CN101265580A - Pre-conditioning a sputtering target prior to sputtering - Google Patents
Pre-conditioning a sputtering target prior to sputtering Download PDFInfo
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- CN101265580A CN101265580A CNA2007100873737A CN200710087373A CN101265580A CN 101265580 A CN101265580 A CN 101265580A CN A2007100873737 A CNA2007100873737 A CN A2007100873737A CN 200710087373 A CN200710087373 A CN 200710087373A CN 101265580 A CN101265580 A CN 101265580A
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Abstract
A sputtering target is pre-conditioned prior to use of the target in a sputtering process by removing a damaged surface layer of a sputtering surface of the target. In one version, the sputtering surface of the sputtering target is lapped to remove a thickness of at least about 25 microns to obtain a sputtering surface having a surface roughness average of from about 4 to about 32 microinches. In another version, an acidic etchant is used to remove the layer. In yet another version, the damaged surface layer is annealed by heating the surface.
Description
Related application
The application submits with non-provisional application, and requires to enjoy the preference that the application number of submitting on March 14th, 2006 is 60/782,740 provisional application, and quotes it in full as a reference at this.
Technical field
Embodiments of the present invention relate to this sputtering target of pre-treatment before sputtering target is used for sputtering technology.
Background technology
In the manufacturing of electronic circuit and indicating meter, sputtering chamber is used for deposition material is splashed to for example substrate, such as, semiconductor wafer or indicating meter.Sputtering chamber uses the sputtering target that is installed in the chamber.This target comprises the sputtering surface of being made up of sputter material, and this sputter material can for example be a metal, such as, aluminium, copper, tantalum, titanium or tungsten.Compound such as sputter material can also be deposited in the chamber, for example, tantalum nitride, titanium nitride and tungsten nitride.Be typically, this chamber comprises the cover (enclosure) that is used to surround the process island of introducing process gas, be used to excite process gas forming the gas excitor of plasma body, and the venting port that is used to discharge gas and control chamber indoor gas pressure.In sputtering technology,, thereby make the material sputter leave target and deposit on the substrate by energetic plasma material bombardment sputtering target.
Yet the manufacturing process that is used to form sputtering target produces the damaging surface layer of this target usually, and this can cause sputter attribute that do not expect or inconsistent.Be typically, sputtering target be processed as discoid by mechanical technology such as lath (lathing) or mill (milling).These complete processings form shearing force on the surface of target, thereby make the surface microstructure viscous deformation and cause other defect in this surface microstructure.In viscous deformation, the vicinal faces of each intragranular atom slides over each other, and causes lattice plane respect to one another permanent laterally mobile, thereby causes hangover (smeared) crystalline-granular texture.Be typically, impaired upper layer also has higher dislocation desity.In sputtering technology, the crystal grain defective effect in the sputtering target spatters distribution from the target material that goes out from target.Impaired crystal grain or upper layer with high bit dislocation density cause variable or uneven sputter attribute on the entire target surface.For example, be damaged upper layer and may cause that the sputter rate that begins from sputtering target changes, and spatters till going out from target up to surface microstructure.This causes the deposition of the sputter material off-gauge on the different substrates of handled a collection of substrate, in the whole lip-deep inhomogeneous deposition of single substrate.Thereby when the sputtering surface of target with on every side or outside atmosphere reaction and when forming the upper layer of not expecting and influencing its sputter attribute, can produce another problem.For example, sputter target material can react with the oxygen in the ambient air, thereby forms the upper layer of oxidation.
In order to remove the impaired upper layer of not expecting of sputtering target, after being installed to sputtering target in the sputtering chamber, being typically and carrying out aging (burn-in) processing step.In aging technique, the sputtering surface of target is exposed to plasma body spatters from going out with the upper layer of not expecting with target.For example, the aging technique step that can carry out target with 150kW-hour plasma body to be removing the adequate thickness on target surface, thereby can provide more uniform sputter rate when using this target subsequently in production technique.Yet the target aging technique needs spended time to finish, and sputtering chamber can not be used for producing during this period.The low utilising efficiency of sputtering chamber has increased processing cost.Therefore, need a kind of technology that is used to remove the impaired upper layer on the sputtering target, this technology more effectively and do not influence the use of sputtering chamber in the target digestion time that prolongs.
Summary of the invention
The invention provides the several method of removing or repairing impaired upper layer on the sputtering target.A kind of method comprises from the surperficial mechanical polishing of target falls impaired upper layer.Other method comprises from the surface etching of target falls impaired upper layer.A method comprises being heated at least about 400 ℃ temperature by the impaired surface with target and repairs this upper layer again.Another method comprises by applying pulsed current spatters impaired upper layer from going out described sputtering surface and making this impaired layer leave this surface by electric arc.
Can use the impaired upper layer on these methods removals or the reparation sputtering target, and need not in the target digestion time that prolongs, to hinder the use of sputtering chamber.
