CN101778962A - Method for thin film formation - Google Patents
Method for thin film formation Download PDFInfo
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- CN101778962A CN101778962A CN200880102838A CN200880102838A CN101778962A CN 101778962 A CN101778962 A CN 101778962A CN 200880102838 A CN200880102838 A CN 200880102838A CN 200880102838 A CN200880102838 A CN 200880102838A CN 101778962 A CN101778962 A CN 101778962A
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 29
- 239000010409 thin film Substances 0.000 title abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 77
- 239000007789 gas Substances 0.000 claims abstract description 72
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000001301 oxygen Substances 0.000 claims abstract description 32
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 32
- 238000005546 reactive sputtering Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000004544 sputter deposition Methods 0.000 claims description 47
- 239000000376 reactant Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 15
- 239000012528 membrane Substances 0.000 claims description 12
- 230000008676 import Effects 0.000 claims description 8
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 238000005240 physical vapour deposition Methods 0.000 claims description 3
- 238000012423 maintenance Methods 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 97
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 23
- 239000010949 copper Substances 0.000 description 22
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 7
- 229910004205 SiNX Inorganic materials 0.000 description 6
- 238000009792 diffusion process Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- 229910052802 copper Inorganic materials 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
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- 125000004429 atom Chemical group 0.000 description 3
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- 238000010586 diagram Methods 0.000 description 3
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
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- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000004044 response Effects 0.000 description 2
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- 238000005245 sintering Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010058490 Hyperoxia Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- 230000003628 erosive effect Effects 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
- H01J37/3411—Constructional aspects of the reactor
- H01J37/3444—Associated circuits
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02266—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by physical ablation of a target, e.g. sputtering, reactive sputtering, physical vapour deposition or pulsed laser deposition
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
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- Optics & Photonics (AREA)
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- Thin Film Transistor (AREA)
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Abstract
This invention provides a method for thin film formation, which, in the formation of an oxide film by reactive sputtering, even when the thin film formation is carried out by a CVD process in the subsequent step, can prevent a lowering in oxygen concentration around the interface of the film and a substrate to avoid a lowering in adhesive strength between the substrate and the oxide film. While introducing a sputter gas and a reactive gas into a sputter chamber (11a) in a vacuum atmosphere, electric power is applied to targets (41a) to (41h) arranged so as to face a substrate (S) to be treated within the sputter chamber (11a), and the targets are sputtered by ions in a plasma atmosphere to form a predetermined thin film on the surface of the substrate by reactive sputtering. In this case, a region having a high reactive gas component concentration is formed in a period where the thin film is formed to a predetermined thickness.
Description
Technical field
The present invention relates to a kind of film formation method that forms the film of regulation by sputtering method at substrate surface to be processed.
Background technology
Sputtering method is as one of method that forms the film of stipulating at substrate surfaces such as glass or silicon wafers, this method is according to make ion under the plasma atmosphere to the target acceleration shock of making in the substrate surface film-forming components, sputtering particle (target atom) is dispersed, adhere to, be deposited in the surface of substrate, thereby form the film of regulation.Simultaneously, import reactant gasess such as oxygen or nitrogen, obtain this film by reactive sputtering.
In recent years, in the manufacturing process of the liquid-crystal display (FPD) that adopts TFT (thin film transistor), the film forming method of above-mentioned sputtering method for example formed in the metallic membranes such as Cu good as the characteristics of electrical conductivity of gate electrode on the surface of glass substrate and also to be utilized.
Wherein, when glass baseplate surface directly formed the Cu film, how improving this Cu film was very big problem to the binding property of glass surface.As one of this way to solve the problem, method in the known patent document 1 is, oxide compound as sintering adjuvant is exposed on the substrate surface, then, form the Cu film by PVD methods such as sputtering methods, guarantee the high bond strength of Cu the oxide compound that constitutes by the sintering adjuvant that is exposed to the substrate top layer.
Patent documentation 1: the spy opens the 2003-3884 communique
Summary of the invention
(problem that invention will solve)
Yet, in the manufacture craft of TFT substrate, for the situation that on the surface of glass substrate, forms the gate electrode that constitutes by Cu, according to the method for record in the above-mentioned patent documentation 1, form the oxide film that contains Cu by reactive sputtering, and form the metallic membrane that contains Cu by sputter.But, after obtaining above-mentioned gate electrode, in next operation, on this gate electrode, generally form the insulating film that constitutes by SiNx with plasma CVD method.When forming film, adopt the N that imports in the treatment chamber by this plasma CVD method
2, NH
3And SiH
4Mixed gas as process gas.
