WO2015182090A1 - Dispositif de formation de film, procédé de mesure d'épaisseur de film d'un film organique, et capteur d'épaisseur de film pour film organique - Google Patents

Dispositif de formation de film, procédé de mesure d'épaisseur de film d'un film organique, et capteur d'épaisseur de film pour film organique Download PDF

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WO2015182090A1
WO2015182090A1 PCT/JP2015/002580 JP2015002580W WO2015182090A1 WO 2015182090 A1 WO2015182090 A1 WO 2015182090A1 JP 2015002580 W JP2015002580 W JP 2015002580W WO 2015182090 A1 WO2015182090 A1 WO 2015182090A1
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Prior art keywords
film
frequency
organic
film thickness
organic material
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PCT/JP2015/002580
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English (en)
Japanese (ja)
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伊藤　敦
万里 深尾
小林　義和
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株式会社アルバック
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Priority to KR1020187015514A priority Critical patent/KR20180063369A/ko
Priority to CN201580020079.7A priority patent/CN106232858A/zh
Priority to KR1020167026478A priority patent/KR102035146B1/ko
Priority to SG11201608133PA priority patent/SG11201608133PA/en
Priority to JP2016523133A priority patent/JP6078694B2/ja
Publication of WO2015182090A1 publication Critical patent/WO2015182090A1/fr

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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/542—Controlling the film thickness or evaporation rate
    • C23C14/545—Controlling the film thickness or evaporation rate using measurement on deposited material
    • C23C14/546—Controlling the film thickness or evaporation rate using measurement on deposited material using crystal oscillators
    • 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
    • C23C14/12—Organic material
    • 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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/50—Substrate holders
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
    • G01B7/02—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness
    • G01B7/06—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness for measuring thickness
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
    • H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition

Definitions

  • the present invention relates to a film forming apparatus including a film thickness sensor, a method for measuring a film thickness of an organic film, and a film thickness sensor for an organic film.
  • a technique called a quartz crystal method (QCM: Quartz Crystal Microbalance) is used to measure the thickness and the film forming speed of a film formed on a substrate.
  • QCM Quartz Crystal Microbalance
  • Patent Document 1 describes a sensor head configured to hold a plurality of quartz plates having a resonance frequency of 5 MHz and to switch the quartz plates to be used individually.
  • the crystal resonator is significantly deteriorated in the resonance characteristics with respect to the adhesion of the organic film, so that it is impossible to perform stable film formation rate control and film thickness control of the organic film. There is a problem. Moreover, the lifetime of the vibrator is short, and the vibrator has to be frequently replaced.
  • an object of the present invention is to form a film forming apparatus, a method for measuring a film thickness of an organic film, and a film for an organic film capable of performing film formation rate control and film thickness measurement with high accuracy. It is to provide a thickness sensor.
  • a film formation apparatus includes a vacuum chamber, an organic material source, a substrate holder, a film thickness sensor, and a measurement unit.
  • the organic material source is disposed inside the vacuum chamber and configured to be able to emit organic material particles.
  • the said substrate holder is arrange
  • the film thickness sensor includes a crystal resonator that is disposed inside the vacuum chamber and has a fundamental frequency of 4 MHz or less.
  • the measurement unit measures the film thickness of the organic film deposited on the substrate on the substrate holder based on the change in the resonance frequency of the crystal resonator.
  • the organic material particles emitted from the organic material source are deposited on the surface of the substrate on the substrate holder and also on the surface of the crystal resonator of the film thickness sensor.
  • the resonance frequency of the quartz crystal unit decreases as the amount of organic material particles deposited increases.
  • the measurement unit measures the film thickness of the organic film formed on the substrate based on the change in the resonance frequency on the crystal resonator.
  • the crystal resonator of the film thickness sensor is composed of a crystal resonator having a fundamental frequency of 4 MHz or less. For this reason, compared to a crystal resonator having a fundamental frequency of 5 MHz or more, the increase in equivalent resistance and half-value frequency width due to the adhesion of the organic film is suppressed, and stable resonance vibration over a long period is ensured. Thereby, it becomes possible to measure the film thickness and film formation rate of the organic film with high accuracy.
  • the above-mentioned crystal resonator is typically composed of an AT cut crystal resonator or an SC cut crystal resonator.
  • the measurement unit may include an oscillation circuit, a reference signal generation circuit, a mixer circuit, a counter, and a controller.
  • the oscillation circuit oscillates the crystal resonator.
  • the reference signal generation circuit oscillates a signal having a reference frequency.
  • the mixer circuit mixes the signal output from the oscillation circuit and the signal of the reference frequency.
  • the counter measures the frequency of a low-frequency component signal among the signals generated by the mixer circuit.
  • the controller calculates an oscillation frequency of the oscillation circuit based on a difference between the frequency measured by the counter and the reference frequency.
  • a film thickness measurement method includes depositing organic material particles emitted from an organic material source on a substrate.
  • the organic material particles are deposited on a crystal resonator that vibrates at a resonance frequency of 4 MHz or less. Based on the change in the resonance frequency of the quartz resonator, the film thickness of the organic material particles deposited on the substrate is measured. Thereby, it becomes possible to measure the film thickness and film formation rate of the organic film with high accuracy.
  • the film thickness sensor for organic films includes a crystal resonator having a fundamental frequency of 4 MHz or less. Thereby, it becomes possible to measure the film thickness and film formation rate of the organic film with high accuracy.
  • the film formation rate control and film thickness measurement of the organic film can be performed with high accuracy.
  • FIG. 1 is a schematic sectional view showing a film forming apparatus according to an embodiment of the present invention.
  • the film forming apparatus of this embodiment is configured as a vacuum vapor deposition apparatus for forming an organic film.
  • the film forming apparatus 10 is disposed in a vacuum chamber 11, an organic material source 12 disposed in the vacuum chamber 11, a substrate holder 13 facing the organic material source 12, and the vacuum chamber 11.
  • a film thickness sensor 14 is disposed in a vacuum chamber 11, an organic material source 12 disposed in the vacuum chamber 11, a substrate holder 13 facing the organic material source 12, and the vacuum chamber 11.
  • the vacuum chamber 11 is connected to an evacuation system 15 and is configured to be able to evacuate and maintain the interior in a predetermined reduced pressure atmosphere.
  • the organic material source 12 is configured to be able to emit organic material particles.
  • the organic material source 12 constitutes an evaporation source that heats and evaporates the organic material to release organic material particles.
  • the type of the evaporation source is not particularly limited, and various methods such as a resistance heating method, an induction heating method, and an electron beam heating method can be applied.
  • the substrate holder 13 is configured to be able to hold a substrate W, which is a film formation target such as a semiconductor wafer or a glass substrate, toward the organic material source 12.
