CN112408394B - Preparation method of tantalum disilicide nano powder - Google Patents
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Abstract
The invention relates to a preparation method of tantalum disilicide nano powder. It sequentially comprises the following steps: (1) Respectively weighing silicon powder and tantalum carbide powder, and ball-milling and uniformly mixing to obtain mixed powder; (2) Placing the mixed powder into a carbonization furnace, vacuumizing, and then introducing protective gas to normal pressure; (3) Under the condition of protective gas atmosphere, the carbonization furnace is heated to 900-1400 ℃, kept for 1-4 hours, and cooled to room temperature. The preparation method has the advantages of simple process, mild reaction condition and environmental friendliness, and the prepared tantalum disilicide nano powder has uniform particles, high purity and no agglomeration phenomenon.
Description
Technical Field
The invention relates to the technical field of special powder, in particular to a preparation method of tantalum disilicide nano powder.
Background
The metal silicide has similar conductivity, high temperature performance, oxidation resistance and compatibility with the production process of silicon integrated circuits, and the transition metal silicide can be used for low-resistance grid gates and interconnects, schottky grids and resistance contacts. Wherein tantalum disilicide (TaSi) 2 ) Is the silicide with the highest melting point, has high hardness and elastic modulus, excellent corrosion resistance and high-temperature oxidation resistance, has both metallic and ceramic properties and can continuously maintain high stability in extremely severe environments. Thus, taSi 2 At high ultrasoundDiffusion barrier layers and high emissivity layers in thermal protective coatings for aerospace structures such as fast-moving aircraft and reentry aircraft are widely used. TaSi 2 The composite ceramic material can be singly used for preparing novel structural components, and can be simultaneously introduced into other ceramic materials or oxidation resistant coatings so as to greatly improve the mechanical properties of the composite ceramic and the oxidation resistance of the ceramic coatings.
Currently, taSi 2 The preparation process mainly comprises a combustion synthesis method, an arc melting method, a mechanochemical reaction method, a solid phase reaction method and the like.
Combustion synthesis is a method for rapidly synthesizing intermetallic compounds using chemical reaction heat. The method has the advantages of high reaction rate, uncontrollable reaction process, and complex phase composition due to the introduction of reaction auxiliary agents, and generally needs purification treatment to obtain high-purity tantalum disilicide powder.
The arc melting method is capable of melting raw powder to achieve homogenization of the material, but it takes a long time to achieve homogenization, and silicon may be lost due to volatilization during arc melting, resulting in generation of impurity phases.
The mechanochemical reaction principle is to prepare nano-scale tantalum disilicide powder by taking nano-scale silicon powder and tantalum powder as raw materials and performing long-time high-energy ball milling. The product prepared by the method has poor purity and low cleanliness, and is not suitable for being used as a raw material for preparing high-performance ceramic materials.
The solid phase reaction rule is Ta 2 O 5 And Si as raw materials, and reacting at 1450-1600 ℃ to obtain TaSi 2 The powder with high emissivity has good crystallinity and smaller particle size. However, the product has more other impurities, and it is difficult to obtain high-purity TaSi 2 And (3) powder.
In summary, the conventional method is adopted to synthesize TaSi with higher purity 2 These methods are difficult to control precisely, and the reaction is incomplete, and an impurity phase (Ta 5 Si 3 ) Resulting in low purity of the product, uneven particles and no use.
Disclosure of Invention
The invention aims to provide a preparation method of tantalum disilicide nano powder, which has the advantages of simple process, mild reaction conditions and environmental friendliness, and the prepared tantalum disilicide nano powder has uniform particles, high purity and no agglomeration phenomenon.
The invention adopts the following technical scheme to realize the aim of the invention:
the preparation method of the tantalum disilicide nano powder is characterized by comprising the following steps in sequence:
(1) Respectively weighing silicon powder and tantalum carbide powder with the granularity of 500 meshes according to the mol ratio of 2:1, then ball-milling and mixing uniformly, wherein the ball-material ratio is 3-8:1, and the ball-milling time is 12-24 hours, so as to obtain mixed powder;
(2) Placing the mixed powder into a ceramic crucible, then placing the ceramic crucible into a high-temperature carbonization furnace, vacuumizing to 5-20 Pa, and then introducing argon to normal pressure;
(3) Under the condition of argon atmosphere, the high-temperature carbonization furnace is heated to 900-1400 ℃ at the speed of 10-20 ℃/min, the temperature is kept for 1-4 h, and then the high-temperature carbonization furnace is naturally cooled to the room temperature.
