CN103403847A - Silicon nitride film deposition method, organic electronic device manufacturing method, and silicon nitride film deposition device - Google Patents
Silicon nitride film deposition method, organic electronic device manufacturing method, and silicon nitride film deposition device Download PDFInfo
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- CN103403847A CN103403847A CN2012800105318A CN201280010531A CN103403847A CN 103403847 A CN103403847 A CN 103403847A CN 2012800105318 A CN2012800105318 A CN 2012800105318A CN 201280010531 A CN201280010531 A CN 201280010531A CN 103403847 A CN103403847 A CN 103403847A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 144
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 238000000151 deposition Methods 0.000 title abstract description 16
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- 239000007789 gas Substances 0.000 claims abstract description 311
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 82
- 238000012545 processing Methods 0.000 claims abstract description 68
- 239000000758 substrate Substances 0.000 claims abstract description 68
- 229910000077 silane Inorganic materials 0.000 claims abstract description 45
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 44
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 230000015572 biosynthetic process Effects 0.000 claims description 55
- 239000001257 hydrogen Substances 0.000 claims description 46
- 229910052739 hydrogen Inorganic materials 0.000 claims description 46
- 238000000034 method Methods 0.000 claims description 43
- 229910052757 nitrogen Inorganic materials 0.000 claims description 40
- 239000012528 membrane Substances 0.000 claims description 30
- 150000002431 hydrogen Chemical class 0.000 claims description 13
- 238000009832 plasma treatment Methods 0.000 claims description 9
- 238000007789 sealing Methods 0.000 abstract description 4
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 54
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 36
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- 229910052786 argon Inorganic materials 0.000 description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 17
- 229910021529 ammonia Inorganic materials 0.000 description 8
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- 238000001035 drying Methods 0.000 description 6
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 description 6
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 6
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- 239000012467 final product Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
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- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 3
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 2
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 2
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- 238000009616 inductively coupled plasma Methods 0.000 description 2
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- 150000002831 nitrogen free-radicals Chemical class 0.000 description 2
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- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910017083 AlN Inorganic materials 0.000 description 1
- 206010027146 Melanoderma Diseases 0.000 description 1
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
- 229910006294 Si—N Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
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- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 description 1
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000006884 silylation reaction Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
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- 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
- H01L21/02271—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 decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/02274—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 decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
- C23C16/345—Silicon nitride
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Abstract
A silicon nitride film deposition method for depositing a silicon nitride film on a substrate housed in a processing vessel, wherein a processing gas containing a silane gas, a nitrogen gas and a hydrogen gas is supplied to the processing vessel, plasma is generated by exciting the processing gas, and a silicon nitride film is deposited on the substrate by means of plasma processing with said plasma. The silicon nitride film is used as a sealing film of an organic electronic device. During the plasma processing with said plasma, the pressure inside the processing vessel is maintained between 20-60Pa.
Description
Technical field
The present invention relates to the film build method of silicon nitride film, the manufacture method of organic electronic device and the film formation device of silicon nitride film.
Background technology
In recent years, developing as the organic EL that comprises the organic electroluminescent (EL:Electro Luminescence) of the luminescent device of organic matter layer.Organic EL is due to for self-luminous,, so power consumption is little, has in addition and compares the advantages such as visual angle is outstanding with liquid crystal display (LCD) etc., and development is from now on expected.
The most basic structure of this organic EL is the lit-par-lit structure (sandwich construction) that forms at glass substrate superimposed layer anodal (anode) layer, luminescent layer and negative pole (negative electrode) layer.Wherein, luminescent layer to water, oxygen a little less than, when sneaking into water, oxygen, its characteristic changes, and produces non-luminous point (blackspot), becomes a reason of the lost of life of organic EL.Therefore, in the manufacturing of organic electronic device, so that the mode that outside water, oxygen do not see through in device seal and stopped organic element.That is, in the manufacturing of organic electronic device, form successively anodal layer, luminescent layer, negative electrode layer on glass substrate, and then form diaphragm seal (sealing film) layer.
, as above-mentioned diaphragm seal, for example can use silicon nitride film (SiN film).This silicon nitride film for example forms by plasma CVD (Chemical Vapor Deposiotion).Particularly, for example utilize the power of microwave to make and comprise silane (SiH
4) gas, nitrogen (N
2) unstrpped gas excite and generate plasma, use the plasma that generates to form silicon nitride film.In addition, there is the problem that sustains damage in organic EL when the temperature of glass substrate reaches high temperature more than 100 ℃, so silicon nitride film forms (patent documentation 1) under the low temperature environment below 100 ℃.
The prior art document
Patent documentation
Patent documentation 1: the JP 2010-219112 of Japan communique
Summary of the invention
The problem that invention will solve
But in the situation that use the method for patent documentation 1 record, silicon nitride film forms under low temperature environment, and therefore the membrane property of this silicon nitride film reduces sometimes.Particularly, for example the stepcoverage of silicon nitride film (step coverage), membranous (for example density relevant to the wet etch rate of hydrofluoric acid) are low sometimes, and the membrane stress of silicon nitride film (film stress) is inappropriate sometimes in addition.
In addition, in above-mentioned, illustrated on glass substrate and to have formed the situation of silicon nitride film as the diaphragm seal of organic electronic device, but this problem is sometimes in the situation that form silicon nitride film and also exist in the purposes beyond the diaphragm seal of organic electronic device.That is, when the temperature of substrate forms silicon nitride film on substrate under the low temperature environment below 100 ℃ for example, same as described above, the membranous reduction of silicon nitride film sometimes.
The present invention In view of the foregoing completes, and purpose is, under the temperature of substrate is low temperature environment below 100 ℃, suitably makes the silicon nitride film film forming on substrate, improves the membrane property of this silicon nitride film.
Be used for solving the technical scheme of problem
In order to achieve the above object, according to a viewpoint of the present invention, it is a kind of film build method of silicon nitride film, to form the film build method of silicon nitride film on the substrate in being accommodated in container handling, to supplying with the processing gas that comprises silane based gas, nitrogen and hydrogen in above-mentioned container handling, above-mentioned processing gas excited and generate plasma, implementing to utilize the plasma treatment that this plasma carries out and form silicon nitride film on substrate.
The result of the deep research of inventors is, as can be known when utilizing method for plasma deposition to make the silicon nitride film film forming on substrate, when use comprises the processing gas of silane based gas, nitrogen and hydrogen, for the etching characteristic of the wet etch rate of silicon nitride film, improve.Particularly, by to processing co-feeding gas hydrogen, wet etch rate reduces, and the stepcoverage of silicon nitride film improves.In addition, when the addition that increases the hydrogen of processing gas, the membrane stress of silicon nitride film becomes minus side.That is, can suitably control as can be known the membrane stress of silicon nitride film.Thereby, according to the present invention, even the temperature of the substrate in container handling under the low temperature environment below 100 ℃ for example, also can improve film forming controlled of the silicon nitride film of film forming on substrate.In addition, to processing co-feeding gas hydrogen, the controlled raising of membrane property, describe in detail in aftermentioned this by like this.
