CN102260802B - Target preparation device and target processing method thereof - Google Patents
Target preparation device and target processing method thereof Download PDFInfo
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- CN102260802B CN102260802B CN 201110203248 CN201110203248A CN102260802B CN 102260802 B CN102260802 B CN 102260802B CN 201110203248 CN201110203248 CN 201110203248 CN 201110203248 A CN201110203248 A CN 201110203248A CN 102260802 B CN102260802 B CN 102260802B
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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 preparation of target materials technical field, particularly a kind of preparation of target materials device and target processing method thereof, can be used for powder sintered preparation large scale, high density, high-melting-point, alloy target material that constituent element fusing point difference is larger.
Background technology
Sputtering method is to prepare the more efficient method of film, but the composition proportion of target used, heterogeneous microstructure and uniformity, purity, density, and target size etc. performance and the plated film efficiency of the film of last formation is had to very important impact.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, as the basic demand of the industries such as display and solar film battery.This has higher requirement also to traditional target technology for producing and equipment.Current, it is powder sintered producing the method that target is commonly used, comprises hot pressed sintering, HIP sintering, microwave sintering, electric current sintering, discharge plasma sintering etc.
Publication number is CN1352375A, disclosing resistive heating device in the Chinese invention patent that application number is 00131150.6 " electric resistor heating type super high temperature vacuum sintering furnace " utilizes two poles to enter the sintering road by the outer heavy-current bus-bars of stove and metal water-cooling electrode, the transition electrode of making via the carbon-graphite material again is connected on the heater grillage, the circuit system of complete, in resistive heating device, the heater grillage adopts the upper and lower heater series connection of a side, the circuit structure of both sides parallel connection, this structural design can be born 2,000 degree above high temperature stable work, but utilize the resistance indirect, certainly will cause a large amount of losses of heat in conductive process.Simultaneously, because heat is to rely on the heat conduction to be passed to sample interior from outside, cause in sample and have thermograde, easily cause the inhomogeneous of target center part and outer portion of tissue structure when the sintering large-size target.This equipment also can't solve the sintering between the constituent element that the fusing point difference is large in addition.
The United States Patent (USP) that publication number is US005234487A discloses by hot isostatic pressing method and has prepared the W/Ti target material, 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 requirement, sintering time needs 2 hours simultaneously, manufacturing cycle is long, easily causes growing up of grain structure.This method also can't solve the sintering between the constituent element that the fusing point difference is large in addition.
Publication number is CN1302707A, and the Chinese invention patent that application number is 01107084.6 " plasma technology for activating sintered material ", disclose plasma technology for activating sintered material; Publication number is CN1676251A, and the Chinese invention patent application that application number is 200510052092.9 discloses a kind of method of nano aluminium oxide plasma sintering.Above two kinds of methods are all to adopt in pressurization, apply pulse voltage and produce plasma, 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, suppressed the activation of grain growth and particle surface, make the performance of agglomerated material obtain raising in essence.But due to the plasma produced along with the difference of composition, electric property, mechanical property, powder shape and the size etc. of powder difference, the resistance heating efficiency difference that causes the heterogeneity powder, finally cause the inhomogeneous of institutional framework and composition, so the plasma agglomeration method generally is only suitable for single constituent element powder or has the sintering of same alloy composition powder; Nor the sintering of applicable large scale sample.If the prolongation sintering time, easily cause grain growth; When the sintering large-size target, due to large cross section, required electric current is large simultaneously, and high to power-supply device and grid power requirement, this method also can't solve the sintering between the constituent element that the fusing point difference is large in addition.
The U.S. Patent Application Publication that publication number is US005896553A prepare single-phase by 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 large, high temperature sintering also makes grain structure easily grow up for a long time simultaneously, and this method also can't solve the sintering between the constituent element that the fusing point difference is large in addition.
Publication number is CN1911599A, the Chinese invention patent that application number is 200510017879.1 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 mould is realized hot pressed sintering under the effect of self and centrifugal medium centrifugal force, heater adopts eddy-current heating or resistance heated, this patent utilization centrifugal force is realized radially evenly hot pressed sintering, improved the uniformity 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 resistance heated, just exist heat time heating time long, the problem that cost is higher, only utilize current flow heats, just exist perpendicular to radial direction, the inhomogeneous problem of being heated.This method also only is suitable for the parts sintering with axial symmetric shape.The method does not solve the Sintering Problem between the constituent element that the fusing point difference is large simultaneously.
Publication number is CN101050121A, the Chinese invention patent that application number is 200710051776.6 discloses the dual heating mode flash sintering method of a kind of current flow heats in conjunction with radiation heating, in agglomerating plant by the current flow heats power with the radiation heating power than 30: 1-5: 1 configures radiant heating device, when the sintering diameter is greater than the sample of 30mm, adopt Fast Sintering under current flow heats and radiation heating dual heating mode, the diameter that utilizes the method can prepare the material internal even structure is greater than the sample of 30mm, and sintering time is short, energy-conservation.But this sintering method still is heated to be the master with Direct Current, during for sintering multicomponent target, due to electric property, mechanical strength, granular size and the shape difference of each component, will there be larger difference in the heating-up temperature of each component, easily cause the volatilization of the inhomogeneous and low-melting component of structure.