  • the film thickness sensor 14 incorporates a crystal resonator having a predetermined fundamental frequency (natural frequency) and, as will be described later, a sensor head for measuring the film thickness and film formation rate of the organic film deposited on the substrate W. Configure.
  • the film thickness sensor 14 is disposed inside the vacuum chamber 11 and at a position facing the organic material source 12.
  • the film thickness sensor 14 is typically disposed in the vicinity of the substrate holder 13.
  • the output of the film thickness sensor 14 is supplied to the measurement unit 17.
  • the measurement unit 17 measures the film thickness and the film formation rate based on the change in the resonance frequency of the crystal resonator, and controls the organic material source 12 so that the film formation rate becomes a predetermined value.
  • the relationship between the frequency change due to the adsorption of the QCM and the mass load is the Sauerbrey equation expressed by the following equation (1).
  • the film forming apparatus 10 further includes a shutter 16.
  • the shutter 16 is disposed between the organic material source 12 and the substrate holder 13, and can open or shield the incident path of organic material particles from the organic material source 12 to the substrate holder 13 and the film thickness sensor 14. Configured.
  • the opening and closing of the shutter 16 is controlled by a control unit (not shown).
  • the shutter 16 is closed at the beginning of deposition until the organic material source 12 stabilizes the emission of organic material particles.
  • the shutter 16 is opened.
  • the organic material particles from the organic material source 12 reach the substrate W on the substrate holder 13 and the film forming process of the substrate W is started.
  • the organic material particles from the organic material source 12 reach the film thickness sensor 14, and the film thickness of the organic film deposited on the substrate W and its film formation rate are monitored.
  • FIG. 2 is a schematic configuration diagram of the film thickness sensor 14.
  • the film thickness sensor 14 includes an oscillator 20 and a case 140 that accommodates the oscillator 20 so as to vibrate.
  • the oscillator 20 is accommodated in the case 140 such that the surface 21 faces the organic material source 12.
  • 3 and 4 are a front view and a rear view of the resonator 20, respectively.
  • Electrode films 31 and 32 having predetermined shapes are respectively formed on the front surface 21 and the back surface 22 of the oscillator 20.
  • the electrode films 31 and 32 are formed in mutually different shapes as shown by the shaded portions in FIGS. 3 and 4, but the shape of the electrode films 31 and 32 is not limited to the illustrated example.
  • the electrode films 31 and 32 are each formed of a metal film such as gold or silver.
  • the oscillator 20 oscillates in a thickness shear vibration mode when a high frequency voltage is applied to the electrode films 31 and 32.
  • a crystal resonator having a fundamental frequency (natural frequency) of 4 MHz is used as the oscillator 20.
  • the film thickness and the film formation rate can be measured with high accuracy.
  • the fundamental frequency of the oscillator 20 is not limited to 4 MHz, and a crystal resonator having any fundamental frequency of 4 MHz or less (for example, 3.25 MHz, 2.5 MHz, etc.) is applicable.
  • the vibration characteristics of the crystal resonator can be evaluated by the equivalent resistance and the Q value. That is, the smaller the equivalent resistance, the easier the vibration, and the higher the Q value, the more stable resonance vibration can be obtained.
  • the inventors prepared AT cut crystal resonator samples having fundamental frequencies of 3.25 MHz, 4 MHz, 5 MHz, and 6 MHz, respectively, and each sample had an organic film (Alq3 (Tris (8 -Equivalent resistance (R1) and Q value when quinolinolato) aluminum)) was attached, respectively.
  • Alq3 Tris (8 -Equivalent resistance (R1) and Q value when quinolinolato) aluminum
  • the half-value frequency width (FW) means a full frequency width ( ⁇ f) at a point 3 dB (decibel) lower than the peak value at the peak frequency (f 0 ) of the amplitude, and the Q value is expressed by f 0 / ⁇ f.
  • both the equivalent resistance (R1) and the half-value frequency width (FW) increase.
  • the equivalent resistance (R1) and the half-value frequency width (FW) when the fundamental frequency is 5 MHz are about 3.5 k ⁇ and about 4 kHz, respectively, and the equivalent resistance (R1) and the half-value frequency width when the fundamental frequency is 4 MHz ( FW) is about 2 k ⁇ and 800 Hz, respectively.
  • the equivalent resistance (R1) increases, the vibrator is less likely to vibrate, and as the half-value frequency width (FW) increases, the Q value of the vibrator decreases. Therefore, it can be said that the smaller the equivalent resistance (R1) and the half-value frequency width (FW), the more advantageous in the formation of the organic film.
  • FIG. 7 shows an experimental result when the film formation rate of the organic film (Alq3 (Tris (8-quinolinolato) aluminum)) is measured using a crystal resonator having a fundamental frequency of 5 MHz. As shown in FIG. 7, it can be seen that the rate of the quartz crystal resonator starts to fluctuate greatly after about 100 minutes.
  • Alq3 Tris (8-quinolinolato) aluminum
  • FIG. 8 shows an experimental result when the film formation rate of the organic film was measured using a crystal resonator having a fundamental frequency of 4 MHz. As shown in FIG. 8, in the crystal resonator, there is almost no fluctuation in the rate, and a stable resonance state can be maintained for a long time.
  • the difference in rate stability due to the difference in the fundamental frequency of the crystal unit has a strong correlation with the magnitude of the above-mentioned equivalent resistance (R1) and half-value frequency width (FW).
  • R1 equivalent resistance
  • FW half-value frequency width
