WO2009154130A1 - プラズマディスプレイパネルの製造方法、成膜装置 - Google Patents

プラズマディスプレイパネルの製造方法、成膜装置 Download PDF

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Publication number
WO2009154130A1
WO2009154130A1 PCT/JP2009/060680 JP2009060680W WO2009154130A1 WO 2009154130 A1 WO2009154130 A1 WO 2009154130A1 JP 2009060680 W JP2009060680 W JP 2009060680W WO 2009154130 A1 WO2009154130 A1 WO 2009154130A1
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Prior art keywords
film
metal oxide
vacuum chamber
display panel
evaporation source
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PCT/JP2009/060680
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English (en)
French (fr)
Japanese (ja)
Inventor
栄一 飯島
宗人 箱守
利春 倉内
礼寛 横山
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株式会社アルバック
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Priority to CN200980122380.3A priority Critical patent/CN102067266B/zh
Priority to KR1020107028164A priority patent/KR101128744B1/ko
Priority to JP2010517878A priority patent/JP5235214B2/ja
Publication of WO2009154130A1 publication Critical patent/WO2009154130A1/ja

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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
    • 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
    • C23C14/08—Oxides
    • C23C14/081—Oxides of aluminium, magnesium or beryllium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02—Manufacture of electrodes or electrode systems
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/20—Manufacture of screens on or from which an image or pattern is formed, picked up, converted or stored; Applying coatings to the vessel

Definitions

  • the present invention relates to a plasma display panel, and more particularly to a technique for forming an MgO film suitable as a protective film for a panel used in a PDP display device.
  • the PDP is mainly a three-electrode surface discharge type in which a front plate having a sustain electrode and a scan electrode formed on a glass substrate and a back plate having an address electrode formed on the glass substrate are bonded together.
  • a discharge gas is enclosed between the front plate and the back plate.
  • the enclosed discharge gas is turned into plasma and ultraviolet rays are emitted.
  • the phosphor is arranged at a position where the emitted ultraviolet rays are irradiated, the phosphor is excited by the ultraviolet rays and visible light is emitted.
  • a dielectric film is formed on the sustain electrode and the scan electrode, and a metal oxide film such as MgO or SrO is formed thereon for the purpose of protecting the dielectric and emitting secondary electrons. .
  • Non-Patent Document 1 Proc. 43rd PDP Technical Discussion Meeting, July 5, 2006, p32-p52 JP 2007-107092 A JP 2007-119831 A JP 2006-149833 A
  • the protective film containing MgO is more likely to emit secondary electrons as the peak intensity of (111) orientation is higher, and that the higher the refractive index, the denser and the higher the sputtering resistance.
  • the crystal orientation is (111)
  • the peak intensity in XRD X Ray Diffraction, X-ray diffraction
  • the filling rate is 82% or more (the refractive index is about 1.6 or more).
  • the film density tends to decrease under the film forming conditions for improving the crystal orientation. Under the film forming conditions for increasing the film density, the crystal orientation tends to decrease. That is, the film forming conditions for improving the above characteristics are contradictory. Therefore, when creating a protective film for PDP having more excellent characteristics than the current situation, it is necessary to make a film forming condition that emphasizes one of the characteristics, or to create an intermediate protective film having both characteristics. Absent.
  • the film formation conditions generally include the substrate temperature, pressure, oxygen, Ar, hydrogen, water and other process gas introduction amounts, gas partial pressure, and the like during film formation. These film formation conditions can be monitored and controlled. However, changing any film formation condition is insufficient for controlling the crystallinity of MgO and controlling necessary film characteristics.
  • a metal oxide such as MgO, SrO, or CaO
  • a metal oxide such as MgO, SrO, or CaO
  • a reaction 2MgO ⁇ 2Mg + O 2
  • MgO magnesium oxide
  • the present inventors Rather than forming a protective film with vapor of metal oxide that has evaporated without dissociating, the present inventors have mixed oxide into the protective film once the metal oxide has been dissociated and then oxidized. It has been found that the (111) crystal orientation of the protective film and the film density are higher when the film is formed. As a result of further studies by the present inventors, in order to dissociate the metal oxide, water was introduced into the vacuum chamber and the electron beam was irradiated so that the film formation rate was 40 nm / second or more. I knew that I should do it.