According to another viewpoint of the present invention, it is a kind of manufacture method of organic electronic device, form organic element on substrate, then, to supplying with the processing gas that comprises silane based gas, nitrogen and hydrogen in the container handling of taking in this substrate, above-mentioned processing gas excited and generate plasma, implementing the plasma treatment of utilizing this plasma to carry out, the mode that covers above-mentioned organic element of using forms silicon nitride film as diaphragm seal.
In addition,, according to another viewpoint of the present invention, be a kind of film formation device that forms the silicon nitride film of silicon nitride film on substrate, possess: take in substrate and to its container handling of processing; To supplying with the processing gas supply part of the processing gas that comprises silane based gas, nitrogen and hydrogen in above-mentioned container handling; Above-mentioned processing gas is excited and generate the plasma exciatiaon section of plasma; And control part, it controls above-mentioned processing gas supply part and above-mentioned plasma exciatiaon section, to implement to utilize the plasma treatment that above-mentioned plasma carries out, forms silicon nitride film on substrate.
The effect of invention
According to the present invention, under the temperature of substrate is low temperature environment below 100 ℃, suitably form silicon nitride film on substrate, can improve membrane property controlled of this silicon nitride film.
Description of drawings
Fig. 1 is the key diagram for the summary of the formation of the base plate processing system of the manufacture method of the organic EL device of implementing present embodiment.
Fig. 2 means the key diagram of manufacturing process of the organic EL device of present embodiment.
Fig. 3 means the longitudinal section of summary of the formation of plasma film forming apparatus.
Fig. 4 is the plane graph of unstrpped gas supplying structure body.
Fig. 5 is the plane graph of plasma exciatiaon with the structure for gas supply body.
Fig. 6 means in the situation that use the method for plasma deposition of present embodiment, the chart of the relation of the supply flow rate of hydrogen and the wet etch rate of silicon nitride film.
Fig. 7 means in the situation that use the method for plasma deposition of present embodiment, the chart of the relation of the supply flow rate of hydrogen and the membrane stress of silicon nitride film.
Fig. 8 means in the situation that use the method for plasma deposition of present embodiment, the chart of the relation of the power of microwave and the membrane stress of silicon nitride film.
Fig. 9 is the key diagram to the mode as present embodiment uses the processing gas that comprises silane gas, nitrogen and hydrogen to form the situation of silicon nitride film and the situation of using the processing gas comprise silane gas and ammonia to form silicon nitride film as prior art compares.
Figure 10 is the plane graph of the unstrpped gas supplying structure body of another execution mode.
Figure 11 is the sectional view of the unstrpped gas supply pipe of another execution mode.
Figure 12 is the sectional view of the unstrpped gas supply pipe of another execution mode.
Embodiment
Below, with reference to accompanying drawing, embodiments of the present invention are described.Wherein, in this specification and accompanying drawing, the identical Reference numeral of inscape mark for the structure that has in fact identical function, omit repeat specification thus.
At first,, about the manufacture method of the organic electronic device of embodiments of the present invention, with the base plate processing system that is used for implementing this manufacture method, describe in the lump.Fig. 1 means the key diagram of summary of the formation of base plate processing system 1.Fig. 2 means the key diagram of the manufacturing process of organic EL device.In addition, in the present embodiment, for making the situation of organic EL device as organic electronic device, describe.
As shown in Figure 1, the base plate processing system 1 of cluster-type (cluster) has conveying chamber 10.Conveying chamber 10 for example has roughly polygon (being hexagon in illustrated example) when overlooking, inside can be airtight.Around conveying chamber 10, be arranged in order load locking room 11, decontaminating apparatus 12, evaporation coating device 13, sputter equipment 14, Etaching device 15, plasma film forming apparatus 16 on clockwise direction when overlooking.
Be provided with the conveying arm 17 of the multi-joint shape that can stretch and rotate in the inside of conveying chamber 10., by this conveying arm 17, as the glass substrate of substrate, be transported to load locking room 11 and each processing unit 12～16.
And being formed in the narration of back of plasma film formation device 16 describes.In addition, about the decontaminating apparatus 12 of the processing unit as other, evaporation coating device 13, sputter equipment 14, Etaching device 15, use general devices to get final product, omit the explanation of its formation.
Then, the manufacture method of the organic EL device that carries out in the base plate processing system 1 forming as described above described.
As shown in Figure 2 (a) shows, the upper surface at glass substrate G makes positive pole (anode) layer 20 film forming in advance.Anodal layer 20 is such as comprising the transparent conductive material such as tin indium oxide (ITO:Indium Tin Oxide).In addition, anodal layer 20 is such as utilizing sputtering method etc. to be formed at the upper surface of glass substrate G.
Then, in decontaminating apparatus 12, after the surface of the anodal layer 20 with on glass substrate G is cleaned, as shown in Figure 2 (a) shows, in evaporation coating device 13, make luminescent layer (organic layer) 21 film forming by vapour deposition method on anodal layer 20.And, luminescent layer 21 such as the sandwich construction that comprises stacked porose transfer layer, non-luminescent layer (electron block layer), blue light-emitting layer, red light emitting layer, green light emitting layer, electron supplying layer etc.
Then, as shown in Fig. 2 (b), in sputter equipment 14, be formed with on luminescent layer 21 such as negative pole (negative electrode) layer 22 that comprises Ag, Al etc.Negative electrode layer 22 for example forms by utilizing sputter to pile up target atom across patterned mask on luminescent layer 21.In addition, these anodal layers 20, luminescent layer 21 and negative electrode layer 22 form organic ELs of the present invention, below sometimes referred to as " organic EL ".
Then, as shown in Fig. 2 (c), in Etaching device 15, take negative electrode layer 22 as mask, luminescent layer 21 is carried out dry ecthing.Like this, luminescent layer 21 patterns are formed the pattern of regulation.
In addition, also can be after the etching of luminescent layer 21, to organic EL and the anodal layer 20 of glass substrate G() exposed portions serve clean, remove the material that is adsorbed in organic EL, such as organic substance etc., namely clean in advance.And then, after pre-cleaning, also can for example use the silylation of coupling agent to process, form very thin adhesion layer (not shown) on negative electrode layer 22.This adhesion layer and organic EL are bonding securely, and adhesion layer and silicon nitride film described later 23 bonding securely.
Then, as shown in Figure 2 (d) shows, in plasma film forming apparatus 16, with cover luminescent layer 21, negative electrode layer 22 around and the mode of the exposed division of anodal layer 20, for example form the silicon nitride film (SiN film) 23 as diaphragm seal.The formation of this silicon nitride film 23 is for example undertaken by microwave plasma CVD technique as described later.
