High-Vacuum Perovskite Glovebox Deposition System

Installation 

Requirements

1. Electricity:  

   a. Three-phase five-wire system: 380 VAC (+/-5%), 50Hz, with three live wires, one ground wire, and one neutral wire. Maximum power: 8KW; maximum current: 32A.  

   b. An additional independent grounding wire is required.  

2.Water:  

   Flow rate: 15-20 liters/minute, temperature: 15 to 25°C. Pressure difference between inlet and outlet: 1 to 2 kg; inlet pressure: 2 to 3 kg. The outer diameter of the inlet and outlet is 12mm (it is recommended to use high-quality rubber hoses). It is suggested to install a ball valve before the water inlet to easily adjust water pressure and flow rate.  

3.Gas:  

   a. Compressed Air: Dry, clean, water-free, and oil-free compressed air, using 8mm plastic tubing, with a pressure of 5.5-6 kg (0.55-0.6 MPa).  

   b. Nitrogen: Dry nitrogen for breaking the vacuum in the equipment chamber, using 8mm plastic tubing, with a pressure of 1-2 kg (0.1-0.2 MPa).

Main 

Features

1. Vacuum Chamber:

   (1). The vacuum chamber is made of dedicated 304 stainless steel, with internal electro-polishing. The dimensions of the chamber are approximately 400mm wide, 400mm deep, and 450mm high, featuring a vertical front and rear door structure.

   (2). The front door track uses an imported dual-track design, preventing the right-side track from extending into the glovebox, saving space while providing a more coordinated appearance. It features manual locking. The rear door employs a manual hinge structure, making sealing operation simple. The system includes a stainless steel liner, which is a multi-piece structure for easy disassembly and installation. Both the interior and exterior surfaces of the vacuum chamber are polished, and interfaces for lighting and thickness measurement devices are reserved.

   (3). The left side of the vacuum chamber connects to the main valve and molecular pump, along with a vacuum measurement interface. The top is equipped with a rotating water-cooled sample stage, a sample stage baffle, and one thickness measurement probe interface. The base includes two sets of metal evaporation electrodes, four organic sources, and two thickness probe installation ports.

   (4). The front and rear doors are equipped with glass observation windows: the front door has one 4-inch observation window with a baffle and anti-contamination glass; the rear door has two small observation windows for observing the source and sample, also equipped with anti-contamination glass.

2. Evaporation Sources: The system is equipped with both metal and non-metal evaporation sources.

3. Comprehensive Alarm System: The system includes detection and protection for low water, low pressure, phase sequence, temperature, and vacuum. It provides alarms for abnormal conditions such as low water, overcurrent, overpressure, and disconnection of pumps and electrodes, along with corresponding protective measures. A complete logic program interlock protection system is included.

4. Control Method:  

   The system uses a Panasonic PLC with a touchscreen for manual and automatic control. Users can input the deposition rate and final thickness, with PID regulation for automatic control of the evaporation power output. Control includes mechanical pumps, molecular pumps, pneumatic and solenoid valves, vacuum gauges, etc. It supports automatic vacuum pumping, automatic deposition, and automatic venting.

   A complete interlock protection system (hardware and software) ensures that the equipment is under full interlock protection in both manual and automatic modes, guaranteeing personnel and equipment safety. Additionally, the system is equipped with a water flow detection alarm device.

5. Structural Features: The integrated electrical control section is located beneath the equipment and glovebox. The system is equipped with casters and leveling feet for easy mobility.

6. Details:  

   A molecular sieve is installed before the mechanical pump, and protective components such as filters and louvers are added to the exhaust port to prevent dust. The organic sources are installed independently inside the chamber.

   All sample stages, source baffles, and the rotation of the sample stage utilize magnetic fluid sealing to ensure long-term stability of the system.

   Components such as relays, terminal blocks, water and gas pipe fittings, and solenoid valves are all made from high-quality products.

Main

Parameters

1. Vacuum System:

   The system uses a Zhongke Keyi oil-lubricated molecular pump (FF-200/1300) with a pumping speed of 1300 L/S, along with a Feiyue VRD-16 mechanical pump. It features an 8-inch pneumatic gate valve and vacuum measurement with one low and one high vacuum gauge (range from atmospheric pressure to 3E-9 torr), allowing for automatic switching between low and high vacuum measurements.

