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Uneven density and numerous bubbles in the sintering furnace for quartz fiber preform?

2025-12-05

The high-frequency induction sintering furnace is the core equipment for preparing quartz fiber preform rods, responsible for sintering high-purity quartz powder into dense and defect free rods (with sintering density ≥ 2.2g/cm ³ and bubble density ≤ 1/cm ³), directly determining the fiber transmission loss and mechanical strength. If there is uneven sintering density (density deviation exceeding 0.1g/cm ³) and more surface bubbles (exceeding 5/cm ³), it will lead to an increase in fiber breakage rate and substandard transmission performance during fiber drawing. Based on the extremely high purity (SiO ₂ ≥ 99.999%) and microstructure requirements of quartz fiber preform, a three-step investigation method is summarized to quickly restore sintering quality.

Step 1: Optimize the heating system and temperature field control - the core power determines density uniformity

Improper configuration of induction coils, temperature distribution, and heating rate are the main causes of uneven density.

Poor adaptation or aging of induction coil parameters: If the deviation of coil turns exceeds 2 turns, it will lead to uneven distribution of heating power, and the radial temperature difference of the prefabricated rod will exceed 5 ℃; Oxidation or deformation of the coil surface, decrease in induction efficiency, and insufficient local heating; The deviation between the coil and the prefabricated rod exceeds 3mm, with high temperature near the coil end and insufficient temperature at the far end. Accurately match the number of turns of the coil according to the diameter of the prefabricated rod (such as 32 turns for a diameter of 100mm), calibrate the coaxiality between the coil and the prefabricated rod, and control the spacing between 2-2.5mm; replace the severely oxidized coil, spray insulation and thermal conductivity coating on the surface to improve heating stability.

Abnormal heating rate or temperature gradient: If the heating rate exceeds 5 ℃/min, the moisture and gas inside the billet cannot be discharged in a timely manner, which can easily form bubbles; A radial temperature gradient exceeding 3 ℃/cm can lead to uneven sintering progress and significant density deviation between the inside and outside. Adopting a "step heating" strategy: room temperature -300 ℃ (2 ℃/min), 300-800 ℃ (3 ℃/min), 800-1200 ℃ (4 ℃/min), and high temperature section insulation for 2 hours; Install an infrared thermometer to monitor the surface temperature of the prefabricated rod in real time, adjust the coil power to make the radial temperature difference ≤ 2 ℃.

Step 2: Calibrate atmosphere control and exhaust mechanism - precise control of gas to reduce bubbles

Improper protection of atmosphere purity, flow rate, and exhaust path can exacerbate bubble problems.

Insufficient purity or flow fluctuation of protective atmosphere: Ar gas with purity below 99.999% contains O ₂ and H ₂ O, which will react with quartz powder to produce gas; The flow rate fluctuates by more than 5L/min, the pressure inside the furnace is unstable, and the exhaust is blocked. Select 99.9995% high-purity Ar gas and install a gas purification device to further remove impurities; Stabilize the flow rate at 20-25 L/min and maintain the furnace pressure at 0.02-0.03 MPa through a mass flow controller to ensure smooth gas flow.

Poor exhaust path or insufficient insulation: The billet is clamped too tightly, and the exhaust channel is blocked; The insulation time in the low-temperature range (300-600 ℃) is less than 1 hour, and the adsorbed water and crystal water cannot be completely discharged. In the high-temperature range, bubbles are formed by evaporation. Optimize the clamping method and reserve a uniform exhaust gap; Extend the low-temperature insulation to 1.5-2 hours, and use vacuum assisted exhaust (evacuate to 10Pa at 300 ℃ and maintain for 30 minutes) to thoroughly remove the gas inside the billet.

Step 3: Adapt to the characteristics of the billet and clean the furnace - avoid defects at the source

The quality of the billet, contamination inside the furnace, and improper cooling methods can affect the sintering stability.

Low density or high impurities in the green body: the green body density is less than 1.6g/cm ³, with many internal pores and easy residual gas; The billet contains over 5ppm of carbon and metal impurities, which can cause gas or chemical reactions during sintering, resulting in the formation of bubbles. Control the raw material preparation process to ensure a density of ≥ 1.7g/cm ³; Select high-purity quartz powder raw materials, avoid pollution during the processing, and wipe the surface of the blank with anhydrous ethanol before entering the furnace.

Residual or rapid cooling in the furnace: residual dust and volatile substances (with a thickness exceeding 0.1mm) on the inner wall of the furnace cavity evaporate and merge into the prefabricated rod at high temperatures, forming bubbles; The cooling rate exceeds 8 ℃/min, and the temperature difference between the inside and outside of the prefabricated rod is large, which is prone to stress cracks, and at the same time, bubbles cannot float up and be discharged. After each sintering, blow the furnace chamber with high-purity Ar gas and regularly clean the inner wall with a plasma cleaning machine; Adopting the "gradient cooling" mode, natural cooling is carried out at 1200-800 ℃ (3 ℃/min), 800-500 ℃ (5 ℃/min), and below 500 ℃ to reduce defects.

Daily maintenance should pay attention to: checking the purity, flow rate, and coil status of Ar gas every day; Calibrate thermometers and mass flow controllers weekly; Clean the furnace cavity and inspect the vacuum system every month; Quarterly testing of coil inductance and heating uniformity. By implementing the above measures, the sintered density of the preform can be stabilized at around 2.25g/cm ³, with a bubble density of ≤ 0.5 bubbles/cm ³, meeting the high-end requirements of optical fiber processing. If there are still problems, it is recommended to contact the manufacturer to optimize the heating coil design and atmosphere control program, and match it with the exclusive sintering process for prefabricated rods.


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