As mentioned above, the organic EL device A that produces,, by to applying voltage between anodal layer 20 and negative electrode layer 22, can make luminescent layer 21 luminous.This organic EL device A can be applicable to display unit, planar light emitting (illumination, light source etc.), in addition, can be used in various electronic equipments.
Then, the film build method for forming above-mentioned silicon nitride film 23, describe in the lump with the plasma film forming apparatus 16 that makes these silicon nitride film 23 film forming.Fig. 3 means the longitudinal section of summary of the formation of plasma film forming apparatus 16.In addition, the plasma film forming apparatus 16 of present embodiment is to use radial line slot antenna to produce the CVD device of plasma.
Plasma film forming apparatus 16 has for example container handling that the round-ended cylinder shape is arranged 30 of upper surface open.Container handling 30 is for example formed by aluminium alloy.In addition, container handling 30 ground connection.The substantial middle section of the bottom of container handling 30 is provided with mounting table 31 as being used for loading for example mounting portion of glass substrate G.
Mounting table 31 is built-in with for example battery lead plate 32, and battery lead plate 32 is connected with the DC power supply 33 of the outside that is arranged on container handling 30.Utilize this DC power supply 33 to produce electrostatic force on the surface of mounting table 31, can be with glass substrate G Electrostatic Absorption on mounting table 31.In addition, battery lead plate 32 can be connected with high frequency electric source (not shown) with for example bias voltage.
At the upper opening of container handling 30 across such as seals 40 such as being used for guaranteeing bubble-tight O type ring, being provided with dielectric window 41.By this dielectric window 41 with container handling 30 inner sealings.Be provided with the plasma exciatiaon section of radial line slot antenna 42 as the microwave of supplying with plasma generation use on the top of dielectric window 41.In addition, dielectric window 41 for example can use aluminium oxide (Al
2O
3).In this case, dielectric window 41 is for the Nitrogen trifluoride (NF that uses in thermal drying
3) gas has patience (corrosion resistance).In addition, in order further to improve the patience to Nitrogen trifluoride, also can be at the surface coverage yttria (Y of the aluminium oxide of dielectric window 41
2O
3), spinelle (MgAl
2O
4) or aluminium nitride (AlN).
Radial line slot antenna 42 possesses the roughly antenna body 50 cylindraceous of lower surface opening.Peristome at the lower surface of antenna body 50 is provided with the discoid aperture plate 51 that is formed with a plurality of gaps.The top of the aperture plate 51 in antenna body 50 is provided with the dielectric plate 52 that is formed by low loss dielectric substance.Be connected with coaxial waveguide pipe 54 by microwave oscillation device 53 at the upper surface of antenna body 50.Microwave oscillation device 53 is arranged at the outside of container handling 30, can be to the microwave of radial line slot antenna 42 vibration assigned frequencies, for example 2.45GHz.Utilize this formation, from microwave oscillation device 53 microwave that vibrates, be passed in radial line slot antenna 42, compressed by dielectric plate 52 and after the short wavelengthization, in aperture plate 51, produce circularly polarized waves, the 30 interior radiation from dielectric window 41 to container handling.
For example be provided with the roughly unstrpped gas supplying structure body (structure) 60 of writing board shape between mounting table 31 in container handling 30 and radial line slot antenna 42.Unstrpped gas supplying structure body 60 profiles form circle larger than the diameter of glass substrate G at least while overlooking., by this unstrpped gas supplying structure body 60, be divided into the unstrpped gas of the plasma formation zone R1 of radial line slot antenna 42 sides and mounting table 31 sides in container handling 30 from separating regional R2.In addition, unstrpped gas supplying structure body 60 for example can be used aluminium oxide.In this case, because aluminium oxide is pottery, therefore compare with the metal material of aluminium etc. have high-fire resistance, high strength.In addition, owing to not capturing (trap) plasma in plasma formation zone R1 generation, so can be to the sufficient ion of glass substrate irradiation.And,, by the sufficient ion of the irradiation of the film on glass substrate, can generate fine and close film.In addition, the gas of nitrogen trifluoride that uses in 60 pairs of thermal dryings of unstrpped gas supplying structure body has patience.And then,, in order to improve the patience to nitrogen trifluoride gas, on the surface of the aluminium oxide of unstrpped gas supplying structure body 60, can cover yttria, spinelle or aluminium nitride.
As shown in Figure 4, unstrpped gas supplying structure body 60 consists of the continuous unstrpped gas supply pipe 61 that roughly configures to clathrate at grade.It is square that unstrpped gas supply pipe 61 forms longitudinal section when axially seeing.Be formed with a plurality of peristomes 62 in unstrpped gas supply pipe 61 gap each other.The plasma that generates in the plasma formation zone R1 of the upside of unstrpped gas supplying structure body 60 and free radical can enter the unstrpped gas of mounting table 31 sides from separating regional R2 by this peristome 62.
As shown in Figure 3, the lower surface at the unstrpped gas supply pipe 61 of unstrpped gas supplying structure body 60 is formed with a plurality of unstrpped gas supply ports 63.These unstrpped gas supply ports 63 are configuration equably in 60 of unstrpped gas supplying structure bodies.Unstrpped gas supply pipe 61 is connected with flue 65, and this flue 65 is communicated with the unstrpped gas supply source 64 of the outside that is arranged at container handling 30.For example can enclose respectively the silane (SiH as silane based gas in unstrpped gas supply source 64
4) gas and hydrogen (H
2) gas is as unstrpped gas.Flue 65 is provided with valve 66, mass flow controller 67.Utilize this formation, import respectively silane gas and the hydrogen of regulation flow from unstrpped gas supply source 64 by 65 pairs of unstrpped gas supply pipes 61 of flue.And these silane gas and hydrogen are supplied with from separating regional R2 from each unstrpped gas supply port 63 unstrpped gas downwards.
At the inner peripheral surface of the container handling 30 of the outer peripheral face that covers plasma formation zone R1, be formed with the plasma exciatiaon of supplying with the raw material that becomes plasma with the first plasma exciatiaon of gas with gas supply port 70.The first plasma exciatiaon for example is formed at a plurality of positions along the inner peripheral surface of container handling 30 with gas supply port 70.The first plasma exciatiaon is connected with gas supply pipe 72 with the first plasma exciatiaon with gas supply port 70, this first plasma exciatiaon for example connects the side wall portion of container handling 30 with gas supply pipe 72, with the first plasma exciatiaon of the outside that is arranged at container handling 30, with gas supply source 71, be communicated with.Be provided with valve 73, mass flow controller 74 at the first plasma exciatiaon with gas supply pipe 72.Utilize this formation, can be from side to supplying with the plasma exciatiaon gas of regulation flow in the plasma formation zone R1 in container handling 30.In the present embodiment, for example enclose in gas supply source 71 and argon gas (Ar) gas is arranged as plasma exciatiaon gas at the first plasma exciatiaon.