   The vacuum readings are input to the PLC for process control.

   Vacuum valves: 2 sets of DN40mm gate valves; 1 set of pneumatic main valve DN200 from Zhongke Keyi.

   Vacuum sealing: Removable static seals use fluororubber O-rings; infrequent removable static seals use oxygen-free copper seals.

2. Ultimate Vacuum: Better than 2.0 × 10^-5 Pa; leak rate: better than 5 × 10^-8 Pa·L/S (national standard); after 12 hours of shutdown, vacuum level ≤ 5 Pa (in a glovebox dry nitrogen environment).

3. Pumping Speed: Pumping time from atmospheric pressure to 5 × 10^-

4 Pa is less than 20 minutes (in a glovebox dry nitrogen environment).

Sample Stage

2. The distance between the substrate and the evaporation source is electrically adjustable, with a maximum adjustable range of 60 mm.

3. The sample stage can rotate and features water cooling functionality: the rotational speed of the sample stage is continuously adjustable from 0 to 30 revolutions per minute.

Evaporation Sources and Power Supply

1. The equipment is equipped with 2 sets of boat-type evaporation sources, with metal sources utilizing water-cooled copper electrodes and evaporation boat structures (temperature limit of 1500 degrees). It includes one 2.4 kW evaporation power supply, which offers both constant current and constant voltage drive modes, allowing for switching between the two. The evaporation power supply can be controlled via software or manually, and it can also automatically adjust the evaporation rate through a PID controller linked to a thickness gauge. It features a digital display.

2. The system is equipped with 4 sets of organic evaporation source furnaces and 4 units of 20-10 organic evaporation power supplies. The organic evaporation sources have temperature display functionality, and the organic source furnaces use a Japanese conductive temperature controller. The setup includes 4 crucibles, with a heating temperature range of 0-700 degrees Celsius and an adjustable angle range of 0-15 degrees.

Film Thickness Control System

1. Power Supply: DC 5V (±10%), with a maximum current of 400 mA.

2. Frequency Resolution: ±0.03 Hz.

3. Thickness Resolution: 0.0136 Å (for aluminum).

4. Thickness Accuracy: ±0.5%, depending on process conditions, particularly sensor position, material stress, temperature, and density.

5. Measurement Speed: 100 ms to 1 s per measurement, adjustable.

6. Measurement Range: 500,000 Å (for aluminum).

### 1. Box Structure

1. A stainless steel box with dimensions of 2440mm (L) x 780mm (W) x 900mm (H), divided into two sections with a flange connection in the middle. The back side has a reserved flange interface for connection to the coating machine (provided by the customer, flange size specified). The material is SUS304 stainless steel with a thickness of 3mm.

2. Detachable safety glass window with a top-hinged design, featuring a slanted operation surface and 10mm thick tempered glass.

3. Four butyl rubber gloves.

4. Ten reserved KF40 standard interfaces.

5. Equipped with a double-layer stainless steel shelf.

6. Safety valve to protect the equipment and materials inside the glovebox.

7. Steel structure support, height 914mm, installed with swivel casters.

### 2. Transition Chamber

1. A large transition chamber:

   - Material: SUS304 stainless steel.

   - Dimensions: Φ360 x 600 mm.

   - Location: Right side of the box.

   - Connection: Sealed flange connection.

   - Transfer method: Via a movable tray that is easy to disassemble for transferring large materials.

   - Operating methods:

     - Manual operation: Touch screen to operate the valve.

     - Automatic operation: Features automatic evacuation and inflating function; users can start the process via the touch screen, with the PLC automatically completing multiple evacuation and inflation cycles, standardizing operations, saving time, and improving efficiency. Users can set the number of cycles, evacuation time, and inflation pressure.

2. Two small transition chambers:

   - Material: SUS304 stainless steel.

   - Dimensions: Φ155 x 320 mm.

   - Location: Right and left sides of the box.

   - Connection: Sealed flange connection.

   - Transfer method: Via movable trays.

   - Operating method: Manual operation via a three-way ball valve.

### 3. Gas Purification System

1. A gas purification column:

   - Utilizes high-performance copper catalysts and molecular sieves suitable for glovebox gas purification, for moisture and oxygen removal.

