CN103966558A - Cu-Mn alloy sputtering target material, Cu-Mn alloy sputtering target material manufacture method and semiconductor element - Google Patents
Cu-Mn alloy sputtering target material, Cu-Mn alloy sputtering target material manufacture method and semiconductor element Download PDFInfo
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Abstract
The invention provides a Cu-Mn alloy sputtering target material, Cu-Mn alloy sputtering target material manufacture method and a semiconductor element. The Cu-Mn alloy sputtering target material can reduce paradoxical discharge in sputtering processes caused by foreign matters such as high concentration Mn and impurity containing oxides and the like. A Cu-Mn apploy which ranges between 5 atom% and 30 atom% in mean concentration and ranges between 10 [mu]m and 50 [mu]m in average crystal grain diameter is adopted as the parent metal of the Cu-Mn alloy sputtering target material, the maximum value and the minimum value of the Mn concentration can be obtained through X-ray energy spectrum analysis, the difference between the the maximum value and the minimum value of the Mn concentration and the average concentration is within +/-2 atom%.
Description
Technical field
The present invention relates to the manufacture method of a kind of Cu-Mn alloy sputtering target, Cu-Mn alloy sputtering target and use the semiconductor element of the Cu-Mn alloy film being formed by this target.
Background technology
In recent years, liquid crystal flat-panel is subject to the impact of large screen, high-precision refinement, pursues further telepresenc and requires the realization of high visual angle (Super High Vision), bore hole 3D flat board.About the thin film transistor for liquid crystal flat-panel (TFT:Thin Film Transistor), constantly carry out utilizing high degree of excursion and carry out that difference high speed motion, threshold voltage is little, the exploitation of the semiconductor material of drive current excellent in uniformity.As such semiconductor material, develop the oxide semiconductors such as Indium sesquioxide gallium zinc (InGaZnO: be designated as below IGZO), zinc oxide (ZnO) and substituted existing non-crystalline silicon (α-Si) semi-conductor.
In addition, as the TFT distribution electrode materials that is applicable to such novel semiconductor material, for example in non-patent literature 1, having recorded copper-manganese (Cu-Mn) alloy is useful for IGZO system TFT., by Cu-4 atom %Mn alloy film film forming on IGZO film, carry out the thermal treatment of 250 DEG C by sputter.Thus, at the interface formation manganese oxide (MnO of alloy film and IGZO film
x) film, the Cu suppressing in alloy film spreads in IGZO film.In this stacked film, having obtained contact resistance is 10
-4the good ohm property of Ω cm.In addition, about the processibility of electrode of utilizing wet etching, the selection of the rate of etch of Cu-4 atom %Mn alloy film and IGZO film, than being 10:1, is good.
The target using in film forming about Cu-Mn alloy film, for example, be recorded in patent documentation 1,2.In patent documentation 1, as the copper alloy of sputtering target material, be to form by melting in a vacuum the also casting of alloying.Now, in the scope of 0.1～20.0at.%, add Mn, the concentration limits of the inevitable impurity element that the spread coefficient in Cu is less than Cu self spread coefficient is decided to be below 0.05at.%.
In addition, in patent documentation 2, the copper alloy that forms sputtering target contains Mn:0.6～30 quality %, and remainder has forming of being made up of Cu and impurity.It is below impurity 40ppm and below oxygen 10ppm, below nitrogen 5ppm, below hydrogen 5ppm, below carbon 10ppm that this impurity is defined as metal.Such Cu alloy is high purity electrolytic copper and electrolytic manganese are carried out to high frequency fusing in the high purity graphite mould in Ar gas atmosphere and manufacture.
In addition, about the control of the foreign matter of target, for example, in patent documentation 3, thereby the vacuum melting in crucible of the metals such as the cobalt containing impurity such as aerobic, phosphorus, sulphur, nickel, iron is manufactured to high purity metal target.After melting of metal, in crucible, solidify or carry out directional freeze carrying out, impurity is concentrated into crucible top or finally solidifies portion, and excise the concentrated part of impurity.
Prior art document
Patent documentation
Patent documentation 1: No. 4065959 communique of Japanese Patent
Patent documentation 2: TOHKEMY 2007-051351 communique
Patent documentation 3: TOHKEMY 2002-327216 communique
Non-patent literature: Pilsang Yun, Junichi Koike, " Microstructure Analysis andElectrical Properties of Cu-Mn Electrode for Back-Channel Etching a-IGZO TFT; " 17th International Display Workshops (IDW ' 10), pp.1873-1876
Summary of the invention
The problem that invention will solve
But, Mn easily with the crucible material using in the fusing of raw material, cast the impurity such as carbon (C) composition contained in flux (flux) composition and react.Therefore, in the tissue of Cu-Mn castings, inevitably there is the foreign matters such as Mn, impure oxide compound.Foreign matter is isolator or semi-conductor, when sputter, can cause charging (parts are charged) thus become paradoxical discharge occur starting point.If generation paradoxical discharge, exists a part of melting of target, thereby the material that is called the droplet-like of splash disperses and causes the bad situation of alloy film.
In addition, in the time of the casting of Cu-Mn alloy, by the solid phases and liquid phase separation of different compositions when liquid phase is solidified, entirety all becomes solid phase.Therefore, in crucible, melt and flow in the cast structure that casting mould is solidified the castings forming and have density unevenness.The essential factor that when Mn of the high density that such density unevenness causes also can become sputter, paradoxical discharge occurs.
Therefore, for the impact of inhibition of impurities, patent documentation 1,2 described above is such, and only the concentration of regulation impurity is inadequate.In patent documentation 1,2, do not record for the problem on the material structure of Cu-Mn alloy as described above, also do not disclose solution.And the method for patent documentation 3 to be considered to be not originally the method about Cu-Mn alloy, in addition, be also unsuitable for expensive volume production manufacture.