  • emission light when Mg is oxidized has characteristic peaks at wavelengths of 285.2 nm and 280.2 nm, and emission light when Sr is oxidized at wavelengths of 242.8 nm and 256.9 nm. There is a characteristic peak.
  • the peak size (intensity) of these specific wavelengths increases as the amount of oxidized metal increases, so if the emission intensity at a specific wavelength is measured, how much the metal oxide is dissociated and re-oxidized? Thus, it can be seen whether the film formation speed and the atmosphere including the electron beam are sufficient to dissociate the metal oxide and oxidize it again.
  • the present invention based on such knowledge, while introducing oxygen into the vacuum chamber, heats the metal oxide disposed in the evaporation source to generate the vapor of the metal oxide, the electrode on the surface
  • the arranged first panel was transported through a transport path in the vacuum chamber, passed through a film forming position facing the evaporation source, and a protective film made of a metal oxide thin film was formed on the electrode. Thereafter, the first panel is bonded to the second panel, and the plasma display panel is manufactured by manufacturing the plasma display panel in which the protective film is exposed to plasma.
  • the protective film when the first panel is stationary at the deposition position while introducing water so that the introduction volume of oxygen is equal to or greater than the introduction volume of oxygen per unit time.
  • Deposition rate is 40n / While evaporating the metal oxide so that the second or higher, a method of manufacturing a plasma display panel for carrying the said first panel.
  • a first panel having an electrode disposed on a surface thereof is disposed at a film forming position facing an evaporation source inside a vacuum chamber, and oxygen is introduced into the vacuum chamber while being disposed at the evaporation source.
  • the metal oxide is heated to generate a vapor of the metal oxide, and a protective film made of a thin film of metal oxide is formed on the electrode of the first panel.
  • Pa It is a manufacturing method of Le.
  • the present invention relates to a method for manufacturing a plasma display panel, wherein the metal oxide is irradiated with an electron beam to evaporate.
  • the present invention is a method for manufacturing a plasma display panel, wherein the total pressure of the vacuum chamber is set to a pressure exceeding 1 ⁇ 10 ⁇ 1 Pa to generate the vapor of the metal oxide. .
  • the present invention is a method for manufacturing a plasma display panel, wherein the metal oxide is MgO.
  • the present invention is a method for manufacturing a plasma display panel, wherein the metal oxide contains MgO, and one or both of SrO and CaO are added.
  • the present invention is a method for manufacturing a plasma display panel, wherein when the metal oxide is evaporated, the emission intensity of light emitted into the vacuum chamber is measured, and the measured value of the emission intensity is preset. This is a method for manufacturing a plasma display panel in which the output of the heating device for evaporating the metal oxide is changed so as to have a value.
  • the present invention is a method for manufacturing a plasma display panel, wherein when the metal oxide is evaporated, the emission intensity of light emitted into the vacuum chamber is measured, and the measured value of the emission intensity is preset.
  • This is a method of manufacturing a plasma display panel in which the irradiation area of the electron beam is changed so as to have a value.
  • the present invention includes a vacuum chamber, an evaporation source disposed in the vacuum chamber, a heating device for heating a vapor deposition material disposed in the evaporation source, a water inlet for introducing water into the vacuum chamber, An apparatus for forming a protective film having an oxygen inlet for introducing oxygen into the vacuum chamber, the measuring device for measuring the emission intensity of light generated inside the vacuum chamber, the measuring device, and the heating device
  • the control device is a film forming device configured to change the output of the heating device based on the emission intensity transmitted from the measurement device.
  • the present invention is a film forming apparatus, wherein the heating device is an electron gun, and the control device is a film forming apparatus that changes an irradiation area of an electron beam emitted from the electron gun.
  • the present invention is a film forming apparatus, and includes a transfer device that transfers a film formation target along a transfer path inside the vacuum chamber, and the evaporation source is moved while moving along the transfer path.