The silicon powder refers to simple substance silicon powder, and is clear in the field.
It is further clear that the particle size of the tantalum disilicide nano-powder is 100 to 200nm.
As a further definition, the surface of the tantalum disilicide nano-powder particles is coated with an amorphous carbon layer.
The invention has the following beneficial effects:
the invention provides a preparation method of tantalum disilicide nano powder, which has the characteristics of simple process, mild reaction condition and environmental friendliness, and the prepared tantalum disilicide nano powder has high purity, uniform particles, controllable scale and no agglomeration phenomenon, and is an ideal preparation raw material of tantalum disilicide ceramic materials. Specifically: (1) The preparation method adopts solid-phase silicon powder and tantalum carbide as raw materials, and is synthesized by direct reaction in a carbonization furnace, and the preparation method has the advantages of simple process, no special equipment requirement and suitability for industrialized mass production; (2) The whole preparation process is free from adding auxiliary reagents or introducing other substances such as hydrogen for purification, the synthesis process is simple and safe, the reaction condition is mild, the method is environment-friendly, the reaction process is controllable, and no raw material silicon source is wasted; (3) The tantalum disilicide nano particles synthesized by direct reaction have high purity, controllable product size, particle size of about 100-200 nm, and particle surface coated by amorphous carbon layer, and the reaction product has obvious expansion compared with the volume of raw materials, so that the particles have no obvious agglomeration, loose agglomerates and no need of breaking.
Drawings
FIG. 1 is an XRD spectrum of tantalum disilicide nano-powder prepared in example 1 of the present invention.
Fig. 2 is a TEM photograph of tantalum disilicide nano-powder prepared in example 1 of the present invention.
Fig. 3 is a HRTEM photograph of tantalum disilicide nano-powder prepared in example 1 of the present invention.
FIG. 4 is an EDS spectrum of a tantalum disilicide nano-powder surface coating layer prepared in example 1 of the present invention.
Detailed Description
The technical solution of the present invention will be clearly and completely described in the following description in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, nor are they limiting the scope of protection.
Example 1
The preparation method of the tantalum disilicide nano powder sequentially comprises the following steps:
(1) Respectively weighing silicon powder and tantalum carbide powder with the granularity of 500 meshes according to the mol ratio of 2:1, and then performing ball milling and mixing uniformly, wherein the ball material ratio is 4:1, and the ball milling time is 12 hours to obtain mixed powder;
(2) Placing the mixed powder into a ceramic crucible, then placing the ceramic crucible into a high-temperature carbonization furnace, vacuumizing to 10Pa, and then introducing argon to normal pressure;
(3) Under the condition of argon atmosphere, the high-temperature carbonization furnace is heated to 1200 ℃ at the speed of 10 ℃/min, the temperature is kept for 2 hours, and then the tantalum disilicide nano powder is prepared after natural cooling to the room temperature, and the granularity of the tantalum disilicide nano powder is 100-130 nm.
Respectively taking the tantalum disilicide nano powder samples prepared in the embodiment for analysis and detection, wherein the detection results are shown in the accompanying figures 1-4: only the diffraction peak of the characteristic tantalum disilicide is detected in the figure 1, which shows that the single-phase tantalum disilicide powder is synthesized, and the product has higher purity; as can be seen from fig. 2, the tantalum disilicide particles formed by the reaction have a size of about 100nm, and the particle surfaces are surrounded by an amorphous layer; as can be seen from FIG. 3, the distance between two adjacent parallel lattice fringes is 0.35nm, and the distance between the adjacent parallel lattice fringes and hexagonal phase TaSi 2 (JCPCDS: 03-065-3548) with similar (101) interplanar spacing, indicating that the formed particles are tantalum disilicide; the analysis of fig. 4 shows that the surface coating layer is composed of carbon element, so that the surface coating layer of the tantalum disilicide particles is amorphous carbon, which is caused by diffusion of carbon in tantalum carbide to the particle surface during the formation of tantalum disilicide phase.
