CN103787651A - Manufacturing method of indium-tin oxide target material - Google Patents
Manufacturing method of indium-tin oxide target material Download PDFInfo
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- CN103787651A CN103787651A CN201210426065.3A CN201210426065A CN103787651A CN 103787651 A CN103787651 A CN 103787651A CN 201210426065 A CN201210426065 A CN 201210426065A CN 103787651 A CN103787651 A CN 103787651A
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Abstract
The invention discloses a manufacturing method of an indium-tin oxide target material. The manufacturing method comprises the following steps of providing ITO powder, carrying out pre-pressing molding on the ITO powder by a static pressing technology to obtain a first ITO target blank material, putting the first ITO target blank material into a first sheath, carrying out vacuum-pumping, carrying out treatment on the first ITO target blank material in the first sheath by a cold isostatic pressing technology to obtain a second ITO target blank material, after removing the first sheath, putting the second ITO target blank material into a second sheath, carrying out vacuum-pumping, carrying out treatment on the second ITO target blank material in the second sheath by a hot isostatic pressing technology to obtain a third ITO target blank material, removing the second sheath, and carrying out machining on the third ITO target blank material to obtain an ITO target material. The manufacturing method solves the problem that ITO powder is not molded easily, can be decomposed easily and can be reduced so that ITO target material processing is limited. Through the manufacturing method, the ITO target material having excellent density and internal microstructure uniformity is obtained.
Description
Technical field
The present invention relates to field of semiconductor manufacture, relate in particular to the making method of a kind of indium tin oxide (ITO) target.
Background technology
ITO(indium tin oxide) film is a kind of N-shaped semiconductive ceramic film, due to its good conductivity, to visible transparent, UV-light had to absorptivity, infrared light is there is to the excellent properties such as highly reflective, thereby be widely used in the field such as optics, electricity.The most ito thin films that adopt magnetron sputtering method to prepare of existing technique, it is good that this quadrat method has technology controlling and process, quality of forming film advantages of higher and be widely used in industrial production.The prerequisite that magnetron sputtering method is prepared high quality ito thin film is the ITO target of preparation high purity, high-density, even density.
The method of conventionally manufacturing now ITO target has sintering process and pressure sintering etc., due to Indium sesquioxide and at high temperature easily decomposition of stannic oxide, and Indium sesquioxide and stannic oxide powder are lean property powder, be difficult for the limitation of the characteristics such as machine-shaping, prior art still has defect in various degree to the making of ITO target:
Sintering legal system ITO target is through colding pressing or casting forms after ITO target blank, high temperature sintering in oxidizing atmosphere by ITO powder.In pressure sintering, at high temperature (particularly temperature higher than 1200 ℃ time), ITO powder easily decomposes, and forms in the ITO sosoloid of gaseous substance from sintering state and escapes, the target forming can have a lot of gas passages and hole, has hindered the raising of ITO target density.
Hot pressing legal system ITO target is to utilize ITO powder being heated to after certain temperature, and the thermoplasticity having and mobility complete two processes of moulding and sintering in an operation simultaneously.The Chinese patent application file that a kind of method of hot pressing legal system ITO target can be 101575203 with reference to publication number.Pressure sintering is high to the requirement of strength of punching block, is generally high-purity high-strength graphite punching block, but at high temperature ITO powder is easily by graphite reduction, and is penetrated into target inside.Pressure sintering is in single shaft direction, exert pressure (for example vertical direction) simultaneously, this makes the crystal grain of powder in the time being molded into target, all directions discontinuity, makes the inner relative density of ITO target of formation inhomogeneous, is difficult to obtain the ITO target that high-quality relative density is high.
In view of this, be necessary to propose in fact a kind of making method of the ITO target that can produce high purity, high-density, even density, to fill up the deficiencies in the prior art, meet and produce and industrial needs.
Summary of the invention
The problem that the present invention solves is the homogeneity of density, internal organizational structure of the indium-tin oxide target material made of existing technique and the grain-size more and more higher sputtering technology that cannot meet the demands.
For addressing the above problem, the invention provides a kind of making method of indium-tin oxide target material, comprising:
ITO powder is provided;
Adopt static pressure technique by ITO powder pre-molding, form an ITO target blank;
The one ITO target blank is put into the first jacket and vacuumized;
Adopt isostatic cool pressing technique to process the ITO target blank in the first jacket, form the 2nd ITO target blank;
Remove after described the first jacket, the 2nd ITO target blank is put into the second jacket, and vacuumize;
Adopt heat and other static pressuring processes to process the 2nd ITO target blank in the second jacket, form the 3rd ITO target blank;
Remove after described the second jacket, described the 3rd ITO target blank is carried out to mechanical workout and form ITO target.
Optionally, the technique of described isostatic cool pressing comprises successively:
Isostatic cool pressing stove is vacuumized to processing;
In isostatic cool pressing stove, fill rare gas element or nitrogen;
The first jacket is placed in isostatic cool pressing stove, and it is 100MPa ~ 200MPa that pressure is set, and pressurize 2 hours ~ 5 hours under this pressure.
Optionally, the technological operation of described hot isostatic pressing comprises:
Hot isostatic pressing stove is vacuumized to processing;
Then in hot isostatic pressing stove, fill rare gas element or nitrogen;
Then will stop vacuumizing and the second jacket of good seal is placed in hot isostatic pressing stove, it be 800 ℃ ~ 1000 ℃ that temperature in hot isostatic pressing stove is set, and it is 90MPa ~ 130MPa that pressure is set, and under this temperature and pressure heat-insulation pressure keeping 2 hours ~ 5 hours;
Finally be cooled to below 200 ℃.