Description of drawings
To understand these features of the present invention, scheme and advantage better by following specification sheets, appended claims and accompanying drawing that the embodiment of the invention is shown.Yet, should be appreciated that generally speaking each feature may be used to the present invention, and be not limited to the content of certain figures, and the present invention includes the arbitrary combination of these features, wherein:
Fig. 1 is the side cross-sectional view of embodiment with sputtering target of sputtering surface;
Fig. 2 A is the partial side view in cross section of embodiment of sputtering target with sputtering surface of impaired upper layer;
Fig. 2 B is the partial side view in cross section of sputtering target after removing impaired upper layer from sputtering surface of Fig. 2 A;
Fig. 3 is the X-ray diffractogram of the sputtering surface of sputtering target, and it shows the X-ray diffraction peak that is obtained by different angle of diffraction;
Fig. 4 A is the synoptic diagram of embodiment of polissoir that is used to polish the sputtering surface of sputtering target;
Fig. 4 B is the synoptic diagram of another embodiment of polissoir that is used to polish the sputtering surface of sputtering target;
Fig. 5 is acidic etchant jar and the fragmentary sectional view of embodiment that is used for holding at this jar the anchor clamps of sputtering target;
Fig. 6 is the explanatory view of laser beam equipment that is used for the sputtering surface of laser treatment sputtering target;
Fig. 7 is the synoptic diagram of electro erosion plant;
Fig. 8 is the cross sectional view of embodiment that can use the sputtering chamber of sputtering target; And
Fig. 9 is the illustrative diagram that is used for the electrolytic process polissoir of electrolytic process polishing sputtering target.
Embodiment
Fig. 1 shows the embodiment that deposition material can be splashed to the sputtering target 20 on the substrate 104.Target 20 comprises the sputtering plates of being made up of sputter material 22, and wherein this sputter material can comprise such as metal, and for example, at least wherein a kind of of titanium, tantalum, tungsten perhaps comprises the alloy of a kind of or other metals of these elements.Sputtering plates 22 comprises sputtering surface 24, can remove material to deposit a material on the substrate 104 from this sputtering surface, for example, utilizes this sputtering surface 24 of high energy gas sputter.Can make sputtering plates 22 by appropriate means, for example comprise, chemical vapour deposition, casting, physical vapor deposition, plating, hot isostatic pressing and additive method.Processing for circular semiconductor wafers is typically, and sputtering plates 22 is discoid.Sputtering plates 22 also can have about 200mm to the interior diameter of about 500mm scope, and about 2.5mm is to the interior thickness of about 25mm scope.Yet sputtering target 20 is not limited to specific geometry, and can have other shapes or other sizes according to the shape of substrate 104.For example, sputtering target 20 can be rectangle or the square that is used for processing display and rectangular substrate.In another program, sputtering target 20 also comprises toroidal coil 25 (as shown in Figure 8), this coil be installed on the sidewall of chamber 106 and be positioned at sputtering plates 22 on the top that is installed in chamber 106 around.The toroidal coil 25 that sputtering plates 22 that install at the top and sidewall are installed all comprises sputtering surface 24, and all is used as sputtering target 20 in this scheme.
In a scheme, sputtering target 20 comprises the sputtering plates 22 that is installed on the backboard 26, and this backboard 26 is used to be supported on the sputtering plates 22 on sputtering chamber 106 tops.Typically, backboard 26 is by forming such as the metal of copper or such as the metal alloy of copper-zinc alloy, and it provides good thermal conduction to cool off to allow sputtering plates 22 during sputtering technology.Backboard 26 comprises peripheral ledge 27, and it is arranged on the annulus (annular ring) in the sputtering chamber 106.The back side 29 of backboard 26 also contacts the heat exchanger in the chamber, further to cool off sputtering plates 22 during sputter process.Be typically, sputtering plates 22 diffusions are connected to backboard 26.The toroidal coil 25 that sidewall is installed can also have sputtering surface 24, with sedimentary sputtering material around the outer peripheral areas that is provided at substrate 104, thereby provides better or more uniform sputter material.
Comprise that by removal the certain thickness pre-treatment target 20 of the sputtering surface 24 of impaired upper layer 32 improves the processing of the substrate 104 that uses sputtering target 20 (it can be sputtering plates 22 or toroidal coil 25).For example, shown in Fig. 2 A, in some targets, impaired upper layer 32 mainly comprises the viscous deformation crystal grain 28 that forms " hangover " surface microstructure structure along sputtering surface 24.Remain with undeformed crystal grain 30 below hangover crystalline-granular texture 28, it provides better or more uniform sputter characteristic usually.Impaired upper layer 32 can also have or optionally only have high dislocation density.The thickness of impaired upper layer 32 depends on the grain-size of target on the surface of target 20, and is typically at least about 25 microns, and more typical is about 50 microns to about 300 microns.Sputtering surface 24 can also have metal oxide or other layers (not shown) that forms on the surface that exposes.
Fig. 3 is the X-ray diffractogram of the sputtering surface 24 of sputtering target 20, and it shows the function of X-ray diffraction peak and angle of diffraction.When impaired upper layer 32 comprised the crystal grain 28 of viscous deformation, the distance between the crystal face differed from one another at each intergranule, thereby diffraction peak is widened.At the FWHM (halfwidth) of the diffraction peak at place, about 38 ° 2 Θ angles is the measurement of the non-homogeneous microstrain that causes of the viscous deformation by crystal face.The crystal plane of level of strain that bigger FWHM value representation is higher and hangover crystal grain 28 changes largely.After initial manufacture, as shown in Figure 3, the FWHM of sputtering surface approximately not 0.69 as can be seen.When with impaired upper layer 32 basically when sputtering surface 24 is removed, shown in Fig. 2 B, following not deformed grains 30 is exposed on the sputtering surface 24, and the FWHM of diffraction peak is reduced to about below 0.4.