Publication number is CN1454736A, the Chinese invention patent application that application number is 03128621.6 discloses casting device and molten-metal supplying device, the induced-current of the metal material of utilization in accepting container heats this metal material and generation makes to stop deposite metal in accepting container to be used in the eddy-current heating coil in Shang magnetic field, this deposite metal from the masterpiece spilt between opening and lid, 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, easily cause first vaporing away of low melting point constituent element, cause the change of final target composition.
The people such as Chen Jianjun disclose the large and more crisp preparation that has the target that preparation is difficult of material self due to component fusing point difference such as ITO target, Tb-Fe-Co/Ti composite graded magneto optical target materials 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, the preparation process more complicated.
From existing document and report, can find out, in the target sintering method, target prepared by pressure sintering, hot isostatic pressing method, compactness is relatively better, but they tend to be subject to the restriction that target requires size, microscopic appearance and low cost etc., and in while hot pressed sintering process, to the activation degree of sample, dynamic process remains further to be improved, and apparatus expensive, the process-cycle is long; Discharge plasma sintering technique has the characteristics that realize at a lower temperature the Fast Sintering dense material, can effectively suppress growing up and the volatilization of constituent element of dusty material particle, energy efficiency is high, but the general only sintering of the small size target of applicable single component powder of the method, the inhomogeneities due to electric current when the sintering large-size target easily causes the inconsistent of target different parts institutional framework; Microwave sintering has special requirement to powder property, and its process easily causes the inefficacy effect, and powder is produced to non-uniform heat flux, thereby has affected 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 center and peripheral density inconsistent.The direct current sintering, produce fuel factor by electric current, can be adapted to the large scale sintering, but can cause equally the inhomogeneous and grain growth of phase constituent when sintering heterogeneity target powder.So, also there is no at present a kind of efficient, low-cost preparation method that high density, high-purity, fusing point fusing point high, constituent differ larger large-size target that can be used in.
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 preparation of target materials device of the alloy target material that the fusing point difference of large scale, high-melting-point, high density and constituent is larger.
Another object of the present invention is to provide the target processing method realized by said apparatus.
For reaching above-mentioned purpose, the present invention adopts following technical scheme:
A kind of preparation of target materials device, comprise sintering body of heater, composite heating mould, pressue device and heater, and the inner chamber of described sintering body of heater is vacuum or atmosphere protection cavity, and the composite heating mould is placed in the inner chamber of sintering body of heater; Described composite heating mould is provided with inner chamber, and processed target powder is placed in the inner chamber of composite heating mould; Described pressue device is connected with the composite heating mould, and heater is connected with composite heating mould, pressue device respectively.
Described composite heating mould is to adopt the skin at the insulation mould to add a conductive die, first DC current or pulse current or alternating current are passed through to conductive die, in certain atmosphere or under vacuum condition, the target material powder to pre-compacted is preheated sintering, and control at a certain temperature, the preferential boiling point of temperature lower than the minimum fusing point constituent element in all constituent elements of controlling, make full and uniformization of low melting point composition at this temperature, it is high that this mold heated mode has energy efficiency, heat temperature raising speed is fast, temperature is controlled, device structure is simple simultaneously, and cost is low.Be specially: described composite heating mould comprises mould inner sleeve and the conductive die that is socketed in mould inner sleeve periphery, and described mould inner sleeve is the insulation mould; The inner chamber of described composite heating mould is the inner chamber of insulation mould; Described pressue device is connected with the insulation mould, and described conductive die is connected with heater.
Described pressue device refers to 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 described transformation is 5MPa～700Mpa; The pressure amplitude scope of described alternation formula transformation mode is pressure of foundation 0～40%, and frequency range is 0.01Hz～200Hz.On the basis at 50MPa pressure, carrying out range value is 30%, i.e. the cyclically-varying of 15MPa, and its frequency is 100Hz.Be specially: described pressue device comprises pressure control device, transformation electrode, pressure head electrode and pressure head, described pressure control device is connected by wire with the transformation electrode, between transformation electrode and pressure head electrode, by non-conductive plate, be connected, the pressure head electrode is connected with the pressure head one; The lower end of described pressure head is stretched into the inner chamber of insulation mould and is connected with the inner chamber of insulation mould, to contact described processed target powder; Described pressure head electrode is connected with heater.
