the powdered material particulate is grown up and the volatilization of constituent element, the Energy efficiency height, but the sintering of the small size target of the general only suitable single component powder of this method, the ununiformity owing to electric current when the sintering large-size target causes the inconsistent of target different sites weave construction 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 spark sintering, especially is unfavorable for the sintering of large size product, causes the center inconsistent with peripheral density.The direct current sintering produces heat effect by electric current, can be adapted to the large size sintering, but can cause the inhomogeneous and grain growth of phase composition equally when sintering heterogeneity target powder.So, also do not have at present a kind of fusing point that can be used in high-density, high purity, fusing point height, moiety to differ efficient, the low-cost preparation method of bigger large-size target.
Summary of the invention
Main purpose of the present invention 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 size, high-melting-point, high-density and moiety.
Another object of the present invention is to provide the target working method that realizes by said apparatus.
For reaching above-mentioned purpose, the present invention adopts following technical scheme:
A kind of target preparation facilities comprises sintering body of heater, compound heating mould, pressurizing device and heating unit, and the inner chamber of described sintering body of heater is vacuum or atmosphere protection cavity, and compound heating mould places in the inner chamber of sintering body of heater; Described compound heating mould is provided with inner chamber, and processed target powder places in the inner chamber of compound heating mould; Described pressurizing device is connected with compound heating mould, and heating unit is connected with compound heating mould, pressurizing device respectively.
Described compound heating mould is to adopt the skin at the insulation mould to add a conductive die, earlier galvanic current or pulsed current or exchange current are passed through conductive die, the target raw material powder to pre-compacted preheats sintering in certain atmosphere or under the vacuum condition, and control at a certain temperature, preferential controlled temperature is lower than the boiling point of the minimum fusing point constituent element in all constituent elements, under this temperature, make full and uniformization of low melting point composition, 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: described 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 described mould; The inner chamber of described compound heating mould is the inner chamber of insulation mould; Described pressurizing device is connected with the insulation mould, and described conductive die is connected with heating unit.
Described pressurizing 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 range of described transformation is 5MPa～700Mpa; The pressure amplitude scope of described alternation formula transformation mode is 0～40% of a pressure of foundation, and range of frequency is 0.01Hz～200Hz.As on the basis of 50MPa pressure, carrying out range value is 30%, i.e. the periodical change of 15MPa, and its frequency is 100Hz.Be specially: described pressurizing device comprises pressure control device, transformation electrode, pressure head electrode and pressure head, described pressure control device is connected by lead with the transformation electrode, be connected by 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 described pressure head stretch into the insulation mould inner chamber and with the insulation mould inner chamber be connected, to contact described processed target powder; Described pressure head electrode is connected with heating unit.
Described insulation mould, conductive die are rectangular mould; Described non-conductive plate, pressure head electrode all place in the inner chamber of sintering body of heater, and described 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 described transformation electrode passes the sintering body of heater is connected with non-conductive plate, and described pressure head is stretched in the inner chamber of insulation mould by the punching press mouth of sintering body of heater.
The effect of described heating unit is to adopt heat conducting mode that the target powder is heated earlier, adopt the current flow heats mode that the target powder of presintering is carried out Fast Sintering by being added in pressure head electrode on the target powder again, obtain the target of desired density and weave construction.Be specially: described heating unit comprises mold heated power supply and target heating power supply, and described mold heated power supply is connected with conductive die by lead, and described target heating power supply is connected with the pressure head electrode by lead.
Described mold heated power supply is direct supply, AC power or the pulse power, and described target heating power supply is direct supply, AC power or the pulse power.The electrically heated current density size of described 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, consider than performance synthesises such as thermal parameter, thermal conduction, powder size size and mechanical characteristics; It can be high frequency, intermediate frequency or low frequency that described alternating current heats used electric current; The peak value of the pulse current density of described pulsed current heating is 0.003～40A/mm
2, base value is 0～20A/mm
2, frequency is 55～500Hz, dutycycle is 57%～89%.
Described insulation mould is the good and resistant to elevated temperatures insulating material of thermal conductivity, is preferably by a kind of or some kinds of moulds that material is made in aluminum oxide, Mo Laishi, quartz, titanium oxide, titanium nitride or the aluminium nitride.
Described conductive die is good conductivity, resistant to elevated temperatures high-strength material, is preferably the mould of being made by graphite, molybdenum, molybdenum alloy, tungsten, tungstenalloy, nichrome or stainless steel.
