JPH05757U - Carbon automatic film thickness vapor deposition equipment - Google Patents

Abstract

(57) [Summary] [Object] The present invention relates to an automatic carbon film thickness vapor deposition apparatus for automatically preparing a sample having a predetermined carbon film thickness deposited during the intermittent vapor deposition. It is intended to be created automatically. [Structure] Carbon vapor deposition is started on a sample 2 arranged in the vicinity by repeatedly supplying a pulsed large current to a contact portion between carbon rods 1 arranged in a vacuum for a short period of time, When the change in the frequency of the vibrator 3 arranged near the sample 2 reaches a preset predetermined value, or when the reference sample 10 and the measurement sample 11 are used to form a bridge and reach a preset value. At this time, the supply of the pulsed large current is stopped.

Description

[Detailed description of the device]

[0001]

[Industrial applications]

  The present invention is a method for automatically preparing a sample in which a predetermined carbon film thickness is vapor-deposited during intermittent vapor deposition. Carbon automatic film thickness deposition apparatus.

[0002]

[Prior art]

  A conventional carbon vapor deposition apparatus is used as shown in FIGS. Make one stick flat and the other one sharp like a pencil, touch them together in a vacuum Place it in the surrounding area to heat the carbon itself and evaporate it by passing an electric current between them. The sample is vapor-deposited on the sample. Also, as suggested by the inventors, As shown in (d) to (f) of 3, there is no pulsed large current in the carbon rod. Pulsed large current is short when using the method of flowing electricity (hereinafter referred to as the intermittent vapor deposition method) Supply for a period of time (eg 1 second or less), repeat after a pause (eg a few seconds) Then, place a blank paper near the sample, estimate the film thickness from the degree of color change, and stop the deposition. Or the number of repetitions of a pulsed large current is experimentally preset (for example, 10 (E.g. times), and evaporation is stopped when this number of times is repeated. It was

[0003]

[Problems to be solved by the device]

  When the above-mentioned deposition method is used, a large pulse current is applied for a short time (for example, 1 second or less). ) During this time, the carbon rod evaporates in an explosive arc-like condition. Therefore, I could not see the color change of carbon deposited on white paper placed near the sample. Practically, the film thickness is experimentally obtained based on the number of times a large pulsed current is supplied The problem is that it is difficult to deposit the carbon film on the sample with the desired thickness because it has to be stopped at was there.

[0004]   The present invention, when supplying a large pulsed current to a carbon rod for vapor deposition, Of the oscillation frequency when carbon is vapor-deposited on the oscillator placed in Configure a bridge with the created reference sample and measurement sample, and based on that value Stop vapor deposition and automatically create a sample with the desired carbon film thickness in the intermittent vapor deposition method Is intended.

[0005]

[Means for Solving the Problems]

  Means for solving the problems will be described with reference to FIGS. 1 and 2.   In FIG. 1 and FIG. 2, the carbon rod 1 generates a large pulse current for a short time. It is a rod that evaporates carbon by repeating supply and rest periods.   The vibrator 3 detects the amount of carbon vapor deposited.

[0006]   The reference sample 10 is a sample in which carbon is vapor-deposited in advance.   The measurement sample 11 is for detecting the carbon vapor deposition amount.

[0007]

[Action]

  The present invention is, as shown in FIG. 1, a contact portion between carbon rods 1 arranged in a vacuum. Repeatedly supplying a large pulsed current to the A vibrator placed in the vicinity of the sample 2 by starting carbon vapor deposition on the sample 2 placed in the vicinity When the change in frequency of 3 reaches a preset value, a large pulse current I am trying to stop the supply. In addition, as shown in FIG. A large pulsed current is supplied to the contact part of the carbon rod 1 for a short period of time and is supplied for a rest period. The carbon deposition was started on Sample 2 by repeating the placement, and the carbon deposition substrate was prepared in advance. A bridge is formed by the quasi sample 10 and the measurement sample 11, and the value of this bridge When the value reaches the preset value, the supply of pulsed large current is stopped. ing.