In a scheme of this technology, shown in Fig. 2 B, on lath after the shape of processing target, the sputtering surface 24 by the glossing in the polissoir 34 polishing sputtering plates 22 is with the whole impaired upper layer 32 of removing sputtering surface 24 places basically and the undeformed crystal grain 30 below exposing or have crystal grain than low-dislocation-density.In a scheme of this technology, shown in Fig. 4 A, target 20 remains on the grinding miller (lapping wheel) 40, from the slurry divider 44 that comprises slurry supply 46 rubbing paste 42 is applied to wheel 40 simultaneously.Swiveling wheel 40 and target 20 exposed surface 24 reciprocally to rub off sputtering plates 22.The glossing typical case is that low pressure, low-speed handing are to obtain the surperficial preferably finishing polish of sputtering surface 24.This slurry comprises the particle size with pre-determined range and the abrasive grains of hardness.Polishing sputtering surface 24 is to remove the certain thickness on surface 24, and this thickness is enough to remove crystal grain and any surface oxide layer of viscous deformation.For example, the sputtering surface 24 that can polish sputtering target 20 to be removing the layer 32 that can have at least about 25 micron thickness, and obtains to have about 4 the sputtering surfaces of average surface roughness to about 32 microinch scopes.
In an embodiment of finishing method, target 20 is placed on the grinding miller 40, and the weight that comprises the sputtering target 20 of sputtering plates 22 and backboard 26 is firmly pressed to sputtering surface 24 on the ground flat of wheel 40.Grinding miller 40 can be installed on the platform of BOGEY WHEEL 48, this BOGEY WHEEL 48 can be minimized in vibrations and the shake that produces during wheel 40 rotations or the concussion.Along with target 20 is pressed mutually each other with grinding miller 40 and rotated, between these two surfaces, introduce the rubbing paste 42 of abrasive grains.Target 20 moves and by this cylinder is stopped towards a pair of cylinder (roller cylinder) 50a that is supported by mounting plate 52 and 50b.Control the polishing Flatness of sputtering surface 24 by the grain-size of abrasive grains.This abrasive grains can be the particle or or even the diamond particles of aluminum oxide, silicon carbide.Ground preferably will comprise size at about 2 to 12 microns, for example 6 microns, the slurry 42 of abrasive grains of diamond particles be suspended in the medium, in deionized water.In one embodiment, comprise that in use slurry 42 polishings of the diamond particles that is of a size of 6 microns are after about 30 minutes, when when test, it is about 0.48 that the FWHM of sputtering surface 24 at 38 ° of X-ray diffraction peaks of locating is reduced to, and its expression is than original FWHM value 0.69 improvement about 30%.
Though described one type glossing, should be appreciated that, also can use other finishing method.For example, can also be in the lath (not shown) sputtering surface 24 of polishing target 20, when substrate 20 during, use and carry out attached to suitable polishing on this lath or abrasive tool around the axle rotation of lath.Equally, can also use other schemes of glossing, for example, shown in Fig. 4 B, can be towards the sputtering surface 24 of last maintenance target 20, and polish along pushing 47 pairs of these sputtering surfaces 24 of polish brush downwards towards sputtering surface 24.In this scheme, when the rubbing paste divider 44 that comprises slurry supply 46 adds the rubbing paste 42 of diamond particles, brush 47 and sputtering surface 24 rotate relative to one another or shake.
In another glossing scheme, use electrochemical etching technology, wherein during polishing, use power supply 56 to apply electric current to the sputtering surface 24 of target 20.Can apply electric current with second brush electrode 59 that contacts rubbing paste 42 by first brush electrode 57 that contacts with target 20.With about 5 to 70mAmps/cm
2Electric current be applied to target 20.In this scheme, rubbing paste 42 for comprise such as the acid solution of HF acid and with the conductive solution of other sour mixtures.Advantageously, because the application of electric current and chemistry and mechanical polishing, electrochemical etching technology provides better removal of the plastic deformation layer 32.
In a scheme again, as shown in Figure 9, use electrolytic process polissoir 300 to remove impaired upper layer 32 from the sputtering surface 24 of target 20.In the electrolytic process glossing, in the electrolytic solution 302 in the target 20 immersion electrolytic process polishing ponds 304.According to target material, electrolytic solution 302 can be an acid solution, such as HCl, HNO
3Or H
2SO
4Dilute solution or its mixture.Make electropolish power supply 312 to applying voltage, also negative electrode 306 is immersed in the solution 302 simultaneously as anodic sputtering target 20.In one embodiment, by applying from about 5 to about 75 volt range, for example about 50 volts, direct current can etching tantalum target 20 sputtering surface 24.By solution 302, electrolytic process polishing power supply 312 provides high electric current to 100mAmps, for example, from about 5 to 70mAmps/cm
2, this current value is based on the area of the sputtering surface 24 that will carry out electrolytic process polishing.In one embodiment, electrolytic solution 302 comprises the alcohol with adding sulphur acid solution, for example, and methyl alcohol or ethanol.Alcohol can be about 5: 1 to about 40: 1 with the volume ratio of acid, for example 20: 1.Other acid such as HF also can join in the electrolytic solution 302.In electrolytic process polissoir 300, for the anode that comprises tantalum target 20, negative electrode 306 can be made by stainless steel.Equally, ground preferably, as shown in the figure, (masking fixture) 310 shelters the back side 29 of target 20 by masking jig, and with the material at the protection back side 29, otherwise it will be corroded by electrolytic solution 302.
