Preparation method of polycrystalline Al2O3-Y3Al5O12 complex-phase fibers or pure YAG fibers

An al2o3-y3al5o12, al2o3-yag technology, applied in the field of inorganic refractory heat insulation, can solve the problems of time-consuming and high cost, and achieve the effects of high process efficiency, large output and good creep resistance.

Inactive Publication Date: 2015-10-28
南京理工宇龙新材料科技股份有限公司
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Problems solved by technology

In their paper "Preparation of polycrystalline YAG / alumina composite fibers and YAG fiber by sol-gel method", Towata et al prepared polycrystalline YAG-Al2O3 fibers and YAG fibers using aluminum isopropoxide and yttrium isopropoxide as raw materials, but using Metal alkoxides are not only time-consuming, but also costly

Method used

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  • Preparation method of polycrystalline Al2O3-Y3Al5O12 complex-phase fibers or pure YAG fibers
  • Preparation method of polycrystalline Al2O3-Y3Al5O12 complex-phase fibers or pure YAG fibers
  • Preparation method of polycrystalline Al2O3-Y3Al5O12 complex-phase fibers or pure YAG fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 30g of anhydrous aluminum chloride in 500ml of water, and then mix it with 27.3g of aluminum powder in a certain ratio (n(Al):n(AlCl 3 )=4.5:1) Put it into a reaction kettle with heating and reflux, heat at 90-100°C for 2-3 hours, cool and filter to obtain pale white polyaluminum chloride mother liquor A (Al 2 o 3 The mass fraction is about 11.2%).

[0031] Press m(Al 2 o 3 ):m(Y 2 o 3 )=85:15 metering composition, add 12.6gY (NO 3 ) 3 ·6H 2 O and 22.2gY(Ac) 3 4H 2 O (the molar ratio of yttrium nitrate to yttrium acetate is 1:2.0), using an electric stirrer to stir, after the yttrium nitrate and yttrium acetate are completely dissolved, add 3wt% (relative to Al 2 o 3 +Y 2 o 3 solid content) of acetic acid as a spinning aid, vacuum concentration at 70° C. for 1 h to obtain a precursor sol with a viscosity of 25-26 Pa·s. When all yttrium sources are yttrium nitrate, due to NO 3 - Excessive, the gel fiber has strong hygroscopicity, at this time the...

Embodiment 2

[0036] Dissolve 30g of anhydrous aluminum chloride in 500ml of water, and then mix it with 30.3g of aluminum powder in a certain ratio (n(Al):n(AlCl 3 )=5.0:1) Put it into a reaction kettle with heating and reflux, heat at 90-100°C for 2-3 hours, cool and filter to obtain pale white polyaluminum chloride mother liquor A (Al 2 o 3 The mass fraction is about 12.1%).

[0037] Press m(Al 2 o 3 ):m(Y 2 o 3 )=85:15 metering composition, add 16.5gY (NO 3 ) 3 ·6H 2 O and 21.2gY(Ac) 3 4H 2 O (the molar ratio of yttrium nitrate to yttrium acetate is 1:1.5), using electric stirrer to stir, after treating that yttrium nitrate and yttrium acetate dissolve completely, add the acetic acid of 5wt% (relative to solid content) as spinning aid, 70 °C and vacuum concentration for 1 h to obtain a precursor sol with a viscosity of 28-30 Pa·s.

[0038] The obtained precursor colloid was centrifugally spun on a self-made centrifugal spinning machine, and the spinning stock solution was thr...

Embodiment 3

[0041] According to the prepared polyaluminum chloride A liquid in Example 1, take one-third of its volume. According to the metering composition of n(Al):n(Y)=5:3, add 31.5gY(NO 3 ) 3 ·6H 2 O and 55.7gY(Ac) 3 4H 2 O (the molar ratio of yttrium nitrate to yttrium acetate is 1:2.0), using an electric stirrer to stir, after the yttrium nitrate and yttrium acetate are completely dissolved, add 3wt% (relative to the solid content) of acetic acid as a spinning aid, 70 °C and vacuum concentration for 0.5 h to obtain a precursor sol with a viscosity of 28-30 Pa·s.

[0042] The obtained precursor colloid is centrifugally spun on a self-made centrifugal spinning machine. The sol forms a gel fiber under the centrifugal force and the secondary traction of the hot air flow, and is collected by a drum to form a fiber cover. The length of the obtained fiber is 10-20cm , with a diameter of 13-15 μm, such as Figure 4 shown. Wherein, the rotational speed of the centrifuge is 5000-7000 ...

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Abstract

The invention discloses a preparation method of polycrystalline Al2O3-Y3Al5O12 complex-phase fibers or pure YAG fibers. The preparation method comprises the following steps that (1) precursor colloids of the polycrystalline Al2O3-Y3Al5O12 complex-phase fibers and the pure YAG fibers are prepared; (2) centrifugal spinning is performed, namely a home-made centrifugal spinning machine is adopted to perform centrifugal spinning so as to obtain uniform-diameter gel fibers under the conditions of appropriate wind seed, appropriate rotation speed and relative humidity; (3) the polycrystalline Al2O3-Y3Al5O12 complex-phase fibers and the YAG fibers are prepared, namely the obtained gel fibers are dried at the temperature of 55-75 DEG C for 12 hours, then heat processing is performed at the temperature interval of 800-1400 DEG C for 2 hours to obtain the required polycrystalline Al2O3-YAG complex-phase fibers and continuous YAG fibers. The fibers prepared by means of the preparation method have good flexibility, higher in high-temperature-resistance degree and better in creep resistance performance, and industrial production can be considered.

Description

technical field [0001] The invention belongs to the technical field of heat insulation of inorganic refractories, in particular to a polycrystalline Al 2 o 3 -Y 3 al 5 o 12 The preparation method of (YAG) composite phase fiber and pure YAG continuous fiber. Background technique [0002] al 2 o 3 Fiber is an important high-performance inorganic ceramic material, which has high strength and elastic modulus, good chemical stability, and can resist the erosion of molten metal and non-oxide in an oxidizing or reducing atmosphere at 1000 °C. At the same time, it also has a high melting point (>2040 ° C), low thermal conductivity (<0.5W m -1 ·K -1 ) and good electrical insulation properties. Compared with carbon fiber, it does not need to be coated with anti-oxidation coating when used, and can be used as a high-temperature heat insulation material, a reinforcement of metal-based or ceramic-based composite materials, etc. However, Al 2 o 3 One of the main disadvan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/08D01F1/10
Inventor 刘和义乔健黄振进陈福金崔宏亮
Owner 南京理工宇龙新材料科技股份有限公司
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