  • the fundamental frequency of the crystal resonator As described above, by setting the fundamental frequency of the crystal resonator to 4 MHz or less, it is possible to extend the lifetime of the resonator as a film thickness sensor as compared with a crystal resonator having a fundamental frequency of 5 MHz or more. At the same time, the thickness and deposition rate of the organic film can be stably measured. Thereby, for example, in the manufacturing process of the organic EL display, the film thickness control and the film formation rate control of the organic layer can be performed with high accuracy.
  • the equivalent resistance and the half-value frequency width are remarkably large as compared with the case of forming an inorganic film.
  • the equivalent resistance (R1) is 1.2 k ⁇
  • the half-value frequency width is 500 Hz. This also shows that when the organic film is formed, it is preferable that the fundamental frequency of the crystal resonator is low in order to ensure stable resonance vibration.
  • the half-value frequency width (FW) can be expressed by the following equation (2).
  • ⁇ Fw is a half value of the half-value frequency width (FW)
  • G is a complex elastic modulus (MPa) of the organic film
  • G ′′ is a loss elastic modulus (dynamic loss) (MPa) of the organic film
  • ⁇ is an angle.
  • Frequency h f is the thickness of the deposited organic film (nm)
  • ⁇ f is the density of the deposited organic film (g / cm 2 )
  • F 0 is the fundamental frequency (Hz)
  • Z q is the shear mode sound of the crystal
  • the impedance (gm / sec / cm 2 ) is shown respectively.
  • FIG. 9 shows the temperature characteristics when an organic film (Alq3 (Tris (8-quinolinolato) aluminum) having a thickness of 60 ⁇ m) is deposited on one surface of each of the vibrator samples.
  • the temperature characteristic means the temperature dependence characteristic of the oscillation frequency of the crystal resonator.
  • FIG. 10 shows thermal shock characteristics of each of the vibrators, both when the organic film having the above thickness is deposited and when it is not deposited.
  • the thermal shock characteristic means a frequency characteristic when the crystal resonator is instantaneously subjected to radiant heat, for example, when the shutter 16 (FIG. 1) is opened.
  • a crystal resonator with a fundamental frequency of 4 MHz or less has a very small frequency change with respect to temperature change and thermal shock compared to a crystal resonator with a fundamental frequency of 5 MHz or more. Therefore, according to the present embodiment, it is possible to perform stable film thickness measurement or film formation rate control without being affected by the temperature change in the chamber or the radiant heat accompanying the opening and closing of the shutter. Further, since complicated temperature compensation calculation based on the temperature characteristics of the vibrator and control such as stopping the calculation until the frequency of the crystal vibrator is stabilized when the shutter is opened, control of the measurement unit 17 is simplified. Can be realized.
  • FIG. 11 is a schematic block diagram showing a configuration example of the measurement unit 17.
  • the measurement unit 17 includes an oscillation circuit 41, a measurement circuit 42, and a controller 43.
  • the oscillation circuit 41 oscillates the oscillator 20 (quartz crystal resonator) of the film thickness sensor 14.
  • the measurement circuit 42 is for measuring the resonance frequency of the oscillator 20 output from the oscillation circuit 41.
  • the controller 43 calculates the resonance frequency of the oscillator 20 from the output of the measurement circuit 42, and based on this, calculates the film formation rate of the organic material particles on the substrate W and the film thickness of the organic film deposited on the substrate W. To do.
  • the controller 43 further controls the organic material source 12 so that the film formation rate becomes a predetermined value.
  • the measurement circuit 42 includes a mixer circuit 51, a low-pass filter 52, a low-frequency counter 53, a high-frequency counter 54, and a reference signal generation circuit 55.
  • the signal output from the oscillation circuit 41 is input to the high frequency counter 54, and first, the approximate value of the oscillation frequency of the oscillation circuit 41 is measured.
  • the approximate value of the oscillation frequency of the oscillation circuit 41 measured by the high frequency counter 54 is output to the controller 43.
  • the controller 43 oscillates the reference signal generation circuit 55 at a reference frequency close to the measured approximate value.
  • a signal having a frequency oscillated at the reference frequency and a signal output from the oscillation circuit 41 are input to the mixer circuit 51.
  • the mixer circuit 51 mixes the two types of input signals and outputs them to the low frequency counter 53 via the low pass filter 52.
  • the signal input from the oscillation circuit 41 is cos (( ⁇ + ⁇ ) t) and the signal input from the reference signal generation circuit is cos ( ⁇ t)
  • cos ( ⁇ t) ⁇ cos
  • An AC signal expressed by the equation ( ⁇ + ⁇ ) t) is generated. This equation is in the form of multiplying cos ( ⁇ t) and cos (( ⁇ + ⁇ ) t), and the AC signal represented by this equation is a high frequency component represented by cos ((2 ⁇ ⁇ + ⁇ ) t). And a low frequency component signal represented by cos ( ⁇ t).
  • the signal generated by the mixer circuit 51 is input to the low-pass filter 52, the high-frequency component signal cos ((2 ⁇ ⁇ + ⁇ ) t) is removed, and only the low-frequency component signal cos ( ⁇ t) is input to the low-frequency counter 53. Entered. That is, the low frequency counter 53 has a low frequency component that is an absolute value
  • the low frequency counter 53 measures the frequency of the low frequency component signal and outputs the measured value to the controller 43.
  • the controller 43 calculates the frequency of the signal output from the oscillation circuit 41 from the frequency measured by the low frequency counter 53 and the frequency of the output signal of the reference signal generation circuit 55. Specifically, when the frequency of the output signal of the reference signal generation circuit 55 is smaller than the frequency of the output signal of the oscillation circuit 41, the frequency of the low frequency component signal is added to the output signal of the oscillation circuit 41, In the opposite case, subtract.