Described insulation mould, conductive die are rectangular mould; Described non-conductive plate, pressure head electrode all are placed in the inner chamber of sintering body of heater, and described sintering body of heater, insulation mould be equipped with the punching press mouth 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; Described transformation electrode is connected with non-conductive plate through the punching press mouth of sintering body of heater, 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 heater is first to adopt heat conducting mode to heat the target powder, by being added in pressure head electrode on the target powder, adopt the current flow heats mode to carry out Fast Sintering to the target powder of presintering again, obtain the target of desired density and institutional framework.Be specially: described heater comprises mold heated power supply and target heating power supply, and described mold heated power supply is connected with conductive die by wire, and described target heating power supply is connected with the pressure head electrode by wire.
Described mold heated power supply is dc source, AC power or the pulse power, and described target heating power supply is dc source, 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, 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 described alternating current heats electric current used; The peak value of the pulse current density of described 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 materials of thermal conductivity, is preferably a kind of in aluminium oxide, Mo Laishi, quartz, titanium oxide, titanium nitride or aluminium nitride or mould that several material is made.
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, tungsten alloy, nichrome or stainless steel.
The target processing method realized by above-mentioned preparation of target materials device, comprise the steps:
(1) pretreatment: under the protection of vacuum or inert gas, adopt ball mill that processed target powder is carried out to ball milling, after described target powder mixes, it is positioned in the inner chamber of insulation mould;
(2) pre-compacted: pressue device is exerted pressure to target powder in described mould by pressure head, 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 to the conductive die 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 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 input current, make electric current flow through the target powder, thereby the target powder is added to hot-working, and simultaneously, pressue device applies pressure changeable to the target powder;
(5) when the temperature of target powder reaches the sintering temperature value, complete the current flow heats sintering, close the target heating power supply, stop the current flow heats sintering, to the cooling of target powder pressure release, complete the processing of target.
In described step (2), first to the inner chamber extracting vacuum of sintering body of heater, so that its internal pressure is 3.2 * 10
-4pa～5 * 10
-4after Pa, then pass into gas (preferably helium, argon gas), so that its pressure becomes 1～10 atmospheric pressure, make the sintering furnace intracoelomic cavity reach the pressure values that preheats sintering;
In described step (4), when the temperature of the target powder after step (3) preheats reaches the pre-sintering temperature value, the target powder first is incubated 0～10h, restarts the target heating power supply and carries out the current flow heats sintering;
In described step (4), if adopt DC current heat-agglomerating, 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, 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 pressure changeable increased progressively to the target powder, when described pressure changeable reaches 5MPa～700Mpa, pressue device applies to the target powder pressure changeable that size fluctuates with 0～40% amplitude on the basis of 5MPa～700Mpa, and frequency range is 0.01Hz～200Hz;
In described step (4), if adopt the Current Heating sintering, the pressure in the sintering body of heater keeps original pressure values, and the peak value of the pulse current density of described 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 the Current Heating sintering, pressue device applies the pressure changeable increased progressively to the target powder, after pressure changeable reaches 5MPa～700MPa, pressue device applies to the target powder pressure changeable that size fluctuates with 15%～20% amplitude on the basis of 5MPa～700Mpa, and frequency is 0.01Hz～200Hz;
Pre-sintering temperature value in described step (4) is than the temperature value of low 10～2000 ℃ of the boiling point of minimum fusing point composition in target powder, and the sintering temperature value in described step (5) is than the temperature value of low 10～1000 ℃ of the fusing point of peak melting point composition in target powder;
In described step (5), after closing the target heating power supply, treat that the target powder drops to 200～100 ℃, then start pressure release; After pressure release completes, treat that temperature is down to 20 ℃～80 ℃ dischargings again.
The average grain diameter of the main component powder of described target is 1～5 μ m, and maximum particle diameter is less than 15um.
Adopt the density of the target of 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 lower than low-melting component, when preventing low-melting component volatilization, can make powder organization obtain homogenising to a certain extent and densified; Heat up while preventing the direct heated sample of electric current too fast, cause the volatilization of low melting point, atmosphere protection can, to the volatilization of low melting point, play certain effect that prevents simultaneously.When sample (target powder) Direct Current sintering subsequently, because presintering powder has had good structural homogeneity, can make the size of current at each position in whole sintered powder more consistent, guarantee large-size target powder each several part sintering uniformity; Simultaneously, owing to having adopted powder directly by the mode of current flow heats, heat time heating time is very short, has effectively avoided the volatilization of low melting point composition, also can not bring that significantly grain growth and phase constituent are inhomogeneous; Adopt first mould resistance heated on the basis of uniform temperature again to the sintered powder current flow heats, can overcome while adopting all the time the mould resistance heated heating slower, in target, the low melting point composition is volatile, the problem of easily growing up with crystal grain, also be conducive to carry out the constituent fusing point simultaneously and differ the sintering of larger target and the sintering of high-melting-point target; Added pressure changeable control, be adapted to the characteristics of various different powder particle sizes and material character, increased the exposure level between powder particle, can effectively increase density and shorten sintering time, and can reduce the wearing and tearing to mould; Whole sintering process energy consumption is lower, and the time is short, has effectively suppressed the grain growth problem, and the sample crystallite dimension of preparation is tiny, even size distribution, and density is larger.In a word, the present invention retained plasma agglomeration or electric current direct sintering method fast, characteristics that efficiency is high, avoided again being not suitable for the shortcoming of sintering large-size target, 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 institutional framework evenly controlled, purity and the higher large-size target of density, is particularly suitable for preparation containing Multiple components and large powder sintered of fusing point difference, reaches high-performance and large scale 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.
