Preparation method of zirconium silicate nanowire

Abstract

The invention discloses a preparation method of a zirconium silicate nanowire, which comprises the following steps: (1) mixing zirconium boride, silicon dioxide and silicon powder to prepare mixed powder A; (2) doping the mixed powder A into silicon resin B to obtain a raw material C; and (3) curing the raw material C, and calcining to obtain the zirconium silicate nanowire. A one-step high-temperature calcination method is adopted, and complex liquid phase reaction control, a high-pressure reaction kettle, expensive vacuum / protective gas deposition equipment or multi-step post-treatment are not needed; the diameter and the length of the final zirconium silicate nanowire can be effectively regulated and controlled by accurately controlling the raw material proportion, the particle size, the resin mixing amount, the curing parameters and the calcination system, namely, the nanowire with the high length-diameter ratio is obtained, and the obtained nanowire is good in morphology uniformity and good in stability. The structure has excellent potential application value in the fields of reinforced and toughened composite materials (ceramics, metals and polymers), high-temperature heat insulation, catalytic carriers, sensors and the like.

Description

TECHNICAL FIELD

[0001] The application relates to a preparation method of zirconium silicate nanowires. BACKGROUND

[0002] Zirconium silicate is a ceramic material with high melting point (>2500 DEG C), excellent chemical stability, low thermal expansion coefficient and good mechanical strength, and is widely used in refractory materials, ceramic glaze, nuclear waste packaging and the like. However, the traditional zirconium silicate exists in the form of micron particles or blocks, has low specific surface area and poor interface activity, and is limited in application in high-end fields such as catalysis, composite material reinforcement and functional coating. The zirconium silicate nanowires can significantly improve the specific surface area and surface activity of the material, and have quantum confinement effect, axial carrier transport capacity and flexible assembly characteristics of one-dimensional nanomaterials, and have great potential in high-temperature sensors, composite reinforcement and photocatalysis. However, the efficient and controllable synthesis of zirconium silicate nanowires still faces great challenges in the prior art. SUMMARY

[0003] The application provides a preparation method of zirconium silicate nanowires, which is safe and environment-friendly in raw materials, simple and efficient in process, easy to scale up and controllable in product morphology (high aspect ratio nanowires).

[0004] The application aims to realize the following technical scheme:

[0005] A preparation method of zirconium silicate nanowires comprises the following steps:

[0006] Step (1) zirconium boride, silicon dioxide and silicon powder are mixed and then ball milled to fully mix the components and prepare a mixed powder A, wherein the mass ratio of the zirconium boride, silicon dioxide and silicon powder is 10-20:5-30:5-40, and the particle size of the zirconium boride, silicon dioxide and silicon powder is 500 nm-5 microns;

[0007] Step (2) the mixed powder A is doped into a silicon resin B and dispersed by using a high-speed dispersing machine to obtain a raw material C, wherein the mass ratio of the mixed powder A and the silicon resin B is 15-55:45, and the silicon resin B comprises at least one of methylphenyl silicone resin, phenyl silicone resin and zirconium silicon resin but is not limited thereto;

[0008] Step (3) the raw material C is solidified and then calcined to obtain zirconium silicate nanowires, wherein the solidification temperature is 150-250 DEG C and the time is 2-4 hours; the calcination temperature is 1300-1500 DEG C, the heating rate is 5-20 DEG C / min, and the holding time is 1-3 hours; and the diameter of the zirconium silicate nanowires is 50-100 nm and the length is 1-50 microns.

[0009] Compared with the prior art, the application has the following advantages:

[0010] 1. Simple and efficient process, easy to scale up: using one-step high-temperature calcination method, without complex liquid phase reaction control, high-pressure reaction kettle, expensive vacuum / protection gas deposition equipment or multi-step post-processing (such as tedious washing, drying, template removal). Among them, the silicone B not only acts as a binder to help form a cured body, but also provides a carbon source (forms a CO reducing atmosphere) at high temperature to guide the growth of nanowires, simplifying the formulation and process. The process has relatively low equipment requirements and is suitable for large-scale production.

[0011] 2. Good controllability of product morphology (nanowires): by accurately controlling the raw material ratio (ZrB2: SiO2: Si), particle size, resin content, curing parameters and calcination system (temperature, heating rate, holding time), the diameter (50-100 nm) and length (1-50 μm) of the final zirconium silicate nanowires can be effectively controlled, i.e. to obtain nanowires with high aspect ratio, and the morphology uniformity of the obtained nanowires is good.

[0012] 3. Superior product performance: the zirconium silicate nanowires prepared by the present application have high aspect ratio, which makes them have excellent potential application value in the fields of reinforced and toughened composite materials (ceramics, metals, polymers), high-temperature insulation, catalyst carriers, sensors, etc. BRIEF DESCRIPTION OF DRAWINGS

[0013] Figure 1 SEM image of zirconium silicate nanowires prepared for Example 1;

[0014] Figure 2 is an enlarged view of Figure 1

[0015] Figure 3 is an EDS element analysis. DETAILED DESCRIPTION

[0016] The technical solutions of the present application will be further described below in combination with examples, but are not limited thereto. Any modification or equivalent replacement of the technical solutions of the present application without departing from the spirit and scope of the present application shall be covered in the protection scope of the present application.