The object of the present invention is to provide a kind of paradoxical discharge can reduce the sputter causing due to the foreign matter such as Mn, impure oxide compound of high density time Cu-Mn alloy sputtering target, Cu-Mn alloy sputtering target manufacture method and use the semiconductor element of this target.
The means of dealing with problems
According to the 1st mode of the present invention, a kind of Cu-Mn alloy sputtering target is provided, it to be to contain the Mn of mean concns more than 5 atom % and below 30 atom % and the Cu-Mn alloy of average crystallite particle diameter more than 10 μ m and below 50 μ m as mother metal, utilizes the maximum value of Mn concentration that X-ray energy spectrum analysis obtains and the difference of minimum value and described mean concns in ± 2 atom %.
According to the 2nd mode of the present invention, provide according to the Cu-Mn alloy sputtering target described in the 1st mode, in described Cu-Mn alloy, exist and contain than at least one the foreign matter in the Mn of described mean concns greater concn and impure oxide compound, in crystal structure in the 1cm × 1cm of described Cu-Mn alloy, maximum diameter is that described foreign matters more than 5 μ m is below 10.
According to the 3rd mode of the present invention, provide according to the Cu-Mn alloy sputtering target described in the 2nd mode, described impurity is at least one in C, S, Si, P.
According to the 4th mode of the present invention, provide according to the Cu-Mn alloy sputtering target described in the 2nd mode, described impurity is at least one in C, S, Si, P, and the mean concns of described impurity in the crystal structure of described Cu-Mn alloy is that C is below 10ppm, S is below 20ppm, Si is below 20ppm, P is below 100ppm.
According to the 5th mode of the present invention, provide according to the Cu-Mn alloy sputtering target described in any in 1st～4 modes, the difference of the maximum value of described Mn concentration and minimum value and described mean concns is in ± 0.5 atom %.
According to the 6th mode of the present invention, a kind of manufacture method of Cu-Mn alloy sputtering target is provided, the raw material that Cu with respect to more than purity 3N is added to Mn more than purity 3N in the mode of the mean concns more than reaching 5 atom % and below 30 atom % melts and casts, thereby obtain castings, then, at the temperature by described castings more than 800 DEG C and below 870 DEG C, thereby heating makes the overall evenly heating of described castings, carries out hot rolling with more than 90% degree of finish.
According to the 7th mode of the present invention, a kind of semiconductor element is provided, it possesses the distribution structure forming by form Cu-Mn alloy film on oxide semiconductor on substrate, and described Cu-Mn alloy uses the Cu-Mn alloy sputtering target described in any in 1st～5 modes or utilizes the Cu-Mn alloy sputtering target of the method manufacture described in the 6th mode to form.
According to the 8th mode of the present invention, provide according to the semiconductor element described in the 7th mode 2 layers of described Cu-Mn alloy film that described distribution structure has pure Cu film and described pure Cu film is clipped in the middle.
Invention effect
According to the present invention, provide a kind of paradoxical discharge can reduce the sputter causing due to the foreign matter of Mn, the impure oxide compound etc. of high density time Cu-Mn alloy sputtering target, Cu-Mn alloy sputtering target manufacture method and use the semiconductor element of this target.
Brief description of the drawings
Fig. 1 is the binary system phase diagram of Cu-Mn alloy.
Fig. 2 is the longitudinal sectional drawing that the sputter equipment of the Cu-Mn alloy sputtering target that an embodiment of the invention relate to is installed.
Fig. 3 is the simple sectional view of the thin film transistor that relates to of an embodiment of the invention.
Fig. 4 is the schematic drawing of the detection device system that uses in the mensuration of arc-over of the Cu-Mn alloy sputtering target that relates to of embodiments of the invention and comparative example.
Fig. 5 is the SEM image that the crystal structure after the hot rolling of Cu-Mn that embodiments of the invention 1,2 are related to is observed.
Fig. 6 is the SEM image that the crystal structure after the hot rolling of Cu-Mn alloy that comparative example 1,2 is related to is observed.
Description of reference numerals
10:Cu-Mn alloy sputtering target
20: sputter equipment
30:IGZO system TFT (thin film transistor)
31: glass substrate
32: gate electrode
33: gate insulating film
34: channel part (oxide semiconductor)
35b: bottom barrier film (Cu-Mn alloy film)
35D: drain electrode
35m: wiring film (Cu film)
35S: source electrode
35t: top barrier film (Cu-Mn alloy film)
36: protective membrane (SiO
2film)
Embodiment
An embodiment of the invention
(1) Cu-Mn alloy sputtering target
Below, copper-manganese (Cu-Mn) alloy sputtering target 10 (with reference to a Fig. 2 described later) mode of the present invention being related to describes.Cu-Mn alloy sputtering target 10 is for example formed as having the external diameter of regulation and the rectangle of thickness, is configured to the formation of the Cu-Mn alloy film using for the distribution structure of various semiconductor elements etc.
Form the Cu-Mn alloy of Cu-Mn alloy sputtering target 10 for example for purity is the alloy that the above oxygen free copper (OFC:Oxygen-Free Copper) of 3N (99.9%) coordinates with requirement ratio with pure manganese (Mn)., Cu-Mn alloy sputtering target 10 is for example taking the Cu-Mn alloy that contains the Mn of mean concns more than 5 atom % and below 30 atom % as mother metal.
As the Cu-Mn alloy of mother metal, its average crystallite particle diameter is adjusted into for example more than 10 μ m and below 50 μ m.Finer crystallization particle diameter so for example can by Cu-Mn alloy is carried out hot rolling with reach degree of finish 90% with on obtain.
