Ultra-High Temperature, Ultra-High Vacuum Distillation Furnace

I. Overview

This equipment is an ultra-high-temperature, ultra-high-vacuum distillation furnace that primarily exploits the principle that components with different vapor pressures and condensation temperatures at a given temperature can be separated, making it suitable for the smelting, distillation, and purification of high-melting-point rare or rare-earth metals.

II. Equipment Features:  

1. Total system power ≤ 1 5 0 kW; the heating power supply is a low-voltage IGBT power supply with constant-current and constant-power capabilities.

2. A tungsten–tantalum composite sheath with hafnium oxide insulation is used for ultra-high-temperature tungsten–rhenium thermocouple measurements, enabling temperature measurement and control over a range from room temperature to 2000°C. After calibration of the thermocouple and adjustment of the heating power, the thermocouple is automatically retracted; periodic recalibration is performed, and constant heating power is maintained via software control, thereby extending the thermocouple’s service life. The instantaneous maximum temperature is 2200°C (determined by infrared pyrometry under vacuum conditions), while the operating temperature is 2000°C (also under vacuum). Temperature control accuracy is better than ±5°C, and the system can be programmed for automated operation. The thermocouple temperature setpoint is located at the center of the crucible, and the infrared temperature setpoint is likewise centered in the crucible; these two setpoints are coordinated and controlled by software, ensuring precise and stable temperature regulation with no overshoot. Over the entire operating cycle, temperature drift is better than ±10°C. The system also provides protection for the furnace heating elements. The thermocouple and electrodes are installed in a cross-through configuration, facilitating maintenance.

3. Furnace Shell All materials 316L Stainless steel, to be installed before the entire vacuum chamber is assembled. 1000 °C, Electropolishing and 4× 10 ^-4 Pa Vacuum degassing For sealing, full-metal seals are used for static seals (with compatibility for fluororubber seals as well), while welded bellows seals are employed for dynamic seals, enabling attainment of a cold-state ultimate vacuum:  9.0 times 10 ^-8 Pa (Measurement point is the vacuum inside the furnace, not the pump inlet vacuum.) 1500 The ultimate vacuum degree in ℃ is 8.0 times 10^-6 Pa (Empty furnace) ,pressure rise rate less than or equal to 0.00 1 Pa/h.

4. A high-temperature, low-vapor-pressure tungsten–rhenium alloy rod heater is employed, with externally mounted, high-purity boron nitride insulators for suspension; the assembly is shielded by low-vapor-pressure, high-temperature tungsten–rhenium alloy and titanium–zirconium–molybdenum alloy. It will not contaminate the product. The purity of the resulting material can be guaranteed. The heater is suspended and mounted, ensuring no deformation prior to installation. to carry out 1200 °C, 4× 10 ^-4 Pa Vacuum Degassing and Deoxidation Handle 。

5. Control method: With manual / Multiple automatic and semi-automatic functions, manufactured by imported Mitsubishi. Programmable Logic Controller Implement overall control: the equipment can be operated automatically via programmed control, or switched to manual mode. / Semi-automatic operation, compatible with imported island-type electric and Raytech program temperature controllers, as well as computers and P LC , the heating power supply, and the program control of heating-up time and holding time, among others, All these parameters can be uploaded to a computer via the communication interface for recording, and the display uses 12 Inch HD touchscreen, elegant and stylish 。

6. Over-temperature alarm: heater power-off; water-loss alarm: heater power-off; gas-leak alarm: heater power-off; thermocouple-break alarm: heater power-off.

III. Equipment Technical Specifications Description:

1 , Feeding method: vertical top inlet and outlet

2 , Maximum operating temperature: 2200 degrees Celsius

Rated maximum operating temperature:  2000 °C, Empty furnace heating time: less than or equal to 200 me n 。

3 , Heater Dimensions F 260 times 400mm

4 , Pressure Rise Rate:   less than or equal to 0.001Pa/h (Under all-metal sealing conditions 24h The residual vacuum level is better than 0. 024Pa， Under fluororubber sealing conditions ，24h The residual vacuum level is better than 1Pa )

5. Cold-state ultimate vacuum:  9.0 times 10 ^-8 Pa (Metal ring seal) / 5.0 times 10^-6 (Fluororubber O-ring seal) Pa (Measurement point is the vacuum inside the furnace, not the pump inlet vacuum.)