In another program, can use or not polish with polishing sputtering surface 24, by acidic etchant the sputtering surface 24 of this sputtering target 20 is etched with and removes impaired layer 32.A kind of method of the sputtering surface of etch sputtered target comprises that the sputtering surface 24 with target 20 is immersed in the acidic etchant 58 that comprises hydrofluoric acid and nitrate mixture.Hydrofluoric acid can have about 10% concentration to about 52% weight percent, for example, and about 49.5wt%.Nitric acid can have about 50% concentration to about 80% weight percent, for example, and about 69.5wt%.The adequate rate of hydrofluoric acid and nitric acid is about 15% to about 20% volume percent.In a scheme, for example as shown in Figure 5, acidic etchant 58 is provided in jars 60 and with target 20 is immersed in the etching reagent 58.Can comprise acidic etchant 58 in jar 60, wherein this jar 60 has recycle pump, and is the filtering system (not shown) alternatively, to remove filter residue from acidic etchant 58.Can also stir the acidic etchant 58 in the jar 60, for example, stir by the ripple vibration that surpasses that the ultrasonic oscillator (not shown) that is connected to jar 60 walls provides.Other agitating methods comprise that the mechanical propeller stirring also can be used to stir acidic etchant 58.
In one embodiment, comprising HF and HNO
3Acidic etchant 58 in chemical milling sputtering surface 24 after about 30 minutes at room temperature, it is about 0.49 that the FWHM at (38 °) peak of sputtering surface 24 is reduced to, it represents to have improved about 30% than the value 0.69 of original FWHM once more.In another embodiment, comprising HF and HNO
3Acidic etchant 58 in chemical milling sputtering surface 24 after about 180 minutes at room temperature, it is about 0.46 that the FWHM at (38 °) peak of sputtering surface 24 is reduced to, it represents to have improved about 30% than 0.69 of original FWHM value once more.Therefore, the impaired layer 32 of sputtering surface 24 has been removed in chemical milling significantly.
In another chemical milling scheme, in water-bath 64, heat the chemical etchant that comprises jar 60, the temperature that heats to keep jar 60 in turn by well heater 62 is at least about 50 ℃.Can determine etch-rate that this temperature provides about fast 5 times than room temperature etch-rate.Jars 60 can comprise water-bath 64 with in the scope that maintains the temperature at a strict control, for example, ± 2 ℃, with the optimal etch of the sputtering surface 24 that obtains target 20.Because etching reaction is thermopositive reaction, it is too fast to prevent that etching reaction from carrying out that the temperature of acidic etchant 58 can be accurately controlled in hope.The sputtering surface 24 of target 20 is exposed in the acidic etchant about 90 to about 180 minutes time.
In a method again, the sputtering surface 24 that at first grinds target 20 is to obtain about 4 surfacenesses to about 32 microinchs.Be typically, grind sputtering surface 24 to remove the thickness at least about 25 microns, perhaps more typical is about 25 thickness to about 300 micrometer ranges.Thereafter, in acidic etchant this sputtering surface 24 of chemical milling to remove about 25 to about 200 microns additional thickness.Initial glossing makes sputtering surface 24 smooth, the sputter attribute that makes the chemical etching process (making surface smoothing) carry out subsequently produce acceptable surfaceness and provide sputtering chamber 106 to hit 20 unanimity.In such embodiment, with the rubbing paste 42 polishing sputtering surface that comprises the diamond particles that is of a size of 6 microns 24 about 15 minutes.Thereafter, chemical milling should grind in above-mentioned acid etching agent solution target 20 about 60 minutes.It is about 0.39 that the FWHM at (38 °) peak of sputtering surface 24 is reduced to, and its expression has improved about 40% than initial FWHM value 0.69.In another embodiment, with comprising the rubbing paste grinding and polishing sputtering surface 24 about 15 minutes that is of a size of about 6 microns diamond particles.Thereafter, chemical milling was ground in the acid etching agent solution target 20 about 120 minutes.The FWHM at (55 °) peak of the sputtering surface 24 of target 20 is reduced to about 0.4.