In addition, the maximum value of the Mn concentration in the mother metal of Cu-Mn alloy and the difference of minimum value and mean concns are in ± 2 atom %, in be preferably ± 0.5 atom %.That is, the value that the maximum value of Mn concentration deducts mean concns gained is no more than "+2 atom % ", and the value that the minimum value of Mn concentration deducts mean concns gained is not less than " 2 atom % ".In addition, preferably, the value that the maximum value of Mn concentration deducts mean concns gained is no more than "+0.5 atom % ", and the value that the minimum value of Mn concentration deducts mean concns gained is not less than " 0.5 atom % ".Such Mn concentration and difference thereof for example can be measured by the mother metal of Cu-Mn alloy being carried out to X-ray energy spectrum (EDX:Energy Dispersive X-ray spectroscopy) analysis.
In addition, in Cu-Mn alloy, the Mn of high density or its oxide compound are separated out and dissociate, and exist sometimes as foreign matter in part.Think that Mn concentration is now at least higher than above-mentioned mean concns, or exceed the scope of above-mentioned difference.In addition, in Cu-Mn alloy, also can mix and have the such regulation element of Mn impurity in addition.This impurity become as a rule independent or with the oxidized state of the form of the reactant of Mn.That is to say, the oxide compound that contains such impurity also can be present in Cu-Mn alloy as foreign matter.
But even under these circumstances, the number that is present in these foreign matters in the crystal structure of Cu-Mn alloy in Cu-Mn alloy sputtering target 10 is also few.That is to say, the maximum diameter for example observing in the crystal structure in the 1cm × 1cm of Cu-Mn alloy is that foreign matters more than 5 μ m is below 10.The shape of foreign matter is various, but the benchmark using its maximum diameter as foreign matter size here.Foreign matter in Cu-Mn alloy for example can be observed by scanning electronic microscope (SEM:Scanning Electron Microscope).Here, the maximum diameter of foreign matter is defined as to " connecting the length of the straight line between 2 points included in the foreign matter region length when maximum ", particularly, draws by measure length by manual line in the photo of SEM.
Here as mixing the impurity being present in Cu-Mn alloy, can enumerate such as carbon (C), sulphur (S), silicon (Si), phosphorus (P) etc..In Cu-Mn alloy sputtering target 10, the mean concns of these impurity in the crystal structure of Cu-Mn alloy is suppressed in prescribed value.As an example based on actual value, for example in present embodiment, C is that 10ppm is following, S is that 20ppm is following, Si is that 20ppm is following, P is below 100ppm.Here, the controlled ultimate value of P concentration is for example below 15ppm, but by making P concentration higher than this, can improve the diffusion barrier of the Cu-Mn alloy film of formation.Thereby, the upper limit taking 100ppm as P concentration here.In addition, C in the application, the concentration of S are measured by " high-frequency combustion infrared absorption ", and the concentration of Si, P is measured by ICP-AES (Inductively CoupledPlasma-Atomic Emission Spectrometry) method.
By forming Cu-Mn alloy sputtering target as above, can form the Cu-Mn alloy film of the high diffusion barrier of performance.
, in the present embodiment, in Cu-Mn alloy, the upper limit of Mn concentration is set as 30 higher atom %.Mn for example, compared with Cu etc., has than being easier to oxidized character.Thereby, for example, by using the sputter of Cu-Mn alloy sputtering target 10, can obtain bringing into play the Cu-Mn alloy film of high diffusion barrier.That is to say, for example, oxidized with the interface Mn of oxide semiconductor that becomes substrate, performance diffusion barrier, the oxygen for example in addition depth direction of film being suppressed spreads.
On the other hand, be high density if make Mn,, in the time of the fusing of target manufacturing process Raw, casting, it is easily oxidized that the raw material of fusing becomes.In addition, in Cu-Mn alloy, become and easily contain impurity.Such oxidation, impurity, not only reduce the quality of the Cu-Mn alloy film of film forming, the occurrence frequency of the paradoxical discharge (arc-over) also can increase sputter time.
But, in present embodiment, by adopting manufacture method described later, contain than the raw material of the Mn of higher concentration even if use, also can, in suppressing the oxidation of raw material and alleviating the impact of impurity, manufacture Cu-Mn alloy sputtering target 10.
Particularly, the present inventors do not limit the impurity concentration in Cu-Mn alloy as above-mentioned patent documentation 1,2, but the difference of Mn concentration of mother metal of Cu-Mn alloy of the reason that becomes these foreign matters is controlled at below prescribed value.If the poor of Mn concentration becomes large, the Mn of the high density in mother metal just has the existence of localization, reacts or oxidized in addition, and become the reason of foreign matter with Mn monomer or with other impurity.First, by making the Mn concentration homogenizing of mother metal of Cu-Mn alloy, thus the foreign matter reason that can forgo such.
In addition, the present inventors are further controlled at size, the number of the foreign matter containing Mn, impurity etc. below prescribed value.Thus, in the plasma body in sputter, suppress the paradoxical discharge taking foreign matter as starting point.
That is to say, if for example contain at least one foreign matter in Mn and the impurity of high density on the surface of the shaping of Cu-Mn alloy sputtering target 10 or the surface occurring by sputter is exposed and existed, the state that easily becomes overshooting shape and give prominence to.Therefore the plasma body, having in for example sputter becomes unsettled situation.If it is unstable that plasma body becomes, cause continually paradoxical discharge.In addition, if come off from the outstanding foreign matter in the surface of Cu-Mn alloy sputtering target 10, can form hole.Around this hole, it is unstable that plasma body easily becomes.
In addition, be that at least one the oxide compound etc. in Mn and the impurity that contains high density, this foreign matter has insulativity or half insulation, becomes easily because of the charged state of plasma body at this foreign matter.Charged due to such foreign matter, it is unstable that plasma body becomes sometimes.
In present embodiment, make the number of the foreign matter more than specified dimension of observing of Cu-Mn alloy in regulation area, the frequency that exists of foreign matter is below prescribed value.The paradoxical discharge that can form taking foreign matter as starting point thus, is difficult to the state occurring.Thereby a part for the Cu-Mn alloy sputtering target 10 that can suppress to be caused by paradoxical discharge melts and the flying (, splash produces) of generation droplet-like.Thereby, can suppress splash and be attached to the Cu-Mn alloy film in film forming and form particle, obtain the Cu-Mn alloy film of high-quality.