The plasma exciatiaon structure for gas supply body 80 that the roughly writing board shape that for example has the formation same with this unstrpped gas supplying structure body 60 is arranged in the upper surface stacked arrangement of unstrpped gas supplying structure body 60.Plasma exciatiaon forms with gas supply pipe 81 with second plasma exciatiaon of structure for gas supply body 80 by clathrate ground configuration as shown in Figure 5.In addition, plasma exciatiaon for example can use aluminium oxide with structure for gas supply body 80.In this case, also as mentioned above, because aluminium oxide is pottery, therefore compare with the metal material such as aluminium have high-fire resistance, high strength.In addition, due to the plasma that does not capture (trap) and generate in plasma formation zone R1, so can be to the sufficient ion of glass substrate irradiation.And,, by the sufficient ion of the irradiation of the film on glass substrate, can generate fine and close film.In addition, plasma exciatiaon has patience with the nitrogen trifluoride gas that uses in 80 pairs of thermal dryings of structure for gas supply body.And then, in order to improve the patience to nitrogen trifluoride gas, can be at surface coverage yttria or the spinelle of plasma exciatiaon with the aluminium oxide of structure for gas supply body 80.
As described in Figure 3, be formed with a plurality of the second plasma exciatiaons gas supply ports 82 at the second plasma exciatiaon with the upper surface of gas supply pipe 81.These a plurality of second plasma exciatiaons with gas supply ports 82 at plasma exciatiaon with configuration equably in 80 of structure for gas supply bodies.Thus, can supply with upward plasma exciatiaon gas from downside by plasma formation zone R1.In addition, in the present embodiment, this plasma excites with gas and for example is argon gas.In addition, except argon gas, also can be from the plasma exciatiaon nitrogen (N of structure for gas supply body 80 plasma formation zone R1 supplies as unstrpped gas
2) gas.
Be formed with peristome 83 at cancellate the second plasma exciatiaon with gas supply pipe 81 gap each other, the plasma that generates in plasma formation zone R1 and free radical can use by plasma exciatiaon structure for gas supply body 80 and unstrpped gas supplying structure body 60 unstrpped gas below entering from separating regional R2.
The second plasma exciatiaon is connected with flue 85 with gas supply pipe 81, and this flue 85 is communicated with gas supply source 84 with the second plasma exciatiaon of the outside that is arranged on container handling 30.For example enclose respectively in gas supply source 84 at the second plasma exciatiaon and have as plasma exciatiaon with the argon gas of gas with as the nitrogen of unstrpped gas.Be provided with valve 86, mass flow controller 87 at flue 85.Utilize this formation, can supply with respectively from the second plasma exciatiaon nitrogen and the argon gas of regulation flow with gas supply port 82 plasma formation zone R1.
In addition, above-mentioned unstrpped gas and plasma exciatiaon form processing gas of the present invention with gas.In addition, unstrpped gas supplying structure body 60 and plasma exciatiaon form processing gas supply part of the present invention with structure for gas supply body 80.
The both sides that clip mounting table 31 in the bottom of container handling 30, be provided with the exhaust outlet 90 that carries out exhaust for the atmosphere in container handling 30.Exhaust outlet 90 is connected with blast pipe 92, and this blast pipe 92 is communicated with the exhaust apparatus 91 such as turbomolecular pump.Be used to the exhaust from this exhaust outlet 90, can will maintain the pressure of regulation in container handling 30, for example hereinafter described 20Pa～60Pa.
Be provided with control part 100 at above plasma film forming apparatus 16.Control part 100 is for example computer, has program incorporating section (not shown).Take in the program that the film forming to the silicon nitride film 23 on glass substrate G in controlling plasma film forming apparatus 16 is processed in the program incorporating section.In addition, also take in the supply of controlling above-mentioned unstrpped gas, plasma exciatiaon in the program incorporating section with the supply of gas, the radiation of microwave, the action of drive system etc., be used for carrying out the program that the film forming of plasma film forming apparatus 16 is processed.In addition, said procedure is the program of storing in the storage medium of the embodied on computer readable such as the hard disk (HD), floppy disk (FD), CD (CD), magneto optical disk (MO), storage card such as embodied on computer readable, can be also to be installed on the program of control part 100 from this storage medium.
Then, illustrate as the plasma film forming apparatus 16 that forms with upper type in the film build method of the silicon nitride film 23 that carries out.
At first, when for example plasma film forming apparatus 16 starts, from the first plasma exciatiaon with the supply flow rate of the argon gas of gas supply port 70 supplies with from the supply flow rate of the second plasma exciatiaon with the argon gas of gas supply port 82 supplies, the concentration that is adjusted to the argon gas of supplying with in plasma formation zone R1 is even.During this supply flow rate is adjusted, for example make exhaust apparatus 91 work, under the state of identical air-flow, from each plasma exciatiaon, with gas supply port 70,82, supply with the argon gas that is set as suitable supply flow rate when the interior formation of container handling 30 is processed with actual film forming.Then, with this supply flow rate, set, implement film forming on the substrate that actual tests is used, check whether this film forming carries out equably in real estate.In the uniform situation of concentration of the argon gas in plasma formation zone R1, carry out equably the film forming in real estate, the result that therefore checks is, in the situation that do not carry out equably film forming in real estate, change the setting of the supply flow rate of each argon gas, again the substrate of test use is implemented film forming.Repeat above step,, in the concentration of evenly carrying out the argon gas in film forming and plasma formation zone R1 in the real estate uniform mode that becomes, set from each plasma exciatiaon with gas supply port 70,82 supply flow rate.
As mentioned above, set each plasma exciatiaon with gas supply port 70,82 supply flow rate after, the film forming that starts the glass substrate G in plasma film forming apparatus 16 is processed.At first, glass substrate G is moved in container handling 30, absorption remains on mounting table 31.At this moment, the temperature of glass substrate G is maintained below 100 ℃, for example 50 ℃～100 ℃.Then, the exhaust that utilizes exhaust apparatus 91 to start in container handling 30, the pressure in container handling 30 is depressurized the pressure into regulation, and for example 20Pa～60Pa, keep this state.In addition, the temperature of glass substrate G is not limited to below 100 ℃, so long as the temperature that organic EL device A does not sustain damage gets final product, material by this organic EL device A etc. determines.
Herein, the result of the deep research of inventors is when the pressure ratio 20Pa in container handling 30 is low as can be known, likely can not be on glass substrate G film forming silicon nitride film 23 suitably.In addition, when the pressure in container handling 30 surpassed 60Pa, the reaction between the gas molecule in gas phase increased, and likely produces particle (particle) as can be known.Therefore, as mentioned above, the pressure in container handling 30 is maintained 20Pa～60Pa.