Target working method by above-mentioned target preparation facilities is realized comprises the steps:
(1) pre-treatment: under the protection of vacuum or rare gas element, adopt ball mill that processed target powder is carried out ball milling, treat that described target powder mixes evenly after, it is positioned in the inner chamber of the mould that insulate;
(2) pre-compacted: pressurizing device is exerted pressure by pressure head target powder in described mould, so that the target powder is by pre-compacted; Extract intravital vacuum of sintering oven or logical protective atmosphere simultaneously, and the intravital pressure of sintering oven is reached preheat the agglomerating pressure values;
(3) preheat sintering: start the mold heated power supply, mold heated power connection conductive die, and to the conductive die received current; Under the effect of electric current, conductive die, insulation mould, processed target powder are realized thermal 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 default 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 received current, make electric current flow through the target powder, thereby the target powder is added hot-work, and simultaneously, pressurizing device applies transformation power to the target powder;
(5) when the temperature of target powder reaches the sintering temperature value, then finish the current flow heats sintering, close the target heating power supply, stop the current flow heats sintering,, finish the processing of target cooling of target powder and pressure release.
In the described 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 oven intracoelomic cavity reach and preheat the agglomerating pressure values so that its pressure becomes 1～10 normal atmosphere;
In the described 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 described step (4), if adopt galvanic current heat-agglomerating, then described 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, consider than performance synthesises such as thermal parameter, thermal conduction, powder size size and mechanical characteristics; When carrying out galvanic current heat-agglomerating, pressurizing device applies the transformation power that increases progressively to the target powder, when described transformation power reaches 5MPa～700Mpa, pressurizing device applies the transformation power that size fluctuates with 0～40% amplitude to the target powder on the basis of 5MPa～700Mpa, range of frequency is 0.01Hz～200Hz;
In the described step (4), if adopt pulsed current heat-agglomerating, then the intravital pressure of sintering oven keeps original pressure values, and the peak value of the pulse current density of described pulsed 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 pulsed current heat-agglomerating, pressurizing device applies the transformation power that increases progressively to the target powder, after transformation power reaches 5MPa～700MPa, pressurizing 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 described 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 described 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 described 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 finished, treat that temperature reduces to 20 ℃～80 ℃ dischargings again.
The median size of the main component powder of described target is 1～5 μ m, and maximum particle diameter is less than 15um.
The density of the target of employing apparatus of the present invention and the described preparation of method can be greater than 99%TD.
Principle of the present invention: 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, prevent that the low-melting component evaporable from can make simultaneously powder organization obtain to a certain degree homogenizing and densification; It is too fast to heat up when preventing electric current direct heating sample, 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 homogeneity because presintering powder has had good structural uniformity; Simultaneously owing to adopted powder directly by the mode of current flow heats, heat-up time is very short, has effectively avoided the volatilization of low melting point composition, can not bring also that significantly grain growth and phase composition are inhomogeneous; Adopt first mould resistive heating to the basis of certain temperature again to the sintered powder current flow heats, it is slower to overcome when adopting the mould resistive heating 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 moiety 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 grain-size of preparation is tiny, even size distribution, and density is bigger.In a word, the present invention 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 present invention has following advantage and beneficial effect:
1, the present invention can prepare the higher large-size target of weave construction 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 size that existing sintering technology can't be realized.
2, the present invention have 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 apparatus of the present invention.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment 1
As shown in Figure 1, this target preparation facilities comprises sintering body of heater 1, compound heating mould, pressurizing device and heating unit, and the inner chamber 2 of described 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; Described compound heating mould is provided with inner chamber 9, and processed target powder places in the inner chamber 9 of compound heating mould; Described pressurizing device is connected with compound heating mould, and heating unit is connected with compound heating mould, pressurizing device respectively.
Described 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 described mould to be the insulation mould; The inner chamber 9 of described compound heating mould is the inner chamber of insulation mould 7; Described pressurizing device is connected with insulation mould 7, and described conductive die 6 is connected with heating unit.
Described pressurizing device comprises pressure control device 5, transformation electrode 12, pressure head electrode 10 and pressure head 8, described pressure control device 5 and transformation electrode 12 are connected by lead, be connected by 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 described 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 described processed target powder; Described pressure head electrode 10 is connected with heating unit.