In addition, in present embodiment, making Cu-Mn alloy is finer crystallization particle diameter.The concavo-convex change on Cu-Mn alloy sputtering target 10 surfaces that thus, can suppress to be caused by sputter is large.Thereby, can suppress sputter applying plasma and become unstable, and form the state that paradoxical discharge is more difficult to generation.
(2) manufacture method of Cu-Mn alloy sputtering target
The manufacture method of the Cu-Mn alloy sputtering target 10 then, relating to for an embodiment of the invention describes.
What at this moment used is the volume production equipment large-scale Cu-Mn alloy sputtering target 10, that carry out air casting, rolling that for example can manufacture the glass substrate size more than generation corresponding to the 8th etc.Utilize such volume production equipment, can make the Mn concentration that contains in Cu-Mn alloy higher, and, by following method, can suppress the poor of Mn concentration in the mother metal of Cu-Mn alloy.In addition, can suppress the oxidation of raw material.In addition, can make the foreign matter miniaturizations such as impurity.
First each material, the chip material that is respectively the above oxygen free copper of 3N (99.9%) and pure Mn by purity being formed coordinates with requirement ratio.It is for example melted, cast at the temperature more than 1100 DEG C and below 1200 DEG C in atmosphere, form and for example contain the castings (ingot casting (Ingot)) that mean concns is the Cu-Mn alloy of the Mn more than 5 atom % and below 30 atom %.
The liquid level of raw material molten metal liquation covers (キ ャ ッ プ) with antioxidant, suppresses with the oxidation that realizes molten metal.The dregs of the impurity such as C, S, its oxide compound etc. containing in crucible material that now, the fusing of raw material is used, casting flux component produce in molten metal.The dregs that produce in molten metal float on liquid level due to density difference as slag.Here, be called slagging-off (ノ ロ か I) thus the purification of molten metal remove slag, this can suppress to become above-mentioned foreign matter.
The moment that becomes full and uniform in concentration is moved liquid to casting mould by molten metal, obtains ingot casting.Now, in the casting bucket to casting mould guiding, casting mould, pulverous casting flux is provided to molten metal surface, slag is absorbed.
But, in present embodiment, in raw material, contain the Mn easily reacting with the impurity such as C, S, become the situation that more easily produces slag.Thereby, even if carry out above operation, be also difficult to from molten metal, slag be removed completely.Therefore, become the state that the impurity of minute quantity in the ingot casting of manufacturing is sneaked into as foreign matter.
In addition, in the time of solidification of molten metal, after liquid phase separates with from the solid phase of its different compositions, entirety becomes solid phase.Therefore, in cast structure, can produce density unevenness.In addition, finally solidify part, the Mn segregation of high density in cast structure.The Mn of high density, its oxide compound also all become the foreign matter in ingot casting like this.Here, for the Mn that contains high density finally solidify part for, also can exist because the thermal contraction of liquid phase produces small hole.
Then, remove the oxide film thereon on the ingot casting surface obtaining,, after so-called casting skin, carry out hot-rolled process to obtain the milled sheet of specific thickness.
For carrying out hot-rolled process, first, for example ingot casting is heated specific time by the temperature more than 800 DEG C and below 870 DEG C, to realize the evenly heating of ingot casting entirety.Then, directly implement by the processing of hot rolling.For hot-rolled process, implement processing so that thickness is reduced more than 90% with respect to the thickness of ingot casting.That is to say, the mode becoming more than 90% with degree of finish in hot-rolled process is processed ingot casting.
Now, realize the evenly heating of ingot casting entirety, namely make ingot casting entirety become uniform temperature roughly to depend on necessary heat-up time the volume of ingot casting.That is to say, ingot casting is larger, and the temperature that fully improves inside ingot more expends time in, and ingot casting is less, needs a small amount of time.For example, if to use the large-scale volume production equipment of the glass substrate more than generation corresponding to the 8th as prerequisite, need to heat more than 2 hours.
As mentioned above, in ingot casting, sneak into the impurity of minute quantity.The foreign matter such as impurity that is brought into inside ingot is diffused, is disperseed by heating under high temperature as much as possible, thereby can realize miniaturization.But if the temperature more than fusing point is heated, ingot casting can melt.In the crystal structure of ingot casting, thus in the case of become due to the segregation concentration of Mn etc. inhomogeneous, due to this concentration difference, the only crystal structure of a part fusing, thereby can there is the solid-liquid separation that solid phase and liquid phase are separated.If implement hot rolling under such state, exist from the situation of the part cracking of liquid phase.As shown in the binary system phase diagram of the Cu-Mn alloy of Fig. 1, in Cu-Mn alloy system, the minimum value of fusing point is 871 DEG C in the time that Mn concentration is 37 atom %.Thereby, if for example in the temperature less than 870 DEG C, in whole compositing range, do not generate the interior heating of the temperature range ingot casting of liquid phase, can suppress solid-liquid separation.
On the other hand, if Heating temperature is too low, be difficult to cause the diffusion of the inhomogeneous part in crystal structure.In addition, ingot casting becomes the just state of hard, and load when rolling uprises.So, make the lower value of above-mentioned Heating temperature be for example 800 DEG C.This temperature be in the scope based on present embodiment hard, the softening temperature of Mn concentration while being 30 atom % be approximately 700 DEG C and determine.
As in the present embodiment, in above-mentioned temperature range, after heating, by implementing hot rolling, thereby realize the homogenizing of the Mn concentration in the crystal structure of Cu-Mn alloy, and can make foreign matter diffusion.Thus, can make foreign matter miniaturization to suppress size below prescribed value, and can reduce the number (having frequency) of the foreign matter in the unit surface of Cu-Mn alloy.