While being depressurized in container handling 30, the first plasma exciatiaon from side in plasma formation zone R1 is supplied with argon gas with gas supply port 70, and from the second plasma exciatiaon of below, with gas supply port 82, supplies with nitrogen and argon gas.At this moment, the concentration of the argon gas in plasma formation zone R1 is maintained evenly in plasma formation zone R1.In addition, nitrogen is supplied with the flow of for example 21sccm.From radial line slot antenna 42 under plasma formation zone R1 with the microwave of the power of frequency radiation 2.5kW～3.0kW of for example 2.45GHz.By the radiation of this microwave, argon gas in plasma formation zone R1 by plasma, nitrogen free radical (or ionization).In addition, at this moment, below the microwave of advancing by the plasma absorption that is generated.This result is, the plasma of generating high density in plasma formation zone R1.
The plasma and the free radical that generate in plasma formation zone R1, use structure for gas supply body 80 and unstrpped gas supplying structure body 60 to enter the unstrpped gas of below from separating in regional R2 by plasma exciatiaon.Unstrpped gas is supplied with silane gas and hydrogen from separating regional R2 from each unstrpped gas supply port 63 of unstrpped gas supplying structure body 60.At this moment, for example with the flow of 18sccm, supply with silane gas, for example with the flow of 64sccm, supply with hydrogen.In addition, the supply flow rate of this hydrogen is set according to the membrane property of silicon nitride film 23 as described later.The plasma that silane gas and hydrogen are entered from top respectively is from solution.And, utilize these free radicals and the free radical of the nitrogen supplied with from plasma formation zone R1, pile up silicon nitride film 23 on glass substrate G.
Then, carry out the film forming of silicon nitride film 23, while forming the silicon nitride film 23 of specific thickness on glass substrate G, the supply of the radiation of microwave, processing gas stops.Then, from container handling 30, take out of glass substrate G, a series of plasma deposition processing finishes.
Herein, the result of the deep research of inventors is as can be known when the processing of the plasma deposition by above-mentioned and in the situation that film forming silicon nitride film 23 on glass substrate G, when use comprises the processing gas of silane gas, nitrogen and hydrogen, the controlled raising of the membrane property of silicon nitride film 23.
Fig. 6 is illustrated in the method for plasma deposition that uses above-mentioned execution mode and makes in the situation that the supply flow rate of processing the hydrogen in gas changes, the appearance that changes for the wet etch rate of the silicon nitride film 23 of hydrofluoric acid.In addition, this moment, the supply flow rate of silane gas was 18sccm, and the supply flow rate of nitrogen is 21sccm.In addition, in plasma deposition was processed, the temperature of glass substrate G was 100 ℃.
With reference to Fig. 6 as can be known, by further add hydrogen in comprising the processing gas of silane gas and nitrogen, the wet etch rate of silicon nitride film 23 reduces.Thereby by processing the hydrogen in gas, the density of silicon nitride film 23 improves, and membranous (resistance to chemical reagents, the compactness) of silicon nitride film 23 improves.In addition, the stepcoverage of silicon nitride film 23 also improves.And the refractive index of silicon nitride film 23 for example is increased to 2.0 ± 0.1 as can be known.Thereby,, by controlling the supply flow rate of hydrogen, can control the wet etch rate of silicon nitride film 23, can control the membrane property of silicon nitride film 23.
The method for plasma deposition that Fig. 7 is illustrated in the above-mentioned execution mode of use makes in the situation of the supply flow rate change of processing the hydrogen in gas, the appearance that the membrane stress of silicon nitride film 23 changes.In addition, this moment, the supply flow rate of silane gas was 18sccm, and the supply flow rate of nitrogen is 21sccm.In addition, during plasma deposition was processed, the temperature of glass substrate G was 100 ℃.
With reference to Fig. 7 as can be known, by further add hydrogen in comprising the processing gas of silane gas and nitrogen, the membrane stress of silicon nitride film 23 changes to minus side (compressed side).Thereby,, by controlling the supply flow rate of hydrogen, can control the membrane stress of silicon nitride film 23.
As mentioned above,, according to present embodiment, by making the changes in flow rate of processing the hydrogen in gas, the membrane property of silicon nitride film 23 is changed.Thereby suitably film forming silicon nitride film 23, as the diaphragm seal in organic EL device A, therefore can suitably be made this organic EL device A.In addition, in the situation that be used for diaphragm seal, the absolute value of the size of the stress of diaphragm seal is little better.
In addition, in the method for plasma deposition of present embodiment, use from the microwave of radial line slot antenna 42 radiation and generate plasma.Herein, the result that inventors study discussion as can be known, comprises silane gas, nitrogen and hydrogen in the situation that process gas, and for example the membrane stress of the power of microwave and silicon nitride film 23 has roughly proportionate relationship as shown in Figure 8.Thereby, according to present embodiment, even, by controlling the power of microwave, also can control the membrane stress of silicon nitride film 23.By making the flow optimization of hydrogen, make the microwave power optimization, can obtain critically to possess the film of desired membrane property.Particularly, after the power that determines microwave, the flow optimization of hydrogen is got final product.
But, in prior art, while forming silicon nitride film on glass substrate, also can use above-mentioned silane gas and the ammonia (NH of comprising
3) the processing gas of gas carries out.But the temperature of glass substrate is under the low temperature environment below 100 ℃, and the ammonia corrosion of supplying with before the film forming of silicon nitride film is formed on metal electrode, for example aluminium electrode of the substrate of this silicon nitride film.In addition, due to film forming under low temperature environment, therefore unreacted ammonia be captured (trap) in silicon nitride film.When in silicon nitride film, ammonia was captured, after having carried out environmental test etc., this ammonia was degassed from silicon nitride film, and organic EL device is worsened.
, to this, in the present embodiment, substitute ammonia and use nitrogen.Thereby, can prevent saprophage, organic EL device deteriorated of the metal electrode of above-mentioned substrate.
And,, as present embodiment, use nitrogen to substitute ammonia, and then in the situation that add hydrogen in processing gas, can improve as shown in Figure 9 the membrane property of the silicon nitride film of film forming.That is, can improve membranous (density) of the silicon nitride film in stage portion.In addition, the epimere of Fig. 9 is illustrated in the appearance of the silicon nitride film in the situation of using the processing gas that comprises silane gas and ammonia gas, and lower floor is illustrated in the appearance of the silicon nitride film in the situation of using the processing gas that comprises silane gas, nitrogen and hydrogen.In addition, the left column of Fig. 9 represents the appearance of the silicon nitride film after film forming, and right list is shown and utilized buffered hydrofluoric acid (BHF) to carry out the appearance of the silicon nitride film of wet etching after 120 seconds.