[0008]   Therefore, when a large pulsed current is supplied to the carbon rod 1 for vapor deposition, the vibrator 3 Of the oscillation frequency when carbon is vapor-deposited on the To form a bridge with the regular sample 11 and stop vapor deposition based on that value Therefore, the desired carbon film thickness can be automatically vapor-deposited on the sample 2 by the intermittent vapor deposition method. And are possible.

[0009]

【Example】

  Next, the configuration and operation of the embodiment of the present invention will be sequentially described in detail with reference to FIGS. 1 and 2. explain.   In FIG. 1, one end of the carbon rod 1 is cut into a thin columnar shape as shown. The other is a flat carbon rod, which is used to supply a large pulsed current for a short time. It is for supplying carbon, depositing a rest period, and depositing carbon on the sample 2.

[0010]   Sample 2 is a sample to be subjected to carbon vapor deposition (for example, observed with a scanning microscope) Therefore, it is a sample that has conductivity).   The vibrator 3 is a vibrator for detecting the amount of carbon deposited on the sample 2. , Is arranged near the sample 2 as shown in the drawing. An example of this oscillator 3 For example, by using a crystal unit and carbon deposition on it, its weight increases. As the natural frequency changes, the rate of change is calibrated and the film thickness of carbon deposited To be able to detect.

[0011]   The crystal film thickness meter 4 drives the vibrator 3 to cause the vibration due to carbon vapor deposition. The change in the natural frequency of the child 3 is detected to measure the thickness of the carbon deposited film. It Here, when the idle period signal from the cantilever oscillator 5 is used, the crystal thickness gauge 4 When the preset carbon film thickness is reached, a stop signal is sent to the intermittent transmitter 5. The notification is stopped and the supply of the pulsed current to the carbon rod 1 is stopped. This , The effect of noise during explosive arc-like carbon evaporation due to pulsed large current Can be avoided.

[0012]   The pulse oscillator 5 is a pulse-shaped, short-time (for example, 1 second or less) large pulse on the carbon rod 1. It oscillates a signal to supply current or provide a rest period (for example, several seconds). It is something. The canned oscillator 5 is generated by pressing the start switch 6. Then, a large pulsed current is started to be supplied to the carbon rod 1 and the When a stop signal indicating that the set carbon film thickness has been reached is sent, the current is supplied. Stop pay.

[0013]   The power supply 7 is an AC commercial power supply.   The transformer 8 is a step-down transformer for supplying a large pulsed current to the carbon rod 1. It is.   The switch 9 is a switch that turns on / off the power source on the primary side of the transformer 8.   Next, the operation of the configuration of FIG. 1A will be described with reference to FIG.

[0014]   (1) The operator turns on (a) the start switch 6 in FIG. 1 (see FIG. 1). (B) of (a)).   (2) Corresponding to (1), the pulse oscillator 5 switches the switch 9 for a short time (for example, For 0.2 seconds) and then switch 9 for the next rest period (eg 2 seconds). Signal to be repeatedly generated. As a result, the power supply 7, A large pulsed current flows through the lance 8 for a short time (for example, 0.2 seconds) (see FIG. 1). (Refer to (b)), an explosive arc is formed and the carbon sublimes, causing sample 2 and vibration. The pendulum 3 is vapor-deposited with carbon, and the carbon rod 1 is electrically charged during the next rest period (for example, 2 seconds). The supply of the flow is stopped to cool the sample 2 or the like whose temperature has risen.

[0015]   (3) In (2), a large pulsed electric current is applied to the carbon rod 1 for a short time, It is sublimated and adheres to the sample 2 and the vibrator 3 (see (b) in FIG. 1). And then When the quiescent period signal is sent from the oscillator 5, the crystal film thickness meter 4 is fixed on the oscillator 3. The change Δf of the frequency is calculated and the carbon film thickness corresponding to this change Δf Compared with the carbon film thickness set in (see (*) in Fig. 1B), the former exceeds the latter. When this happens, a stop signal is sent to the intermittent oscillator 5 to supply a pulsed large current. Stop. On the other hand, the carbon film thickness corresponding to Δf is set in advance by the operator. When the thickness of the carbon film is less than the thickness, the stop signal is not output. Then, a pulsed large current is supplied and the rest period is repeated.

