Mullite fiber preparation method

A kind of mullite fiber and mullite technology, which is applied in the field of green low-cost mullite fiber preparation, can solve the problems of large internal and external temperature gradient, low material consistency, and fiber grain growth, and achieve short holding time , Improve energy utilization, reduce fiber brittle fracture and pulverization ratio

Inactive Publication Date: 2012-07-25
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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Problems solved by technology

[0004] At present, in the production and research of mullite fiber, traditional resistance furnace heating is used for heat treatment. The heat is mainly transferred from outside to inside through heat conduction, heat radiation and convection. Due to the thermal conductivity of mullite fiber Low, so the efficiency of the traditional heating method is low, the heating rate is slow, and the required holding temperature is as high as 1300°C, and the holding time is about 3 hours. The entire heating and holding process generally takes 8-10 hours, which shows that the production efficiency is low and the production cycle long, high energy consumption
At the same time, due to the high heat treatment temperature and long holding time in the traditional method, the fiber grains grow abnormally, and the brittle fracture and pulverization of the fibers are serious.
In addition, the traditional heating method has a large internal and external temperature gradient, low material consistency, prone to black heart problems, and low yield

Method used

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Examples

Experimental program
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Embodiment 1

[0032] In this embodiment, the chemical expression of mullite fiber is 3Al 2 o 3 2SiO2 2 , the specific preparation method is as follows:

[0033] (1) Weigh 241.5g aluminum chloride hexahydrate (AlCl 3 ·6H 2 (2), 135g aluminum powder, add 400ml deionized water, stir 20min with the rotating speed of 800rpm and make mixed solution A, then add 480ml silica sol (SiO 2 Content is 0.25g / ml), and 1% polyvinyl alcohol, heated to 80 ° C, and fully stirred, during the stirring process, 1mol / L of HCl was added dropwise to adjust the pH to 5±1. A sol was obtained after stirring for 12 h.

[0034] (2) The sol obtains colloidal fibers through spinning into fibers;

[0035] (3) The colloidal fiber was heated to 500°C at a heating rate of 2°C / min, and heat-treated for 2 hours to obtain an amorphous fiber;

[0036] (4) Put the amorphous fiber obtained in (3) into a professional microwave oven for heat treatment, the sintering atmosphere is air, and the temperature is raised to 1000°C at...

Embodiment 2

[0039] In Examples 2 to 8, the chemical expression of mullite fiber is the same as that of Example 1, and the specific preparation method is basically the same as that of Example 1, except that the heating rate, sintering temperature, and holding time are shown in Table 1 below. .

[0040] Chemical expression and process conditions of mullite fiber in Table 1 embodiment 2~8

[0041]

[0042]

[0043] The polycrystalline mullite fiber sample prepared above was measured and analyzed, and the phase of the sample was analyzed by an X-ray diffractometer. figure 1 As shown, it is shown that the fiber is in the mullite phase at the microwave treatment temperature shown in Table 1; the fracture morphology, grain size, and structural characteristics of the sample are observed with a scanning electron microscope, and similar figure 2 In the image shown, the grain size is 30-60nm, the fiber diameter is 6-10μm, and the fiber section is dense.

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Abstract

The invention discloses a mullite fiber preparation method which is efficient, rapid, environment-friendly and low in cost. The method includes: taking raw materials according to stoichiometric ratio of elements in the mullite fiber chemical formula, preparing colloid, performing fiber forming and drying for colloid discharging to obtain mullite non-crystal fiber, adding the fiber into a sagger made of wave permeable materials, placing the sagger in a special microwave oven, controlling heating rate by adjusting the microwave power under the air or oxygen atmosphere, heating to a heat treatment temperature, and cooling to the room temperature to obtain the mullite fiber. The mullite fiber prepared by the method is high in impurity and low in porosity, the grain size is about 30nm, and the fiber diameter ranges from 6 micrometers to 10 micrometers. Further, the mullite fiber is excellent in uniformity, brittle fracture and chalking of the fiber are greatly reduced, yield is increased, heat treatment temperature is lowered, heat insulation time is shortened, and production efficiency is greatly improved.

Description

technical field [0001] The invention relates to the technical field of high-temperature refractory fiber preparation, in particular to a method for preparing green and low-cost mullite fiber. Background technique [0002] Mullite fiber is a kind of high-tech basic material in the field of high-temperature technology, because it has a series of excellent properties, including: high melting point (1850 ° C), excellent high-temperature creep resistance, excellent high-temperature strength, electrical insulation and Chemical stability, low thermal conductivity and thermal expansion coefficient (5.3×10 -6 K), as well as excellent corrosion resistance and high shear modulus, play a very prominent role in the development of the national economy, and are closely related to the development of steel, nonferrous metals, building materials, energy and new technology industries. Important Guarantee. Therefore, mullite fiber has been paid more and more attention as a light-weight and hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/185C04B35/622C04B35/66
Inventor 黄庆周小兵胡春峰
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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