After polishing, etching or any other process of surface treatment, can use the profilograph (not shown) to measure the surfaceness of the sputtering surface 24 of sputtering plates 22.Surface properties is of value to the attribute of crystal grain 28 on the performance sputtering surface 24.For example, it is 24 surface average roughness of averaging again apart from the absolute value of the middle line shift of the peak of rough features and paddy surfacewise, can be used as the slick rough measure on surface 24.Too coarse surface is not expected, because it provides the mutability of not expecting in sputtering technology.Profilograph generally includes the probe that is installed on the surperficial transverse arm, and this surface transverse arm is connected to a right cylinder and by engine driven.Probe can exchange with the different schemes that is applicable to different surfaces attribute or measurement.This right cylinder is installed on the stable pedestal, such as heavy metal or granite platform.Measure the surface properties of sputtering surface 24 by dilatory probe on the evaluation length on surface 24.Along with probe moves up and down along contact sputtering surface 24, it produces the surface profile signal trajectory of uneven surface height fluctuation from the teeth outwards, the transmitter that this signal trajectory is sent to such as induction pick-up is converted into sensor signal with the vibration with probe, and then by Computer Processing.Selected sample length and signal trajectory are used for determining one group of surface profile numeral corresponding to surperficial different positions, and are used for the surface profile track that provides visual on indicating meter.Suitable surface profiler is the FormTalysurf Model12 type probe contourgraph from England Leicester's Taylor Hobson.Can also use scanning electronic microscope, it uses from the electron beam of surface 24 reflections and produces this surperficial image.In a kind of measuring method, sputtering plates 22 is cut to a plurality of test pieces and each test piece is taken multiple measurements.Then, the surfaceness measuring result is averaged to determine the mean value on this surface 24.In one embodiment, use three test pieces, and four surface profile tracks of the height change of valley roughness are provided for each test piece.In a scheme, can determine that suitable average roughness value for example is, from about 4 to about 32 microinchs.Use and specify the international standard ANSI/ASME of suitably fix a point length and evaluation length B.46.1-1995 to carry out these measurements.
In an embodiment again, use sputtering surface 24 such as the energy heating target of laser beam or lamp.Set the characteristic of the energy,, be heated to the temperature that is enough to annealing grains 28 with impaired upper layer 32 selectivity with sputtering surface 24 such as focal length, shape of beam and beam diameter.In one embodiment, use the energy that sputtering surface 24 is heated to deep thickness less than 300 microns, more particularly less than 200 microns.For example, the laser beam of focusing can be used for optionally the temperature that local surfaces 24 with sputtering plates 22 is heated to the dislocation desity that is enough to reduce impaired layer 32, and does not need too to increase the bulk temperature of entire target 20.The proper temperature that reduces dislocation is at least about 400 ℃.The typical case is, annealing temperature is less than 2/3 of the melting point of the material of sputtering surface 24.For example, temperature can be about 400 ℃ to about 1000 ℃.In another embodiment, the proper temperature for the sputtering surface 24 that comprises the tantalum with about 3017 ℃ of melt temperatures is about 600 ℃.The local heat energy that is provided to the impaired upper layer 32 of sputtering surface 24 by laser apparatus causes the softening and fusion in local heating zone, causes the dislocation in the layer 32 to move in crystal grain, to reduce physical damage and strain.The heating sputtering surface 24 impaired upper layer 32 with after it is annealed, only by just rapid quenching taking place with during heat is from the surface conductance to the surrounding environment.
Can use laser apparatus annealing device 80 to carry out the annealing of crystal grain in the sputtering surface 24 of sputtering plates 22, figure 6 illustrates an exemplary embodiment.Laser apparatus annealing device 80 is included in the laser apparatus 82 in the laser beam cover 84.Be provided with power and controlled laser apparatus 82 by controller 86, laser apparatus 82 can also comprise scanning mechanism 88, passes the laser beam 90 of sputtering surface 24 with scanning.Operable suitable laser apparatus 82 comprises, for example, and Ar, CO
2With the KrF laser apparatus.Argon laser sends the visible wavelength of about 5145 dusts.CO
2Laser apparatus is for source of infrared energy with 10.6 mum wavelengths and the light beam with 10 kilowatts of energy levels can be provided.CO
2Laser apparatus is higher than 100 times and have higher intensity than argon laser is effective, compares with argon laser and allows sweep velocity and bigger spot size faster.The laser apparatus of another type is the KrF excimer laser, has Eg, about 3% efficient and the output energy of 350mJ of wavelength, the 5.0eV of about 248nm.Laser beam 90 typical cases are the circular light beams that have less than the beam diameter of about 10nm, and more typical is that about 0.5mm is to about 4mm.Suitable laser beam 90 can have about 190nm to about 10, the wavelength of 600nm.The typical case operates this laser apparatus 82 with about 50 watts to about 2000 watts power stage.
Though with the laser beam heat treatment described is schematic annealing process, also can use other surface annealing processings.For example, alternative annealing process comprises the one group of rapid thermal annealing system such as the lamp of quartz lamp that uses, with the sputtering surface 24 of heating target 20.In a scheme, by directly infrared radiation heating sputtering surface 24 to the sputtering surface 24 of target 20 being carried out annealing process, for example, via the one group of quartz lamp that in the rapid thermal annealing chamber, is installed in above the target 20.Can also be by well heater be set, the resistance heater such as contiguous target perhaps heats target 20 by target is set in stove.Radiant heat energy heats sputtering surface 24 apace to redirect in 24 on the surface and/or the crystal grain 28 of the viscous deformation of regenerating.Can also scanning radiation can be to provide required thermal treatment on the surface 24 of entire target 20.Yet other heating means and system comprise plasma jet heating, electric-arc heating and flame heating.Therefore, scope of the present invention should not be confined to exemplary arrangement described here, and the present invention also comprises other localized surface annealing technology and equipment, and this is conspicuous to those of ordinary skill in the art.
