How to put materials into the vertical tube furnace?

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How to put materials into the vertical tube furnace?

How to strictly follow the equipment structure and process safety to achieve material loading of vertical tube furnace to ensure operation efficiency and experimental/production quality? Next, let's take a look at the furnace loading process, core precautions, and typical cases!

Vertical Tube Furnace Click the picture to view detailed parameters

1. Standardized process for loading vertical tube furnace

a. Equipment pre-inspection and safety confirmation

① Check the integrity of the furnace tube: confirm that there are no cracks in the furnace tube and no residue on the inner wall (such as oxides or carbides from the previous experiment). It is recommended to use an endoscope to detect the deep hole area.

② Verify the sealing: fill argon gas to 0.1MPa and maintain the pressure for 10 minutes, observe whether the pressure gauge fluctuation is ≤0.005MPa to avoid danger caused by gas leakage at high temperature.

③ Calibrate the temperature control system: Use a standard thermocouple (such as K type) to check the temperature uniformity at multiple points in the middle and both ends of the furnace tube. The error must be ≤±2℃ (high-precision experiments require ≤±1℃).

b. Material loading strategy

① Rigid support system:

Use high-purity alumina or silicon carbide boat (purity ≥99.9%), the boat length should be ≤ the effective heating zone length of the furnace tube (usually 70%-80% of the total length of the furnace tube).

② Loading density control: Powder samples need to be flattened to a thickness of ≤5mm, and the spacing between block materials should be ≥10mm (such as when sintering lithium-ion battery positive electrode materials to prevent particle agglomeration).

③ Flexible suspension solution:

Fiber cloth/net bag (such as alumina fiber, temperature resistance 1600℃) is suitable for fragile or special-shaped parts, fixed by the top ring of the furnace tube to avoid contact with the inner wall of the furnace tube.

The suspension spacing needs to be ≥30mm (such as carbon nanotube growth experiment, to prevent air flow disturbance from causing material to fall off).

c. Atmosphere pipeline pretreatment

① Inert gas replacement: introduce argon/nitrogen at a flow rate of ≥500ml/min for more than 30 minutes to ensure that the oxygen content is ≤1ppm (using an oxygen probe for real-time monitoring).

② Premixing of reaction gases: If hydrogen/ammonia is needed, first mix it with inert gas at 10% volume fraction, and then adjust it through a gas mixer (accuracy ±0.5%FS) before introducing it.

2. Key operational risks and solutions

① Furnace tube rupture

Cause analysis: Rapid cooling and heating lead to thermal stress concentration

Solution: Heating/cooling rate ≤5℃/min, high temperature section (>1000℃) insulation time extended by 20%

② Sample contamination

Cause analysis: volatilization of furnace tube residue or impure atmosphere

Solution: After each experiment, burn the furnace tube at high temperature (1200℃) for 1 hour, and add 5 minutes of purge time when the atmosphere is switched

③ Temperature uniformity is too poor

Cause analysis: The axial temperature difference of the furnace tube is too large

Solution: Use three-zone independent temperature control technology, or use graphite felt to wrap the middle section of the furnace tube (reduce radial heat loss)

④ Seal failure

Cause analysis: Insufficient preload of flange bolts or aging of sealing rings

Solution: Use a torque wrench to tighten diagonally 3 times (recommended torque: M16 bolts are 80-100N·m), and replace the sealing ring regularly

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