[0017] Example 1:

[0018] Step (1) Mix zirconium boride, silicon dioxide and silicon powder, then ball mill to fully mix the components, to prepare a mixed powder A, wherein: the mass ratio of zirconium boride, silicon dioxide and silicon powder is 4:1:3, and the particle size of zirconium boride, silicon dioxide and silicon powder is 1 μm;

[0019] ​Step (2) mixed powder A is doped into silicone B, and a high-speed dispersion machine is used for dispersion to obtain raw material C, wherein the mass ratio of the mixed powder A to the silicone B is 5:9, and the silicone B is methyl phenyl silicone resin;

[0020] Step (3) after curing the raw material C, calcination is carried out to obtain zirconium silicate nanowires, wherein the curing temperature is 200℃, the time is 4h; the calcination temperature is 1300℃, the heating rate is 10℃ / min, and the holding time is 1h; the diameter of the zirconium silicate nanowires is 50-100nm, and the length is 1-10μm.

[0021] Example 2:

[0022] Step (1) zirconium boride, silicon dioxide and silicon powder are mixed and ball milled to fully mix the components to prepare mixed powder A, wherein the mass ratio of the zirconium boride, silicon dioxide and silicon powder is 2:2:1, and the particle size of the zirconium boride, silicon dioxide and silicon powder is 1μm;

[0023] Step (2) mixed powder A is doped into silicone B, and a high-speed dispersion machine is used for dispersion to obtain raw material C, wherein the mass ratio of the mixed powder A to the silicone B is 1:2.5, and the silicone B is zirconium silicon resin;

[0024] Step (3) after curing the raw material C, calcination is carried out to obtain zirconium silicate nanowires, wherein the curing temperature is 250℃, the time is 2h; the calcination temperature is 1500℃, the heating rate is 10℃ / min, and the holding time is 2h; the diameter of the zirconium silicate nanowires is 50-100nm, and the length is 10-50μm.

[0025] Example 3:

[0026] Step (1) zirconium boride, silicon dioxide and silicon powder are mixed and ball milled to fully mix the components to prepare mixed powder A, wherein the mass ratio of the zirconium boride, silicon dioxide and silicon powder is 4:2:1, and the particle size of the zirconium boride, silicon dioxide and silicon powder is 2μm;

[0027] Step (2) mixed powder A is doped into silicone B, and a high-speed dispersion machine is used for dispersion to obtain raw material C, wherein the mass ratio of the mixed powder A to the silicone B is 1:2.5, and the silicone B is a mixture of methyl phenyl silicone resin and zirconium silicon resin, and the Zr / Si ratio is 1:3;

[0028] In step (3), the raw material C is solidified and calcined to obtain zirconium silicate nanowires, wherein the solidification temperature is 250 DEG C, the time is 4 h, the calcination temperature is 1300 DEG C, the temperature rising rate is 10 DEG C / min, the holding time is 2 h, the diameter of the zirconium silicate nanowires is 50-100 nm, and the length is 10-50 microns.

[0029] Examples 1-3 can prepare zirconium silicate nanowires with similar morphology, which are prepared by Figure 1 and Figure 2 It can be seen from the above that the nanowires are uniform in thickness, with a diameter of 50-100 nm and a high aspect ratio, as shown in Figure 3 EDS element analysis shows that the composition is zirconium silicate.

Claims

1. A method for preparing zirconium silicate nanowires, characterized in that... The method includes the following steps: Step (1) Mix zirconium boride, silicon dioxide, and silicon powder to form mixed powder A, wherein the mass ratio of zirconium boride, silicon dioxide, and silicon powder is 10~20:5~30:5~40; Step (2) The mixed powder A is incorporated into the silicone resin B to obtain raw material C, wherein the mass ratio of the mixed powder A to the silicone resin B is 15~55:45; Step (3) After the raw material C is cured, it is calcined to obtain zirconium silicate nanowires.

2. The method for preparing zirconium silicate nanowires according to claim 1, characterized in that... The zirconium boride, silicon dioxide, and silicon powder have a particle size of 500 nm to 5 μm.

3. The method for preparing zirconium silicate nanowires according to claim 1, characterized in that... The silicone resin B is at least one of methylphenyl silicone resin, phenyl silicone resin, and zirconium silicone resin.

4. The method for preparing zirconium silicate nanowires according to claim 1, characterized in that... The curing temperature is 150~250℃, and the time is 2~4h.

5. The method for preparing zirconium silicate nanowires according to claim 1, characterized in that... The calcination temperature is 1300~1500℃, the heating rate is 5~20℃ / min, and the holding time is 1~3h.

6. The method for preparing zirconium silicate nanowires according to claim 1, characterized in that... The zirconium silicate nanowires have a diameter of 50~100nm and a length of 1~50μm.

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