Like this, when forming film by the CVD method, the radiant heat of plasma body etc. are with the glass substrate heating, thereby the oxygen in making oxide film takes place in the diffusion, again the hydrogen that is decomposed in plasma body, NH
3Or SiH
4Reduction is released to outside the film, and consequently the oxygen concn in the oxide film (reactant gas composition contain concentration) reduces.At this moment, when the oxygen concn of the near interface of glass substrate is reduced to the threshold value of regulation, there is the significantly reduced problem of bond strength.In this case, can consider when forming oxide film, to improve in advance the oxygen concn in the film, but this makes again the ratio resistance value of oxide film too high.
Therefore, in view of the above problems, the invention provides a kind of film formation method, even in next operation, undertaken under the situation of formation of film by the CVD method, the oxygen concn that also can prevent the near interface of glass substrate reduces, and can not cause the bond strength of substrate and oxide film to reduce.
(means of dealing with problems)
In order to address the above problem, film formation method according to claim 1 record, when importing sputter gas and reactant gases in the sputtering chamber under vacuum atmosphere, in sputtering chamber, apply electric power to being set to the target relative with substrate to be processed, carry out sputter by the ion pair target under the plasma atmosphere, form the film of regulation at substrate surface by reactive sputtering, it is characterized in that, described film reach regulation thickness during in, form the zone contain high density reactant gases composition.
According to the present invention, in during the thickness that reaches regulation at described film, form the zone of containing high density reactant gases composition, interface from substrate in this film increases direction to thickness, there is gradient in the concentration that contains of reactant gases composition, even so in next operation, causing under the condition of diffusion and reduction reaction, the glass substrate that has for example formed oxide film is implemented predetermined process, also can inhibited oxidation thing film and the oxygen diffusion of the near interface of substrate, thus prevent to reduce at this near interface oxygen concn.
In the present invention, in sputter, keep importing to the flow rate of reactive gas constant while in the sputtering chamber, by being transformed into low power from superpower to the electric power that target applies, carry out the described formation that contains high density reactant gases composition range, just can be by only changing the power supply control of original sputter equipment, at the film forming sputter rate that reduces of thickness according to the rules, thereby realize to improve the concentration that contains of reactant gases composition in the film midway.
In addition, by carry out the described switching that applies electric power according to certain cycle, just can form a plurality of zones of containing high density reactant gases composition partly, in addition, sputtering time when shortening low power, it is elongated to suppress the film forming sputtering time of thickness that is used for according to the rules.
Can also adopt in sputter, to keep in the power invariability that target applies, being transformed into high flow capacity from low flow, form the described zone of containing high density reactant gases composition by the flow rate of reactive gas that will import in the sputtering chamber.
Also can carry out the switching of described reaction gas flow in this case according to certain cycle.
And, in the present invention, for the big substrate of area being formed efficiently the film of regulation, can also constitute described target by the multi-disc target with same composition of spacing parallel arranging setting in sputtering chamber with regulation, after in a single day described reactant gases is diffused into the space of back face of target side, supply with described reactant gases to substrate by each target gap each other.Thus, it is unbalanced just can to prevent that by simple structure substrate is imported reactant gases, can prevent the reaction of real estate internal cause uneven and cause become inhomogeneous in that real estate internal ratio resistance value etc. is membranous.
Also have, with the gas that contains aerobic as reactant gases, can be applicable to the film formation method that comprises following operation: require the 1 film formation method of putting down in writing in any one claim to the claim 6 on substrate surface, to form the operation of the oxide film that contains Cu by aforesaid right, on the surface of this oxide film, form the operation of the metallic membrane that contains Cu, on the surface of this metallic membrane, form the operation of insulating film by the CVD method with the process gas of regulation by the PVD method.
Thus, in the manufacture craft of TFT substrate, after use film formation method of the present invention has formed the oxide film that contains Cu, the stacked metallic membrane of Cu that contains is to form gate electrode, form under the situation of the insulating film that constitutes by SiNx with plasma CVD method in next operation, can prevent to reduce, thereby guarantee the bond strength height of copper the oxide compound that on substrate surface, forms at the oxygen concn of the near interface of substrate.In addition, only form the high zone of oxygen concn midway what film formed, the ratio resistance value of this oxide film can't become so high.