Described insulation mould 7, conductive die 6 are rectangular mould; Described non-conductive plate 11, pressure head electrode 10 all place in the inner chamber 2 of sintering body of heater 1, and described 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 described transformation electrode 12 passes sintering body of heater 1 is connected with non-conductive plate 11, and described 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 described heating unit 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 by being added in pressure head electrode 10 on the target powder again, obtain the target of desired density and weave construction.Be specially: described heating unit comprises mold heated power supply 3 and target heating power supply 4, and described mold heated power supply 3 is connected with conductive die 6 by lead, and described target heating power supply 4 is connected with pressure head electrode 10 by lead.
Described mold heated power supply is a direct supply; Described target heating power supply is a direct supply.
Described insulation mould 7 is the good and resistant to elevated temperatures insulating material of thermal conductivity, is the mould of being made by aluminum oxide.
Described conductive die 6 is good conductivity, resistant to elevated temperatures high-strength material, is the mould of being made by graphite.
Target working method by above-mentioned target preparation facilities is realized comprises the steps:
(1) pre-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 median size is Cu (copper) powder, the Ga powder of 0.5～30 μ m, in required ratio weighing, in rare gas element (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 galvanic current is passed through conductive die 6, the target raw material powder to pre-compacted under certain atmosphere preheats sintering, carries out the galvanic 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 normal atmosphere;
(3) preheat sintering: begin to preheat, be warming up to 403 ℃ by 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 tightness, 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 the target powder is added hot-work to pressure head electrode, pressure head input dc power stream; Wherein galvanic current density size is 1.5A/mm
2; In current flow heats, pressurizing device applies transformation power to the target powder, 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% periodical change (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 finished 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 constitutional featuress with embodiment 1: the mould of described insulation mould 7 for making by titanium nitride.The mould of described conductive die 6 for making by tungsten.
Described mold heated power supply is a direct supply; Described target heating power supply is the pulse power.
Target working method by above-mentioned target preparation facilities is realized comprises the steps:
(1) pre-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 median size is titanium valve, the aluminium powder of 0.5～30 μ m, at rare gas element (Ar gas) protection ball milling 6 hours down, after mixing under rare gas element (He gas) protection, it is positioned in 800mm * 580mm rectangle high strength, the high temperature resistant and mould 7 that insulate;
Adopt earlier galvanic current by conductive die 6, the target raw material powder to pre-compacted under certain atmosphere preheats sintering, carries out pulse electric current sintering again, as step (2)～(5):
(2) pre-compacted: pre-compacted also is evacuated to 3.2 * 10
-4Pa feeds helium, and pressure becomes four normal atmosphere;
(3) preheat sintering: begin to preheat, be warming up to 1000 ℃ by the powder of die coat heating power supply device output DC stream to compacting;
(4) carry out pulsed 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 tightness, start the target heating power supply, the target heating power supply is connected pressure head electrode and pressure head, and, make pulsed current flow through the target powder, thereby the target powder is added hot-work 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, pressurizing 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 described transformation power was on the basis of 50MPa, and the amplitude of carrying out is 20% periodical change (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 ℃, processing is finished 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 constitutional featuress with embodiment 2: pressure becomes 10 normal atmosphere after feeding gas in the described step (3), in the described 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 pulsed current heat-agglomerating, pressurizing device applies the transformation power that increases progressively to the target powder, and after transformation power reached 700MPa, the size of described transformation power amplitude with 20% on the basis of 700Mpa fluctuated, and frequency is 200Hz;
In the described 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 finished, treat that temperature reduces to 50 ℃ of dischargings again.
Embodiment 4
Present embodiment except that following characteristics other constitutional featuress with embodiment 2: in the described 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 pulsed current heat-agglomerating, pressurizing device applies the transformation power that increases progressively to the target powder, and after transformation power reached 5MPa, the size of described transformation power amplitude with 15% on the basis of 5Mpa fluctuated, and frequency is 0.01Hz;
In the described 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 finished, treat that temperature reduces to 50 ℃ of dischargings again.
Embodiment 5
Present embodiment except that following characteristics other constitutional featuress with embodiment 1: the mould of described insulation mould 7 for making by aluminium nitride.The mould of described conductive die 6 for making by nichrome.