  • the water introduction port is a film forming apparatus that is closer to the evaporation source than the oxygen introduction port and farther from the transfer path.
  • the present invention is a film forming apparatus, comprising a substrate holder that holds a substrate at a position facing the evaporation source inside the vacuum chamber, wherein the water introduction port is closer to the evaporation source than the oxygen introduction port In addition, the film forming apparatus is located far from the substrate held by the substrate holder.
  • the present invention is configured as described above, and the protective film to be formed has good crystal orientation and high film density.
  • the crystal orientation is good, the (111) peak intensity of the protective film becomes high, and when the film density is high, the sputtering resistance is improved and the film thickness of the protective film can be reduced.
  • the (111) peak intensity is 40% higher and the film density is high, the required film thickness can be reduced by 20% to 50%.
  • the amount of water introduced is the same as or larger than that of oxygen.
  • the amount of water and oxygen introduced may be defined by the partial pressure in the vacuum chamber, but since water is decomposed by an electron beam, it is difficult to accurately measure the partial pressure of water. Therefore, in the present invention, instead of the partial pressure, the introduction amount of water and oxygen is defined by the introduction volume (sccm) per unit time.
  • the crystal orientation is good, the secondary electron emission property of the protective film is high.
  • Spatter resistance of the protective film is good due to high filling rate (film density), secondary electron emission is high, and sputter resistance of the protective film is good, so not only the life of the PDP is long, but also the film thickness can be reduced.
  • PDP can be made thin. Thinning saves vapor deposition materials and reduces panel costs. Since the film formation rate is faster than the conventional one, not only the manufacturing time of the PDP is shortened, but also the possibility that impurities such as CO and CO 2 are mixed is reduced. By monitoring the emission wavelength and feeding back to the power of the electron gun, the MgO film quality can be stabilized.
  • Reference numeral 1 in FIG. 1 shows an example of a plasma display panel.
  • the plasma display panel 1 includes first and second panels 10 and 20.
  • the first panel 10 has a first glass substrate 11, and a sustain electrode 15 and a scan electrode 16 are arranged on the surface of the first glass substrate 11 (one in FIG. 1 is illustrated). ).
  • the sustain electrodes 15 and the scan electrodes 16 are alternately arranged at a predetermined interval. Sustain electrode 15 and scan electrode 16 are separated from each other, and dielectric film 12 is formed between the surface and sustain electrode 15 and scan electrode 16. Therefore, the sustain electrode 15 and the scan electrode 16 are insulated from each other.
  • a protective film 14 is disposed on the entire surface of the dielectric film 12. Accordingly, the protective film 14 is located on each sustain electrode 15 and each scan electrode 16.
  • the second panel 20 has a second glass substrate 21.
  • address electrodes 25 are arranged in parallel to each other, and the address electrodes 25 are separated from each other.
  • a dielectric layer 24 (insulating layer) is disposed between the surface of the address electrode 25 and the address electrode 25, and the address electrodes 25 are insulated from each other.
  • a partition wall 23 is disposed along the longitudinal direction of the address electrodes 25. Any one of the phosphor films (red phosphor film 22R, green phosphor film 22G, and blue phosphor film 22B) containing fluorescent dyes of different colors is disposed between the adjacent barrier ribs 23. Each address electrode 25 is covered with a phosphor film 22R, 22G, or 22B of any one color through the dielectric layer 24.
  • the surface on which the protective film 14 is formed and the surface on the side on which the partition wall 23 is formed face each other, and the sustain electrode 15 and the scan electrode 16 are opposed to the address electrode 25. Are stuck together so that they are orthogonal to each other, and the space between the first and second panels 10 and 20 is sealed.
  • the partition wall 23 protrudes high from the surface of the second panel 20, and the tip thereof is in contact with the surface of the first panel 10. Accordingly, the space between the first and second panels 10 and 20 is divided by the partition wall 23, and each of the divided spaces (light emitting space 29) is filled with a sealed gas (for example, a mixed gas of Ne and Xe). ing.
  • a sealed gas for example, a mixed gas of Ne and Xe.