In addition, in present embodiment, the degree of finish that makes hot rolling is more than 90%.Thus, can make in Cu-Mn alloy is the finer crystalline particle more than average crystallite particle diameter 10 μ m and below 50 μ m.
Then, the milled sheet of the crystalline texture that becomes afore mentioned rules is implemented to the mechanical workouts such as mirror ultrafinish, for example, be configured as and there is the external diameter of regulation and the rectangle of thickness.By above operation, manufacture Cu-Mn alloy sputtering target 10.
As mentioned above, according to present embodiment, in the impact of the paradoxical discharge that can bring at reduction foreign matter, adopt and utilize the volume production operation of the casting of air melting and the low price of hot rolling to manufacture Cu-Mn alloy sputtering target 10.
(3) the formation method of Cu-Mn alloy film
Then the Cu-Mn alloy sputtering target 10, relating to for an embodiment of the application of the invention in conjunction with Fig. 2 carries out the method that sputter forms Cu-Mn alloy film and describes.This Cu-Mn alloy film is for example for having the distribution structure of stacked distribution of the semiconductor elements such as TFT, and the formation method of the Cu-Mn alloy film of the following stated is for example implemented as an operation of the manufacturing process of semiconductor element.
Fig. 2 is the longitudinal sectional drawing that the sputter equipment 20 of the Cu-Mn alloy sputtering target 10 that an embodiment of the invention relate to is installed.Here, the sputter equipment 20 shown in Fig. 2 is only an example.
As shown in Figure 2, sputter equipment 20 has vacuum chamber 21.Top in vacuum chamber 21 is provided with substrate maintaining part 22s, the substrate S that becomes film forming object be retained as by film forming facing to below.Bottom in vacuum chamber 21 is provided with the not shown target maintaining part 22t that possesses the cooling bodies such as water cooler and magnetite, for example, maintain the not shown backboard that has engaged Cu-Mn alloy sputtering target 10.Thus, Cu-Mn alloy sputtering target 10 with substrate S be retained as sputter face upward by the relative mode of film forming face.Here can, at the multiple substrate S of the interior maintenance of sputter equipment 20, these substrates S be handled together or be processed continuously.In addition, also can on substrate S, be pre-formed and become the IGZO film of Cu-Mn alloy film substrate etc.
In addition, be connected with gas supply pipe 23f at a wall of vacuum chamber 21, be connected with gas exhaust pipe 23v at another wall relative with gas supply pipe 23f.Gas supply pipe 23f is connected with the not shown gas supply system at non-active gas such as the interior supply argon of vacuum chamber 21 (Ar) gas.Gas exhaust pipe 23v is connected with the not shown gas exhaust system of the atmosphere in Ar gas equal vacuum chamber 21 being carried out to exhaust.
While utilizing this sputter equipment 20 to carry out film forming to substrate S, at the interior supply of vacuum chamber 21 Ar gas etc., by Cu-Mn sputtering target material 10 ground connection (Earth), substrate S is applied to positive high-tension mode, vacuum chamber 21 is thrown in to DC discharged power (DC power).
Thus, mainly between Cu-Mn alloy sputtering target 10 and substrate S, produce plasma body, the argon (Ar of positively charged
+) the sputter face collision of ion G and Cu-Mn alloy sputtering target 10.Pass through Ar
+the collision of ion G, sputtering particle P being piled up by film forming face to substrate S of the element that contains Cu, the Mn etc. knocking-on from Cu-Mn alloy sputtering target 10.
Now, utilize the magnetite of the target maintaining part 22t that is disposed at Cu-Mn alloy sputtering target 10 belows, form magnetic field space on the surface of Cu-Mn alloy sputtering target 10, thereby make plasma body densification, sputtering rate can be brought up to realistic scale.In addition wherein, utilize the cooling Cu-Mn alloy sputtering target 10 of water cooler across backboard, can suppress unnecessary temperature rise.
By above operation, on substrate S, make to have with Cu-Mn alloy sputtering target 10 the Cu-Mn alloy film film forming of substantially same composition.
Now, as mentioned above, the average crystallite particle diameter in Cu-Mn alloy sputtering target 10 is that fine 10 μ m are above and below 50 μ m.In addition, the size of the foreign matter of the Mn, the impurity etc. that contain high density, number are suppressed at below prescribed value.Thus, be difficult to occur the paradoxical discharge in sputter.Thereby, can suppress the generation of the particle that paradoxical discharge causes, obtain the Cu-Mn alloy film M of high-quality.
Here, as producing the structure on the device of impact of foreign matter for alleviating by arc-over as described above, device etc., for example, for the above-mentioned sputter equipment of enumerating 20, below Cu-Mn alloy sputtering target 10 is disposed at device, ventricumbent film forming substrate S is disposed to device top.But Cu-Mn alloy sputtering target 10 can be installed in various types of sputter equipments such as the vertically opposite device of device, target and substrate that the upper-lower position of target and substrate puts upside down and use.
By aforesaid operations, the mean concns that makes for example to contain in film is the Cu-Mn alloy film M film forming of the Mn more than 5 atom % and below 30 atom %.Thereby the substrate S that is formed with such Cu-Mn alloy film M for example forms after distribution at the Wiring pattern that Cu-Mn alloy film M is patterned as to expectation, is used as with the various semiconductor elements headed by TFT.
(4) structure of thin film transistor
The Cu-Mn alloy film that uses Cu-Mn alloy sputtering target 10 to form, for example can be applicable to as mentioned above as the distribution structure of thin film transistor (TFT:Thin Film Transistor) of semiconductor element with IGZO film.Now, the distribution structure as TFT by Cu-Mn alloy film separately, but in order to obtain more low-resistance distribution structure, also can obtain for example Cu-Mn alloy film being used as the TFT with the stacked distribution of Cu-Mn/Cu/Cu-Mn that there is the barrier film of diffusion barrier, pure Cu film is used as to wiring film.