The accompanying drawing explanation
Fig. 1 is the structural representation of apparatus of the present invention.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
As shown in Figure 1, this preparation of target materials device, comprise sintering body of heater 1, composite heating mould, pressue device and heater, and the inner chamber 2 of described sintering body of heater 1 is vacuum cavity, and the composite heating mould is placed in the inner chamber 2 of sintering body of heater 1; Described composite heating mould is provided with inner chamber 9, and processed target powder is placed in the inner chamber 9 of composite heating mould; Described pressue device is connected with the composite heating mould, and heater is connected with composite heating mould, pressue device respectively.
The conductive die 6 that described composite heating mould comprises mould inner sleeve 7 and is socketed in mould inner sleeve 7 peripheries, described mould inner sleeve is the insulation mould; The inner chamber that the inner chamber 9 of described composite heating mould is insulation mould 7; Described pressue device is connected with insulation mould 7, and described conductive die 6 is connected with heater.
Described pressue device comprises pressure control device 5, transformation electrode 12, pressure head electrode 10 and pressure head 8, described pressure control device 5 is connected by wire with transformation electrode 12, between transformation electrode 12 and pressure head electrode 10, by non-conductive plate 11, be connected, pressure head electrode 10 is connected with pressure head 8 one; The lower end of described pressure head 8 is stretched into the inner chamber 9 of insulation mould 7 and is connected with the inner chamber 9 of insulation mould 7, to contact described processed target powder; Described pressure head electrode 10 is connected with heater.
Described insulation mould 7, conductive die 6 are rectangular mould; Described non-conductive plate 11, pressure head electrode 10 all are placed 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 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; Described transformation electrode 12 is connected with non-conductive plate 11 through the punching press mouth of sintering body of heater 1, 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 heater is first to adopt heat conducting mode to heat the target powder, by being added in pressure head electrode on the target powder 10, adopt the current flow heats modes to carry out Fast Sintering to the target powder of presintering again, obtain the target of desired density and institutional framework.Be specially: described heater 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 wire, and described target heating power supply 4 is connected with pressure head electrode 10 by wire.
Described mold heated power supply is dc source; Described target heating power supply is dc source.
Described insulation mould 7 is the good and resistant to elevated temperatures insulating materials of thermal conductivity, is the mould of being made by aluminium oxide.
Described conductive die 6 is good conductivity, resistant to elevated temperatures high-strength material, is the mould of being made by graphite.
The target processing method realized by above-mentioned preparation of target materials device, comprise the steps:
(1) pretreatment: Ga (gallium) powder (purity >=99.5%) that the copper powder (purity >=99.5%) that the fusing point of take is 1084 ℃, fusing point are 2403 ℃ as 29.8 ℃, boiling point is raw material powder;
Cu (copper) powder, Ga powder that the average grain diameter of take is 0.5～30 μ m, in required ratio weighing, after the lower ball milling of inert gas (Ar gas, i.e. argon gas) protection mixes in 4 hours, it is positioned in 800mm * 580mm rectangle high strength, high temperature resistant and insulation mould 7;
Adopt first DC current is passed through to conductive die 6, the target material powder to pre-compacted under certain atmosphere is preheated sintering, then carries out the DC current sintering, carries out step (2)～(5):
(2) pre-compacted: pre-compacted also is evacuated to 5 * 10
-4pa, pass into helium, and pressure becomes five atmospheric pressure;
(3) preheat sintering: start the powder to compacting by die coat heating power supply device output direct current and preheated, be warming up to 403 ℃, 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, 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, to pressure head electrode, pressure head input direct-current electric current, make electric current flow through the target powder, thereby the target powder is added to hot-working; Wherein DC current density size is 1.5A/mm
2; In current flow heats, pressue device applies pressure changeable to the target powder, pressure changeable is pressurized to 50MPa continuously from 30MPa, when the pressure changeable size reaches 50MPa, pressure changeable on the 50MPa basis, the cyclically-varying that the amplitude of carrying out is 10% (fluctuating), i.e. 5MPa, frequency is 200Hz, and the circulation variable pressure scope is in 45MPa～55MPa;
(5) when the temperature of target powder reaches sintering temperature value (in than target powder, the fusing point of peak melting point composition hangs down the temperature value of 10 ℃, 1074 ℃), insulation 8min, close subsequently DC heating, temperature drops to 200 ℃, starts pressure release, temperature is down to 80 ℃, and discharging, complete processing.