  • the protective film 14 is mainly composed of an MgO film mainly composed of a protective material composed of MgO, an SrO—CaO film composed mainly of a protective material composed of SrO and CaO, or a protective material composed of MgO and SrO. It is composed of an MgO—SrO film or the like.
  • Such a protective film 14 has a high electron emission characteristic, and in the light emitting cell in which wall charges are accumulated by address discharge, electrons are discharged from the protective film 14 to cause a sustain discharge, the sealed gas is turned into plasma, and ultraviolet rays are generated.
  • ultraviolet light is emitted from the light emitting cell where the selected scanning electrode 16 and the address electrode 25 intersect, when the ultraviolet light is incident on the phosphor films 22R, 22G, and 22B located in the light emitting cell, the phosphor films 22R and 22G. , 22B are excited, and visible light of any one of red, green, and blue is emitted.
  • the first glass substrate 11 and the dielectric film 12 are each transparent.
  • the protective film 14 is also made of a transparent metal oxide such as MgO or SrO, and its film thickness distribution is ⁇ 5% to ⁇ 10% so that the transparency is not impaired. It is transparent. Therefore, light (visible light) emitted from the light emitting cell is transmitted through the first panel 10 and emitted to the outside.
  • the protective film 14 is exposed in the space between the first and second panels 10 and 20, and when the light emitting cell emits light, the protective film 14 is exposed to plasma.
  • the protective film 14 is made of a material that is difficult to be etched by plasma, such as MgO or SrO.
  • the protective film 14 formed according to the present invention has a high filling rate as will be described later, it is more difficult to etch, and the dielectric film 12, the sustain electrode 15, and the scanning electrode 16 are protected by the protective film 14.
  • the display panel 1 has a longer life than conventional ones.
  • Reference numeral 3 in FIG. 2 is an example of a film forming apparatus and has a vacuum chamber 32.
  • the vacuum chamber 32 has a film forming chamber 34 and a material chamber 35, and the material chamber 35 is disposed below the film forming chamber 34 and connected to the film forming chamber 34.
  • a preparation chamber 31 and an extraction chamber 33 are connected to the film formation chamber 34 via a gate valve 39.
  • the film forming chamber 34 is provided with a transfer device 50, and an object to be formed is carried into the film forming chamber 34 from the preparation chamber 31 while being held by the holding means 47 (carrier). The film is carried out to the take-out chamber 33 through a predetermined transfer path 51 in the film formation chamber 34.
  • the material chamber 35 is connected to the film forming chamber 34 at a position directly below the transfer path 51.
  • an evaporation source 36 is disposed immediately below a connection portion between the material chamber 35 and the film forming chamber 34. Therefore, the evaporation source 36 is positioned directly below the transport path 51, and the film formation target faces the evaporation source 36 while moving along the transport path 51.
  • the evaporation source 36 has a crucible (container), and a vapor deposition material is disposed in the crucible.
  • the vapor deposition material is a metal oxide.
  • the material chamber 35 is provided with an electron gun (electron beam generator) 41.
  • An evacuation system 52 b is connected to the vacuum chamber 32, and when the inside of the vacuum chamber 32 is put into a vacuum atmosphere and the electron gun 41 is operated, an electron beam (electron beam) 42 is irradiated to the metal oxide of the evaporation source 36. The metal oxide vapor is released into the material chamber 35.
  • a restriction plate 38 is disposed in a portion of the vacuum chamber 32 where the material chamber 35 and the film forming chamber 34 are connected.
  • An opening (discharge port) 37 is formed at a position of the restriction plate 38 directly above the evaporation source 36, and the vapor passing through the discharge port 37 is discharged into the film forming chamber 34.
  • the film formation target passes through the film formation position 49 facing the evaporation source 36 through the discharge port 37 while moving along the transport path 51.
  • the limiting plate 38 restricts the spread angle of the vapor discharged into the film forming chamber 34, so that the vapor enters the film forming object passing through the film forming position 49 with an incident angle within a predetermined range.
  • a water inlet 55 and an oxygen inlet 56 are provided at a position between the limiting plate 38 and the evaporation source 36 inside the vacuum chamber 32 (that is, inside the material chamber 35).
