CN112408394A - 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 comprises the following steps in sequence: (1) respectively weighing silicon powder and tantalum carbide powder, and performing ball milling and mixing uniformly to obtain mixed powder; (2) putting the mixed powder into a carbonization furnace, vacuumizing, and introducing protective gas to normal pressure; (3) and under the condition of protective gas atmosphere, heating the carbonization furnace to 900-1400 ℃, preserving heat for 1-4 h, and cooling to room temperature. The preparation method has the advantages of simple process, mild reaction conditions and environmental friendliness, and the prepared product 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 metal-like 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 gate and interconnection, Schottky gate and resistance contact. Wherein tantalum disilicide (TaSi)2) The silicon compound has the highest melting point, high hardness and elastic modulus, excellent corrosion resistance and high-temperature oxidation resistance, and has both metallicity and ceramic properties, and can continuously maintain high stability in extremely severe environment. Thus, TaSi2The composite material is widely applied to a diffusion barrier layer and a high radiation layer in the thermal protection coating of aerospace structural members such as hypersonic aircrafts, reentry aircrafts and the like. TaSi2The composite ceramic can be used independently to prepare a novel structural component, and can be introduced into other ceramic materials or an anti-oxidation coating so as to greatly improve the mechanical property of the composite ceramic and the anti-oxidation property of the ceramic coating.
At present, TaSi2The preparation process mainly comprises a combustion synthesis method, an electric arc melting method, a mechanochemical reaction method, a solid-phase reaction method and the like.
The combustion synthesis method is a method for rapidly synthesizing an intermetallic compound by using the heat of chemical reaction. The method has the advantages of high reaction rate, uncontrollable reaction process and often need of introducing reaction auxiliary agents, so that the phase components are relatively complex, and purification treatment is usually needed to obtain high-purity tantalum disilicide powder.
The arc melting method can melt raw material powder to achieve homogenization of the material, but it takes a long time to achieve homogenization, and silicon loss may also occur due to volatilization during the arc melting process, resulting in the generation of an impurity phase.
The mechanochemical reaction method takes nano-scale silicon powder and tantalum powder as raw materials and prepares nano-scale tantalum disilicide powder by long-time high-energy ball milling. The product prepared by the method has poor purity and lower cleanliness, and is not suitable for being used as a raw material for preparing high-performance ceramic materials.
The solid-phase reaction method is Ta2O5And Si as raw materials, and reacting at 1450-1600 ℃ to obtain TaSi2High emissivity powder, good crystallinity of the obtained powder particles and small particle size. However, the product has more other impurities, and high purity TaSi is difficult to obtain2And (3) powder.
In conclusion, the conventional method is adopted to synthesize TaSi with higher purity2It is difficult to precisely control these methods, and the reaction is incomplete and an impurity phase (Ta) is easily generated5Si3) Resulting in low purity product, non-uniform particles and unusable product.
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 product tantalum disilicide nano powder has uniform particles, high purity and no agglomeration phenomenon.
The invention specifically adopts the following technical scheme to realize the purpose of the invention:
a preparation method of tantalum disilicide nano powder is characterized by sequentially comprising the following steps:
(1) respectively weighing silicon powder and tantalum carbide powder with the particle sizes of 500 meshes according to the molar ratio of 2: 1, and 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 introducing argon to normal pressure;
(3) under the condition of argon atmosphere, heating the high-temperature carbonization furnace to 900-1400 ℃ at the speed of 10-20 ℃/min, preserving the heat for 1-4 h, and then naturally cooling to room temperature.
Wherein, the silicon powder refers to simple substance silicon powder, and the field is clear.
As a further definition, the particle size of the tantalum disilicide nanopowder is 100 to 200 nm.
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 conditions and environmental friendliness, and the prepared product tantalum disilicide nano powder has high purity, uniform particles, controllable size and no agglomeration phenomenon, and is an ideal raw material for preparing tantalum disilicide ceramic materials. Specifically, the method comprises the following steps: (1) the preparation method adopts solid-phase silicon powder and tantalum carbide as raw materials, and adopts one-step reaction synthesis through direct reaction in a carbonization furnace, so that the preparation method is simple in process, free of special equipment requirements and suitable for industrial mass production; (2) the whole preparation process does not need to add auxiliary reagents or introduce other substances such as hydrogen and the like for purification, the synthesis process is simple and safe, the reaction condition is mild, the environment is friendly, the reaction process is controllable, and no raw material silicon source is wasted; (3) the product tantalum disilicide nano-particles synthesized through direct reaction have high purity and controllable product size, the particle size is about 100-200 nm, the particle surface is coated by an amorphous carbon layer, and the volume of the reaction product is obviously expanded compared with that of the raw material, so that the particles do not obviously agglomerate, the lumps are loose, and the particles do not need to be crushed.