Embodiment
With reference to Fig. 1, the 1st, the sputter equipment of Magnetron Mode of the present invention (below be called " sputter equipment ").Sputter equipment 1 is a continuous-flow type, has the vacuum chamber 11 that keeps having the specified vacuum degree by rotor pump, turbomolecular pump equal vacuum gas barrier (not shown).On the top of vacuum chamber 11 substrate transfer apparatus 2 is set.This substrate transfer apparatus 2 has known structure: have the supporting plate 21 that substrate S such as glass substrate are installed, not shown drive unit is intermittently driven, substrate S is transported on the position relative with target described later successively.
In vacuum chamber 11, by to be moved to the target relative position on substrate S when carrying out sputter and forming the film of regulation, in order to prevent that sputtering particle is attached on the sidewall of supporting plate 21 surface and vacuum chamber 11 etc., between substrate transfer apparatus 2 and target, be provided with and be formed with towards the 1st shielding slab 31 of the opening 31a of substrate S, the lower end of the 1st shielding slab 31 extend to the 2nd shielding slab described later near, and cathode electrode C is set at the downside of vacuum chamber 11.
Cathode electrode C has relative multi-disc (being 8 in the present embodiment) the target 41a to 41h that uniformly-spaced is provided with substrate S, thereby can form film efficiently to large-area substrate S.The composition of the film that each target 41a to 41h will form on the surface of substrate S according to oxide compound (ITO) of Cu, Al, Ti, Mo and alloy thereof or indium and tin etc., the employing known method is made, and for example forms roughly cubes identical shapes such as (see and be rectangle) in the above.In the sputter, each target 41a to 41h joins on the backboard 42 of each target of cooling 41a to 41h by matrix materials such as indium or tin.
Each target 41a to 41h is installed on the framework (not shown) of cathode electrode C by insulating element, thereby the sputter face 411 when not using is positioned on the same plane parallel with substrate S.In addition, around the target 41a to 41h that is set up in parallel the 2nd shielding slab 32 is set, the space that is surrounded by the 1st and the 2nd shielding slab 31,32 in vacuum chamber 11 constitutes sputtering chamber 11a.
In addition, cathode electrode C has magnet set zoarium 5 respectively on the position of the rear that is positioned at target 41a to 41h (with sputter face 411 opposite sides).Each magnet set zoarium 5 of same structure has the back up pad (yoke) 51 that be arranged in parallel with each target 41a to 41h.Target 41a to 41h sees when being rectangle in the front, back up pad 51 is made of rectangular flat board, described flat board is made by the magneticsubstance that the adsorptive power of magnet is amplified, this rectangular sheet width is less than each target 41a to 41h, extends to its both sides along the length direction of each target 41a to 41h.On back up pad 51, the rim magnet 53 that the portion in the central of disposing is central magnet 52 that wire is provided with along its length and is provided with around central magnet 52 along the peripheral ring of back up pad 51 is to change the polarity of sputter face 411 sides.
With central magnet 52 be scaled with the volume in when magnetization and for example rim magnet 53 be scaled with magnetization the time volume with (rim magnet: central magnet: rim magnet=1: 2: 1) be designed to equate, form the tunnel-like magnetic line of force of uniform closed loop in the place ahead of each target 41a to 41h respectively.Thus,, the electron density in each target 41a to 41h the place ahead is uprised, thereby can improve plasma density, improve sputter rate by catching the secondary electron that ionized electronics and sputter produce on the side of the place ahead of each target 41a to 41h (sputter face 411).
Each magnet set zoarium 5 links with the drive shaft D1 of the drive unit D that is made of electric motor or cylinder etc. respectively, along parallel between two positions that are set up in parallel direction of target 41a to 41h and constant speed ground one to-and-fro movement.Thus, change the zone that sputter rate uprises, on whole of each target 41a to 41h, all obtain even erosive zone.
Two adjacent targets constitute a pair of target (41a and 41b, 41c and 41d, 41e and 41f, 41g and 41h) among each target 41a to 41h, distribution is provided with AC power E1 to E4 to target to each, and the output cable K1, the K2 that come from AC power E1 to E4 are connected with a pair of target 41a, 41b (41c and 41d, 41e and 41f, 41g and 41h).So apply voltage of alternating current to each a pair of target 41a to 41h by AC power E1 to E4 with alternately changing polarity.