Below, as an example as the TFT of barrier film by Cu-Mn alloy film, the structure of IGZO system TFT30 is described in conjunction with Fig. 3.Fig. 3 is the simple sectional view of the IGZO system FTF30 that relates to of present embodiment.
As shown in Figure 3, IGZO system TFT30 for example there is glass substrate 31, be formed at gate electrode 32 on glass substrate 31, on gate electrode 32 across the source of gate insulating film 33 electrode 35S and drain electrode 35D (hereinafter referred to as source-drain electrode 35S, 35D).These electrodes 32,35S, 35D are for example formed at each element, and glass substrate 31 is for example cut to multiple elements and is in array-like arrangement.
Gate electrode 32 is for example connected with not shown grid distribution.On grid distribution, be formed with the not shown electronic pads with outside switching telecommunication number.
Mainly, gate electrode 32, grid distribution and electronic pads etc. become the gate electrode structure of the thin film transistor (TFT) that present embodiment relates to.
On gate electrode 32, be for example formed with by SiN film or SiO
2the gate insulating film 33 that film etc. form.
In addition, on gate electrode 32, be formed with as the channel part 34 of oxide semiconductor that is configured as predetermined pattern across gate insulating film 33.Channel part 34 is for example with InGaZnO
4for starting material, formed by Indium sesquioxide gallium zinc (InGaZnO:IGZO) film forming by sputter etc.
On channel part 34, be formed with the source-drain electrode 35S, the 35D that are configured as predetermined pattern, make the two clip rear passage 34b that channel part 34 has and relatively.Source-drain electrode 35S, 35D are connected with not shown source and leak distribution.Source is leaked distribution and is formed with and the not shown electronic pads of outside switching telecommunication number.
Mainly, distribution and electronic pads etc. are leaked in source-drain electrode 35S, 35D, source becomes the source leakage electrode structure of the thin film transistor (TFT) that present embodiment relates to.
The stacked distribution that contains source-drain electrode 35S, 35D has the distribution structure that stacks gradually bottom barrier film 35b, wiring film 35m, top barrier film 35t on glass substrate 31.
Any one of bottom barrier film 35b and top barrier film 35t or two above-mentioned Cu-Mn alloy sputtering targets 10 of use form, and are made up of for example Cu-Mn alloy film above for 50nm and below 100nm of thickness.The mean concns that Cu-Mn alloy film for example contains in film is the Mn more than 5 atom % and below 30 atom %.
Wiring film 35m, for example using oxygen free copper more than purity 3N (99.9%) as raw material, by formation such as sputters, is that 200nm pure Cu film above and below 300nm forms by for example thickness.Here in pure Cu film, can contain inevitable impurity.
Like this, by forming the wiring film 35m being formed by the low-resistance pure Cu barrier film 35b being formed by Cu-Mn alloy, the structure that 35t clips, can suppress the resistance of source-drain electrode 35S, 35D, TFT distribution.In addition, by the Cu-Mn/Cu/Cu-Mn stacked film forming is implemented to thermal treatment, can (IGZO film/Cu-Mn alloy film) form manganese oxide (MnO at the interface of channel part 34 and bottom barrier film 35b
x) film, improve for example diffusion barrier of bottom barrier film 35b.
Like this, IGZO system TFT30 has above-mentioned each electrode 32,35S, 35D and the distribution that is connected respectively with them etc.
Mainly, by above-mentioned source leakage electrode structure, distribution and electronic pads etc. are leaked in source-drain electrode 35S, 35D, source, the distribution structure of the thin film transistor (TFT) that formation present embodiment relates to.Now, can consider to contain above-mentioned gate electrode structure in the distribution structure of TFT, i.e. gate electrode 32, grid distribution, electronic pads.
In addition, at the protective membrane 36 that roughly forms the rear passage 34b that covers source-drain electrode 35S, 35D and expose on whole of glass substrate 31.
The SiO that protective membrane 36 is for example formed by plasma CVD etc.
2film forms.By making protective membrane 36 for SiO
2film, different from silicon nitride (SiN) film etc. using as protective membrane in α-Si system TFT, can not under hydrogen reduction atmosphere but under oxidizing gas atmosphere, form protective membrane 36, can suppress rotten to metallic character of IGZO film.
In addition; even the in the situation that of forming protective membrane 36 under oxidizing gas atmosphere; by being separated with the top barrier film 35t being formed by the Cu-Mn alloy film with high diffusion barrier; thereby can suppress the wiring film 35m that by pure Cu film the formed diffusion oxidation of oxygen to lower floor, suppress the rising of resistance value.
Here the TFT structure that uses Cu-Mn alloy sputtering target 10 to form, is not limited to foregoing.For example, can be by the Cu film that has added any interpolation material in pure Cu for wiring film.In addition, distribution structure can be made in the mode at the one-sided Cu-Mn of the being provided with alloy film of Cu film only and form, do not use Cu film to be only made up of etc. and above-mentioned different membrane structure Cu-Mn alloy film.
The Cu-Mn alloy film that present embodiment can be related in addition, is for the gate electrode structure of above-mentioned TFT structure.Now, for example can obtain pure Cu film as gate electrode film, only one-sided or there is the stepped construction of Cu-Mn alloy film in upper and lower both sides.
Here can, by the Cu film that has added any interpolation material in pure Cu as gate electrode film, in addition, can only form gate electrode structure by Cu-Mn alloy film.
In addition, except using the IGZO system TFT of IGZO film, in the formation of the Cu-Mn alloy film using in ZnO system TFT or α-Si system TFT etc., also can use Cu-Mn alloy sputtering target 10.
In addition, the purposes of TFT is not limited to liquid crystal flat-panel etc., also applicable to TFT etc. for the driving for organic EL.In addition, be not TFT, also go for the distribution structure of the semi-conductive various semiconductor elements of use Si such as Si solar cell device, the distribution structure of touch pad.