  • the oscillation frequency of the reference signal generation circuit 55 is It becomes lower than the actual oscillation frequency of the circuit 41. Therefore, in order to obtain the actual oscillation frequency of the oscillation circuit 41, the frequency
  • the resolution of the low-frequency counter 53 has an upper limit, the resolution can be assigned to measure the difference frequency
  • the oscillation frequency of the reference signal generation circuit 55 is controlled by the controller 43, and the oscillation frequency can be set so that the difference frequency
  • the obtained frequency value is stored in the controller 43.
  • high frequency resolution can be maintained even when a crystal resonator having a relatively low oscillation frequency of 4 MHz or less is used by using the measurement unit 17 having the above configuration. As a result, it is possible to ensure a film thickness measurement accuracy equal to or higher than that of a crystal resonator having a fundamental frequency of 5 MHz or higher.
  • the resonance frequency of the crystal unit gradually decreases as the deposition amount increases, and when the predetermined frequency is reached, stable film thickness measurement is no longer possible. The frequency variation becomes so large that it cannot be performed. For this reason, when the resonance frequency is lowered by a predetermined value or more, it is determined that the lifetime has been reached, and the quartz crystal unit is replaced.
  • a sensor head configured to hold a plurality of crystal resonators and switch each crystal resonator individually is used.
  • a film thickness sensor used for vapor deposition of a metal film or an oxide film generally has a crystal resonator (surface roughness (Ra) of about 0. 27 ⁇ m) is used. The purpose of this was to make it difficult to peel off when the metal film or oxide film was deposited thickly on the film formation surface.
  • FIG. 12 shows a result of an experiment in which 12 crystal units are sequentially switched every 5 minutes by using 12 sensor heads, and the film formation rate is measured.
  • the vertical axis indicates the measurement rate [ ⁇ / s].
  • the horizontal axis represents time [minutes].
  • FIG. 13 is a plot of the average rate variation of each of the above-mentioned crystal resonators.
  • the vertical axis represents the variation [%] with respect to the average rate of the crystal resonator immediately before switching, and the horizontal axis represents the crystal resonator. No. is shown respectively.
  • the measurement unit 17 described with reference to FIG. 11 was used to measure the film formation rate, and a crystal resonator having a fundamental frequency of 5 MHz was used as the crystal resonator (oscillator 20).
  • the measurement rate has changed by about ⁇ 5 to 10% before and after switching of the crystal unit. Further, as shown in FIG. 13, the variation in the rate of each crystal resonator is not constant, and it is difficult to stably measure the film formation rate.
  • the inventors pay attention to the fact that the above-mentioned phenomenon is caused by the roughness of the electrode of the quartz plate on the film quality of the organic film deposited on the film-forming surface of the crystal resonator. It has been found that the organic film is uniformly applied on the quartz plate, and variation in the measurement rate is reduced. Therefore, the present inventors have suppressed the variation in the measurement rate before and after switching the crystal resonator by smoothing the surface of the crystal resonator so that the surface of the film is a mirror surface.
  • FIG. 14 shows a sequence of twelve quartz crystal resonators (hereinafter referred to as “sample 1”) having a fundamental frequency of 5 MHz and having a film surface roughness (Ra) of 0.27 ⁇ m.
  • the variation in the measurement rate is compared with the variation in the measurement rate when twelve crystal resonators (hereinafter referred to as sample 2) having a surface roughness (Ra) of 0.02 ⁇ m are sequentially switched.
  • a gold thin film having a thickness of 0.25 ⁇ m was formed on each surface of samples 1 and 2 as electrode films 31 and 32 (see FIGS. 3 and 4).
  • the surface roughness (Ra) of the electrode films 31 and 32 was equivalent to the surface roughness (Ra) of the crystal resonator.
  • sample 2 has a smaller variation in measurement rate than sample 1, so sample 2 can measure the deposition rate stably and with high accuracy. It becomes.
  • FIG. 15 shows a case where twelve crystal resonators (hereinafter referred to as “sample 3”) having a fundamental frequency of 4 MHz and having a surface roughness (Ra) of 0.02 ⁇ m are sequentially switched. The variation in the measurement rate is shown in comparison with Sample 2.
  • the variation in the measurement rate can be reduced as the crystal resonator film formation surface is closer to the mirror surface or the crystal resonator has a lower fundamental frequency. It becomes possible to measure.
  • the surface roughness (Ra) of the film formation surface of the crystal resonator is, for example, 0.2 ⁇ m or less, and more preferably 0.1 ⁇ m or less. This makes it possible to measure the film formation rate of the organic film with high accuracy.
  • the fundamental frequency may be 5 MHz or less, but is more preferably 4 MHz or less as described above.
  • Alq3 tris (8-quinolinolato) aluminum
  • the organic film is not limited to this, and other organic materials such as a synthetic resin thin film can be used.
  • the present invention can also be applied to a membrane.
  • the vacuum deposition apparatus has been described as an example of the film forming apparatus.
  • the present invention is not limited to this, and the present invention can be applied to other film forming apparatuses such as a sputtering apparatus.
  • the organic material source is constituted by a sputtering cathode including a target made of an organic material.