In the plasma film forming apparatus 16 of above execution mode, supply with silane gas and hydrogen from unstrpped gas supplying structure body 60, supply with nitrogen and argon gas from plasma exciatiaon with structure for gas supply body 80, but hydrogen can be supplied with structure for gas supply body 80 from plasma exciatiaon also.Perhaps, hydrogen also can be supplied with structure for gas supply body 80 both sides from unstrpped gas supplying structure body 60 and plasma exciatiaon.Under any circumstance, as mentioned above,, by controlling the supply flow rate of hydrogen, can both control the membrane property of silicon nitride film 23.
Herein, the result that inventors study discussion as can be known, silicon nitride film 23 membranous, particularly the Si-N in film is in conjunction with density at most in the membranous situation of the densification of (greatly), the refractive index of this silicon nitride film 23 is approximately 2.0.In addition, from the viewpoint of the barrier (sealing) of silicon nitride film 23 as can be known, preferred index is 2.0 ± 0.1.
Thereby, be 2.0 ± 0.1 in order to make above-mentioned refractive index, preferably in plasma film forming apparatus 16, the supply flow rate that makes nitrogen is 1～1.5 with respect to the ratio of the supply flow rate of silane gas.To this, usually in the plasma CVD equipment of (having now), utilize silane gas and nitrogen to make in the situation of silicon nitride film film forming, the supply flow rate of nitrogen is generally 10～50 with respect to the ratio of the supply flow rate of silane gas.In common plasma CVD equipment, due to nitrogen as a large amount of in above-mentioned needs, therefore when improving the silane gas flow in order to improve film forming speed, need to the nitrogen flow of above-mentioned increase balance, produce boundary in gas extraction system.Therefore, under the large condition of film forming speed, keep above-mentioned refractive index 2.0 ± 0.1 as the refractive index of silicon nitride film and become difficult.Thereby the plasma film forming apparatus 16 of present embodiment is compared and is played very good effect with common plasma CVD equipment.
In addition, the supply flow rate by controlling nitrogen is with respect to the ratio of the supply flow rate of silane gas, in refractive index is 2.0 ± 0.1 scope, can control the membrane stress of silicon nitride film 23.Particularly, can make this membrane stress approach zero.And then this membrane stress also can be adjusted the power from the microwave of radial line slot antenna 42, the supply flow rate of hydrogen is controlled.
In addition, as mentioned above, with common plasma CVD equipment, compare, can make the supply flow rate of the nitrogen in plasma film forming apparatus 16 for a small amount of, be because of the nitrogen activate that easily makes supply, can improve the degree of dissociation.Namely, while from plasma exciatiaon, with structure for gas supply body 80, supplying with nitrogen, be positioned at very the position of the dielectric window 41 that generates near plasma, compare with gas supply port 82 the easy ionization of nitrogen that is released to the interior plasma formation zone R1 of container handling 30 with the state than higher pressure with the second plasma exciatiaon of structure for gas supply body 80 with above-mentioned plasma exciatiaon thus and generate in large quantities the nitrogen free radical etc. of activity.And as mentioned above, in order to improve the degree of dissociation of nitrogen, plasma exciatiaon is disposed at apart from radial line slot antenna 42(strictly speaking for dielectric window 41 with structure for gas supply body 80) 30mm is with interior position.When inventors investigated, in the situation that this position configuration plasma exciatiaon structure for gas supply body 80, plasma exciatiaon self was disposed at plasma formation zone R1 with structure for gas supply body 80.Therefore, can improve the degree of dissociation of nitrogen.
In the plasma film forming apparatus 16 of above execution mode, the supply of unstrpped gas also can be carried out or plasma carries out before generating simultaneously in the generation of plasma.That is, at first, from unstrpped gas supplying structure body 60, supply with silane gas and hydrogen (or only silane gas).In the supply of this silane gas and hydrogen or after the gas supply, supply with argon gas and nitrogen (and hydrogen) from plasma exciatiaon with structure for gas supply body 80, from radial line slot antenna 42 microwave radiations.And, generate plasma at plasma formation zone R1.
Form the negative electrode layer 22 that contains metallic element herein, on the glass substrate G that forms silicon nitride film 23.When the organic EL device A that for example comprises negative electrode layer 22 was exposed in plasma, negative electrode layer 22 was peeled off from luminescent layer 21, and organic EL A sustains damage sometimes in addition., to this, in the present embodiment,, owing to generating plasma in the supply at silane gas and hydrogen or after supplying with, therefore start the film forming of silicon nitride film 23 in the generation of this plasma.Thereby, this negative electrode layer 22 surperficial protected, organic EL device A is not exposed in plasma, can suitably make organic EL device A.
In the above embodiment, unstrpped gas supply port 63 forms from unstrpped gas supplying structure body 60 downward, the second plasma exciatiaon forms from plasma exciatiaon and uses structure for gas supply body 80 towards top with gas supply port 82, but, these unstrpped gas supply ports 63 and the second plasma exciatiaon also can be the incline direction beyond horizontal direction or vertical below with gas supply port 82, more preferably form from the direction of horizontal direction towards 45 degree that tilt.
In this case, as shown in figure 10, be formed with a plurality of unstrpped gas supply pipes 61 that extend in parallel to each other at unstrpped gas supplying structure body 60.Unstrpped gas supply pipe 61 is equally spaced configuration in unstrpped gas supplying structure body 60.Be formed with as shown in figure 11 the unstrpped gas supply port 63 of base feed gas in the horizontal direction in the both sides, side of unstrpped gas supply pipe 61.Unstrpped gas supply port 63 equally spaced is disposed on unstrpped gas supply pipe 61 as shown in figure 10.In addition, adjacent unstrpped gas supply port 63 forms the rightabout towards mutual horizontal direction.In addition, plasma exciatiaon also can have the formation identical with upper note unstrpped gas supplying structure body 60 with structure for gas supply body 80.And, unstrpped gas supply pipe 61 and plasma exciatiaon with unstrpped gas supplying structure body 60 are roughly cancellate mode with the second plasma exciatiaon of structure for gas supply body 80 with gas supply pipe 81, dispose unstrpped gas supplying structure body 60 and plasma exciatiaon structure for gas supply body 80.
The unstrpped gas of supplying with from unstrpped gas supply port 63 is piled up in unstrpped gas supply port 63 mainly as the silicon nitride thing, and the silicon nitride thing of therefore piling up is removed by thermal drying when safeguarding.In this case, in the situation that unstrpped gas supply port 63 is downward to forming, plasma is difficult to enter in unstrpped gas supply port 63, therefore sometimes can not will be piled up in the silicon nitride thing of this unstrpped gas supply port 63 until internally remove fully.This point, as present embodiment, unstrpped gas supply port 63 is in the situation of horizontal direction, and the plasma that generates during thermal drying enters to the inside of this unstrpped gas supply port 63.Therefore, silicon nitride can be removed fully to the inside of unstrpped gas supply port 63.Thereby, after maintenance, can, from unstrpped gas supply port 63 base feed gas suitably, can more suitably make silicon nitride film 23 film forming.