  • the water inlet 55 and the oxygen inlet 56 are connected to a gas supply system (not shown). From the water inlet 55 and the oxygen inlet 56, H 2 O gas (water vapor, gaseous water), oxygen gas, Is introduced into the material chamber 35.
  • the water inlet 55 is closer to the evaporation source 36 than the oxygen inlet 56, the H 2 O gas is exposed to the electron beam 42 to generate hydrogen, and the vapor of the metal oxide is exposed to the H 2 O gas containing hydrogen. Then, a part of the vapor is reduced and the metal is dissociated.
  • the water inlet 55 is farther from the transport path 51 than the oxygen inlet 56. That is, the distance between the film formation target and the water introduction port 55 when the film formation target is closest to the water introduction port 55 is the distance when the film formation target is closest to the oxygen introduction port 56. It is longer than the distance between the film formation target and the oxygen inlet 56.
  • the vapor exposed to the H 2 O gas is also exposed to oxygen gas before reaching the film formation target, and the dissociated metal is oxidized to become a metal oxide before reaching the film formation target.
  • the dissociated metal oxidizes, it emits light (ultraviolet rays).
  • a window portion 44 for example, a quartz window
  • a spectroscopic monitor 43 is disposed outside the material chamber 35. The light transmitted through the window 44 enters the light receiving unit of the spectroscopic monitor 43, and the spectroscopic monitor 43 measures the emission intensity of the incident light.
  • the amount of evaporation of the metal oxide per unit time increases.
  • the film formation rate is increased and the emission intensity is increased.
  • the electron gun 41 and the spectral monitor 43 are connected to the control device 45. The measured value of the emission intensity is transmitted to the control device 45.
  • the control device 45 investigates the relationship between the emission intensity and the deposition rate, and setting the relationship in the control device 45. If a desired film formation rate is set in the control device 45, the control device 45 compares the measured value of the emission intensity with the set relationship, and the irradiation area of the electron gun 41 so that the film formation rate becomes the set value. change.
  • the protective film is formed under the same conditions (metal oxide type, film forming pressure, heating temperature, transport speed, etc.) as when the protective film was actually formed, and formed at the film forming position.
  • the relationship between the film thickness growth amount per unit time (static deposition rate) when the object is stationary and the emission intensity of a specific wavelength when the metal oxide evaporates is obtained.
  • the static film formation rate is determined in the range of 40 nm / second or more, and the determined static film formation rate and the relationship obtained in the preliminary test are set in the controller 45.
  • the preparation chamber 31, the extraction chamber 33, and the vacuum chamber 32 are evacuated by the evacuation systems 52a to 52c to form a vacuum atmosphere at a predetermined pressure.
  • the first panel 10 in which the electrodes (sustain electrodes 15 and scanning electrodes 16) and the dielectric film 12 are formed on the first glass substrate 11 is used as a film formation target, and is held by the holding means 47 and charged. Carry it into the chamber 31.
  • Heating means 59 is disposed inside the preparation chamber 31 and the film forming chamber 34, and the first panel 10 is heated to a predetermined temperature and then carried into the film forming chamber 34.
  • a granular metal oxide is disposed in the evaporation source 36.
  • the amount of water (steam) and oxygen introduced can be controlled by a flow controller (mass flow controller) (not shown) so that the introduced volume per unit time of water is larger than the introduced volume per unit time of oxygen.
  • the metal oxide vapor is generated by irradiating the electron beam 42 while introducing water and oxygen.
  • the first panel 10 When the first panel 10 is transported through the transport path 51 with the surface on which the sustain electrode 15 and the scan electrode 16 are formed facing downward, and passes through the position facing the evaporation source 36, the first panel 10 and the scan electrode 15 are scanned.
  • the metal oxide vapor reaches the electrode 16 (here, the surface of the dielectric film 12) to form a metal oxide thin film (protective film 14).
  • the controller 45 measures the emission intensity every predetermined time or continuously measures the emission intensity, changes the irradiation area of the electron beam 42 so that the measured value of the emission intensity becomes a set value, and the protective film
  • the static deposition rate of 14 is set to a predetermined rate of 40 nm / second or more. Since the static film formation rate is 40 nm / second or more and water is introduced in a larger amount than oxygen, the protective film 14 is oriented to (111), and the filling rate exceeds 82%.