Optionally, the main component of described ITO powder is In
2o
3and SnO
2mixed powder.
Optionally, described In
2o
3and SnO
2mass ratio be 9:1.
Optionally, described ITO powder also comprises tamanori, and described tamanori is glycerine or acetone.
Optionally, described static pressure technique comprises:
By the processing of static pressure stove evacuation;
Vacuumize after processing, ito powder is put into mould, described mould is put into static pressure stove, the pressure head in described static pressure stove applies static pressure pressure to described ito powder, carries out compaction treatment and forms an ITO target blank, and described static pressure pressure is 20MPa ~ 30MPa.
Optionally, described the first jacket is carried out to first and vacuumize processing, be evacuated to vacuum tightness and be less than 10
-2pa.
Optionally, described the first jacket is rubber package set or aluminium jacket.
Optionally, described the second jacket is carbon steel jacket or stainless steel jacket, comprises jacket body and lid.
Optionally, the 2nd ITO target blank is put into after the second jacket, described the second jacket is carried out to second and vacuumize before processing, be also included in the jacket body upper cover upper cover body of the second jacket, and by the mode of argon arc welding, jacket body and lid are welded, described the second jacket is shut.
Optionally, vacuumizing of the second jacket being carried out is treated to and is evacuated to vacuum tightness in described the second jacket is 2 × 10
-3more than Pa.
Optionally, the second jacket is evacuated to 2 × 10
-3after Pa is above, carry out also comprising step before hip treatment: maintain and vacuumize 2 × 10
-3state more than Pa, is then heated to the second jacket 250 ℃ ~ 500 ℃, and is incubated 2 hours ~ 5 hours;
After insulation finishes, keep the vacuum tightness in the second jacket constant, stop vacuumizing, and simultaneously by the second jacket sealing.
Optionally, vacuumizing that described the first jacket is carried out process or described the second jacket is carried out vacuumize processing, comprise the step of shutting described the first jacket or the second jacket and therefrom drawing degassed mouthful, vacuumize processing by described degassed mouth.
Optionally, described to after the vacuumizing processing and finish of the first jacket, the degassed mouth of described the first jacket is carried out to mechanical seal.
Optionally, described mechanical seal is that degassed mouthful on described the first jacket is tightened.
Optionally, described to after the vacuumizing processing and finish of the second jacket, degassed mouthful of described the second jacket is held one's breath to realize by described the second jacket sealing.
Optionally, the method for described the second jacket of described removal is turning.
Compared with prior art, technical solution of the present invention has the following advantages:
The pre-molding of ITO powder is carried out in employing, and then carry out isostatic cool pressing and hot isostatic pressing and form ITO target blank, aforesaid method has been broken through ITO powder and has easily been decomposed, the feature such as can be reduced bring in the limitation that is processed into ITO target, make to form ITO target blank and there is good density, the homogeneity of internal organizational structure.
In isostatic cool pressing technique and heat and other static pressuring processes, can all directions, transmit by liquid or gas the ultra-high voltage of formed objects to target blank, with respect to, in the time of the fine and close equipment of other unidirectional pressurizations of application or Bidirectional-pressure, it is each to impartial pressure that isostatic cool pressing technique and heat and other static pressuring processes can provide, making target blank is consistent by the degree of densification everywhere, thereby realizes the uniform ITO target of interior tissue.
And with respect to isostatic cool pressing technique, the hot environment that heat and other static pressuring processes provides, can make the diffusion aggravation of ITO particulate, to fill up the space between ITO atom, and at high temperature, described ITO molecule can be realized recrystallize, make the crystal grain moulding of target inside and evenly.
In addition, wherein the technique design parameter of isostatic cool pressing is set to: the temperature that described isostatic cool pressing stove provides is normal temperature, and isostatic cool pressing pressure is 100Mpa ~ 200MPa, and pressurize 2 hours ~ 5 hours.After the pressure of isostatic cool pressing is applied to 200MPa, the effect of the increase to isostatic cool pressing technique can be too unobvious.And if the not enough 100MPa of isostatic cool pressing operation pressure makes the 2nd ITO target blank be difficult to realize finer and close.Be 100Mpa ~ 200MPa in the isostatic cool pressing pressure range applying, if the time of the maintenance of isostatic cool pressing pressure is less than 2 hours, the 2nd ITO target blank is good not by the degree of densification, and the 2nd ITO target blank is inner and submarginal place, even not by the degree of densification; If the time of the maintenance of isostatic cool pressing pressure is greater than 5 hours, the 2nd ITO target blank is not too significantly changed by the degree of densification and homogeneity, easily causes process costs waste.