Annealing process can also use together in conjunction with other technologies described here.In one embodiment, after processing target 20, use glossing to polish the sputtering surface 24 of this target 20.After glossing, the sputtering surface 24 of etching target 20 in described acidic etchant 58.Thereafter, by being heated to about 400 ℃ to 1000 ℃ temperature, the sputtering surface 24 of annealing target 20.In conjunction with polishing, etching and annealing, can expect provides the target 20 with low defect level and less impaired surface microstructure 28.
In other method, well-known electrodischarge machining(E.D.M.) (EDM) can be removed the crystal grain layer of viscous deformation on the sputtering surface 24 by discharge.As shown in Figure 7, in typical EDM equipment 200, come the high-frequency spark discharge of self-electrode 202 to be used to decompose the electro-conductive material of sputtering surface 24, have the layer of the sputtering plates 22 of viscous deformation crystal grain 28 with removal.In the embodiment of this expection, electrode 202 and sputtering surface 24 are immersed in the insulating material 204 in jars 210, and electrode mechanically moving device 206 is used to keep about spark gap of 0.013 to about 0.5mm between electrode 202 and the target 20.Electrode mechanically moving device 206 can be screw thread or hydro-cylinder, and it is used for vertically moving up and down electrode 202 on whole surperficial 24, also is used to be provided with the gap size between electrode 202 and the sputtering surface 24.The electrical spark that forms in the gap melts or the small-particle of evaporation target 20, and this small-particle is along with electrode 202 is 24 up and then be rinsed on the surface.Electrode 202 uses discharge and removes material from sputtering surface 24, the temperature between each spark produces 10,000 to 20,000 ℃.Along with electrode 202 moves on whole sputtering surface, the arc erosion of generation falls part sputtering surface 24.In a scheme, electrode 202 is a metal wire, this metal wire for example comprises Al, Cr, Cr/Ni, Cu/Co, Cu/Mn, Cu/Sn, Cu/W, Ni, Ni/Co, Ni/Fe, Ni/Mn, Ni/Si, Ti, Ti/Al, TiC/Ni, W/CrC/Cu or WC/Co, and wherein the typical case uses copper cash.EDM can use molding (die-sinking) or electrode wires cutting, and wherein molding uses finished graphite or copper electrode that sputtering plates 22 is burnt till required shape, and the electrode wires cutting uses very thin line to downcut the impaired part of sputtering surface 24.
In EDM technology, it is negative polarity that discharge power supply 208 keeps electrodes 202, and for example about 100 straight polarity is applied to sputtering plates 22 to about 400 volts voltage.Controller 212 control power supplys 208 are applied to electrode 202 will hang down pulsed current under stable recurrence interval, go back control electrode mechanically moving device 206 traveling electrode 202 on whole sputtering surface 24 simultaneously.Power supply 208 can comprise that the pulsed current of the electric current formation pulse that control produces produces power unit.For example, power supply 208 can be to produce the pulse of 1000Amp electric current during discharge processes less than the interval of a microsecond.In precision work, it is that time length nanosecond level is to stablize and repeatedly to produce less pulsed current that this pulse can be set.
In a scheme, in embodiment as shown in Figure 8, after pre-treatment, can in sputtering chamber 106, use sputtering target 20, such as one or more of tantalum, tantalum nitride, aluminium, aln precipitation, titanium, titanium nitride, tungsten, tungsten nitride and copper with sputtering depositing layer on substrate 104.Substrate support 108 is set with support substrates 104 in chamber 106.By the substrate load port (not shown) in chamber 106 sidewalls substrate 104 is incorporated in the chamber 106 and with this substrate and is placed on the support 108.Can promote the lifting of corrugated tube (bellows) (not shown) or reduce support 108 by support.
Can be by chamber controller 54 these chambers 106 of control, this chamber controller 54 comprises the program code with instruction set, with the assembly of operation chamber 106, thereby handles substrate 104 in chamber 106.For example, controller 54 can comprise the substrate orientation instruction set, operating one or more substrate supports 108 and substrate forwarder, thereby in chamber 106 position substrate 104; Air-flow steering order collection is with supply 103 of operation sputter gas and flow director 126; Gaseous tension steering order collection, with operation exhaust system 128 and throttling valve 137, thus the pressure in the maintenance chamber 106; Gas excitor steering order collection with operating air excitor 190, thereby is provided with the gas excitation level; The temperature control instruction collection is with the temperature in the control chamber 106; And the process monitoring instruction set, with the technology in the monitoring chamber 106.