Above, embodiments of the present invention are illustrated, but the invention is not restricted to above-mentioned embodiment, in the scope that does not depart from its purport, can carry out various changes.
Embodiment
(1) embodiment 1～3
The various evaluation results of the Cu-Mn alloy film relating to about embodiments of the invention 1～3, together describe with comparative example 1,2.
The making of Cu-Mn alloy sputtering target
First, make and contain the embodiment 1～3 of Mn that mean concns is 10 atom % and the Cu-Mn alloy sputtering target that comparative example 1,2 relates to by the gimmick same with above-mentioned embodiment.But, in comparative example 1,2, the processing that contains the prerequisite that exceeds above-mentioned embodiment.In addition, in order to be installed on the sputter equipment of experiment use, Cu-Mn alloy sputtering target be shaped as the discoideus of diameter 100mm, thickness 5mm.
The crystal structure observation of Cu-Mn alloy
To before being configured as Cu-Mn alloy sputtering target, i.e. the milled sheet of the Cu-Mn alloy after just rolling, analyzes Mn concentration in mensuration milled sheet and poor by EDX.The mensuration of analyzing by EDX is to cut out and carry out for the block milled sheet of 1cm × 1cm size for 3.Now, in order not to be subject to the impact of the easy degree difference of etching of Cu and Mn, do not carry out the etching after mirror ultrafinish.For each milled sheet, in the visual field of 200 μ m × 100 μ m, carry out the surface analysis of EDX in 10 positions choosing at random, by the mean concns of the Mn concentration of the each point of the EDX surface analysis gained in the visual field of 200 μ m × 100 μ m of each position, as the mean concns of Mn.And for 10 positions measuring point separately, the highest part to Mn concentration and lowermost portion are implemented the point analysis of EDX, obtain the poor of the maximum value of Mn concentration and minimum value and mean concns.Concrete mensuration flow process is below shown.
Use S-4300 that Hitachi manufactures, utilize 500 times of multiplying powers (the ≈ 250 μ m visuals field, μ m × 180)～multiplying power 1000 times (≈ 120 μ m visuals field, μ m × 70) to obtain SEM images.Now, the acceleration voltage that makes electron beam gun is 15kv, and W.D. (operating distance: the distance of object lens and sample) is 15mm.Foreign matter, the impurity when casting, brought into should be got rid of by measuring, and select not have the visual field of foreign matter, hole.
For the whole region in this visual field, the face tracing (Mapping) that uses EDX to carry out Cu and Mn element is analyzed.Be more than 30 minutes analysis time,, utilizes determinator to continue scanning therebetween.Here, note making analysis time not long, unclear with the aberration of the tracing avoiding representing with different colours.
Then, confirm the darkest part (Mn concentration the best part) of the color that represents Mn and the most shallow part (part of Mn concentration minimum) by range estimation, carry out point analysis in these parts by EDX.The probe diameter of EDX analyzer is used common size, and (m～tens of μ m) for number μ.The time of point analysis is 1 minute.
By above EDX point analysis, obtain the spectrum for the intensity of each wavelength.For each peak of this spectrum, be accredited as Cu, Mn, other elements.In addition, the quantitative analysis results that is obtained forming by spectral intensity, obtains the poor of the maximum value of Mn concentration and minimum value and its mean concns.
In addition, for the milled sheet of the Cu-Mn alloy after just rolling, record by SEM the number that maximum diameter is foreign matter more than 5 μ m.The observation that utilizes SEM is to cut out and carry out for the block milled sheet of 1cm × 1cm for 3.Now, the number of the foreign matter that the surface of each milled sheet is exposed is counted, the number using the mean value of 3 milled sheets as the foreign matter of this embodiment or comparative example, the foreign matter in each 1cm × 1cm there is frequency.In addition, now, the average crystallite particle diameter in the crystal structure of mensuration Cu-Mn alloy.
The evaluation of paradoxical discharge
The Cu-Mn alloy sputtering target obtaining as mentioned above (diameter 100mm, thickness 5mm) is installed on as shown in Figure 4 to the sputter equipment 120 of the detection device system 60 that is provided with arc-over, measures the number of times of arc-over.
Particularly, be connected with the substrate maintaining part 122s as electrode of substrate by the analyzer 61(DC power supply 124 of being located between outgoing side and the substrate maintaining part 122s of DC power supply 124), detect the electric current and the voltage that put between substrate maintaining part 122s and target maintaining part 122t relative with substrate maintaining part 122s, that become negative potential.For the electric current detecting and voltage, the arc monitor 62 of controlling by the control part 63 being made up of computer etc. is monitored, and is determined with without arc-over and occurs, and measure the frequency of arc-over simultaneously.
The condition of sputter is now shown in following table 1.For arc-over is easily occurred, be here high by DC power setting.Depth of corrosion under this condition is about 2mm in the time of continuous sputter in 2 hours.
Table 1
| DC power | 1kW |
| Process gas | Ar |
| Cavity pressure | 0.5Pa |
| Sputtering time | 2 hours |
That is to say, thereby the condition of table 1 is the limiting condition due to temperature rise that for a long time sputter the causes degree that according to circumstances bonding of target and backboard is peeled off.Here the impact that the paradoxical discharge that, sputter has occurred in 30 seconds of sputter after just having started contacts with atmosphere as target and within number of times not included in paradoxical discharge.
Evaluation result
Be shown in following table 2 by the various evaluation results that obtain above.
Table 2
In addition, the SEM image that the crystal structure after the hot rolling of the Cu-Mn alloy that embodiment 1,2 is related to is observed has been shown in Fig. 5.In addition, the SEM image that the crystal structure after the hot rolling of the Cu-Mn alloy that comparative example 1,2 is related to is observed has been shown in Fig. 6.