AC power E1 to E4 has identical structure, alternately changes polarity by power feeding section 6 that can supply capability and frequency according to the rules and constitutes to the oscillating portion 7 of a pair of target 41a, 41b (41c and 41d, 41e and 41f, 41g and 41h) output AC voltage.Waveform to the voltage of each target 41a to 41h output roughly is sinusoidal wave, but is not limited to this, can roughly be rectangular wave also for example.The structure of AC power E1 is described below with reference to Fig. 2.
In addition, in power feeding section 6, be provided with: thus be arranged at the switching transistor 65 between DC power line 64a, the 64b and be connected with 1CPU circuit 61 freedom of correspondence ground and the operation of trip switch transistor 65 is controlled to the output voltage of oscillating portion 7 or the 1st driving circuit 66a and the 1PMW pilot circuit 66b of outward current, determine the electric power that applies between a pair of target 41a, the 41b by this output voltage or outward current.In this case, testing circuit 67a and A/D convertor circuit 67b are set, testing circuit 67a has current detection sensor and voltage detecting transformer, detect electric current, voltage between DC power line 64a, the 64b, and described electric current, voltage are input to cpu circuit 61 by testing circuit 67a and A/D convertor circuit 67b.
On the other hand, in oscillating portion 7, be provided with: the 2CPU circuit 71 that is connected with 1CPU circuit 61 freedom of correspondence ground; The formation that is arranged between DC power line 64a, the 64b is vibrated with 4 the 1st to the 4th switching transistor 72a, 72b, 72c, the 72d of switch circuit 72; And be connected, control the 2nd driving circuit 73a and the 2PMW pilot circuit 73b of the operation of each switching transistor 72a, 72b, 72c, 72d with 2CPU circuit 71 freedom of correspondence ground.
So, by the 2nd driving circuit 73a and 2PMW pilot circuit 73b, control the operation of each switching transistor 72a, 72b, 72c, 72d, so that for example the 1st and the 4th switching transistor 72a, 72d, when opposite with the timing of the connection of the 2nd and the 3rd switching transistor 72b, 72c, disconnection, can be by coming from vibration with the alternating-current line of force 74a of switch circuit 72, the alternating-current of 74b sine wave output.The testing circuit 75a and the A/D convertor circuit 75b that detect oscillating voltage, oscillating current are set, and described voltage, electric current are input to 2CPU circuit 71 by testing circuit 75a and A/D convertor circuit 75b.
Alternating-current line of force 74a, 74b use lc circuit through serial or parallel connection and the resonance of this dual mode bonded, are connected with the output transformer 76 with known configurations, and the output cable K1, the K2 that come from output transformer 76 are connected with a pair of target 41a, 41b respectively.In this case, setting has current detection sensor and voltage detecting transformer, detection is input to 2CPU circuit 71 to the output voltage of a pair of target 41a, 41b, the testing circuit 77a and the A/D convertor circuit 77b of outward current by testing circuit 77a and A/D convertor circuit 77b.Thus, can in sputter,, alternately change polarity ground applies any setting to a pair of target 41a, 41b constant power according to certain frequency by AC power E1 to E4.
Have, the 1CPU circuit 61 of each AC power E1 to E4 connects on freedom of correspondence ground each other again, and the output signal that comes from any one cpu circuit 61 makes each AC power E1 to E4 synchronous operation.
In addition, gas gatherer 8 is set in vacuum chamber 11, the sputter gas that will constitute by rare gas such as Ar, according to the forming of the film that will on the surface of substrate S, form, suitably reactant gasess such as oxygen of selecting or nitrogen import in the sputtering chamber (with reference to Fig. 1).Gas gatherer 8 has the flue 81 on the sidewall that is installed in vacuum chamber 11, and flue 81 is communicated with gas source 83a, the 83b of sputter gas and reactant gases respectively by mass flow controller 82a, 82b.
In addition, be used for the downstream side branch of the part of supply response gas in the flue 81 at mass flow controller 82b, be connected with a gas supply pipe 84, this supply-pipe 84 extends by the center of each target in the direction that is set up in parallel of target 41a to 41h at rear side and each target 41a to 41h interval of each magnet set zoarium 5.The size of gas supply pipe 84 is more equal or longer than the whole width of the target 41a to 41h that is set up in parallel, forms a plurality of jet orifice 84a on the position below the gap on the face of these targets 41a to 41h side, between each target 41a to 41h.