Described heat and other static pressuring processes design parameter is, it is 800 ℃ to 1000 ℃ that hip temperature is set, and applying argon gas or nitrogen in hot isostatic pressing stove keep the environmental stress 90Mpa to 130Mpa at jacket place, and be incubated 2 hours under this temperature pressure ~ 5 hour.Cool to afterwards 200 ℃ with the furnace.If wherein hip temperature is too high, not only waste fuel, very uneconomical, but also the crystal grain that can impel the ITO target crystallization of follow-up formation to form is excessive, the performance of follow-up ITO target is worsened.And particularly in temperature during higher than 1200 ℃, the ito powder in ITO target easily decomposes, and forms in the ITO sosoloid of gaseous substance from sintering state and escapes, the target of formation can have a lot of gas passages and hole, has hindered the raising of ITO target density.And if hip temperature is too low, the 3rd ITO target blank is difficult to produce moulding distortion and forms ITO target.After the pressure of hot isostatic pressing is applied to 130MPa, the effect of the increase to isostatic cool pressing technique can be too unobvious.And if the not enough 90MPa of isostatic cool pressing operation pressure makes the 3rd ITO target blank be difficult to realize finer and close.If the time of the maintenance of hot isostatic pressing pressure is less than 2 hours, the 3rd ITO target blank is good not by the degree of densification, and the 3rd ITO target blank is inner and submarginal place, even not by the degree of densification; If the time of the maintenance of hot isostatic pressing pressure is greater than 5 hours, the 3rd ITO target blank is not too significantly changed by the degree of densification and homogeneity, easily causes process costs waste.
And, in embodiment provided by the invention, first make the density of the 2nd ITO target blank reach 70% by isostatic cool pressing, be based upon on such basis, follow-up hot isostatic pressing can be realized the complete densification of the 3rd ITO target blank, forms density and is at least more than 99% ITO alloy target material.Contriver repeatedly puts into practice discovery, if without isostatic cool pressing technique, and directly carries out an ITO target to carry out heat and other static pressuring processes, can not make the ITO target forming meet the requirements.If carry out isostatic cool pressing technique and first carry out heat and other static pressuring processes, the effect of the further densification of the ITO target blank of described isostatic cool pressing after to hip treatment is not too remarkable again, can not make the final ITO target forming meet the requirements.Through the repeatedly summary of practice and experience, carry out again heat and other static pressuring processes to first carrying out isostatic cool pressing technique in making employing the present invention of ITO target, and in conjunction with the method for the parameter providing in the present embodiment, be the most effectively, the method for the minimizing process costs waste of saving processing step most and trying one's best few.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of manufacturing ITO target in the embodiment of the present invention;
Fig. 2 to Fig. 3 is the schematic diagram that in the embodiment of the present invention, ITO powder is carried out to pre-molding formation the one ITO target blank;
Fig. 4 to Fig. 5 adopts isostatic cool pressing technique to form the schematic diagram of the 2nd ITO target blank the one ITO target blank in the embodiment of the present invention;
Fig. 6 is the schematic diagram of the second jacket of use while the 2nd ITO target blank being carried out to heat and other static pressuring processes in the embodiment of the present invention.
Embodiment
Contriver's discovery, the powder of preparation ITO target is mainly the mixture of Indium sesquioxide and stannic oxide, and the two kinds of lean property of oxide powder powders, are difficult for machine-shaping, and the in the situation that of high temperature, also easily decompose, and be easily reduced.Due to these characteristics, make the very difficult of ITO target that preparation quality is good.And the sintering process using in existing technique or pressure sintering are prepared the problem that characteristic that ITO target all can not comprehensively solve ITO powder is brought.
Given this, contriver proposes mainly to prepare ITO target in the mode of isostatic cool pressing and hot isostatic pressing combination.Because isostatic cool pressing and hot isostatic pressing can provide each to impartial pressure, making target blank is consistent by the degree of densification everywhere, thereby realizes the uniform ITO target of interior tissue.
And hot isostatic pressing has each advantage to isobaric and hot pressing concurrently, on the basis that can process in isostatic cool pressing technique above etc., further densification ITO target blank, makes the ITO target of formation realize densification completely.Thereby the ITO target of the high purity of making, high-density, even density, to meet the needs of magnetron sputtering method of high request.
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.
Below by specific embodiment, technical scheme of the present invention is carried out to clear, complete description.
As shown in Figure 1, in the present embodiment, the step that forms ITO target of the present invention comprises:
Step S11, provides ITO powder;
Step S12, puts into punching block by ITO powder, carries out pre-molding and forms an ITO target blank;
Step S13, puts into the first jacket by an ITO target blank, and described the first jacket is carried out to first vacuumizes processing, is evacuated to vacuum tightness and is less than 10
-2pa, seals described the first jacket;
Step S14, carries out isostatic cool pressing technique to described the first jacket, and an ITO target blank is formed to the 2nd ITO target blank, removes described the first jacket;
Step S15, puts into the second jacket by the 2nd ITO target blank, and described the second jacket is carried out to second vacuumizes processing, and being evacuated to vacuum tightness in described the second jacket is 2 × 10
-3more than Pa, maintain the state of vacuumizing, then the second jacket is heated to 250 ℃ ~ 500 ℃, and is incubated 2 hours ~ 3 hours;
Step S16, carries out heat and other static pressuring processes to described the second jacket, and described the 2nd ITO target blank is formed to the 3rd ITO target blank;
Step S17, removes described the second jacket, described the 3rd ITO target blank is carried out to mechanical workout and form ITO target.
Concrete, its technological process is as follows:
First, in conjunction with reference to figure 1, perform step S11, ITO powder is provided;
In the present embodiment, described ITO powder is that main component is In
2o
3and SnO
2mixed powder, described In
2o
3and SnO
2mass ratio be 9:1.In order to make the uniform ITO target of density distribution, two kinds of powder need to mix fully.Be more than or equal to 90% ITO target in order to make purity, the purity of described ITO powder is more than or equal to 90%.In order to make the ITO target that compactness is good, described powder diameter is the smaller the better.And, in order to increase the stickiness between powder, can in powder, sneak into glycerine or acetone and other organic solvent as tamanori.