[0016]   In addition, in (b) of FIG. 1, is the heating current I and is the car of (a) of FIG. It is the current I flowing through the bomb 1. The shaded area is the area where a large pulsed current flows. The other part represents a rest period in which no current flows. Of this rest period, At the time of * part, the (b) oscillator 5 of FIG. Notify and let them compare.

[0017]   Is a schematic representation of the film thickness of carbon deposited on sample 2.   Indicates start / stop. This is the start switch in (a) of Fig. 1. When the operator presses 6, (a) starts, and the oscillator 5 Switch 9 is repeatedly turned on and off to generate a large pulsed current for a short time Repeat feeding bar 1.

[0018]   As described above, the cantilever oscillator 5 controls the on / off of the switch 9, Repeatedly applying a pulsed large current to 1 for a short time and then putting a rest period Then, carbon is vapor-deposited on sample 2. At this time, notify the quartz film thickness meter 4 of the pause period signal. The car calculated from the change Δf of the natural frequency due to carbon deposition on the vibrator 3 When the Bon film thickness exceeds the preset value, a stop signal is output to the interrupt oscillator 5. To stop the current supply. As a result, the sample 2 was measured by the vibrator 3. It is possible to easily and automatically deposit a carbon film thickness equivalent to the carbon film thickness. It Here, during the rest period, the carbon film thickness is obtained from Δf and the preset value is set. The carbon film 1 is compared with the carbon film thickness. Carbon is not in an arc state during vapor deposition, so it may be affected by noise. Without, malfunction can be eliminated.

[0019]   Next, the configuration and operation of another embodiment will be described with reference to FIG.   FIG. 2A shows an example of measuring the resistance value.   In (a) of FIG. 2, the reference sample 10 is carbon-vapor-deposited on a glass plate or the like in advance. It is a sample that serves as a reference for comparison of the deposited resistance values. This reference sample 10 is As shown in (b) of 2, a low resistance conductor (for example, silver paint) is placed on the glass plate. Coating and vapor deposition of a conductive substance) are provided on both sides, and carbon is vapor-deposited on this. It

[0020]   The measurement sample 11 is a sample for measuring the resistance of the carbon film thickness. this Is a glass plate with low-resistance conductors on both sides, as shown in Fig. 2B. Is.   The amplifier 12 amplifies the bridge-connected signal.   The meter 13 measures a differential signal bridge-connected.

[0021]   R0, R1, R2, and RX are reference samples when bridge-connected as shown. Resistance value of the sample 10, reference resistance value, switchable reference resistance value, measurement sample 11 It is the resistance value. Here, by arbitrarily switching R2, the meter 13 becomes zero. When (R0 · R2 = RX · R1), the resistance value of the reference sample 10 is measured. The resistance value of the constant sample 11 is switched arbitrarily, and the sample 2 with an arbitrary carbon film thickness is automatically It is possible to create.

[0022]   FIG. 2C shows a specific circuit example. In this specific circuit example, the reference sample 10 Resistance value R0, resistance value RX of the measurement sample 11 and reference resistance R1 as shown in the figure. , R2 to form a bridge, and the difference signal at this time is compared by the comparator 14, For example, the resistance value RX of the measurement sample 11 is smaller than the resistance value R0 of the reference sample 10. When it gets cold, the stop signal shown in the figure is sent to the oscillator 5, and the carbon rod The current supply to 1 is stopped. The operation will be described in detail below.

[0023]   (1) The operator presses the start switch 6 to start carbon vapor deposition. It   (2) Corresponding to (1), the intermittent oscillator 5 closes the switch 9, and the power supply 7, A large pulsed current is passed through the transformer 8 for a short time (for example, 0.2 seconds) It is supplied between the rods 1 to cause explosive arc-like carbon evaporation. Then pause During the period (for example, 2 seconds), the switch 9 is opened, the current supply is stopped, the sample 2 and the like. Cool down. By repeating these steps, carbon is added to sample 2 and measurement sample 1 Attach to 1.

