JP5784885B2 - Oxygen partial pressure control heat treatment equipment - Google Patents

Description

  The present invention relates to an oxygen partial pressure control heat treatment apparatus.

  For the development of advanced devices, oxygen partial pressure control devices are used in combination with temperature control devices such as electric furnaces.

The oxygen partial pressure control device reduces the oxygen partial pressure in argon gas (generally synonymous with oxygen concentration in gas) to 10 ⁻³⁰ atm or less.

If a filter or adsorbent is used to remove oxygen in the argon gas, it is not easy to reduce the oxygen partial pressure to 10 ⁻⁹ atm (lppb) or less. The pressure is reduced. In the case of using this solid electrolyte, oxygen is removed using zirconium (zirconia), which is a solid electrolyte that transmits oxygen ions.

  In Patent Document 1, a voltage is applied between electrodes of an oxygen molecule discharging device having a hollow ceramic solid electrolyte body, an inner electrode and an outer electrode, a heating device, a voltage applying means, and an oxygen molecule discharging device. And providing a control device for controlling the oxygen partial pressure in the gas passing through the hollow.

  Patent Document 2 describes a heat treatment method and apparatus that are continuously performed in a controlled oxygen partial pressure atmosphere by a horizontal furnace.

JP 2008-231466 A JP-A-4-110034

  Patent Document 1 describes means for controlling oxygen partial pressure, and Patent Document 2 describes heat treatment means using oxygen partial pressure. Developers involved in advanced device development must individually handle each device. Procured and used in combination. For this reason, “temperature” and “oxygen concentration” are individually controlled, and the control is not performed in conjunction with the two, and the highly linked “temperature” and “oxygen concentration” control necessary for the experiment is not performed. Not realized.

  In view of the above, an object of the present invention is to provide an oxygen partial pressure control processing apparatus excellent in usability (user usability) capable of controlling the “temperature” and the “oxygen concentration” in a unified manner.

The present invention includes a heat treatment part for heat-treating a sample disposed therein with an atmospheric gas whose oxygen partial pressure is controlled, a heat treatment part temperature sensor for measuring the temperature of the heat treatment part, and a temperature for controlling the temperature of the heat treatment part. A controller, an atmosphere gas supply line that is connected to the heat treatment section and supplies an atmosphere gas under oxygen partial pressure control, a discharge line that discharges the atmosphere gas subjected to heat treatment, and oxygen partial pressure control of the atmosphere gas In an oxygen partial pressure control heat treatment apparatus including an oxygen partial pressure controller and an oxygen partial pressure sensor,
A box-shaped body that integrally incorporates the heat treatment section, temperature controller, atmospheric gas supply line, discharge line, oxygen partial pressure controller, and oxygen partial pressure sensor;
The oxygen partial pressure sensor is a downstream oxygen partial pressure sensor disposed on the discharge line and downstream of the heat treatment section;
A measuring oxygen partial pressure signal transmitted from the downstream oxygen partial pressure sensor, a measured temperature signal transmitted from the previous heat treatment temperature sensor, and an input operation; Based on the operation control information, the heat controller temperature control diagram and the oxygen partial pressure control diagram are displayed on the screen unit with a common time axis, and the temperature controller is displayed based on these displayed diagrams. An oxygen partial pressure control heat treatment apparatus is provided, comprising an operation controller that transmits a temperature control signal to the oxygen partial pressure controller and an oxygen partial pressure control signal to the oxygen partial pressure controller.

  The present invention is also characterized in that the operation controller displays a heat treatment part temperature diagram and an oxygen partial pressure diagram showing a control state on the screen part with a common time axis. Providing the device.

  According to the present invention, the heat treatment part includes an infrared heat treatment part and a cooling gas cooling means, and a rapid crunch part is formed inside the box-like body, whereby rapid heating and cooling are performed in the box-like body. An oxygen partial pressure control device is provided.