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
The present embodiment except following characteristics other architectural features with embodiment 1: the mould of described insulation mould 7 for being made by titanium nitride.The mould of described conductive die 6 for being made by tungsten.
Described mold heated power supply is dc source; Described target heating power supply is the pulse power.
The target processing method realized by above-mentioned preparation of target materials device, comprise the steps:
(1) pretreatment: the aluminium powder (purity >=99.5%) that the titanium valve (purity >=99.5%) that the fusing point of take is 1660 ℃, fusing point are 2467 ℃ as 660 ℃, boiling point is raw material powder;
Titanium valve, aluminium powder that the average grain diameter of take is 0.5～30 μ m, under inert gas (Ar gas) protection, ball milling is 6 hours, after mixing under inert gas (He gas) protection, it is positioned in 800mm * 580mm rectangle high strength, high temperature resistant and insulation mould 7;
Adopt first DC current by conductive die 6, the target material powder to pre-compacted under certain atmosphere is preheated sintering, then carries out pulse electric current sintering, as step (2)～(5):
(2) pre-compacted: pre-compacted also is evacuated to 3.2 * 10
-4pa, pass into helium, and pressure becomes four atmospheric pressure;
(3) preheat sintering: start the powder to compacting by die coat heating power supply device output DC current and preheated, be warming up to 1000 ℃;
(4) then carry out the Current Heating sintering: 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, 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, to pressure head electrode, pressure head input pulse electric current, make pulse current flow through the target powder, thereby the target powder is added to hot-working; The pulse current density amplitude is from 1A/mm
2be increased to 1.2A/mm
2, and frequency falls less to 68Hz from 89Hz, and the dutycycle perseverance is 57%; In current flow heats, pressue device applies pressure changeable to the target powder, and pressure changeable is pressurized to 50MPa continuously from 10MPa therebetween; When pressure changeable reaches 50MPa, the size of described pressure changeable on the basis of 50MPa, the cyclically-varying that the amplitude of carrying out is 20% (fluctuating), i.e. 10MPa, frequency is 100Hz, the circulation variable pressure scope, in 40MPa～60MPa, is closed sintering;
(5) when the temperature of target powder reaches sintering temperature value (in than target powder, the fusing point of peak melting point composition hangs down the temperature value of 140 ℃, 1520 ℃), be incubated 10min, temperature drops to 200 ℃ subsequently, starts pressure release, and temperature is down to 80 ℃, discharging, complete processing.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.
The present embodiment except following characteristics other architectural features with embodiment 2: after passing into gas in described step (3), pressure becomes 10 atmospheric pressure, in described step (4), when the temperature of the target powder after step (3) preheats reaches the pre-sintering temperature value, the target powder first is incubated 10h, 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 the Current Heating sintering, pressue device applies the pressure changeable increased progressively to the target powder, and after pressure changeable reaches 700MPa, the size of described pressure changeable amplitude with 20% on the basis of 700Mpa fluctuates, and frequency is 200Hz;
In described step (5), after closing the target heating power supply, treat that the target powder drops to 100 ℃, then start pressure release; After pressure release completes, treat that temperature is down to 50 ℃ of dischargings again.
Embodiment 4
The present embodiment except following characteristics other architectural features with embodiment 2: in described step (4), when the temperature of the target powder after step (3) preheats reaches the pre-sintering temperature value, the target powder first is incubated 10h, 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 the Current Heating sintering, pressue device applies the pressure changeable increased progressively to the target powder, and after pressure changeable reaches 5MPa, the size of described pressure changeable amplitude with 15% on the basis of 5Mpa fluctuates, and frequency is 0.01Hz;
In described step (5), after closing the target heating power supply, treat that the target powder drops to 150 ℃, then start pressure release; After pressure release completes, treat that temperature is down to 50 ℃ of dischargings again.
The present embodiment except following characteristics other architectural features with embodiment 1: the mould of described insulation mould 7 for being made by aluminium nitride.The mould of described conductive die 6 for being made by nichrome.