So, when making mass flow controller 82a, 82b operation,, sputter gas is imported in the sputtering chamber 11a by between the 1st and the 2nd each shielding slab 13, the 43 and gap between the 1st shielding slab 13 and the substrate transfer apparatus 2.Reactant gases just is supplied to substrate S by each target 41a to 41h each gap each other in case mainly be diffused in the space of rear side of each target 41a to 41h.Thus, can be to substrate S supply response gas lopsidedly, reactant gases roughly exists equably in the space of the target 41a to 41h of substrate S one side, this reactant gases disperses to substrate S from target 41a to 41h, with reacted by plasma-activated sputtering particle, adhere to, be deposited on the surface of substrate.Consequently, can prevent that generation is reactive inhomogeneous in substrate S face, thereby can prevent from substrate S face, to take place than membranous inequalities such as resistance values.
Next as an example of film formation method of the present invention, illustrate in the manufacture craft of TFT substrate and contain the oxide film of Cu, the insulating film (with reference to Fig. 3) that contains the metallic membrane of Cu and constitute by SiNx in the formation of the surface of the glass substrate that utilizes.
With the sputter equipment shown in Fig. 11, at first on the surface of glass substrate S, form the oxide film that contains Cu.In this case, use in Cu, added Mg the Cu alloys target as target 41a to 41h.
Next, with being vented to specified vacuum degree (for example 10-5Pa) in the vacuum chamber 11, glass substrate S is transported on the position relative with target 41a to 41h by substrate transfer apparatus 2.Then, according to the constant flow Ar gas and oxygen are imported in the sputtering chamber 11a, apply voltage of alternating current (applying power for example is 20kW) to each paired target 41a to 41h respectively by AC power E1 to E4 by gas gatherer 8.Necessary sputtering time of the thickness that consideration will obtain stipulating and mass production are suitably set the power that applies.In addition, suitably set the gas flow of oxygen, so that caused within the limits prescribed than resistance value place by the oxygen concn in the oxide film.
When each target 41a to 41h applied electric power, each target 41a to 41h alternately switched to anode electrode, cathode electrode, between anode electrode and cathode electrode glow discharge takes place, and formed plasma atmosphere.So, ion in the plasma atmosphere becomes side's acceleration shock of cathode electrode in target 41a to 41h, target atom (sputtering particle) disperses, reacted by plasma-activated sputtering particle and oxygen, adhere to, be deposited on the surface of glass substrate S, thickness according to the rules forms the CuMgO film.
Wherein, in above-mentioned sputter equipment 1, the 1st and the 2nd each shielding slab 31,32 and substrate transfer apparatus 2 are around constituting sputtering chamber 11a.Therefore, import to oxygen flow among the sputtering chamber 11a when constant, according to the power that applies to each target 41a to 41h, that the supply of oxygen is produced is not enough for the amount of dispersing of sputtering particle relatively.In this case, the oxygen concn in the CuMgO film (in the film reactant gases composition contain concentration) reduces (in such CuMgO film, at the oxygen of the near interface of glass substrate S easily to the diffusion of CuMgO film top layer) along with its thickness thickening.
Therefore, in the sputter of present embodiment, in the flow rate of reactive gas constant while that keeps importing among the sputtering chamber 11a, by the pwm control circuit 66b trip switch transistor 65 of each AC power E1 to E4, the power (superpower: for example 20kW) that applies in the time of will applying from common sputter to the power of target 41a to 41h applies the low power of electric power (low power) (with reference to Fig. 4) when being transformed into than common sputter.Wherein, during low power to apply power setting be common sputter the time the scope of the 5-90% that applies power in, preferred 25% (5kW).In addition, the transition period that applies power suitably is set in the scope of 5-95% of sputtering time.
Thus, the CuMgO film reach regulation thickness during in, be low power by applying power transfer, thereby reduce the amount of dispersing of sputtering particle, the high zone of concentration when in the CuMgO film, forming oxygen concn than common sputter.Have again,, can not make this zone effectively surpassing under 90% the situation apply power; In addition, under than 5% little power, it is long that sputtering time becomes, and is unfavorable for mass production.On the other hand, if, can not make this zone effectively surpassing 95% time internal conversion power of sputtering time; In addition, in the time than 5% weak point, it is long that sputtering time becomes, and is unfavorable for mass production.