6 1. Power supply: 380V 50HZ 。

7、 Maximum equipment height 3500 ㎜, occupying a area 4000 millimeter times 4000 millimeter

Four . Equipment composition:

The equipment comprises a furnace body (double-layer water cooling), a reflector screen, heating elements, a crucible assembly, a temperature measurement and control system, a vacuum unit, a vacuum measurement system, an upper-cover condensation device, a lower-cover crucible assembly, a frame, an electrical control system, and software. System Wait until it's done.

1. Furnace body

The furnace body features a double-layer water-cooling structure, and all materials are 316L Stainless steel; with water cooling through the interior. The vacuum chamber is divided into three independent sections: a water-cooled upper cover, a water-cooled chamber body, and a water-cooled lower base. The chamber body and the lower base are sealed using high-purity silver or high-purity copper wire, while the upper cover can be sealed either with high-purity silver or copper wire, or with a fluororubber gasket. Water-cooled electrodes and thermocouples are mounted on the furnace side. 、 Observation ports and infrared temperature measurement ports; the furnace bottom has C F200 Ash-Removal Hole , all components are inspected before the entire vacuum chamber is installed. 1000 ℃4× 10 ^-4 Pa24 Hour-long vacuum degassing and electrolytic polishing Processing.

Structural configuration: vertical, with top-opening lid and top discharge; the top lid is of a bell-shaped design.

Structural dimensions: Effective internal dimensions of the vacuum chamber F 600 times 1200mm；

Sealing method: sealed with high-purity silver, high-purity copper wire, or fluororubber O-rings;

2. Thermal insulation screen

The thermal insulation screen is made of 3 Tungsten-rhenium alloy screen, 3 High-temperature tungsten screen, 6-layer titanium-zirconium-molybdenum shield ( TZM) , consisting of a single layer of high-temperature molybdenum shell, with each insulation screen as an independent unit; prior to installation, all components are 1200 ℃4× 10 ^-4 Pa24 Hourly vacuum degassing and deoxidation Processing.

3. Heating element, crucible, and collection cylinder

The heating element is made of high-temperature tungsten rod, with hot-pressed boron nitride as the insulating material; heater dimensions: Φ26 0 ×40 0mm , Tungsten crucible (provided by the user) dimensions: ≤Φ16 0 ×24 0mm。

Tungsten or tantalum collection tube dimensions: Collection tube dimensions: ≤Φ16 0 ×50 0mm (To be provided by the user.)

4.  Temperature Measurement and Control System

Heating power supply ( 120KW ) Adopt low voltage IGBT constant-current DC power supply. Temperature measurement and control using the imported Shima FP9. 3 Temperature controller that allows setting of temperature profiles and heating rates, with precise temperature measurement and control. less than or equal to 1600 ±2℃ at ℃, 2000 ± at ℃ 5 °C, 16 Above 0°C, the measurement automatically switches to infrared thermometry. The tungsten–rhenium thermocouple is an ultra-high-temperature thermocouple with a tungsten–tantalum composite sheath and hafnium oxide insulation, and it can be electrically inserted into and withdrawn from the heating zone. 1600 Temperatures above °C are permitted only for short periods in the heating zone, and are intended solely for calibrating constant-current/constant-power power supplies and infrared thermometers. Infrared thermometers used for this purpose are also intended for calibrating the power of constant-current/constant-power power supplies and should not be used for prolonged temperature measurements.

The infrared temperature-measurement window is sapphire-welded and features a magnetic-coupling baffle inside.

5. Vacuum system

The vacuum system consists of Two sets of Tianyuan Stars CF 2 00 /2000 L/s High speed, high limit Molecular Pumps and Fustern 15 L/S Composed of a direct-drive mechanical pump.

The vacuum valve is 2 Taipei Scientific Instruments High Vacuum CF200 Electric plug valve and CF35 Composition of the angle valve.

In the vacuum chamber 2 Cs F200 Each outlet is equipped with a water-cooled radiation trap.

6. Rack

The equipment is fixed to a 1000 millimeter times 3000 On the mm platform, the top cover is equipped with an electric lifting mechanism, and the chamber is fitted with a lifting and moving crane.

7. Electrical control components

Industrial control computers and PLC controller with a user-friendly panel design for the control cabinet, offering intuitive and straightforward operation; the control circuit is equipped with protection features against water shortage, overheating, and overcurrent. 、 Lid Lifting and Alignment Limit Device 、 Sound and light alarms, automatic protection, and other functions.