Target working method by above-mentioned target preparation facilities is realized comprises the steps:
(1) pre-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 median size is Ni powder, the Al powder of 10～30 μ m, in required ratio weighing, in rare gas element (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 galvanic current by conductive die 6, the target raw material powder to pre-compacted under certain atmosphere preheats sintering, carries out the galvanic current sintering again, as step (2)～(5):
(2) pre-compacted: pre-compacted also is evacuated to 3.5 * 10
-4Pa feeds argon gas, and pressure becomes three normal atmosphere;
(3) preheat sintering: begin to preheat, be warming up to 800 ℃ by 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 reaches the pre-sintering temperature value (temperature value of low 1667 ℃ of the boiling point of minimum fusing point composition in than target powder, promptly 800 ℃) time, the target powder is insulation 10min earlier, restart the target heating power supply and carry out galvanic current heat-agglomerating, keep original vacuum tightness, the target heating power supply is connected pressure head electrode and pressure head, and to pressure head electrode, pressure head received current, make electric current flow through the target powder, thereby the target powder is added hot-work; Wherein, galvanic current density size is 1.7A/mm
2When carrying out galvanic current heat-agglomerating, pressurizing device applies the transformation power that increases progressively to the target powder again, transformation power is pressurized to 60MPa continuously from 40MPa therebetween, and when transformation power reached 60MPa, the size of transformation power was on the 60MPa basis, the amplitude of carrying out is 15% periodical change (fluctuating), be 9MPa, frequency is 200Hz, and circulation transformation scope is in 51MPa～69MPa, frequency is 200Hz, closes DC heating subsequently;
(5) reach the sintering temperature value (temperature value of low 145 ℃ of the fusing point of peak melting point composition in than target powder when the temperature of target powder, promptly 1310 ℃) time, 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 constitutional featuress with embodiment 1: the serve as reasons mould of Mo Lai one-tenth made of stones of described insulation mould 7.The mould of described conductive die 6 for making by stainless steel.Described mold heated power supply is an AC power.
Embodiment 7
Present embodiment except that following characteristics other constitutional featuress with embodiment 1: described insulation mould 7 mould that quartz is made of serving as reasons.
In the described 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;
Described galvanic current density size is 40A/mm
2When carrying out galvanic current heat-agglomerating, pressurizing device applies the transformation power that increases progressively to the target powder again, and when transformation power reached 700Mpa, the size of described 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 constitutional featuress with embodiment 1: the mould of described insulation mould 7 for making by titanium oxide.
In the described 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;
Described galvanic current density size is 0.0003A/mm
2, its voltage swing is 1V; When carrying out galvanic current heat-agglomerating, pressurizing device applies the transformation power that increases progressively to the target powder again, and when transformation power reached 5Mpa, the size of described transformation power amplitude with 1% on the basis of 5Mpa fluctuated, and frequency is 0.01Hz;
Described 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 described 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 described 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 finished, treat that temperature reduces to 20 ℃ of dischargings again.
Embodiment 9
With fusing point is that 1565 ℃ indium trioxide 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 median size is the In of 10～30 μ m
2O
3Powder, SnO
2Powder in required ratio weighing, in rare gas element (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 galvanic current is passed through conductive die, the target raw material powder to pre-compacted under certain atmosphere preheats sintering, and carry out the galvanic current sintering again: pre-compacted also is evacuated to 3.5 * 10
-4Pa feeds helium, and pressure becomes two normal atmosphere, begin to preheat by 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 tightness, carry out the heating of sample galvanic current again, wherein galvanic current density size is 0.9A/mm
2, be warming up to 1500 ℃, insulation 8min, pressure is pressurized to 60MPa continuously from 40MPa therebetween, is on the 60MPa basis at pressure simultaneously, and the amplitude of carrying out is 15% periodical change, be 9MPa, frequency is 200Hz, and circulation transformation scope is in 51MPa～69MPa, frequency is 200Hz, close DC heating subsequently, 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 1336 ℃; boiling point is 3023 ℃ a terbium powder (purity 〉=99.5%); fusing point is 1535 ℃; boiling point is that 2750 ℃ iron powder (purity 〉=99.5%) fusing point is 1495 ℃; boiling point is 2870 ℃ a cobalt powder; fusing point is 1660 ℃; boiling point is that 3287 ℃ titanium valve is a raw material powder; preparation Tb-Fe-Co/Ti complex gradient magneto-optic target is the Tb powder of 10～30 μ m with median size; the Fe powder; the Co powder; in required ratio weighing; after ball milling mixed in 6 hours under rare gas element (Ar gas) protection, it is positioned over 800mm * 580mm rectangle high strength; high temperature resistant and the insulation mould in.Adopt earlier galvanic current is passed through conductive die, the target raw material powder to pre-compacted under certain atmosphere preheats sintering, and carry out the galvanic current sintering again: pre-compacted also is evacuated to 3.5 * 10