  In the present invention, the oxygen partial pressure control processing apparatus is connected to a personal computer via a network, and the temperature controller and the oxygen partial pressure controller are controlled from the personal computer having the operation controller function described above. An oxygen partial pressure control heat treatment apparatus is provided.

  The present invention includes the operation controller as described above, and transmits the temperature control signal to the temperature controller and the oxygen partial pressure control signal to the oxygen partial pressure controller. Based on the measured oxygen partial pressure signal from the downstream oxygen partial pressure sensor, the measured temperature signal from the heat treatment section temperature sensor, and the input operation control information, the heat treatment section temperature control diagram and the oxygen partial pressure control chart are timed. Since the axes are displayed in common, an oxygen partial pressure control processing apparatus excellent in usability capable of controlling “temperature” and “oxygen concentration” in a unified manner is provided.

The figure which shows the concept of the Example of this invention. The figure which shows the structure of the present Example integrated. The figure which shows the control method and means of a present Example. The figure which shows the diagram displayed on a screen part.

Embodiments of the present invention will be described below with reference to the drawings.

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

  In FIG. 1, an oxygen partial pressure control processing apparatus 100 according to an embodiment of the present invention includes a box-like body 1, and the box-like body has a tubular infrared heat treatment furnace as a heat treatment section, for example, a cooling gas, as will be described later. The temperature of an infrared heat treatment unit, an oxygen partial pressure control unit, and a tubular infrared rapid quenching heat treatment furnace that can be configured by an infrared rapid quenching heat treatment furnace that can be introduced (hereinafter, an infrared rapid quenching heat treatment furnace will be described as an example). Infrared rapid quenching furnace temperature sensor as heat treatment temperature sensor, temperature controller for controlling temperature of tubular infrared rapid quenching heat treatment section, oxygen gas pressure controlled atmosphere gas supply line, atmosphere gas used in experiment A discharge line, an oxygen partial pressure control unit, an oxygen partial pressure controller for providing a control signal, and an oxygen partial pressure sensor are integrally provided. An operation controller is provided in the box-like body in association with the temperature controller and the oxygen partial pressure controller. As will be described later, the driving operation controller has screen display means 5, and a screen portion which is a part of the screen display means is installed on the surface of the box-shaped body 1. This screen unit can be a touch panel using a GUI as shown in FIG. The infrared rapid quenching heat treatment furnace may be a vertical type or a two-chamber type for heating and cooling. An infrared heating and cooling furnace capable of raising the temperature up to 1000 ° for about 12 seconds and cooling speed up to 100 ° for about 12 seconds in the gas can be used.

  The oxygen partial pressure control device 100 can be connected to a large number of personal computers (PCs) 2 via the network 3, and controls the “temperature” and “oxygen concentration” not only from the screen display means 5 but also from each personal computer. Controllable. Further, it is possible to similarly control the “temperature” and “oxygen concentration” using the USB 4 from the personal computer 2. Software for program pattern operation that enables such control is incorporated in the oxygen partial pressure control apparatus 100.

  FIG. 2 shows a state in which the tubular infrared rapid quenching heat treatment furnace section 11 and the oxygen partial pressure control section 12 are incorporated in the box-shaped body 1. FIG. 2 does not show a tubular infrared rapid quenching heat treatment furnace temperature sensor, a temperature controller, an atmosphere gas supply line, a discharge line, an oxygen partial pressure controller, and an oxygen partial pressure sensor, but these devices are also integrated. Built in. In FIG. 2, each device incorporated in the box-like body 1 should be indicated by a dotted line, but is drawn by a solid line for clear display. As illustrated in FIG. 2, according to the example illustrated in FIG. 2, the tubular infrared rapid quenching heat treatment furnace unit 11 and the oxygen partial pressure control unit 12 are disposed close to each other in the box. Along with this, each sensor is also arranged integrally in the box, and a signal for accurate control is obtained.