Then, in conjunction with reference to figure 1, perform step S12, ITO powder is put into punching block, carry out pre-molding and form an ITO target blank;
Fig. 2 is the schematic diagram that ito powder is carried out to the technique of pre-molding of the embodiment of the present invention; Fig. 3 is the schematic diagram of the ITO target blank that forms after the technique of pre-molding of the embodiment of the present invention.Please refer to Fig. 2, ito powder 20 is put into punching block 23, then punching block 23 is put into static pressure machine 21, in static pressure machine 21, be provided with pressure head 22, in the time that pressure head 22 moves down, make ito powder 20 in punching block 23 be under pressure to be compacted to form an ITO target blank 24.
Applied pressure in the present embodiment is 20MPa ~ 30MPa, and pressure head 22 is 20MPa ~ 30MPa to ito powder 20 applied pressures in punching block 23, and the process of exerting pressure is single axial pressure.In this step, pressure is too little, little when the not enough 20MPa, can make ito powder 20 be difficult to moulding.When pressure is greater than after 20MPa, the pressure of employing is larger, and ito powder can more easily be pressed into bulk, and powder wherein can be pressed closelyr, makes the quality of target of follow-up formation finer and close; Easily cause breaking of punching block 23 and cross conference when the pressure adopting.In the present embodiment, put into practice discovery through contriver, when pressure does not exceed 30MPa, can maintain punching block 23 and be not easy to break.
The shape of the ITO target that wherein, the shape of described punching block 23 and expectation form adapts.The surface shape of ITO target can be circular, square etc., and corresponding, described punching block is cylindrical or square column type.In the present embodiment, described punching block is cylinder shape, this step complete after an ITO target blank of formation also for cylinder shape.
The method of the pre-molding of this step can have two kinds: the first, for once all ITO powders being put into punching block, completes by a precompressed; The second, for putting into several times ITO powder, is pressed when putting at every turn.In these two kinds of modes: first kind of way need once all ITO powders to compacting, need to impose severe pressure quickly, the pressure that punching block 23 bears is larger, easily causes breaking of punching block 23.Need to select to there is the punching block compared with hard intensity; And in the second way, because ITO powder is that gradation is put into, when each compacting, needing the applied pressure can be less, the pressure that punching block 23 need to bear is less.But repeatedly put into and repeatedly compacting meeting bring repeated pollution, the purity of ITO target that impact forms.And in the present embodiment, described punching block 23 adopts punching block, because punching block intensity is high, it is little to be out of shape, only need filling step one time to the filling of carrying out ITO powder in punching block, can avoid the repeated pollution of ITO powder, meet the sputtering technology more and more higher to purity requirement with the purity that improves follow-up ITO target.
Then, continue in conjunction with reference to figure 1, execution step S13, puts into the first jacket by an ITO target blank, and described the first jacket is carried out to first vacuumizes processing, is evacuated to vacuum tightness and is less than 10
-2pa, seals described the first jacket;
Incorporated by reference to reference to figure 4, the one ITO target blank 24 is placed in the first jacket to 251, pack in the first jacket 251, with rope 260 fasten the first jackets 251 so that the first jacket 251 is sealed, and drawing deaeration pipe 261 from described jacket 251, this deaeration pipe 261 is connected with vaccum-pumping equipment, can vacuumize described the first jacket 251.The vacuum tightness being evacuated in described the first jacket is less than 10
-2pa.To the vacuum canning technique of holding one's breath, make that the first jacket 251 is inner forms an airtight vacuum environment.
In this step, the object vacuumizing is that the foreign gas in described the first jacket is pumped, and forms a vacuum environment in the first jacket.When vacuum tightness is less than 10
-2when Pa, can reach this object.
In this step, described in hold one's breath technique be with rope by tight deaeration pipe 12 tyings on the first jacket 251, hold one's breath after technique, the vacuum tightness of described vacuum canning is less than or equal to 10
-2pa.
Wherein, the effect of the first jacket 251 isolates the isostatic cool pressing stove in ITO powder and follow-up isostatic cool pressing technique on the one hand, prevent from mutually polluting between ITO powder and isostatic cool pressing stove, on the other hand, carry out in the process of isostatic cool pressing technique, must transmit cold isostatic pressure by the distortion of the first jacket 251, make the ITO target blank 24 can be by densification, moreover, can also prevent that an ITO target blank 24 is oxidized in air.The size of the first jacket 251 can be determined according to ITO target blank 24 sizes.The material of the first jacket 251 is selected to need to meet two conditions, and first condition is: jacket has good snappiness, otherwise jacket easily breaks; Second condition is: in conjunction with the thickness of jacket, the material of jacket can realize preferably pressure conduction, otherwise causes the densification of ITO powder inhomogeneous.
In the present embodiment, the material of the first jacket 251 is preferably used rubber, and thickness is 3mm ~ 5mm, and the first jacket is too thin, and the follow-up jacket that vacuumizes in step is easily cracked; The first jacket 251 is too thick, and in follow-up isostatic cool pressing process, the first jacket 251 is not easy to realize pressure conduction.In other embodiment, the material of the first jacket 251 is not limited to rubber, can be used as the first jacket 251 as long as meet the material of above-mentioned two conditions, and for example, the material of described the first jacket 251 can also be aluminium.Different from rubber package set is, now the formation method of aluminium jacket can be by Machine Design, for example CAD, make its shape meet the shape of the ITO target of follow-up formation, afterwards aluminium sheet is spliced, employing argon arc welding sealing, and leave deaeration pipe to aluminium jacket is vacuumized, the thickness of aluminium jacket is 2.5mm ~ 3.0mm.Vacuumizing step is by completing from the deaeration pipe of aluminium jacket.The technique of holding one's breath of described aluminium jacket is to realize by mechanical workout and welding, for example, can the afterbody of aluminium jacket deaeration pipe be pounded and flatly then be sealed with argon arc welding with iron hammer.Hold one's breath after technique, the vacuum tightness of described aluminium jacket is at least 10
-2pa.