  • the film thickness is 14. That is, when the film thickness of the protective film 14 is determined, the value obtained by dividing the film thickness by the static film formation rate is the residence time.
  • the first panel 10 in a state where the protective film 14 is formed moves on the transport path 51, then is carried out to the take-out chamber 33, cooled, and then carried out of the film forming apparatus 3. If the carried out first panel 10 and the above-described second panel 20 are bonded together, and the sealed gas is disposed between the first and second panels 10 and 20, the plasma display panel 1 of FIG. can get.
  • the protective film 14 is formed on the first panel 10 of the three-electrode AC type PDP has been described above.
  • the present invention is not limited to this, and the protective film 14 is formed only on the second panel 20.
  • the film may be formed on both the first and second panels 10 and 20.
  • the protective film 14 is disposed on at least each address electrode 25.
  • the metal oxide used in the present invention is MgO alone or a mixture of MgO and another metal oxide (either SrO or CaO or both).
  • the electron gun is controlled to stabilize film characteristics by measuring the emission intensity during oxidation of the dissociated metal for any one or more metal oxides in the mixture. It is possible to measure.
  • the vapor deposition material is not limited to the metal oxide, but includes at least one kind selected from the group consisting of the above-described metal oxide, Ca, Al, Si, Mn, Eu, and Ti. An agent can also be added.
  • the metal oxide may be excessively dissociated and unoxidized metal may be mixed in the protective film. Since an unoxidized metal, particularly Mg, has high ignitability, in the present invention, the electron gun 41 is used and the metal oxide is evaporated by the electron beam 42.
  • the electron gun 41 is not particularly limited, but a piercing electron gun is suitable in consideration of controllability and stability of the evaporation rate.
  • the film thickness distribution of the protective film 14 becomes non-uniform, the optical characteristics deteriorate and it is not suitable for the first panel 10, so the film thickness distribution is ⁇ 5% to ⁇ 10% of the target film thickness (for example, 800 nm).
  • the oscillation waveform of the electron beam 42 is determined.
  • the control device 45 changes the irradiation area of the electron beam 42 to set the light emission intensity to the set value.
  • the present invention is not limited to this, and the power density (W / cm 2 ) of the electron gun 41 Alternatively, the emission intensity may be set to a set value.
  • the preparation chamber 31 and the take-out chamber 33 are connected to the film formation chamber 34.
  • a heating chamber is installed between the preparation chamber 31 and the film formation chamber 34.
  • a cooling chamber is provided between the film formation chamber 34 and the take-out chamber 33.
  • the protective film 14 may be formed by placing a substrate holder directly above the evaporation source 36 inside the material chamber 35 and holding the substrate holder so that the film formation target faces the evaporation source 36. . In this case, the distance between the evaporation source 36 and the film formation target does not change at least during the formation of the protective film 14.
  • the film formation target held on the substrate holder has a film thickness growth amount per unit time (that is, film formation speed) of 40 nm / second or more, and other conditions (such as the amount of water and oxygen introduced) are film formation. This is the same as when film formation is performed while the object is being conveyed.
  • the oxygen introduction port 56 is disposed closer to the film formation target of the substrate holder than the water introduction port 55, and the water introduction port 55 is introduced with oxygen. It is arranged near the evaporation source 36 rather than the mouth 56.
  • the water is preferably pure water (absorbance 0.01 or less at a wavelength of 210 nm to 400 nm, nonvolatile 5 ppm or less).
  • the discharge characteristics deteriorate, so the total organic carbon content is preferably 4 ppb or less.
  • the installation location of the water introduction port 55 is not particularly limited, but if it directly faces the vapor discharge port of the evaporation source 36 (for example, the opening of the crucible), the metal oxide may be deposited and the water introduction port 55 may be clogged. Therefore, it is desirable that the water inlet 55 does not face the vapor outlet or a shield is disposed between the water inlet 55 and the evaporation source 36.