The target processing method realized by above-mentioned preparation of target materials device, comprise the steps:
(1) pretreatment: the aluminium powder (purity >=99.5%) that the fusing point of take is 2467 ℃ as 660 ℃, boiling point, the nickel powder (purity >=99.5%) that fusing point is 1455 ℃ are raw material powder;
Ni powder, Al powder that the average grain diameter of take is 10～30 μ m, in required ratio weighing, under inert gas (Ar gas) protection, after ball milling mixes in 6 hours, be positioned over it in 800mm * 580mm rectangle high strength, high temperature resistant and insulation mould 7;
Adopt first DC current by conductive die 6, the target material powder to pre-compacted under certain atmosphere is preheated sintering, then carries out the DC current sintering, as step (2)～(5):
(2) pre-compacted: pre-compacted also is evacuated to 3.5 * 10
-4pa, pass into argon gas, and pressure becomes three atmospheric pressure;
(3) preheat sintering: start the powder to compacting by die coat heating power supply device output DC current and preheated, be warming up to 800 ℃;
(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, 800 ℃) time, the target powder first is incubated 10min, 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 the target powder is added to hot-working; Wherein, DC current density size is 1.7A/mm
2; When carrying out DC current heat-agglomerating, pressue device applies to the target powder pressure changeable increased progressively again, pressure changeable is pressurized to 60MPa continuously from 40MPa therebetween, and when pressure changeable reaches 60MPa, the size of pressure changeable is on the 60MPa basis, the cyclically-varying that the amplitude of carrying out is 15% (fluctuating), be 9MPa, frequency is 200Hz, and the circulation variable pressure scope is in 51MPa～69MPa, frequency is 200Hz, closes subsequently DC heating;
(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, 1310 ℃) time, insulation 8min, close the target heating power supply, stop the current flow heats sintering, temperature drops to 200 ℃ subsequently, starts pressure release, temperature is down 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
The present embodiment except following characteristics other architectural features 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 being made by stainless steel.Described mold heated power supply is AC power.
The present embodiment except following characteristics other architectural features with embodiment 1: described insulation mould 7 mould that quartz is made of serving as reasons.
In described step (4), when the temperature of the target powder after step (3) preheats reaches the pre-sintering temperature value, the target powder first is incubated 10h, restarts the target heating power supply and carries out the current flow heats sintering;
Described galvanic current density size is 40A/mm
2; When carrying out DC current heat-agglomerating, pressue device applies to the target powder pressure changeable increased progressively again, and when pressure changeable reaches 700Mpa, the size of described pressure changeable amplitude with 0～40% on the basis of 700Mpa fluctuates, and frequency is 200Hz.
Embodiment 8
The present embodiment except following characteristics other architectural features with embodiment 1: the mould of described insulation mould 7 for being made by titanium oxide.
In described step (4), when the temperature of the target powder after step (3) preheats reaches the pre-sintering temperature value, the target powder does not need insulation, directly starts the target heating power supply and carries out the current flow heats sintering;
Described galvanic current density size is 0.0003A/mm
2, its voltage swing is 1V; When carrying out DC current heat-agglomerating, pressue device applies to the target powder pressure changeable increased progressively again, and when pressure changeable reaches 5Mpa, the size of described pressure changeable amplitude with 1% on the basis of 5Mpa fluctuates, and frequency is 0.01Hz;
Described pre-sintering temperature value is than the temperature value of low 10 ℃ of the boiling point of minimum fusing point composition in target powder, and described sintering temperature value is than the temperature value of low 10 ℃ of the fusing point of peak melting point composition in target powder;
In described step (5), after closing the target heating power supply, treat that the target powder drops to 200 ℃, then start pressure release; After pressure release completes, treat that temperature is down to 20 ℃ of dischargings again.
Embodiment 9
The putty powder (purity >=99.5%) that the indium sesquioxide powder (purity >=99.5%) that the fusing point of take is 1565 ℃, fusing point are 1800 ℃ as 1127 ℃, boiling point is raw material powder, preparation ITO target.
Take the In of average grain diameter as 10～30 μ m
2o
3powder, SnO
2powder, in required ratio weighing, under inert gas (Ar gas) protection, after ball milling mixes in 6 hours, be positioned over it in 800mm * 580mm rectangle high strength, high temperature resistant and insulation mould.Adopt first DC current is passed through to conductive die, the target material powder to pre-compacted under certain atmosphere is preheated sintering, then carries out the DC current sintering: pre-compacted also is evacuated to 3.5 * 10
-4pa, pass into helium, and pressure becomes two atmospheric pressure, starting the powder to compacting by die coat heating power supply device (being the mold heated power supply) output DC current is preheated, be warming up to 1200 degree, insulation 10min, pressure is pressurized to 30MPa continuously from 10MPa therebetween; Keep original vacuum, then carry out the heating of sample DC current, 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, at pressure, is on the 60MPa basis simultaneously, the cyclically-varying that the amplitude of carrying out is 15%, be 9MPa, frequency is 200Hz, and the circulation variable pressure scope is in 51MPa～69MPa, frequency is 200Hz, close subsequently DC heating, temperature drops to 200 ℃, starts pressure release, temperature is down to 80 ℃, discharging processing.The density of target is 7.02g/cm
3, the main particle average dimension that relative density is greater than 99%, ITO target is no more than 5 μ m.