Because the manufacture craft of aluminium jacket is than rubber package set complexity, and aluminium jacket can not can reuse as rubber package set.Combined process cost and working efficiency, preferred rubber jacket.
Then, continue, in conjunction with reference to figure 1, to perform step S14, described the first jacket is carried out to isostatic cool pressing technique, an ITO target blank is formed to the 2nd ITO target blank, remove described the first jacket;
Isostatic cool pressing (Cold Isostatic Pressing, CIP) technique is under normal temperature, sample to be pressed is placed in to high pressure vessel, utilizes the character of the incompressible character of liquid or gaseous media and even transmission of pressure from all directions, sample evenly to be pressurizeed.According to fluid mechanics principle, when liquid or gaseous media are during by pressure pump injection pressure container, the constant and Transmit evenly of its pressure size is to all directions.The pressure that now sample to be pressed in high pressure vessel is subject in all directions is uniformly with of the same size.
Set forth the principle that forms the 2nd ITO target blank in this step by isostatic cool pressing below in conjunction with the principle of isostatic cool pressing technique.As shown in Figure 5, the first jacket 251 that the one ITO target blank 24 is housed is placed in to airtight liquid or atmosphere surrounding, all directions, transmit the ultra-high voltage of formed objects to an ITO target blank 24 by liquid or gas, the one ITO target blank 24 is carried out to densification for the first time, form the 2nd finer and close ITO target blank.
In the time of the fine and close equipment of other unidirectional pressurizations of application or Bidirectional-pressure, an ITO target blank of different positions is stressed and varies in size, and compressed degree varies causes, and makes the 2nd ITO target blank interior tissue of formation inhomogeneous.And it is not by the place that directly exerts pressure, its densification degree is inadequate.And in the present embodiment, adopt the mode of isostatic cool pressing, what make that the 2nd ITO target blank in described the first jacket 251 is subject to is each to impartial cold isostatic pressure, as shown in Figure 5, wherein the arrow of four direction represent that isostatic cool pressing stove 11 produces respectively to equalization pressure.Like this, the 2nd ITO target blank is consistent by the degree of densification everywhere, thereby can obtain uniform the 2nd ITO target blank of interior tissue.And, the fine and close equipment of other the unidirectional pressurizations of corresponding use or Bidirectional-pressure, the density of the 2nd ITO target blank that the present embodiment forms can improve 5 ~ 15 times, and density is 70% left and right.
In carrying out isostatic cool pressing technique, the isostatic cool pressing pressure applying is larger, the inner ITO particle packing of the 2nd ITO target blank in the first jacket 251 can be tightr, the deflection that particle is extruded is larger, contact area between particle is also larger, and isostatic cool pressing technique makes target blank faster by fine and close speed.But find by contriver's test of many times, after the pressure of isostatic cool pressing is applied to 200MPa, the effect of the increase to isostatic cool pressing technique can be too unobvious.And if the not enough 100MPa of isostatic cool pressing operation pressure makes the 2nd ITO target blank be difficult to realize finer and close.
And the hold-time of isostatic cool pressing pressure need to maintain the sufficiently long time, such the first jacket 251 can have time enough to carry out pressure conduction, makes the 2nd ITO target blank interior tissue of follow-up formation even.Creative work through contriver is found, be 100Mpa ~ 200MPa in the isostatic cool pressing pressure range applying, if the time of the maintenance of isostatic cool pressing pressure is less than 2 hours, the 2nd ITO target blank is good not by the degree of densification, and the 2nd ITO target blank is inner and submarginal place, even not by the degree of densification; If the time of the maintenance of isostatic cool pressing pressure is greater than 5 hours, the 2nd ITO target blank is not too significantly changed by the degree of densification and homogeneity, easily causes process costs waste.
Therefore in this step, the technique design parameter of described isostatic cool pressing is set to: the temperature that described isostatic cool pressing stove 11 provides is normal temperature, the isostatic cool pressing pressure of isostatic cool pressing stove 11 is 100Mpa ~ 200MPa, and makes the first jacket 251 the interior pressurize of isostatic cool pressing stove 11 2 hours ~ 5 hours.
After isostatic cool pressing completes, remove the first jacket 251.In the present embodiment, the material of the first jacket 251 is rubber, and the method for removing the first jacket is the rope of untiing on rubber package set, directly rubber package set is peeled off to removal from the 2nd ITO target blank.
Through this step, the density of the 2nd ITO target blank forming is 70% left and right, still can not meet the demands, and need to carry out follow-up heat and other static pressuring processes to realize the further densification of described the 2nd ITO target blank.