-4Pa feeds helium, and pressure becomes two normal atmosphere, begin to preheat by 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 tightness, carry out the heating of sample galvanic current again, wherein galvanic current density size is 0.8A/mm
2Be 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% periodical change, i.e. 9MPa, and frequency is 200Hz, circulation transformation scope is in 51MPa～69MPa, frequency is 200Hz, closes DC heating subsequently, and temperature drops to 800 ℃, the beginning pressure release, temperature is reduced to 80 ℃, after the discharging processing, and fragmentation, and mistake 400 mesh sieves (aperture is 38 μ m), obtain needed magneto-optic target raw material powder, after this target powder and titanium valve are mixed, be positioned over 800mm * 580mm rectangle high strength, high temperature resistant and the insulation mould in, adopt and earlier galvanic current is passed through conductive die, target raw material powder to pre-compacted under certain atmosphere preheats sintering, carries out the galvanic current sintering again, and pre-compacted also is evacuated to 3.5 * 10
-4Pa feeds helium, and pressure becomes a normal atmosphere, begins to preheat by 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 tightness, carry out the heating of sample galvanic current again, wherein galvanic current density size is 1.1A/mm
2, be warming up to 1600 ℃, insulation 8min, pressure is pressurized to 60MPa continuously from 40MPa therebetween, is on the 60MPa basis at pressure simultaneously, and the amplitude of carrying out is 15% periodical change, be 9MPa, frequency is 200Hz, and circulation transformation scope is in 51MPa～69MPa, frequency is 200Hz, close DC heating subsequently, 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 working method by the target preparation facilities is realized comprises the steps:
(1) pre-treatment: under the protection of rare gas element, adopt ball mill that processed target powder is carried out ball milling, treat that described target powder mixes evenly after, it is positioned in the inner chamber of the mould that insulate;
(2) pre-compacted: pressurizing device is exerted pressure to the target powder by pressure head, so that the target powder is by pre-compacted; Then, extract the intravital vacuum of sintering oven, preheat the agglomerating pressure values so that the intravital pressure of sintering oven reaches by pressurizing device;
(3) preheat sintering: start the mold heated power supply, mold heated power connection conductive die, and to the conductive die input current signal; Under the effect of current signal, conductive die, insulation mould, processed target powder are realized thermal 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 received current, make electric current flow through the target powder, thereby the target powder is added hot-work; In current flow heats, pressurizing 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,, finish the processing of target cooling of target powder and pressure release.
Described 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 described sintering temperature value is to hang down 1000 ℃ temperature value than the fusing point of a target powder peak melting point composition;
In the described step (5), close the target heating power supply after, treat that the target powder drops to 1000 ℃, begins pressure release again; After pressure release is finished, treat that temperature reduces to 50 ℃ of dischargings again.
Embodiment 12
Present embodiment except that following characteristics other features with embodiment 11: described 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 described 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 described 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 finished, treat that temperature reduces to 20 ℃ of dischargings again.
Embodiment 13
Present embodiment except that following characteristics other features with embodiment 1: described mold heated power supply is an AC power, and described target heating power supply is a direct supply.
Embodiment 14
Present embodiment except that following characteristics other features with embodiment 1: described mold heated power supply is the pulse power, and described target heating power supply is the pulse power.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. target preparation facilities, it is characterized in that: comprise sintering body of heater, compound heating mould, pressurizing device and heating unit, the inner chamber of described sintering body of heater is vacuum or atmosphere protection cavity, and compound heating mould places in the inner chamber of sintering body of heater; Described compound heating mould is provided with inner chamber, and processed target powder places in the inner chamber of compound heating mould; Described pressurizing device is connected with compound heating mould, and heating unit is connected with compound heating mould, pressurizing device respectively.
2. target preparation facilities according to claim 1 is characterized in that: described 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 described mould; The inner chamber of described compound heating mould is the inner chamber of insulation mould; Described pressurizing device is connected with the insulation mould, and described conductive die is connected with heating unit.