   - Adsorption capacity for oxygen and water is 60 liters and 2 kilograms, respectively.

2. After saturation, the purification column is regenerated using hydrogen-containing nitrogen or argon:

   - A mixture of hydrogen/nitrogen is used for regeneration: H2: 5%; N2: 95%.

   - Due to the glovebox's ultra-low leakage rate, the regeneration frequency for the purification column is approximately once a year.

3. A circulating fan:

   - Flow rate: 90 m³/h.

4. An organic solvent adsorption column:

   - Contains activated carbon particle adsorbents.

5. Electrically controlled main valve with KF40 standard interface.

6. All gas paths are controlled by solenoid valves, with complete automatic control for the purification column regeneration.

7. Gas filters are installed at the inlet and outlet of the circulation system.

### 4. Control System

1. The control system consists of an imported PLC and a 7-inch color touchscreen with a bilingual (Chinese and English) interface.

2. Control functions include:

   1) Automatic pressure control within the box:

      - Users can set the working pressure range between +10 and -10 mbar; the PLC will automatically regulate the pressure within the set range. The default working pressure range is 0 to +5 mbar.

      - If the box pressure exceeds 12 mbar, the PLC automatically opens the safety valve to relieve pressure, protecting gloves, equipment, and materials inside the box.

      - A footswitch allows for fine adjustments of the box pressure.

   2) One-button operation for multiple evacuation/inflation cycles in the transition chamber, saving time:

      - Users can set the number of evacuation cycles, evacuation time, and inflation pressure, then start the automatic process for completion within the set time.

   3) Manual leakage rate monitoring:

      - Users can initiate a manual test by pressing the start button, and the PLC will automatically test the airtightness of the box and report the leakage rate.

   4) Automatic gas cleaning function:

      - Users can set the cleaning time and touch the start button on the touchscreen; the system will begin cleaning the box and stop automatically after the set time.

   5) Automatic recording and display of historical data, with the option to export data such as box pressure, moisture content, and oxygen content via a USB drive.

   6) Displays operation errors and prompts.

   7) Automatic alarm for box atmosphere.

   8) All operations have preset conditions and interlocks to prevent unsafe operations that could damage equipment or compromise the atmosphere inside the box.

### 5. Technical Specifications

1. Leakage Rate: < 0.02 vol%/h.

2. H2O: < 1 ppm, O2: < 1 ppm.

### 6. Other Accessories

1. One oxygen analyzer:

   - Measurement range: 0-1000 ppm.

   - Accuracy: 1% of the range or 0.2 ppm.

   - Installation location: The oxygen sensor from Kejing is installed on the box, continuously monitoring the atmosphere inside the glovebox, regardless of gas circulation, displaying oxygen content.

   - Sensor: Zirconia cell, known for zero-point accuracy and low drift.

   - Display: The analyzer's output connects to the PLC, with values displayed on the touchscreen and alarm values set by the user.

   - Control: Kejing employs real-time monitoring to ensure rapid purification of oxygen, maintaining the user's set oxygen concentration.

   - Calibration method: Accurate detection of oxygen levels inside the glovebox is crucial. Kejing provides calibration methods for users to ensure the analyzer accurately detects impurity concentrations, avoiding erroneous readings that could impact experimental results and waste valuable time and materials.

2. One water analyzer:

   - Measurement range: 20°C to -100°C (dew point).

   - Accuracy: 2°C.

   - Display: The analyzer's output connects to the PLC, with values displayed on the touchscreen and alarm values set by the user.

   - Control: Similar to the oxygen analyzer, it can automatically control the gas circulation system based on user settings.

3. Power interface inside the box, equipped with a multi-port socket.

4. One vacuum valve.

### 7. Acceptance Method

Using a 99.999% inert gas source, operate the empty box, ensuring that the water and oxygen content inside the box is below 1 ppm.

VRD-16

- Molecular pump

- Inflation valve

- Interfaces

- Vacuum gauges

- Evaporation electrodes

- Metal evaporation power supply

- Organic source

- Organic power supply

- Sample stage

- Magnetic fluid seal

- Sealing and other accessories

- Electrical control system

- Electrical control cabinet

- Main frame