  The tubular infrared rapid quenching heat treatment furnace 11 is a horizontally long shape arranged in a horizontal direction, and is a heat treatment furnace 13 capable of rapidly heating a sample in a clean atmosphere and an infrared lamp for heating the heat treatment furnace 13. The infrared part 14 formed is provided. A sample can be inserted into the space inside the heat treatment furnace 13. The heat treatment furnace 13 is connected with a cooling gas introduction pipe 36 for introducing a cooling gas and a cooling gas discharge pipe 37 for discharging the used cooling gas. These pipes are provided with valves (not shown), and a cooling gas introduction control device (not shown) is attached to the cooling gas introduction pipe 36. The cooling gas is introduced into the heat treatment furnace 13 from the cooling gas introduction pipe 36. The introduced cooling gas flows through the heat treatment furnace 13 to cool the sample on the sample holder 15, and from the cooling gas discharge pipe 37 to the outside. Discharged. As the cooling gas, for example, helium gas having good thermal conductivity is used, and the flow rate of the cooling gas is controlled by a cooling gas introduction control device. In this way, the cooling gas cooling means is configured.

  A temperature controller 34 for controlling the temperature of the heat treatment furnace 13 controls the temperature of the sample on the sample holder 15 to a temperature increase rate, a cooling rate or a constant temperature state programmed in advance. The temperature controller 34 performs PID control on the input power to the infrared part 14 formed by the infrared lamp while detecting the sample temperature with the heat treatment part temperature sensor (thermocouple 35), and also controls the cooling temperature.

  The oxygen partial pressure control unit 12 is disposed below the heat treatment furnace 13. As described in Patent Document 1 and other documents, the oxygen partial pressure control unit 12 includes a hollow ceramic (SiOC) solid electrolyte body, an oxygen molecule discharging device having an inner electrode and an outer electrode, and a heating device. And a voltage applying means, and configured to control the oxygen partial pressure in a gas passing through the hollow, for example, argon gas, by applying a voltage between the electrodes of the oxygen molecule discharging apparatus. In the oxygen molecule discharging apparatus, the PID constant is defined as a function of the oxygen partial pressure, and each time the current value of the oxygen partial pressure is sampled from the oxygen sensor, it is automatically adjusted to a value corresponding to the function, and the PID after adjustment PID control of the oxygen molecule discharge operation is performed based on the constant.

  The box-shaped body 1 includes an integrated controller 16. The integrated controller 16 includes the screen display means 5 shown in FIG. 1, and further includes an operation controller 35, a temperature controller 34, and an oxygen partial pressure controller 33 shown in FIG.

  As described above, the screen display means 5 includes the screen unit 17, and driving operation information (data) is easily set from the touch panel of the screen unit 17. In this way, the operating conditions are set and the state is displayed using the touch panel.

FIG. 3 shows the oxygen partial pressure control method and means of the oxygen partial pressure control apparatus 100.
In FIG. 3, the heat treatment furnace 13 of the tubular infrared rapid quenching heat treatment furnace section 11 is connected to the oxygen partial pressure control section 12 (indicated by SiOC in FIG. 13) via a connection line 21.

  An atmosphere gas (for example, argon gas) supply line 22 is connected to the inlet side, that is, the upstream side of the oxygen partial pressure control unit 12, and a stop valve 23 is provided in the supply line 22. The supply line 22 is branched into three lines, and a stop valve 24 and a flow rate regulator 25 are provided in each branch line, and atmosphere gas 1, atmosphere gas 2 or atmosphere gas 3 is provided in each branch line. Supplied.

  An exhaust line 26 of the atmospheric gas used for the experiment is connected to the outlet side of the heat treatment furnace 13, that is, the downstream side, and a stop valve 27 is provided in the exhaust line 26.

  As described above, the solid electrolyte is formed in a tube shape, electrodes are formed on the inner and outer surfaces, and a voltage is applied. When commercially available argon gas is supplied from one end of the tube, oxygen contained as impurities obtains electrons on the inner surface electrode and becomes oxygen ions. Oxygen ions pass through the tube wall and reach the outer electrode, release electrons, return to oxygen, and are discharged.