Then, when the CuMgO film reaches the thickness (setting sputtering time) of regulation, stop the supply of oxygen, will apply to the power of target 41a to 41h simultaneously and be transformed into superpower once more.Thus, the sputtered atom that has dispersed adheres to, is deposited on the surface of CuMgO film, and thickness according to the rules forms the CuMg film that is made of the metallic membrane that contains Cu.
Then, after in accordance with regulations thickness has formed CuMgO film and CuMg film, glass substrate S is transported in the not shown plasma CVD equipment, forms the insulating film that constitutes by SiNx by substrate transfer apparatus 2.Plasma CVD equipment has known structure, and the treatment temp of glass substrate is set at 300 ℃, uses N
2, NH
3And SiH
4Mixed gas as process gas, form above-mentioned insulating film.
Wherein, when forming insulating film because the radiant heat of plasma body etc. are glass substrate S heating, thus when diffusion takes place in the oxygen in the CuMgO film, again by plasma decomposes hydrogen, NH
3And SiH
4Reduction is released to outside the film.Yet, owing in the CuMgO film, there is the high zone of oxygen concn, in this film, have the concentration gradient of the direction that increases to thickness from the interface of glass substrate S,, prevented reduction at this near interface oxygen concn so suppressed the diffusion of oxygen of the near interface of CuMgO film and glass substrate S.Consequently, can guarantee the high bond strength of copper to the oxide compound that forms at substrate surface.In addition, owing to only improve oxygen concn midway in that CuMgO is film formed, so the ratio resistance value of CuMgO film can't become so high.
In addition, in the sputter of present embodiment, in the flow rate of reactive gas constant while that keeps importing among the sputtering chamber 11a, to be transformed into low power from superpower to the power that target 41a to 41h applies, but be not limited thereto, also the power that AC power E1 to E4 is applied is the alternately pulse type (with reference to Fig. 5) of conversion of superpower and low power.Can the cycle according to the rules in insulating film, form partial hyperoxia concentration range thus.At this moment, for the sputtering time that makes the CuMgO film that obtains the regulation thickness not elongated, apply power and sputtering time when suitably setting low power, but, can the power that applies when the not elongated scope of sputtering time makes low power be 0 also according to the oxygen concn that obtains in the CuMgO film.
In addition, in the present embodiment, in sputter, keep importing to the flow rate of reactive gas constant while among the sputtering chamber 11a, the power that conversion applies to target 41a to 41h, but be not limited thereto, also can controlling quality flow director 82a, 82b, the gas flow of the flow that makes oxygen during (low flow: apply the flow (high flow capacity: 500-1000sccm) (with reference to Fig. 6) that power is Duoed when 10-500sccm) being converted to than common sputter from common sputter.At this moment, also can carry out the increase of described reactant gases feed rate according to certain cycle.
And, in the present embodiment, form the oxide film that contains Cu, contain the metallic membrane of Cu and be that example is illustrated to the surface of glass substrate with what in the manufacture craft of TFT substrate, utilize by the insulating film that SiNx constitutes, but be not limited thereto, can be applicable to that also the metallic membrane that forms regulation is as the source electrode of TFT substrate and the situation of drain electrode.
In embodiment 1, the sputter equipment 1 with shown in Fig. 1 has formed the CuMgO film by reactive sputtering on glass substrate S.In this case, as target, be shaped, engage with backboard 32 with known method with the CuMg that consists of 0.7wt%.
As the condition of reactive sputtering, the controlling quality flow director is set at 890sccm with the gas flow of Ar gas, and the flow set of oxygen in the scope of 240-700sccm, is imported in the vacuum chamber.And the power setting that applies during with superpower is 20kW, and the power setting that applies during with low power is 5kW, and suitably conversion applies power, sets sputtering time to obtain 300
Thickness.
Wherein, sample # 1 and #2 keep applying power invariability on superpower, make the example (comparative example) of the fluctuations in discharge of oxygen, and sample # 3 keeps applying the example (comparative example) of power invariability on low power.On the other hand, sample # 4 to #6 is the example (embodiment) when suitably conversion applies power between superpower and low power.Have, under the situation of sample # 4, the setting power conversion period is to obtain 150 under superpower again
Thickness, under low power, obtain 150
Thickness (with reference to Fig. 4).