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  • Electroluminescent Light Sources (AREA)

Abstract

　La présente invention concerne un dispositif de formation de film, un procédé de mesure de l'épaisseur de film d'un film organique, et un capteur d'épaisseur de film pour un film organique, au moyen desquels il est possible, avec une très haute précision, de contrôler le taux de formation de film et de mesurer l'épaisseur de film d'un film organique. Le dispositif (10) de formation de film est équipé d'une chambre à vide (11), d'une source (12) de matière organique, d'un support (13) de substrat, d'un capteur (14) d'épaisseur de film, et d'une unité de mesure (17). La source (12) de matière organique est agencée à l'intérieur de la chambre à vide (11) et est conçue de sorte à pouvoir libérer des particules de matière organique. Le support (13) de substrat est agencé de sorte à faire face à la source (12) de matière organique et est conçu de sorte à pouvoir maintenir un substrat (W). Le capteur (14) d'épaisseur de film est agencé à l'intérieur de la chambre à vide (11) et comporte un oscillateur à cristal ayant une fréquence fondamentale inférieure ou égale à 4 MHz. L'unité de mesure (17) mesure l'épaisseur de film d'un film organique déposé sur le substrat (W) sur le support (13) de substrat sur la base de variations dans la fréquence de résonance de l'oscillateur à cristal.
PCT/JP2015/002580 2014-05-26 2015-05-22 Dispositif de formation de film, procédé de mesure d'épaisseur de film d'un film organique, et capteur d'épaisseur de film pour film organique WO2015182090A1 (fr)

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KR1020187015514A KR20180063369A (ko) 2014-05-26 2015-05-22 성막 장치, 유기막의 막후 측정 방법 및 유기막용 막후 센서
CN201580020079.7A CN106232858A (zh) 2014-05-26 2015-05-22 成膜装置、有机膜的膜厚测量方法以及有机膜用膜厚传感器
KR1020167026478A KR102035146B1 (ko) 2014-05-26 2015-05-22 성막 장치, 유기막의 막후 측정 방법 및 유기막용 막후 센서
SG11201608133PA SG11201608133PA (en) 2014-05-26 2015-05-22 Film-forming device, method for measuring film thickness of organic film, and film thickness sensor for organic film
JP2016523133A JP6078694B2 (ja) 2014-05-26 2015-05-22 成膜装置、有機膜の膜厚測定方法および有機膜用膜厚センサ

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JP2014107816 2014-05-26
JP2014-107816 2014-05-26

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JP (1) JP6078694B2 (fr)
KR (2) KR102035146B1 (fr)
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TWI606134B (zh) * 2016-08-05 2017-11-21 財團法人工業技術研究院 膜厚度監測系統及使用所述系統的方法
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KR20180110004A (ko) 2016-05-06 2018-10-08 가부시키가이샤 알박 박막 제조 장치, 박막 제조 방법
KR20180137512A (ko) 2016-05-13 2018-12-27 울박, 인크 유기 박막 제조 장치, 유기 박막 제조 방법
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TWI701641B (zh) * 2019-10-01 2020-08-11 龍翩真空科技股份有限公司 無線傳輸薄膜厚度監控裝置
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CN106232858A (zh) 2016-12-14
KR20160127078A (ko) 2016-11-02
SG11201608133PA (en) 2016-11-29

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