Sputtering target 20 of the present invention can use with any sputtering technology.Exemplary sputtering technology has been described in following patent, and quote its full content as a reference: authorize to the denomination of invention of Kumagai U.S. Patent No. 6 for " Sputtering Method and Apparatus (sputtering method and equipment) " at this, 616,402, the denomination of invention of authorizing to people such as Gregor is the U.S. Patent No. 3 of " Apparatus and Method forSputter Etching (equipment and the method that are used for sputter etching) ", 617,463, the denomination of invention of authorizing to people such as Macaulay is the U.S. Patent No. 4 of " Sputtering Apparatus and Method (sputtering equipment and method) ", 450,062, the denomination of invention of authorizing to people such as Makino is the U.S. Patent No. 5 of " Method for Producing a Specified Zirconium-Silicon Amorphous Oxide FilmComposition by Sputtering (by the method for the definite zirconium-amorphized silicon oxide film synthetics of sputter manufacturing) ", 209,835, the denomination of invention of authorizing to people such as Nihei is the U.S. Patent No. 5 of " Methodof and Apparatus for Sputtering and Integrated Circuit Device (device that is used for sputter closes method and unicircuit) ", 175,608 and authorize to people's such as Hiraki denomination of invention U.S. Patent No. 5 for " Titanium-Tungsten Target Material for Sputtering and ManufacturingMethod Therefor (titanium-tungsten target material and the manufacture method thereof that is used for sputter) ", 160,534.
Although illustrate and described illustrative embodiments of the present invention, those of ordinary skill in the art can design other embodiment in conjunction with the present invention, and these also belong to protection scope of the present invention.For example, target 20 can comprise the material except exemplary materials described here, and also can carry out other treatment step to target 20.Equally, except clearly describe, also can handle target 20 with different shapes or heterogeneity.In addition, interchangeable about the relevant or position terms shown in the illustrative embodiments.Therefore, appended claims should not be limited to the description that is used to explain preferred version of the present invention, material or arrangement space described here.
Claims (19)
1. the method for this sputtering target of pre-treatment before sputtering target is used for sputtering technology, described method comprises:
(a) provide the sputtering target of sputtering surface with impaired upper layer; And
(b) the described sputtering surface of the described sputtering target of polishing to be removing the thickness at least about 25 microns, and obtains to have about 4 sputtering surfaces to the average surface roughness of about 32 microinchs.
2. method according to claim 1 is characterized in that, described (b) comprises electrochemical etching, wherein during described glossing, electric current is applied to the described sputtering surface of described target.
3. method according to claim 2 is characterized in that, comprises applying from about 5 to about 70mAmps/cm
2Electric current.
4. method according to claim 1 is characterized in that, described (b) comprises the described sputtering surface that polishes described sputtering target by following arbitrary method:
(1) described sputtering surface is pressed to grinding miller with himself weight, between described plate and described sputtering surface, apply rubbing paste simultaneously;
(2) use the rubbing paste that is included in the diamond particles in the deionized water;
(3) use comprises that size is at about 2 rubbing pastes to about 15 microns diamond particles;
(4) sputtering surface that described sputtering target is set towards top and with polish brush towards sputtering surface to pressing down.
5. method according to claim 1 is characterized in that, is included in described (b) carries out following steps afterwards at least one:
(1) the described sputtering surface by the described sputtering target of electrochemical etching etching; And
(2) utilize the described sputtering surface of the described sputtering target of acidic etchant etching.
6. method according to claim 5 is characterized in that, comprises hydrofluoric acid and nitric acid in acidic etchant described in described (2), and comprise following at least one of them:
(1) described hydrofluoric acid comprises about 10% concentration to about 52% weight percent;
(2) described nitric acid comprises about 50% concentration to about 80% weight percent;
(3) volume ratio of described hydrofluoric acid and nitric acid is about 10% to about 20%.
7. method according to claim 1 is characterized in that, also is included at least one of described (b) following steps afterwards:
(i) utilize the described sputtering surface of the described sputtering target of acidic etchant etching; And
(ii) described sputtering surface is heated to about 400 ℃ to about 1000 ℃ temperature.
8. method according to claim 1 is characterized in that, comprising provides the sputtering target that comprises the sputtering surface of being made up of titanium, tantalum or tungsten.
9. method according to claim 1 is characterized in that, described sputtering target comprise following at least one of them:
(i) sputtering plates, it is to have about 200 disks to about 500mm diameter;
(ii) has 2.5 to about 25mm thickness; And
The backboard that (iii) comprises copper-zinc alloy.
10. method according to claim 1 is characterized in that, also comprises:
(1) described sputtering target is installed in sputtering zone;
(2) in described sputtering zone, be positioned adjacent the substrate of described target; And
(3) form plasma body to sputter material to described substrate from described sputtering target.
11. the method for the described sputtering target of pre-treatment before sputtering target is used for sputtering technology, described method comprises:
(a) provide the sputtering target of sputtering surface with impaired upper layer; And
(b) the described sputtering surface of the described sputtering target of etching in the acidic etchant that comprises hydrofluoric acid and nitric acid, described hydrofluoric acid comprises about 30% concentration to about 52% weight percent, described nitric acid comprises about 50% concentration to about 80% weight percent, and the volume ratio of described hydrofluoric acid and nitric acid is about 10% to about 20%.
12. method according to claim 11 is characterized in that, also comprises by described sputtering surface is exposed in the electrolytic solution applying electric current by described electrolytic solution simultaneously, makes the described sputtering surface of the described sputtering target of electropolish.
13. method according to claim 12 is characterized in that, comprises to described electrolytic solution applying about 5 to 70mAmps/cm
2Electric current.