Take fusing point as 1336 ℃, the terbium powder that boiling point is 3023 ℃ (purity >=99.5%), fusing point is 1535 ℃, the iron powder that boiling point is 2750 ℃ (purity >=99.5%) fusing point is 1495 ℃, the cobalt powder that boiling point is 2870 ℃, fusing point is 1660 ℃, the titanium valve that boiling point is 3287 ℃ is raw material powder, preparation Tb-Fe-Co/Ti composite graded magneto optical target materials be take the Tb powder of average grain diameter as 10～30 μ m, the Fe powder, the Co powder, in required ratio weighing, after under inert gas (Ar gas) protection, ball milling mixes in 6 hours, it is positioned over to 800mm * 580mm rectangle high strength, high temperature resistant and the insulation mould in.Adopt first DC current is passed through to conductive die, the target material powder to pre-compacted under certain atmosphere is preheated sintering, then carries out the DC current sintering: pre-compacted also is evacuated to 3.5 * 10
-4pa, pass into helium, and pressure becomes two atmospheric pressure, starting the powder to compacting by die coat heating power supply device (being the mold heated power supply) output DC current is preheated, be warming up to 1500 degree, insulation 10min, pressure is pressurized to 30MPa continuously from 10MPa therebetween, keep original vacuum, then carry out the heating of sample DC current, 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, at pressure, be on the 60MPa basis simultaneously, the cyclically-varying that the amplitude of carrying out is 15%, be 9MPa, frequency is 200Hz, the circulation variable pressure scope is in 51MPa～69MPa, frequency is 200Hz, close subsequently DC heating, temperature drops to 800 ℃, start pressure release, temperature is down to 80 ℃, after discharging processing, broken, and mistake 400 mesh sieves (aperture is 38 μ m), obtain needed magneto optical target materials material powder, by this target powder with after titanium valve mixes, be positioned over 800mm * 580mm rectangle high strength, high temperature resistant and the insulation mould in, adopt and first DC current is passed through to conductive die, target material powder to pre-compacted under certain atmosphere is preheated sintering, carry out again the DC current sintering, pre-compacted also is evacuated to 3.5 * 10
-4pa, pass into helium, and pressure becomes an atmospheric pressure, starts the powder to compacting by die coat heating power supply device output DC current and preheated, and is warming up to 1000 degree, insulation 10min, and pressure is pressurized to 30MPa continuously from 10MPa therebetween, keep original vacuum, then carry out the heating of sample DC current, 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, at pressure, is on the 60MPa basis simultaneously, the cyclically-varying that the amplitude of carrying out is 15%, be 9MPa, frequency is 200Hz, and the circulation variable pressure scope is in 51MPa～69MPa, frequency is 200Hz, close subsequently DC heating, temperature drops to 200 ℃, starts pressure release, temperature is down to 80 ℃, discharging processing.The density of target is for being 7.298g/cm
3, the main particle average dimension that relative density is greater than 99%, Tb-Fe-Co/Ti target is no more than 5 μ m.
Embodiment 11
The target processing method realized by the preparation of target materials device, comprise the steps:
(1) pretreatment: under the protection of inert gas, adopt ball mill that processed target powder is carried out to ball milling, after described target powder mixes, it is positioned in the inner chamber of insulation mould;
(2) pre-compacted: pressue device is exerted pressure to the target powder by pressure head, so that the target powder is by pre-compacted; Then, by pressue device, 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;
(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 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 the target powder is added to hot-working; In current flow heats, pressue device applies pressure changeable to the target powder;
(5) when the temperature of target powder reaches the sintering temperature value, close the target heating power supply, stop the current flow heats sintering, to the cooling of target powder pressure release, complete the processing of target.
Described pre-sintering temperature value is than the temperature value of low 2000 ℃ of the boiling point of minimum fusing point composition in target powder, and described sintering temperature value is than the temperature value of low 1000 ℃ of the fusing point of a target powder peak melting point composition;
In described step (5), after closing the target heating power supply, treat that the target powder drops to 1000 ℃, then start pressure release; After pressure release completes, treat that temperature is down to 50 ℃ of dischargings again.
Embodiment 12
The present embodiment except following characteristics other features with embodiment 11: described pre-sintering temperature value is than the temperature value of low 10 ℃ of the boiling point of minimum fusing point composition in target powder, and described sintering temperature value be to hang down 10 ℃ of temperature values than the fusing point of peak melting point composition in target powder;
In described step (5), after closing the target heating power supply, treat that the target powder drops to 100 ℃, then start pressure release; After pressure release completes, treat that temperature is down to 20 ℃ of dischargings again.
Embodiment 13
The present embodiment except following characteristics other features with embodiment 1: described mold heated power supply is AC power, and described target heating power supply is dc source.
Embodiment 14
The present embodiment except 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.