Then, continue in conjunction with reference to figure 1, execution step S15, puts into the second jacket by the 2nd ITO target blank, and described the second jacket is carried out to second vacuumizes processing, and being evacuated to vacuum tightness in described the second jacket is 2 × 10
-3more than Pa, maintain the state of vacuumizing, then the second jacket is heated to 250 ℃ ~ 500 ℃, and is incubated 2 hours ~ 3 hours;
Wherein, described the second jacket can be by Machine Design, and for example CAD makes its shape meet the shape of target, afterwards by seamless tubular goods or sheet material through splicing formation welded together.Concrete, as shown in Figure 6, this second jacket 252 generally comprises jacket body and lid, and deaeration pipe 262 can be arranged on lid or jacket body.In the time vacuumizing processing, described deaeration pipe is connected with vaccum-pumping equipment, realizes vacuumizing in jacket.On lid, the 2nd ITO target blank is placed into after the second jacket 252, by argon arc welding, this lid is shut on this jacket body and formed complete jacket, this step also claims to shut jacket step.It should be noted that, the material of the second jacket 252 is selected to need satisfied what time following: the one, and, the fusing point of the second jacket 252 is higher than the temperature in heat-processed; The thickness of two, the second jackets 252 need to be enough thick, guarantee vacuumize and heat-processed in, weld can not split; Three, the second jackets 252 need to not can make ITO be reduced.And the inventor finds to adopt carbon steel or stainless steel, the jacket thickness that is 1.0mm ~ 2.0mm in conjunction with thickness, can realize preferably pressure conduction effect, also there will not be weld easily to split, and causes the phenomenon of gas leakage, and also can not make ITO be reduced.In the present embodiment, to adopt thickness be the soft steel welding fabrication of 1.0mm ~ 2.0mm to the second jacket 252.In addition, shut in jacket step, this deaeration pipe is not shut.
After shutting jacket step and finishing, then start to vacuumize by deaeration pipe, reach 2 × 10 to vacuum tightness
-3when Pa is above, start jacket to heat.Until be heated to after certain temperature within the scope of 250 ℃ ~ 500 ℃, carry out incubation step, in described heating and insulating process, continue to vacuumize, keep the vacuum tightness in the second jacket 252 to be at least 2 × 10
-3pa.The object of this step has two: the one, and vacuumize and make gas residual in jacket be drawn out of by limit heating edge, and the impurity that is made the volatile or lower boiling in the 2nd ITO target blank or be easily decomposed into gas by heating energy becomes gaseous state, discharges jacket by vacuumizing.The 2nd, for the step of follow-up hot isostatic pressing is carried out abundant preheating, after making the 2nd ITO target blank to be first incubated for some time at lower temperature, again temperature is elevated to comparatively high temps, and then the insulation long period, be that the temperature in order to make the 2nd ITO target blank each several part is consistent.And if be warmed up to faster comparatively high temps, can cause the 2nd ITO target blank place's temperature that keeps to the side very high, and the temperature of centre portions is still very low.Thereby the structural performance inside and outside the target that makes to form is inconsistent.
In this step, the temperature raising is too low, does not realize deimpurity object, and the temperature of rising is too high, make the 2nd ITO target blank first make the consistent object of its inner each several part temperature in a lesser temps and then intensification thereby do not realize, and easily cause excessive power consumption.The inventor has analyzed the impurity in ito powder, preferably adopts 250 ℃ ~ 500 ℃, substantially can remove most impurity, can not cause again excessive power consumption.In vacuum, the vacuum tightness that the second jacket 252 keeps, if too small, the gas that can cause impurity to produce can not be extracted out completely, the density of the ITO target forming after having a strong impact on.The inventor finds, in the time that soaking time is 2 ~ 3 hours, can realizes and allow the internal temperature of whole material can reach uniformly design temperature, can guarantee to remove the object of volatile or lower boiling impurity simultaneously.Soaking time is too much, can cause excessive power consumption.The 2nd ITO target blank is after above-mentioned heating and incubation step, and purity increases, but now density is still inadequate.Need to process again.
Then, continue, in conjunction with reference to figure 1, to perform step S16, described the second jacket is carried out to heat and other static pressuring processes, described the 2nd ITO target blank is formed to the 3rd ITO target blank;
Similar isostatic cool pressing technique, heat and other static pressuring processes utilizes liquid or γ-ray emission respectively to impartial pressure.But it is a kind of processing method of at high temperature suppressing.Concrete, heat and other static pressuring processes is in the hot isostatic pressing stove of High Temperature High Pressure sealing, take high-pressure inert gas or nitrogen (being generally argon gas or nitrogen) as medium, sample is applied to each processing method of suppressing to impartial static pressure.And, the method for applying the fine and close equipment of other unidirectional pressurizations or Bidirectional-pressure with respect to other, density and the homogeneity of the 3rd ITO target blank after hip treatment are better.With respect to isostatic cool pressing technique, the hot environment that the 3rd ITO target blank provides at heat and other static pressuring processes, can make the diffusion aggravation of ITO particulate, to fill up the space between ITO atom, and at high temperature, described ITO molecule can be realized recrystallize, makes the crystal grain moulding of target inside and evenly.
Set forth the principle that forms ITO target in this step by hot isostatic pressing below in conjunction with the principle of heat and other static pressuring processes.
After insulation in step S15 finishes, take out the second jacket, under the state that continues to keep its inner vacuum, hold one's breath (be about to the duct occlusion of holding one's breath, make an airtight vacuum environment of the inner formation of the second jacket), now the vacuum tightness of described vacuum canning is at least 2 × 10
-3pa.Afterwards, the jacket of holding one's breath is placed in hot isostatic pressing (Hot Isostatic Pressing, HIP) stove and carries out hot isostatic pressing step.