Next, the sample # 1 to #6 that has formed the CuMgO film by above-mentioned condition on the surface of glass substrate is continued to form the CuMg film by above-mentioned sputter equipment.As sputtering condition, the controlling quality flow director is set at 890sccm with the gas flow of Ar gas, imports in the vacuum chamber.And will apply power setting is 75kW, sets sputtering time to obtain 3000
Thickness.
Next, the sample # 1 to #6 that has formed CuMgO film and CuMg film is formed the SiNx film by known plasma CVD equipment.As the condition of plasma CVD, substrate temperature is set at 300 ℃, use N
2, NH
3And SiH
4Mixed gas as process gas, form 3000
Thickness.
Fig. 7 is the table of the relation between the binding property of the ratio resistance value of CuMgO film monofilm of sample # 1 to #6 of the above-mentioned making of expression and CuMg/CuMgO stack membrane.Wherein, binding property is estimated with following so-called band method of inspection.That is,, according to certain interval 10 cut line are set respectively in the horizontal direction with on the vertical direction, attach adhesive tape being provided with on the zone of these cut line then, peel off with ciamond cutter to the sample # 1 to #6 that obtains as mentioned above.Then, the average evaluation that the area that only has in the film that cut line centered on below 5% is not attached on the band is that binding property is good.On the other hand, measure with known method than resistance value.
Judge thus, the gas flow during reactive sputtering can not obtain sufficient binding property (sample #1) after a little while, on the other hand, the gas stream quantitative change for a long time, binding property improves, but uprise (sample #2) than resistance value.In addition, when under low power, carrying out reactive sputtering, obtaining the sufficient fusible while, also can make, but sputtering time is 32 seconds, is unfavorable for producing in batches than resistance value step-down.
At this problem, during the conversion reaction sputter apply power the time, also can make than resistance value step-down obtaining the sufficient fusible while, in addition, can also make sputtering time shorten to 20 seconds.Especially, can judge sample # 4 be sample # 2 the ratio resistance value about 1/6.
Description of drawings
Fig. 1 is a constructed profile of implementing the sputter equipment of film formation method of the present invention.
Fig. 2 is the structural representation of the AC power that adopts in the sputter equipment shown in the explanatory view 1.
Fig. 3 is the figure that the film in the explanation TFT substrate manufacture technology forms.
Fig. 4 implements to apply the control synoptic diagram of electric power and reaction gas flow under the situation of film formation method of the present invention.
Fig. 5 is that explanation is implemented to apply the variation synoptic diagram of the control of electric power and reaction gas flow under the situation of film formation method of the present invention.
Fig. 6 is that explanation is implemented to apply the variation synoptic diagram of electric power and reaction gas flow control under the situation of film formation method of the present invention.
Fig. 7 is the film formation condition that is illustrated among the embodiment 1 sample of making, than the table of resistance value and fusible experimental result.
Description of reference numerals
1 sputter equipment
The 11a sputtering chamber
31,32 shielding slabs
41a to 41h target
65 switching elements
8 gas gatherers
E1 to E4 AC power
The S substrate
Claims (7)
1. film formation method, described method is when importing sputter gas and reactant gases in the sputtering chamber under vacuum atmosphere, in sputtering chamber, apply electric power to being set to the target relative with substrate to be processed, carry out sputter by the ion pair target under the plasma atmosphere, form the film of regulation at substrate surface by reactive sputtering, it is characterized in that
During described film reaches the thickness of regulation, form the zone of containing high density reactant gases composition.
2. film formation method as claimed in claim 1, it is characterized in that, the flow rate of reactive gas that imports in the sputtering chamber by maintenance in sputter is constant, will be transformed into low power from superpower to the electric power that target applies simultaneously, forms the described zone of containing high density reactant gases composition.
3. film formation method as claimed in claim 2 is characterized in that, carries out the described switching that applies electric power according to certain cycle.
4. film formation method as claimed in claim 1, it is characterized in that, by in sputter, keeping when target applies firm power, the flow rate of reactive gas that imports in the sputtering chamber being transformed into high flow capacity from low flow, form the described zone of containing high density reactant gases composition.
5. film formation method as claimed in claim 4 is characterized in that, carries out the increase of described reactant gases feed rate according to certain cycle.