Above-described embodiment is preferably embodiment 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 Essence of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (7)
1. a preparation of target materials device, it is characterized in that: comprise sintering body of heater, composite heating mould, pressue device and heater, the inner chamber of described sintering body of heater is vacuum or atmosphere protection cavity, and the composite heating mould is placed in the inner chamber of sintering body of heater; Described composite heating mould is provided with inner chamber, and processed target powder is placed in the inner chamber of composite heating mould; Described pressue device is connected with the composite heating mould, and heater is connected with composite heating mould, pressue device respectively;
Described composite heating mould comprises mould inner sleeve and the conductive die that is socketed in mould inner sleeve periphery, and described mould inner sleeve is the insulation mould; The inner chamber of described composite heating mould is the inner chamber of insulation mould; Described pressue device is connected with the insulation mould, and described conductive die is connected with heater;
Described pressue device comprises pressure control device, transformation electrode, pressure head electrode and pressure head, and described pressure control device is connected by wire with the transformation electrode, between transformation electrode and pressure head electrode, by non-conductive plate, is connected, and the pressure head electrode is connected with the pressure head one; The lower end of described pressure head is stretched into the inner chamber of insulation mould and is connected with the inner chamber of insulation mould, to contact described processed target powder; Described pressure head electrode is connected with heater.
2. preparation of target materials device according to claim 1, it is characterized in that: described non-conductive plate, pressure head electrode all are placed in the inner chamber of sintering body of heater, and described sintering body of heater, insulation mould are equipped with the punching press mouth be communicated with its inner chamber, the punching press mouth of the punching press mouth of sintering body of heater and insulation mould is on same straight line; Described transformation electrode is connected with non-conductive plate through the punching press mouth of sintering body of heater, and described pressure head is stretched in the inner chamber of insulation mould by the punching press mouth of sintering body of heater.
3. preparation of target materials device according to claim 1, it is characterized in that: described heater comprises mold heated power supply and target heating power supply, described mold heated power supply is connected with conductive die by wire, and described target heating power supply is connected with the pressure head electrode by wire.
4. preparation of target materials device according to claim 3, it is characterized in that: described mold heated power supply is dc source, AC power or the pulse power; Described target heating power supply is dc source, AC power or the pulse power.
5. preparation of target materials device according to claim 1 is characterized in that: described insulation mould is a kind of in aluminium oxide, Mo Laishi, quartz, titanium oxide, titanium nitride or aluminium nitride or mould that several material is made.
6. preparation of target materials device according to claim 1, is characterized in that: the mould of described conductive die for being made by graphite, molybdenum, molybdenum alloy, tungsten, tungsten alloy, nichrome or stainless steel.
7. the target processing method realized by the described preparation of target materials device of claim 3, is characterized in that, comprises the steps:
(1) pretreatment: under the protection of vacuum or inert gas, adopt ball mill that processed target powder is carried out to ball milling, after described target powder mixes, it is positioned in the inner chamber of insulation mould;
(2) pre-compacted: pressue device is exerted pressure to target powder in described mould by pressure head, so that the target powder is by pre-compacted; Extract the vacuum in the sintering body of heater simultaneously, then pass into protective atmosphere, 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 to the conductive die 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: 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 input current, make electric current flow through the target powder, thereby the target powder is heated; In current flow heats, pressue device applies pressure changeable to the target powder;
(5) after the temperature of target powder reaches the sintering temperature value and is incubated the time that reaches default, close the target heating power supply, stop the current flow heats sintering, to the cooling of target powder pressure release, complete the processing of target;
In described step (2), first to the inner chamber extracting vacuum of sintering body of heater, making its internal pressure is 3.2 * 10
-4pa～5 * 10
-4after Pa, then pass into protective gas, so that the sintering furnace intracoelomic cavity reaches the pressure values that preheats sintering;
In described step (4), when the temperature of the target powder after step (3) preheats reaches the pre-sintering temperature value, the target powder first is incubated and was greater than for 0 time that is less than or equal to 10h, restarts the target heating power supply and carries out the current flow heats sintering;
In described step (4), if adopt DC current heat-agglomerating, described galvanic current density size is 0.0003～40A/mm
2, its voltage swing is 1～700V; When carrying out DC current heat-agglomerating, pressue device applies the pressure changeable increased progressively to the target powder, when pressure changeable reaches 5MPa～700Mpa, pressue device applies size to the target powder and be less than or equal to be greater than 0 the pressure changeable that 40% amplitude fluctuates on the basis of 5MPa～700Mpa, and frequency is 0.01Hz～200Hz;
If adopt the Current Heating sintering, 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 the Current Heating sintering, pressue device applies the pressure changeable increased progressively to the target powder, after pressure changeable reaches 5MPa～700MPa, pressue device applies to the target powder pressure changeable that size fluctuates with 15%～20% amplitude on the basis of 5MPa～700Mpa, and frequency is 0.01Hz～200Hz;
Pre-sintering temperature value in described step (4) is than low 10～2000 ℃ of the boiling point of minimum fusing point composition in target powder, and the sintering temperature value in described step (5) is than the temperature value of low 10～1000 ℃ of the fusing point of peak melting point composition in target powder;
In described step (5), after closing the target heating power supply, treat that the target powder drops to 200 ℃～100 ℃, then start pressure release; After pressure release completes, treat that temperature is down 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 |
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