3. target preparation facilities according to claim 2, it is characterized in that: described pressurizing device comprises pressure control device, transformation electrode, pressure head electrode and pressure head, described pressure control device is connected by lead with the transformation electrode, be connected by 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 described pressure head stretch into the insulation mould inner chamber and with the insulation mould inner chamber be connected, to contact described processed target powder; Described pressure head electrode is connected with heating unit.
4. target preparation facilities according to claim 3, it is characterized in that: described non-conductive plate, pressure head electrode all place in the inner chamber of sintering body of heater, and described 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 described transformation electrode passes the sintering body of heater is connected with non-conductive plate, and described 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: described heating unit comprises mold heated power supply and target heating power supply, described mold heated power supply is connected with conductive die by lead, and described target heating power supply is connected with the pressure head electrode by lead.
6. target preparation facilities according to claim 5 is characterized in that: described mold heated power supply is direct supply, AC power or the pulse power; Described target heating power supply is direct supply, AC power or the pulse power.
7. target preparation facilities according to claim 2 is characterized in that: described insulation mould is by a kind of or some kinds of moulds that material is made in aluminum 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 described conductive die for being made by graphite, molybdenum, molybdenum alloy, tungsten, tungstenalloy, nichrome or stainless steel.
9. the target working method that is realized by the described target preparation facilities of claim 5 is characterized in that, comprises the steps:
(1) pre-treatment: under the protection of vacuum or rare gas element, adopt ball mill that processed target powder is carried out ball milling, treat that described target powder mixes evenly after, it is positioned in the inner chamber of the mould that insulate;
(2) pre-compacted: pressurizing device is exerted pressure by pressure head target powder in described mould, so that the target powder is by pre-compacted; Extract the intravital vacuum of sintering oven simultaneously or feed protective atmosphere, and the intravital pressure of sintering oven is reached preheat the agglomerating pressure values;
(3) preheat sintering: start the mold heated power supply, mold heated power connection conductive die, and to the conductive die received current; Under the effect of electric current, conductive die, insulation mould, processed target powder are realized thermal conduction successively, and then realize the sintering that preheats of target powder;
(4) current flow heats target sintering: after the temperature of target powder reaches default pre-sintering temperature value and is incubated the time that reaches default, 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 received current, make electric current flow through the target powder, thereby the target powder is heated; In current flow heats, pressurizing device applies transformation power to the target powder;
(5) after the temperature of target powder reaches the sintering temperature value and is incubated the time that reaches default, then close the target heating power supply, stop the current flow heats sintering,, finish the processing of target cooling of target powder and pressure release.
10. target working method according to claim 9 is characterized in that: in the described step (2), to the inner chamber extracting vacuum of sintering body of heater, making its internal pressure is 3.2 * 10 earlier
-4Pa～5 * 10
-4Behind the Pa, feed shielding gas again, preheat the agglomerating pressure values so that the sintering oven intracoelomic cavity reaches;
In the described 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 described step (4), if adopt galvanic current heat-agglomerating, then described galvanic current density size is 0.0003～40A/mm
2, its voltage swing is 1～700V; When carrying out galvanic current heat-agglomerating, pressurizing device applies the transformation power that increases progressively to the target powder, when transformation power reaches 5MPa～700Mpa, pressurizing device applies the transformation power that size fluctuates with 0～40% amplitude to the target powder on the basis of 5MPa～700Mpa, frequency is 0.01Hz～200Hz;
If adopt pulsed current heat-agglomerating, then the peak value of pulse current density is 0.003～40A/mm
2, base value is 0～20A/mm
2, frequency is 55～500Hz, dutycycle is 57%～89%; When carrying out pulsed current heat-agglomerating, pressurizing device applies the transformation power that increases progressively to the target powder, after transformation power reaches 5MPa～700MPa, pressurizing 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 described step (4) is than low 10～2000 ℃ of the boiling point of minimum fusing point composition in the target powder, and the sintering temperature value in the described step (5) be to hang down 10～1000 ℃ temperature value than the fusing point of peak melting point composition in the target powder;
In the described 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 finished, treat that temperature reduces to 20 ℃～80 ℃ dischargings again.
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Denomination of invention: Target preparation device and target processing method thereof Effective date of registration: 20190429 Granted publication date: 20130612 Pledgee: Guangdong Nanhai Rural Commercial Bank branch branch of Limited by Share Ltd Pledgor: Foshan City Jushitai Powder Metallurgy Co., Ltd. Registration number: 2019440000168 |