In addition, unstrpped gas supply pipe 61 and plasma exciatiaon with unstrpped gas supplying structure body 60 are roughly cancellate mode with the second plasma exciatiaon of structure for gas supply body 80 with gas supply pipe 81, dispose unstrpped gas supplying structure body 60 and plasma exciatiaon structure for gas supply body 80.Therefore, and make each unstrpped gas supplying structure body 60 self be roughly clathrate with plasma exciatiaon with structure for gas supply body 80 to compare, can easily make unstrpped gas supplying structure body 60 and plasma exciatiaon with structure for gas supply body 80.In addition, the plasma that generates in plasma formation zone R1 also can easily pass through.
In addition, as shown in figure 12, unstrpped gas supply port 63 also can form its internal diameter and go toward the outer side tapered expansion from inboard.In this case, when thermal drying, plasma is more prone to enter the inside of unstrpped gas supply port 63.Thereby, can remove more reliably the silicon nitride thing that is piled up in unstrpped gas supply port 63.In addition,, can form too its internal diameter and go toward the outer side tapered expansion from inboard with gas supply port 82 for the second plasma exciatiaon.
In the above embodiment, the situation of having used silane gas as silane based gas has been described, but silane based gas is not limited to silane gas.The inventor studies after discussion as can be known, is for example using disilane (Si
2H
6) in the situation of gas, with the situation of using silane gas, compare, the stepcoverage of silicon nitride film 23 further improves.
In addition, in the plasma film forming apparatus 16 of above execution mode, be used to generate plasma from the microwave of radial line slot antenna 42, but the generation of this plasma is not limited to present embodiment., as plasma, also can use for example CCP(capacitance coupling plasma), the ICP(inductively coupled plasma), the ECRP(Ecr plasma), HWP(helicon wave plasma, the helicon activated plasma) etc.In either case, the film forming of silicon nitride film 23 is all carried out under the temperature of glass substrate G is low-temperature environment below 100 ℃, therefore preferably uses highdensity plasma.
And then, in the above embodiment, film forming silicon nitride film 23 has been described on glass substrate G as diaphragm seal, make the situation of organic EL device A, but the present invention also can be applicable to make the situation of other organic electronic device.For example as organic electronic device, make in the situation of organic transistor, organic solar batteries, organic FET (Field Effect Transistor, field-effect transistor) etc., also can use the film build method of silicon nitride film of the present invention.And the present invention except the manufacturing of this organic electronic device, under the temperature of substrate is low temperature environment below 100 ℃, also can be widely used in the situation of film forming silicon nitride film on substrate.
Above, with reference to accompanying drawing, suitable execution mode of the present invention is illustrated, but the present invention is not limited to this example., if those skilled in the art in the category of the thought of putting down in writing in the scope of Patent right requirement, can expect various variation and fixed case certainly, for those, certainly also belong to technical scope of the present invention.
Symbol description
1 base plate processing system
16 plasma film forming apparatus
20 anodal layers
21 luminescent layers
22 negative electrode layers
23 silicon nitride films
30 container handlings
31 mounting tables
42 radial line slot antenna
60 unstrpped gas supplying structure bodies
62 peristomes
63 unstrpped gas supply ports
70 the 1st plasma exciatiaon gas supply ports
80 plasma exciatiaons structure for gas supply body
82 the 2nd plasma exciatiaon gas supply ports
83 peristomes
90 exhaust outlets
100 control parts
The A organic EL device
The G glass substrate
R1 plasma formation zone
R2 unstrpped gas is from separating zone
Claims (27)
1. the film build method of a silicon nitride film, be to form the film build method of silicon nitride film on the substrate in being accommodated in container handling, and the film build method of this silicon nitride film is characterised in that:
To supplying with the processing gas that comprises silane based gas, nitrogen and hydrogen in described container handling,
Described processing gas excited and generate plasma, implementing to utilize the plasma treatment that this plasma carries out and form silicon nitride film on substrate.
2. the film build method of silicon nitride film as claimed in claim 1 is characterized in that:
Described silicon nitride film uses as the diaphragm seal of organic electronic device.
3. the film build method of silicon nitride film as claimed in claim 1 is characterized in that:
Utilize in the plasma treatment that described plasma carries out, the pressure in described container handling is maintained 20Pa～60Pa.
4. the film build method of silicon nitride film as claimed in claim 1 is characterized in that:
Control the supply flow rate of described hydrogen, thereby control the membrane stress of described silicon nitride film.
5. the film build method of silicon nitride film as claimed in claim 1 is characterized in that:
Described plasma utilizes the described processing gas of microwave-excitation and generates.
6. the film build method of silicon nitride film as claimed in claim 5 is characterized in that:
Control the power of described microwave, thereby control the membrane stress of described silicon nitride film.
7. the film build method of silicon nitride film as claimed in claim 1 is characterized in that:
Described processing gas comprises:
Be used to form the unstrpped gas of described silicon nitride film; With
Be used for generating the plasma exciatiaon gas of described plasma,
Supply with described unstrpped gas when utilizing described plasma exciatiaon to generate described plasma with gas or before generating described plasma.
8. the film build method of silicon nitride film as claimed in claim 1 is characterized in that:
In the described processing gas of supplying with in to described container handling, the supply flow rate of described nitrogen is 1～1.5 with the ratio of the supply flow rate of described silane based gas.
9. the manufacture method of an organic electronic device is characterized in that:
Form organic element on substrate,
Then, to supplying with the processing gas that comprises silane based gas, nitrogen and hydrogen in the container handling of taking in this substrate, described processing gas is excited and generate plasma, the plasma treatment that enforcement utilizes this plasma to carry out, form silicon nitride film as diaphragm seal so that cover the mode of described organic element.
10. the manufacture method of organic electronic device as claimed in claim 9 is characterized in that:
In the plasma treatment of utilizing described plasma to carry out, the pressure in described container handling is maintained 20Pa～60Pa.
11. the manufacture method of organic electronic device as claimed in claim 9 is characterized in that:
Control the supply flow rate of described hydrogen, thereby control the membrane stress of described silicon nitride film.
12. the manufacture method of organic electronic device as claimed in claim 9 is characterized in that:
Described plasma utilizes the described processing gas of microwave-excitation and generates.
13. the manufacture method of organic electronic device as claimed in claim 12 is characterized in that:
Control the power of described microwave, thereby control the membrane stress of described silicon nitride film.
14. the manufacture method of organic electronic device as claimed in claim 9 is characterized in that:
Described processing gas comprises:
Be used to form the unstrpped gas of described silicon nitride film; With
Be used for generating the plasma exciatiaon gas of described plasma,
When utilizing described plasma exciatiaon to generate described plasma with gas or before generating described plasma, supply with described unstrpped gas.