6. as any one the described film formation method in the claim 1 to 5, it is characterized in that, the multi-disc target with same composition of the spacing parallel arranging setting that can also stipulate by being separated by in sputtering chamber constitutes described target, after in a single day described reactant gases is diffused into the space of back face of target side, supply with described reactant gases to substrate by each target gap each other.
7. film formation method, it is characterized in that, comprise following operation: use oxygen-containing gas as reactant gases, by aforesaid right require 1 to the claim 6 any one film formation method of putting down in writing on substrate surface, form the operation of the oxide film that contains Cu, on the surface of this oxide film, form the operation of the metallic membrane that contains Cu, on the surface of this metallic membrane, form the operation of insulating film by the CVD method with the process gas of regulation by the PVD method.
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| JP2007208789A JP5186152B2 (en) | 2007-08-10 | 2007-08-10 | Thin film formation method |
| JP2007-208789 | 2007-08-10 | ||
| PCT/JP2008/064007 WO2009022573A1 (en) | 2007-08-10 | 2008-08-05 | Method for thin film formation |
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| CN101778962B CN101778962B (en) | 2012-11-28 |
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| KR (1) | KR101209019B1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2014079097A1 (en) * | 2012-11-26 | 2014-05-30 | Cai Shiquan | Evaporated metal film, manufacturing intermediate therefor and method for preparing same |
| CN104064454A (en) * | 2014-06-11 | 2014-09-24 | 京东方科技集团股份有限公司 | Thin film and array substrate preparation method and array substrate |
| CN111902562A (en) * | 2018-03-16 | 2020-11-06 | 株式会社爱发科 | Film forming method |
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| JP5339965B2 (en) | 2009-03-02 | 2013-11-13 | 株式会社アルバック | AC power supply for sputtering equipment |
| JP5604056B2 (en) * | 2009-05-15 | 2014-10-08 | 関東化学株式会社 | Etching solution for copper-containing laminated film |
| US20140083841A1 (en) * | 2011-05-13 | 2014-03-27 | Sharp Kabushiki Kaisha | Thin film-forming method |
| KR101673224B1 (en) * | 2014-11-17 | 2016-11-16 | 전영권 | Solar cells and manufacturing method for the same |
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| JPS63114965A (en) * | 1986-11-01 | 1988-05-19 | Tosoh Corp | Production of laminated film |
| JP2001192822A (en) | 2000-01-07 | 2001-07-17 | Nippon Sheet Glass Co Ltd | Film deposition method, and article obtained by the same |
| JP4071020B2 (en) * | 2002-03-18 | 2008-04-02 | 株式会社アルバック | Photocatalyst layer forming method |
| JP4780972B2 (en) * | 2004-03-11 | 2011-09-28 | 株式会社アルバック | Sputtering equipment |
| JP2006302975A (en) * | 2005-04-15 | 2006-11-02 | Toshiba Corp | Semiconductor device and manufacturing method thereof |
| JP4669992B2 (en) * | 2005-09-28 | 2011-04-13 | Ｄｏｗａホールディングス株式会社 | Nitrogen-containing chromium coating, method for producing the same, and mechanical member |
| CN1966758A (en) * | 2005-11-18 | 2007-05-23 | 电子科技大学 | Process for preparing vanadium oxide film |
| JP5291907B2 (en) * | 2007-08-31 | 2013-09-18 | 株式会社アルバック | Sputtering equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2014079097A1 (en) * | 2012-11-26 | 2014-05-30 | Cai Shiquan | Evaporated metal film, manufacturing intermediate therefor and method for preparing same |
| CN104064454A (en) * | 2014-06-11 | 2014-09-24 | 京东方科技集团股份有限公司 | Thin film and array substrate preparation method and array substrate |
| US9487867B2 (en) | 2014-06-11 | 2016-11-08 | Boe Technology Group Co., Ltd. | Method for preparing a film and method for preparing an array substrate, and array substrate |
| CN111902562A (en) * | 2018-03-16 | 2020-11-06 | 株式会社爱发科 | Film forming method |
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| KR20100041821A (en) | 2010-04-22 |
| WO2009022573A1 (en) | 2009-02-19 |
| JP2009041082A (en) | 2009-02-26 |
| TW200912022A (en) | 2009-03-16 |
| CN101778962B (en) | 2012-11-28 |
| JP5186152B2 (en) | 2013-04-17 |
| KR101209019B1 (en) | 2012-12-10 |
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