[0024]   (3) When carbon is repeatedly vapor-deposited as in (2), initially measured sample 1 If the resistance value RX of 1 was infinite, the value gradually decreased and the reference sample When it becomes smaller than the resistance value R0 of the loop 10, the signal of the output of the comparator 14 is inverted and Notify the chip oscillator 5 of the top signal and leave the switch 9 open to Stop evaporation. Here, the measurement of the resistance value by the bridge is performed during the rest period. , Avoid being affected by noise caused by explosive arc-like carbon deposition.

[0025]   As described above, the carbon-deposited reference sample 10 and the measurement sample 1 1 and a bridge is formed, and the resistance value RX of the measurement sample 11 is the reference sample. When the resistance value of R10 is less than R0, or a predetermined ratio (depending on the reference resistance When the ratio falls below a predetermined ratio, the oscillation of the signal by the intermittent oscillator 5 is stopped. Then, by stopping the carbon vapor deposition, the sample 2 having a desired carbon film thickness is automatically operated. Can be achieved. Further, regarding the resistance value RX of the measurement sample 11, A sample 2 having a desired carbon film thickness is prepared by comparing with the resistance value R0 of the quasi sample 10. As a result, the resistance value of carbon vapor deposition is 1000 MΩ to several tens of KΩ, depending on the film thickness. Furthermore, it is possible to easily set a wide range that is less than that.

[0026]

[Effect of device]

  As described above, according to the present invention, a large pulsed current is supplied to the carbon rod 1. When the carbon was vapor-deposited on the vibrator 3 arranged in the vicinity of the sample 2 during the supply and vapor deposition. Measurement by the change of the oscillation frequency Because it uses a structure that forms a bridge with the sample 11 and stops vapor deposition , It is possible to automatically deposit a desired carbon film thickness on the sample 2 in the intermittent deposition method. it can. This enables explosive arc-like carbon vapor deposition by intermittent vapor deposition. It is possible to control the thickness of the carbon film as desired and heat the carbon rod 1. Measure the carbon film thickness during the rest period when no current is supplied, and compare it with the reference sample. Therefore, the ring with extremely noisy arc-shaped noise is produced by the vacuum deposition method. Despite the boundaries, carbon is not affected by noise and is accurate and reproducible. It is possible to control the film thickness.

[Brief description of drawings]

FIG. 1 is a configuration diagram of an embodiment of the present invention.

FIG. 2 is a block diagram of another embodiment of the present invention.

FIG. 3 is an explanatory diagram of a conventional technique.

[Explanation of symbols]

1: Carbon rod 2: Sample 3: Transducer 4: Quartz film thickness meter 5: Canned oscillator 6: Start switch 7: Power supply 8: Transformer 9: Switch 10: Reference sample 11: Measurement sample 12: Amplifier 14: Comparator

Claims (2)

[Scope of utility model registration request] 1. An automatic carbon film thickness vapor deposition apparatus for automatically preparing a sample vapor-deposited with a predetermined carbon film thickness during intermittent vapor deposition, in which a large pulsed current is applied to a contact portion between carbon rods (1) arranged in vacuum. Carbon deposition is started on the sample (2) arranged in the vicinity by repeating supply and rest periods for a short time, and the change in frequency of the vibrator (3) arranged in the vicinity of the sample (2) is changed in advance. An automatic film thickness vapor deposition system for carbon, characterized in that the supply of said pulsed large current is stopped when the set predetermined value is reached. 2. In a carbon automatic film thickness deposition apparatus for automatically preparing a sample having a predetermined carbon film thickness deposited during intermittent deposition, a short pulse-like large current is applied to a contact portion of a carbon rod (1) placed in a vacuum. Carbon deposition is started on the sample (2) by repeatedly supplying and resting for a period of time, and a reference sample (10) preliminarily carbon-deposited on carbon and a measurement sample (11) arranged in the vicinity of the sample (2). A carbon automatic film thickness vapor deposition apparatus characterized in that a bridge is formed by using and the supply of the pulsed large current is stopped when the value of the bridge reaches a preset value. .