Example 2
The preparation method of the tantalum disilicide nano powder sequentially comprises the following steps:
(1) Respectively weighing silicon powder and tantalum carbide powder with the granularity of 500 meshes according to the mol ratio of 2:1, then ball-milling and mixing uniformly, wherein the ball-material ratio is 3:1, and the ball-milling time is 12 hours, so as to obtain mixed powder;
(2) Placing the mixed powder into a ceramic crucible, then placing the ceramic crucible into a high-temperature carbonization furnace, vacuumizing to 15Pa, and then introducing argon to normal pressure;
(3) Under the condition of argon atmosphere, the high-temperature carbonization furnace is heated to 1000 ℃ at the speed of 15 ℃/min, the temperature is kept for 1h, and then the tantalum disilicide nano powder is prepared after natural cooling to room temperature, and the granularity of the tantalum disilicide nano powder is 120-160 nm.
XRD detection is carried out on the tantalum disilicide nano powder sample prepared in the embodiment, and the detection result shows that the product is single-phase tantalum disilicide powder.
Example 3
The preparation method of the tantalum disilicide nano powder sequentially comprises the following steps:
(1) Respectively weighing silicon powder and tantalum carbide powder with the granularity of 500 meshes according to the mol ratio of 2:1, and then performing ball milling and mixing uniformly, wherein the ball material ratio is 5:1, and the ball milling time is 18 hours to obtain mixed powder;
(2) Placing the mixed powder into a ceramic crucible, then placing the ceramic crucible into a high-temperature carbonization furnace, vacuumizing to 20Pa, and then introducing argon to normal pressure;
(3) Under the condition of argon atmosphere, heating a high-temperature carbonization furnace to 1300 ℃ at a speed of 20 ℃/min, preserving heat for 3 hours, and naturally cooling to room temperature to obtain tantalum disilicide nano powder, wherein the granularity of the tantalum disilicide nano powder is 130-180 nm.
XRD detection is carried out on the tantalum disilicide nano powder sample prepared in the embodiment, and the detection result shows that the product is single-phase tantalum disilicide powder.
Example 4
The preparation method of the tantalum disilicide nano powder sequentially comprises the following steps:
(1) Respectively weighing silicon powder and tantalum carbide powder with the granularity of 500 meshes according to the mol ratio of 2:1, and then performing ball milling and mixing uniformly, wherein the ball material ratio is 8:1, and the ball milling time is 24 hours to obtain mixed powder;
(2) Placing the mixed powder into a ceramic crucible, then placing the ceramic crucible into a high-temperature carbonization furnace, vacuumizing to 20Pa, and then introducing argon to normal pressure;
(3) Under the condition of argon atmosphere, heating a high-temperature carbonization furnace to 1400 ℃ at a speed of 20 ℃/min, preserving heat for 4 hours, and naturally cooling to room temperature to obtain tantalum disilicide nano powder, wherein the granularity of the tantalum disilicide nano powder is 150-200 nm.
XRD detection is carried out on the tantalum disilicide nano powder sample prepared in the embodiment, and the detection result shows that the product is single-phase tantalum disilicide powder.
Claims (3)
1. The preparation method of the tantalum disilicide nano powder is characterized by comprising the following steps in sequence:
(1) Respectively weighing silicon powder and tantalum carbide powder with the granularity of 500 meshes according to the mol ratio of 2:1, then ball-milling and mixing uniformly, wherein the ball-material ratio is 3-8:1, and the ball-milling time is 12-24 hours, so as to obtain mixed powder;
(2) Placing the mixed powder into a ceramic crucible, then placing the ceramic crucible into a high-temperature carbonization furnace, vacuumizing to 10-20 Pa, and then introducing argon to normal pressure;
(3) Under the condition of argon atmosphere, the high-temperature carbonization furnace is heated to 1000-1400 ℃ at the speed of 10-20 ℃/min, the temperature is kept for 1-4 h, and then the high-temperature carbonization furnace is naturally cooled to the room temperature.
2. The tantalum disilicide nano-powder prepared by the method of preparing the tantalum disilicide nano-powder according to claim 1, wherein: the particle size of the tantalum disilicide nano powder is 100-200 nm;
the surface of the tantalum disilicide nano powder particles is coated by an amorphous carbon layer.
3. Use of tantalum disilicide nanopowder according to claim 2, wherein: the tantalum disilicide nano powder is used for preparing tantalum disilicide ceramic materials.
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