  • the film formation rate was the same as before (less than 40 nm / second), the peak intensity of the (111) crystal orientation was small and did not reach the practical level.
  • it is essential to introduce water into the vacuum chamber and to set the film formation rate to 40 nm / second or more (more desirably 140 nm / second or more).
  • the amount of water introduced is not particularly limited as long as it is larger than the amount of oxygen introduced, but it is preferably 200 sccm or more.
  • the internal pressure (film formation pressure) of the vacuum chamber 32 when forming the protective film 14 is not particularly limited.
  • the impurity concentration of the protective film even if the film forming pressure is as high as 5 ⁇ 10 ⁇ 2 Pa or higher (for example, 0.2 Pa, 0.3 Pa, etc.)
  • impurities containing C), film density, (111) crystal orientation, and the like were not deteriorated, and the intensity distribution of crystal orientation was improved as compared with the prior art.
  • the vacuum chamber 32 needs to be periodically cleaned.
  • the film forming pressure was as low as less than 5 ⁇ 10 ⁇ 2 Pa, the inside of the vacuum chamber 32 had to be evacuated for a long time (5 to 6 hours) after cleaning. If the film forming pressure is 5 ⁇ 10 ⁇ 2 Pa or more, more desirably 1 ⁇ 10 ⁇ 1 Pa or more, it is not necessary to evacuate the inside of the vacuum chamber 32 for a long time after cleaning.
  • ⁇ Crystal orientation and film density> E1 to E4 in FIG. 3 show the relationship between the (111) strength and the filling rate of the protective film formed by introducing water so that the amount of oxygen introduced into the material chamber 35 is larger than the amount of oxygen introduced into the material chamber 35.
  • Typical film forming conditions are shown in Table 1 below, and analysis results of water (H 2 O gas) introduced into the material chamber 35 are shown in Table 2 below.
  • C1 to C3 in FIG. 3 show the relationship between the (111) strength and the filling rate of the protective film formed by introducing only oxygen without introducing H 2 O.
  • the diffraction intensity and refractive index of (111) orientation were measured, and the filling factor (film
  • the refractive index was measured with an ellipsometer.
  • the refractive index is n
  • the filling rate (film density) is p
  • the spatial refractive index is nv
  • the refractive index n is expressed by the following formula (1).
  • the (111) strength of the MgO film for obtaining a filling rate of 90% was 2450 CPS in the comparative example, but 3500 CPS in the example, which was improved by about 40% or more. From the above results, it can be seen that the protective film formed according to the present invention has both high film density (filling rate) and high (111) orientation.
  • FIG. 8 shows the result of measuring the emission intensity at a wavelength of 285.2 nm by increasing the power applied to the electron gun without introducing water. From FIG. 8, it can be seen that if the input power is increased, the emission intensity increases, but the emission intensity is extremely lower than when water is introduced. Is dissociated and recombined.
  • FIGS. 9 and 10 show electron micrographs of the protective film when water is introduced and the protective film when water is not introduced.
  • the portions that appear black in FIGS. 9 and 10 are gaps between the MgO columnar crystals and the MgO columnar crystals. As the gap between the columnar crystals is smaller, the amount of impure gas adsorbed is reduced and etching is difficult. 9 and 10, it can be seen that FIG. 9 has fewer gaps between the columnar crystals, and that a protective film that is less likely to adsorb impure gas and less etched is formed when water is introduced.
  • the dynamic film formation speed is a unit representing the film formation speed when forming a film while transporting the substrate. It is the film thickness that is formed while the substrate moves 1 m per minute. If the dynamic film formation rate is converted by multiplying by a predetermined coefficient, the static film formation rate when the substrate is fixed to the evaporation source can be obtained.
  • the coefficient for converting the static deposition rate varies depending on the deposition apparatus to be used, but in this case, it is 2.12. If the static deposition rate is Rs and the dynamic deposition rate is Rd, the static deposition rate is static.

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PCT/JP2009/060680 2008-06-16 2009-06-11 プラズマディスプレイパネルの製造方法、成膜装置 WO2009154130A1 (ja)

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JP5235214B2 (ja) 2013-07-10
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