14. method according to claim 11 is characterized in that, also comprises following at least one:
(1) the described sputtering surface of electrochemical etching; Perhaps
(2) by under the own wt of described sputtering surface, being pressed to grinding miller and simultaneously applying rubbing paste and polish described sputtering surface to described the wheel.
15. the method for the described sputtering target of pre-treatment before sputtering target is used for sputtering technology, described method comprises:
(a) provide the sputtering target of sputtering surface with impaired upper layer; And
(b) the described impaired upper layer of described sputtering surface is heated to temperature at least about 400 ℃.
16. method according to claim 15 is characterized in that, is included in the described sputtering surface of heating under following at least one condition:
(1) described sputtering surface is heated to 2/3 temperature less than the described fusing point of the described material of described sputtering surface;
(2) described sputtering surface is heated to less than about 1000 ℃ temperature;
(3) described sputtering surface is heated to deep thickness less than 300 microns;
(4) use the described sputtering surface of laser beam heats; And
(5) use one group of quartz lamp to heat described sputtering surface.
17. the method for the described sputtering target of pre-treatment before sputtering target is used for sputtering technology, described method comprises:
(a) provide the sputtering target of sputtering surface with impaired upper layer; And
(b) keep described sputtering surface one clearance distance of electrode distance; And
(c) apply pulsed current between described electrode and described sputtering surface, forming electric arc to described electrode, thereby remove the described impaired upper layer of described sputtering surface basically.
18. the method for the described sputtering target of pre-treatment before sputtering target is used for sputtering technology, described method comprises:
(a) sputtering surface with sputtering target is immersed in the electrolytic solution, and described sputtering surface has impaired upper layer; And
(b) apply electric current to remove the described impaired upper layer of described sputtering surface by described electrolytic solution.
19. method according to claim 18 is characterized in that, comprise following at least one of them:
(1) applies about 5 to about 70mAmps/cm by described electrolytic solution
2Electric current;
(2) described sputtering surface is immersed in comprises HCl, HNO
3, H
2SO
4Perhaps in the electrolytic solution of its mixture; And
(3) apply volts DS to described target and electrode in described electrolytic solution, described volts DS is about 5 to about 75 volts.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US60/782,740 | 2006-03-14 | ||
| US11/685,151 US20070215463A1 (en) | 2006-03-14 | 2007-03-12 | Pre-conditioning a sputtering target prior to sputtering |
| US11/685,151 | 2007-03-12 |
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| Publication Number | Publication Date |
|---|---|
| CN101265580A true CN101265580A (en) | 2008-09-17 |
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| CNA2007100873737A Pending CN101265580A (en) | 2006-03-14 | 2007-03-14 | Pre-conditioning a sputtering target prior to sputtering |
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| CN102029570A (en) * | 2010-10-29 | 2011-04-27 | 宁波江丰电子材料有限公司 | Method and device for machining tungsten and titanium alloy target material |
| CN102842478A (en) * | 2011-06-24 | 2012-12-26 | 初星太阳能公司 | Non-bonded rotary semiconducting targets and methods of their sputtering |
| CN104470681A (en) * | 2012-06-21 | 2015-03-25 | 国立大学法人鹿儿岛大学 | Observation camera |
| CN107630221A (en) * | 2016-07-18 | 2018-01-26 | 宁波江丰电子材料股份有限公司 | The cleaning method of titanium focusing ring |
| CN107868940A (en) * | 2016-09-27 | 2018-04-03 | 宁波江丰电子材料股份有限公司 | The manufacture method of target |
| CN108396307A (en) * | 2018-01-18 | 2018-08-14 | 昆明理工大学 | A kind of preparation method of the diamond thin with strong film base adhesion strength |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102029570A (en) * | 2010-10-29 | 2011-04-27 | 宁波江丰电子材料有限公司 | Method and device for machining tungsten and titanium alloy target material |
| CN102029570B (en) * | 2010-10-29 | 2012-09-26 | 宁波江丰电子材料有限公司 | Method and device for machining tungsten and titanium alloy target material |
| CN102842478A (en) * | 2011-06-24 | 2012-12-26 | 初星太阳能公司 | Non-bonded rotary semiconducting targets and methods of their sputtering |
| CN104470681A (en) * | 2012-06-21 | 2015-03-25 | 国立大学法人鹿儿岛大学 | Observation camera |
| US9804067B2 (en) | 2012-06-21 | 2017-10-31 | Kagoshima University, National University Corporation | Observation and photography apparatus |
| CN107630221A (en) * | 2016-07-18 | 2018-01-26 | 宁波江丰电子材料股份有限公司 | The cleaning method of titanium focusing ring |
| CN107630221B (en) * | 2016-07-18 | 2019-06-28 | 宁波江丰电子材料股份有限公司 | The cleaning method of titanium focusing ring |
| CN107868940A (en) * | 2016-09-27 | 2018-04-03 | 宁波江丰电子材料股份有限公司 | The manufacture method of target |
| CN107868940B (en) * | 2016-09-27 | 2020-07-31 | 宁波江丰电子材料股份有限公司 | Method for manufacturing target material |
| CN108396307A (en) * | 2018-01-18 | 2018-08-14 | 昆明理工大学 | A kind of preparation method of the diamond thin with strong film base adhesion strength |
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