Hot isostatic pressing method have the hot pressing of gathering, etc. the plurality of advantages such as static pressure, but the concrete technology parameter that will obtain adopting this method to process the target that meets standard is but and be not easy.Above-mentioned parameter mainly comprises: the disproportionate relation of temperature, environmental stress and soaking time and three.The rising of hip temperature is conducive to the diffusion of ITO atom in the 3rd ITO target blank equally, the voidage of the ITO target inside of follow-up formation is reduced, density and intensity improve constantly, and can make ITO molecule can realize recrystallize, make the crystal grain moulding of target inside and evenly.If but hip temperature is too high, not only waste fuel, very uneconomical, but also the crystal grain that can impel the ITO target crystallization of follow-up formation to form is excessive, the performance of follow-up ITO target is worsened.And particularly in temperature during higher than 1200 ℃, the ito powder in ITO target easily decomposes, and forms in the ITO sosoloid of gaseous substance from sintering state and escapes, the target of formation can have a lot of gas passages and hole, has hindered the raising of ITO target density.And if hip temperature is too low, the 3rd ITO target blank is difficult to produce moulding distortion and forms ITO target.In the present embodiment, before the heat and other static pressuring processes of this step carries out, described the 3rd ITO target blank has passed through pre-molding, isostatic cool pressing and has vacuumized the processing such as preheating insulation, and the density of described the 3rd ITO target blank is higher than 70%.Repeatedly put into practice and analyze through contriver, finally determining in this step, the temperature that hot isostatic pressing is set is 800 ℃ to 1000 ℃, can realize compactness, the homogeneity of the last ITO target forming are met the demands, and not cause the decomposition of ITO powder.
In carrying out heat and other static pressuring processes, the hot isostatic pressing pressure applying is larger, in the second jacket, the ITO particle packing of the 3rd ITO target blank inside can be tightr, the deflection that particle is extruded is larger, contact area between particle is also larger, and described heat and other static pressuring processes makes target blank faster by fine and close speed.And under the environment of the high temperature of hot isostatic pressing, it is too large that required applied pressure does not need, but too little, can make the 3rd ITO target blank be difficult to realize finer and close.Find by contriver's test of many times, after the pressure of the hot isostatic pressing in this step is applied to 130MPa, the effect of the increase to isostatic cool pressing technique can be too unobvious.And if the not enough 90MPa of isostatic cool pressing operation pressure makes the 3rd ITO target blank be difficult to realize finer and close.
And the hold-time of hot isostatic pressing pressure need to maintain the sufficiently long time, such the second jacket can have time enough to carry out pressure conduction, makes follow-up formation ITO target interior tissue even.Creative work through contriver is found, it is 800 ℃ to 1000 ℃ in the temperature of hot isostatic pressing, in the situation that the hot isostatic pressing pressure range applying is 90Mpa ~ 130MPa, if the time of the maintenance of hot isostatic pressing pressure is less than 2 hours, the 3rd ITO target blank is good not by the degree of densification, and the 3rd ITO target blank is inner and submarginal place, even not by the degree of densification; If the time of the maintenance of hot isostatic pressing pressure is greater than 5 hours, the 3rd ITO target blank is not too significantly changed by the degree of densification and homogeneity, easily causes process costs waste.
In this step, described heat and other static pressuring processes design parameter is, set temperature is 800 ℃ to 1000 ℃, and applying argon gas or nitrogen in hot isostatic pressing stove keep the environmental stress 90Mpa to 130Mpa at jacket place, and be incubated 2 hours under this temperature pressure ~ 5 hour.Cool to afterwards 200 ℃ with the furnace.
The isostatic cool pressing of carrying out before the heat and other static pressuring processes of this step makes the density of the 2nd ITO target blank reach 70%, be based upon on such basis, the hot isostatic pressing of this step can be realized the complete densification of the 3rd ITO target blank, forms density and is at least more than 99% ITO alloy target material.Contriver repeatedly puts into practice discovery, if without isostatic cool pressing technique, and directly carries out an ITO target to carry out heat and other static pressuring processes, can not make the ITO target forming meet the requirements.If carry out isostatic cool pressing technique and first carry out heat and other static pressuring processes, the effect of the further densification of the ITO target blank of described isostatic cool pressing after to hip treatment is not too remarkable again, can not make the final ITO target forming meet the requirements.Through the repeatedly summary of practice and experience, carry out again heat and other static pressuring processes to first carrying out isostatic cool pressing technique in making employing the present embodiment of ITO target, and in conjunction with the method for the parameter providing in the present embodiment, be the most effectively, the method for the minimizing process costs waste of saving processing step most and trying one's best few.
Finally, continue, in conjunction with reference to figure 1, to perform step S17, remove described the second jacket 252, described the 3rd ITO target blank is carried out to mechanical workout and form ITO target.
After cooling, the sharp method of crossing turning is removed described the second jacket 252 and is obtained the 3rd ITO target blank, and then the 3rd ITO target blank is carried out mechanical workout and makes the ITO target finished product that final size needs.
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; can utilize method and the technology contents of above-mentioned announcement to make possible variation and modification to technical solution of the present invention; therefore; every content that does not depart from technical solution of the present invention; any simple modification, equivalent variations and the modification above embodiment done according to technical spirit of the present invention, all belong to the protection domain of technical solution of the present invention.