As shown in Figure 5, in the crystal structure of embodiment 1,2 (being respectively Fig. 5 (a), (b)), do not confirm foreign matter, hole.On the other hand, as shown in Fig. 6 (a), in comparative example 1, in crystal structure, confirm foreign matters (in figure, arrow) more than maximum diameter 5 μ m.If analyze by EDX, foreign matter is the Mn that contains high density and the oxide compound that contains C, S, Si etc.In addition, as shown in Fig. 6 (b), in comparative example 2, in crystal structure, confirming maximum diameter is holes (in figure, arrow) more than 5 μ m.If analyze by EDX, divide in hole portion the Mn, the C that detect high density.Thereby, think that this hole is the vestige that the foreign matter that is made up of such composition comes off.
In addition, as shown in table 2, temperature when hot rolling is higher, and degree of finish is higher, and the number of the foreign matters more than corresponding 5 μ m of unit surface (1cm × 1cm) (foreign matter exist frequency) has the tendency tailing off.Think by the hot rolling under such condition, make the crystal structure homogenizing of Cu-Mn alloy, foreign matter is spread and tail off.
In addition, temperature when hot rolling is higher, and degree of finish is higher, and poor (the Mn concentration difference) of the maximum value of Mn concentration and minimum value and mean concns has the tendency diminishing.Think by the hot rolling under such condition, make the crystal structure homogenizing of Cu-Mn alloy, foreign matter is spread and tail off.
In addition, by having crystal structure such shown in table 2, the frequency of the paradoxical discharge of any in embodiment 1～3 is 0 time～1 time.On the other hand, in comparative example 1,2, the frequency of paradoxical discharge is respectively 11 times, 18 times, and paradoxical discharge occurs with high frequency.
(2) embodiment 4～7
The various evaluation results of the Cu-Mn alloy film relating to about embodiments of the invention 4～7, together describe with comparative example 3～6.
By the gimmick same with above-described embodiment, make and contain the embodiment 4～7 of Mn that mean concns is 5 atom % and 30 atom % and the Cu-Mn alloy sputtering target that comparative example 3～6 relates to, carry out same evaluation with above-described embodiment.Evaluation result is shown in following table 3.
Table 3
As shown in table 3, meet in the embodiment 4～7 of above-mentioned condition at temperature and the degree of finish of hot-rolled process, the difference of Mn concentration and foreign matter exist frequency all in specialized range.But the mean concns of the Mn in Cu-Mn alloy is high if think, foreign matter exist frequency high, become easily because Mn and impurity reaction produce foreign matter.In addition, particularly, if the difference of Mn concentration in ± 0.5 atom %, can make the frequency that has frequency and paradoxical discharge of foreign matter be respectively zero, obtain preferred result.
On the other hand, do not meet in the comparative example 3～6 of above-mentioned condition at temperature and the degree of finish of hot-rolled process, the difference of Mn concentration and foreign matter there is at least one specialized range exceeding of frequency.
Claims (8)
1. a Cu-Mn alloy sputtering target, is characterized in that, to contain the Mn of mean concns more than 5 atom % and below 30 atom % and the Cu-Mn alloy of average crystallite particle diameter more than 10 μ m and below 50 μ m as mother metal,
Utilizing the maximum value of Mn concentration and the difference of minimum value and described mean concns that X-ray energy spectrum analysis obtains is in ± 2 atom %.
2. Cu-Mn alloy sputtering target according to claim 1, it is characterized in that, in described Cu-Mn alloy, exist and contain than at least one the foreign matter in the Mn of described mean concns greater concn and impure oxide compound, in crystal structure in the 1cm × 1cm of described Cu-Mn alloy, maximum diameter is that described foreign matters more than 5 μ m is below 10.
3. Cu-Mn alloy sputtering target according to claim 2, is characterized in that, described impurity is at least one in C, S, Si, P.
4. Cu-Mn alloy sputtering target according to claim 2, it is characterized in that, described impurity is at least one in C, S, Si, P, and the mean concns of described impurity in the crystal structure of described Cu-Mn alloy is that C is below 10ppm, S is below 20ppm, Si is below 20ppm, P is below 100ppm.
5. according to the Cu-Mn alloy sputtering target described in any one in claim 1～4, it is characterized in that, the difference of the maximum value of described Mn concentration and minimum value and described mean concns is in ± 0.5 atom %.
6. the manufacture method of a Cu-Mn alloy sputtering target, it is characterized in that, the raw material that the Cu with respect to more than purity 3N has been added to Mn more than purity 3N in the mode of the mean concns more than reaching 5 atom % and below 30 atom % melts and casts, thereby obtains castings, then
At the temperature by described castings more than 800 DEG C and below 870 DEG C, thereby heating makes the overall evenly heating of described castings, carries out hot rolling with more than 90% degree of finish.
7. a semiconductor element, it is characterized in that, on substrate, possess the distribution structure forming by form Cu-Mn alloy film on oxide semiconductor, described Cu-Mn alloy right to use requires the Cu-Mn alloy sputtering target described in any one in 1～5 or utilizes the Cu-Mn alloy sputtering target of the method manufacture described in claim 6 to form.
8. semiconductor element according to claim 7, is characterized in that, 2 layers of described Cu-Mn alloy film that described distribution structure has pure Cu film and described pure Cu film is clipped in the middle.
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| CN109695021A (en) * | 2017-10-23 | 2019-04-30 | 迪睿合株式会社 | Mn-Zn-W-O base sputtering target material and preparation method thereof |
| CN115612872A (en) * | 2022-09-27 | 2023-01-17 | 同创普润(上海)机电高科技有限公司 | Smelting process of ultra-pure copper-manganese alloy |
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| TW201529877A (en) * | 2013-12-27 | 2015-08-01 | Jx Nippon Mining & Metals Corp | High-purity copper or copper alloy sputtering target, and method for producing same |
| JP6435981B2 (en) * | 2015-04-28 | 2018-12-12 | 三菱マテリアル株式会社 | Copper alloy sputtering target |
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