On the other hand, since the argon gas cannot pass through the tube wall of the solid electrolyte, it passes through the tube as it is. As a result, the argon gas from which oxygen has been removed flows out at the tube outlet. According to this method, the oxygen partial pressure in the argon gas can be reduced to 10 ⁻³⁰ atm or less.

  An oxygen partial pressure sensor 31 is provided in the connection line 21 on the outlet side of the oxygen partial pressure control unit 12, and another oxygen partial pressure sensor 32 is provided in the exhaust line 26 on the outlet side of the heat treatment furnace 13. The measured oxygen partial pressure signals from the oxygen partial pressure sensors 31 and 32 are input to the oxygen controller 33 and the operation controller 35. The horizontal furnace 13 and the coil 14 are provided with a thermocouple 35, and a temperature signal is input to the temperature controller 34.

  The operation controller 35 is connected to the oxygen partial pressure controller 33 and the temperature controller.

  In order to control the atmospheric gas to the target oxygen partial pressure, the upstream oxygen partial pressure sensor 31 on the upstream side of the tubular infrared rapid quenching heat treatment furnace section 11 connected to the oxygen partial pressure control section 12 or the downstream downstream stage. The oxygen concentration pressure sensor (downstream oxygen partial pressure sensor) 32 measures and monitors the oxygen concentration and feeds it back to the oxygen pump, but it affects the shape, size, temperature, etc. of the tubular infrared rapid quenching heat treatment furnace 11 The subsequent oxygen partial pressure sensor 32 controls the oxygen partial pressure side constant value. The use of the oxygen partial pressure sensor 32 at the latter stage becomes possible by the integration of the above-described configuration, which meets high needs, and enables unified control of the oxygen partial pressure and temperature. Furthermore, rapid quench control is also possible.

  In the tubular infrared rapid quenching heat treatment furnace unit 11, the sample is heated and cooled in an atmosphere controlled by the oxygen partial pressure control unit 12 with the sample holder 15 positioned in the center of the heat treatment furnace 13. After the predetermined rapid heating process is completed, the rapid cooling process is performed by switching. As a result, the steps from the rapid heating process to the rapid quenching in the heat treatment furnace 13 can be continuously performed in the controlled oxygen partial pressure atmosphere without exposing the box-shaped body 1 to the atmosphere.

  The driving operation controller 40 includes an input unit 41, an arithmetic processing unit 42, an output unit 43, a recording unit 44, and a screen display unit 45. The screen display unit 45 corresponds to the screen display unit 5 of FIG. 1 and includes a screen unit 17 (see FIG. 2).

  The operation controller 40 is transmitted from the measured oxygen partial pressure signal transmitted from the downstream oxygen partial pressure sensor 32 disposed close to the heat treatment furnace 13 in the box-shaped body 1, and from the heat treatment section temperature sensor, that is, the thermocouple 35. Based on the measured temperature signal and the operation control information input to the input means 41, a heat treatment part temperature control diagram and an oxygen partial pressure control diagram are displayed on the screen part.

  In the above example, an infrared rapid quenching heat treatment furnace is used, but instead of this, a box-type electric furnace and a rapid crunch device may be provided to perform rapid heating and rapid cooling separately.

  FIG. 4 shows a state in which the heat treatment part temperature control diagram 46 and the oxygen partial pressure control diagram 47 are displayed on the screen unit 17.

As shown in FIG. 4, a heat treatment part temperature control diagram 46 and an oxygen partial pressure control diagram 47 are displayed with a common time axis. Each diagram can also be displayed individually. These displays can be performed for both setting of operating conditions and status display. When operating conditions are set, based on these displayed diagrams, a temperature control signal 48 is transmitted to the temperature controller 34, and an oxygen partial pressure control signal 49 is transmitted to the oxygen partial pressure controller. The tubular electric furnace unit 11 and the oxygen partial pressure control unit 12 are controlled through the control unit 34 and the oxygen partial pressure controller 33, respectively. In this way, unified control of “temperature” and “oxygen concentration” is performed.
Further, the operation controller 35 displays a heat treatment temperature diagram and an oxygen partial pressure diagram showing the control state on the screen unit 17 with a common time axis. These diagrams can be displayed individually.