Claims (18)
1. a making method for indium-tin oxide target material, is characterized in that, comprising:
ITO powder is provided;
Adopt static pressure technique by ITO powder pre-molding, form an ITO target blank;
The one ITO target blank is put into the first jacket and vacuumized;
Adopt isostatic cool pressing technique to process the ITO target blank in the first jacket, form the 2nd ITO target blank;
Remove after described the first jacket, the 2nd ITO target blank is put into the second jacket, and vacuumize;
Adopt heat and other static pressuring processes to process the 2nd ITO target blank in the second jacket, form the 3rd ITO target blank;
Remove after described the second jacket, described the 3rd ITO target blank is carried out to mechanical workout and form ITO target.
2. the making method of indium-tin oxide target material according to claim 1, is characterized in that, the technique of described isostatic cool pressing comprises successively:
Isostatic cool pressing stove is vacuumized to processing;
In isostatic cool pressing stove, fill rare gas element or nitrogen;
The first jacket is placed in isostatic cool pressing stove, and it is 100MPa ~ 200MPa that pressure is set, and pressurize 2 hours ~ 5 hours under this pressure.
3. the making method of indium-tin oxide target material according to claim 1, is characterized in that, the technological operation of described hot isostatic pressing comprises:
Hot isostatic pressing stove is vacuumized to processing;
Then in hot isostatic pressing stove, fill rare gas element or nitrogen;
Then will stop vacuumizing and the second jacket of good seal is placed in hot isostatic pressing stove, it be 800 ℃ ~ 1000 ℃ that temperature in hot isostatic pressing stove is set, and it is 90MPa ~ 130MPa that pressure is set, and under this temperature and pressure heat-insulation pressure keeping 2 hours ~ 5 hours;
Finally be cooled to below 200 ℃.
4. the making method of indium-tin oxide target material according to claim 1, is characterized in that, the main component of described ITO powder is In
2o
3and SnO
2mixed powder.
5. the making method of indium-tin oxide target material according to claim 4, is characterized in that, described In
2o
3and SnO
2mass ratio be 9:1.
6. the making method of indium-tin oxide target material according to claim 4, is characterized in that, described ITO powder also comprises tamanori, and described tamanori is glycerine or acetone.
7. the making method of indium-tin oxide target material according to claim 1, is characterized in that, described static pressure technique comprises:
By the processing of static pressure stove evacuation;
Vacuumize after processing, ito powder is put into mould, described mould is put into static pressure stove, the pressure head in described static pressure stove applies static pressure pressure to described ito powder, carries out compaction treatment and forms an ITO target blank, and described static pressure pressure is 20MPa ~ 30MPa.
8. the making method of indium-tin oxide target material according to claim 1, is characterized in that, described the first jacket is pumped down to vacuum tightness and is less than 10
-2pa.
9. the making method of indium-tin oxide target material according to claim 8, is characterized in that, described the first jacket is rubber package set or aluminium jacket.
10. the making method of indium-tin oxide target material according to claim 1, is characterized in that, described the second jacket is carbon steel jacket or stainless steel jacket, comprises jacket body and lid.
The making method of 11. indium-tin oxide target materials according to claim 10, it is characterized in that, the 2nd ITO target blank is put into after the second jacket, described the second jacket is carried out to second to be vacuumized before processing, also be included in the jacket body upper cover upper cover body of the second jacket, and by the mode of argon arc welding, jacket body and lid are welded, described the second jacket is shut.
The making method of 12. indium-tin oxide target materials according to claim 1, is characterized in that, vacuumizing that the second jacket is carried out is treated to and is evacuated to vacuum tightness in described the second jacket is 2 × 10
-3more than Pa.
The making method of 13. indium-tin oxide target materials according to claim 12, is characterized in that, the second jacket is evacuated to 2 × 10
-3after Pa is above, carry out also comprising step before hip treatment: maintain and vacuumize 2 × 10
-3state more than Pa, is then heated to the second jacket 250 ℃ ~ 500 ℃, and is incubated 2 hours ~ 5 hours;
After insulation finishes, keep the vacuum tightness in the second jacket constant, stop vacuumizing, and simultaneously by the second jacket sealing.
The making method of 14. indium-tin oxide target materials according to claim 1, it is characterized in that, vacuumizing that described the first jacket is carried out process or described the second jacket is carried out vacuumize processing, comprise the step of shutting described the first jacket or the second jacket and therefrom drawing degassed mouthful, vacuumize processing by described degassed mouth.
The making method of 15. indium-tin oxide target materials according to claim 14, is characterized in that, described to after the vacuumizing processing and finish of the first jacket, and the degassed mouth of described the first jacket is carried out to mechanical seal.
The making method of 16. indium-tin oxide target materials according to claim 15, is characterized in that, described mechanical seal is that degassed mouthful on described the first jacket is tightened.
The making method of 17. indium-tin oxide target materials according to claim 14, is characterized in that, described to after the vacuumizing processing and finish of the second jacket, and degassed mouthful of described the second jacket is held one's breath to realize by described the second jacket sealing.
The making method of 18. indium-tin oxide target materials according to claim 1, is characterized in that, the method for described the second jacket of described removal is turning.
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| CN105478756A (en) * | 2014-09-17 | 2016-04-13 | 宁波江丰电子材料股份有限公司 | Ti-A1 alloy forming method |
| CN112592173A (en) * | 2020-12-15 | 2021-04-02 | 株洲火炬安泰新材料有限公司 | Preparation method of ITO (indium tin oxide) sintered target material |
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