15. the manufacture method of organic electronic device as claimed in claim 9 is characterized in that:
In the described processing gas of supplying with in to described container handling, the supply flow rate of described nitrogen is 1～1.5 with the ratio of the supply flow rate of described silane based gas.
16. a film formation device that forms the silicon nitride film of silicon nitride film on substrate, is characterized in that, comprising:
Take in substrate and to its container handling of processing;
To supplying with the processing gas supply part of the processing gas that comprises silane based gas, nitrogen and hydrogen in described container handling;
Described processing gas is excited and generate the plasma exciatiaon section of plasma; With
Control part, it controls described processing gas supply part and described plasma exciatiaon section,, to implement the plasma treatment of utilizing described plasma to carry out, forms silicon nitride film on substrate.
17. the film formation device of silicon nitride film as claimed in claim 16 is characterized in that:
Described silicon nitride film uses as the diaphragm seal of organic electronic device.
18. the film formation device of silicon nitride film as claimed in claim 16 is characterized in that:
Described control part, control described processing gas supply part, makes in the plasma treatment of utilizing described plasma to carry out, and the pressure in described container handling is maintained 20Pa～60Pa.
19. the film formation device of silicon nitride film as claimed in claim 16 is characterized in that:
Described control part is controlled the supply flow rate of described hydrogen, thereby controls the membrane stress of described silicon nitride film.
20. the film formation device of silicon nitride film as claimed in claim 16 is characterized in that:
The described processing gas of described plasma exciatiaon section's supply microwave-excitation.
21. the film formation device of silicon nitride film as claimed in claim 20 is characterized in that:
Described control part is controlled the power of described microwave, thereby controls the membrane stress of described silicon nitride film.
22. the film formation device of silicon nitride film as claimed in claim 16 is characterized in that:
Described processing gas comprises:
Be used to form the unstrpped gas of described silicon nitride film; With
Be used for generating the plasma exciatiaon gas of described plasma,
Described control part is controlled described processing gas supply part and described plasma exciatiaon section, makes when utilizing described plasma exciatiaon to generate described plasma with gas or before generating described plasma and supplies with described unstrpped gas.
23. the film formation device of silicon nitride film as claimed in claim 16 is characterized in that:
Described control part is controlled described processing gas supply part, and the supply flow rate that makes described nitrogen is 1～1.5 for the ratio of the supply flow rate of described silane based gas.
24. the film formation device of silicon nitride film as claimed in claim 16 is characterized in that:
Described processing gas comprises:
Be used to form the unstrpped gas of described silicon nitride film; With
Be used for generating the plasma exciatiaon gas of described plasma,
Be provided with described plasma exciatiaon section on the top of described container handling,
Be provided with the mounting portion of mounting substrate in the bottom of described container handling,
Between described plasma exciatiaon section and described mounting portion, be provided with plasma exciatiaon structure for gas supply body and the unstrpped gas supplying structure body dividing in described container handling and form described processing gas supply part,
Be formed with in the structure for gas supply body at described plasma exciatiaon: the plasma exciatiaon gas supply port of described plasma exciatiaon with gas supplied with in the zone to described plasma exciatiaon section side; With the peristome that makes the described plasma that generates in the zone of described plasma exciatiaon section side by the zone of described mounting portion side,
Be formed with in described unstrpped gas supplying structure body: the unstrpped gas supply port of the zone of described mounting portion side being supplied with described unstrpped gas; With the peristome that makes the described plasma that generates in the zone of described plasma exciatiaon section side by the zone of described mounting portion side.
25. the film formation device of silicon nitride film as claimed in claim 24 is characterized in that:
Described plasma exciatiaon is disposed at apart from the described plasma exciatiaon 30mm of section with interior position with the structure for gas supply body.
26. the film formation device of silicon nitride film as claimed in claim 24 is characterized in that:
Described unstrpped gas supply port forms towards horizontal direction.
27. the film formation device of silicon nitride film as claimed in claim 26 is characterized in that:
Described unstrpped gas supply port forms its internal diameter and goes toward the outer side tapered shape to enlarge from inboard.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011-038342 | 2011-02-24 | ||
| JP2011038342 | 2011-02-24 | ||
| JP2011-233620 | 2011-10-25 | ||
| JP2011233620A JP5941653B2 (en) | 2011-02-24 | 2011-10-25 | Silicon nitride film forming method and silicon nitride film forming apparatus |
| PCT/JP2012/052608 WO2012114856A1 (en) | 2011-02-24 | 2012-02-06 | Silicon nitride film deposition method, organic electronic device manufacturing method, and silicon nitride film deposition device |
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| CN103403847A true CN103403847A (en) | 2013-11-20 |
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| CN2012800105318A Pending CN103403847A (en) | 2011-02-24 | 2012-02-06 | Silicon nitride film deposition method, organic electronic device manufacturing method, and silicon nitride film deposition device |
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| Country | Link |
|---|---|
| JP (1) | JP5941653B2 (en) |
| KR (1) | KR101881470B1 (en) |
| CN (1) | CN103403847A (en) |
| TW (1) | TWI533378B (en) |
| WO (1) | WO2012114856A1 (en) |
Cited By (6)
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| CN107275507A (en) * | 2016-03-31 | 2017-10-20 | 株式会社日本有机雷特显示器 | Organic EL display panel and preparation method thereof |
| CN107507774A (en) * | 2016-06-14 | 2017-12-22 | 东京毅力科创株式会社 | The processing method of silicon nitride film and the forming method of silicon nitride film |
| CN109468613A (en) * | 2017-09-07 | 2019-03-15 | 东京毅力科创株式会社 | Film formation device and film build method |
| CN109952632A (en) * | 2016-11-11 | 2019-06-28 | 朗姆研究公司 | Reduce method of the wet etch rate of SiN film without damaging the substrate that underlies |
| CN110408909A (en) * | 2018-04-26 | 2019-11-05 | Spts科技有限公司 | The method for depositing SiN film |
| US11832533B2 (en) | 2018-08-24 | 2023-11-28 | Lam Research Corporation | Conformal damage-free encapsulation of chalcogenide materials |
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| JP2014060378A (en) * | 2012-08-23 | 2014-04-03 | Tokyo Electron Ltd | Silicon nitride film deposition method, organic electronic device manufacturing method and silicon nitride film deposition device |
| KR102418092B1 (en) | 2016-03-11 | 2022-07-06 | 다이요 닛산 가부시키가이샤 | Silicon nitride film manufacturing method and silicon nitride film |
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Also Published As
| Publication number | Publication date |
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| KR20140006907A (en) | 2014-01-16 |
| JP2012188735A (en) | 2012-10-04 |
| WO2012114856A1 (en) | 2012-08-30 |
| TW201248729A (en) | 2012-12-01 |
| JP5941653B2 (en) | 2016-06-29 |
| KR101881470B1 (en) | 2018-07-24 |
| TWI533378B (en) | 2016-05-11 |
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