  As shown in FIG. 1, the oxygen partial pressure control apparatus 100 configured as described above is connected to a personal computer 2 at various locations via a network 3, and the personal computer 2 has the function of the operation controller 40. Operating conditions can be input to the oxygen partial pressure control device 100 from the screen of the personal computer 2 (corresponding to the drawing unit 17), and the temperature controller 34 and the oxygen partial pressure controller 33 can be controlled. In addition, the control state can be displayed on the same screen. The same applies when USB is used.

  DESCRIPTION OF SYMBOLS 1 ... Box-shaped body, 2 ... Personal computer, 3 ... Network, 5 ... Screen display apparatus, 11 ... Tubular type infrared rapid quenching heat treatment furnace part (heat treatment part), 12 ... Oxygen partial pressure control part, 16 ... Integrated control part, DESCRIPTION OF SYMBOLS 17 ... Screen part, 21 ... Connection line, 22 ... Supply line, 26 ... Exhaust line, 31, 32 ... Oxygen partial pressure sensor, 33 ... Oxygen partial pressure controller, 34 ... Temperature controller, 35 ... Thermocouple, 40 ... Operation operation Controller, 42 ... arithmetic processing means, 45 ... screen display means, 46 ... heat treatment part temperature control diagram, 47 ... oxygen partial pressure control diagram, 48 ... temperature control signal, 49 ... oxygen partial pressure control signal, 100 ... oxygen content Pressure control device.

Claims (3)

A heat treatment part for heat-treating a sample disposed therein with an atmospheric gas whose oxygen partial pressure is controlled, a heat treatment part temperature sensor for measuring the temperature of the heat treatment part, a temperature controller for controlling the temperature of the heat treatment part, and An atmospheric gas supply line that supplies an atmospheric gas that is connected to the heat treatment section and that is subjected to oxygen partial pressure control, a discharge line that discharges the atmospheric gas subjected to the heat treatment, and an oxygen partial pressure controller that controls the oxygen partial pressure of the atmospheric gas And an oxygen partial pressure control heat treatment apparatus comprising:
A box-shaped body that integrally incorporates the heat treatment section, temperature controller, atmospheric gas supply line, discharge line, oxygen partial pressure controller, and oxygen partial pressure sensor;
The oxygen partial pressure controller performs oxygen partial pressure reduction control for removing oxygen contained as impurities in the atmospheric gas and reducing the oxygen partial pressure to 10 ⁻³⁰ atm or less. Introduced in
An oxygen partial pressure sensor disposed on the downstream side of the heat treatment section in the discharge line detects an oxygen partial pressure of the atmospheric gas discharged from the heat treatment section, and the detected oxygen partial pressure is the oxygen partial pressure. Input to the pressure controller, used for controlling the oxygen partial pressure reduction control,
A measuring oxygen partial pressure signal transmitted from the downstream oxygen partial pressure sensor, a measured temperature signal transmitted from the previous heat treatment temperature sensor, and an input operation; Based on the operation control information, the heat treatment section temperature control chart and oxygen partial pressure control chart are displayed on the screen section with a common time axis , the temperature controller displays a temperature control signal, and the oxygen partial pressure controller An oxygen partial pressure control heat treatment apparatus, comprising: an operation controller that transmits an oxygen partial pressure control signal.   In Claim 1, the said heat processing part is comprised by the infrared heat processing part and the cooling gas cooling means, and rapid heating cooling is performed in the said box-shaped body by making a quick quench part inside the said box-shaped body. An oxygen partial pressure control device characterized by being configured as described above.   The oxygen partial pressure control processing apparatus according to claim 1 is connected to a personal computer via a network, and the temperature controller and the oxygen partial pressure controller are controlled from the personal computer having the operation controller function described above. Oxygen partial pressure control heat treatment equipment.

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