Drawings
FIG. 1 is an XRD spectrum of the tantalum disilicide nano powder prepared in example 1 of the present invention.
FIG. 2 is a TEM photograph of the tantalum disilicide nanopowder prepared in example 1 of the present invention.
FIG. 3 is a HRTEM photograph of the tantalum disilicide nanopowder prepared in example 1 of the present invention.
FIG. 4 is an EDS spectrum of the surface coating layer of tantalum disilicide nanopowder prepared in example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments, and not a limitation on the scope of the present invention.
Example 1
A preparation method of tantalum disilicide nano powder sequentially comprises the following steps:
(1) respectively weighing silicon powder and tantalum carbide powder with the particle sizes of 500 meshes according to the molar ratio of 2: 1, and then 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 in a ceramic crucible, then placing the ceramic crucible in a high-temperature carbonization furnace, vacuumizing to 10Pa, and then introducing argon to normal pressure;
(3) heating the high-temperature carbonization furnace to 1200 ℃ at the speed of 10 ℃/min under the argon atmosphere condition, preserving the heat for 2 hours, and then naturally cooling to room temperature to obtain the tantalum disilicide nano powder, wherein the particle size of the tantalum disilicide nano powder is 100-130 nm.
The tantalum disilicide nano powder samples prepared in the embodiment were respectively taken for analysis and detection, and the detection results are shown in the attached fig. 1-4: only the characteristic diffraction peak of tantalum disilicide is detected in fig. 1, indicating that single-phase tantalum disilicide powder is synthesized and the product has higher purity; it can be seen from FIG. 2 that the tantalum disilicide formed by the reaction has a particle size of about 100nm, and the surface of the particles is coated with an amorphous layer; as can be seen from FIG. 3, the distance between two adjacent parallel lattice fringes is 0.35nm, which is equal to that of the hexagonal phase TaSi2(JCPDS: 03-065-3548) that the (101) interplanar spacings were similar, indicating that the particles formed were tantalum disilicide; the results of the analysis of FIG. 4 show that the surface coating layer is composed of elemental carbon, and therefore, the surface coating layer of the tantalum disilicide particles is amorphous carbon, which is caused by the diffusion of carbon in the tantalum carbide to the surface of the particles during the formation of the tantalum disilicide phase.
Example 2
A preparation method of tantalum disilicide nano powder sequentially comprises the following steps:
(1) respectively weighing silicon powder and tantalum carbide powder with the particle sizes of 500 meshes according to the molar ratio of 2: 1, and then ball-milling and mixing uniformly, wherein the ball-material ratio is 3:1, and the ball-milling time is 12 hours to obtain mixed powder;
(2) placing the mixed powder in a ceramic crucible, then placing the ceramic crucible in a high-temperature carbonization furnace, vacuumizing to 15Pa, and then introducing argon to normal pressure;
(3) and under the condition of argon atmosphere, heating the high-temperature carbonization furnace to 1000 ℃ at the speed of 15 ℃/min, preserving the heat for 1h, and then naturally cooling to room temperature to obtain the tantalum disilicide nano powder, wherein the particle size of the tantalum disilicide nano powder is 120-160 nm.
The tantalum disilicide nano powder sample prepared in the embodiment is detected by XRD, and the detection result shows that the product is single-phase tantalum disilicide powder.
Example 3
A preparation method of tantalum disilicide nano powder sequentially comprises the following steps:
(1) respectively weighing silicon powder and tantalum carbide powder with the particle sizes of 500 meshes according to the molar ratio of 2: 1, and then 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 in a ceramic crucible, then placing the ceramic crucible in a high-temperature carbonization furnace, vacuumizing to 20Pa, and then introducing argon to normal pressure;
(3) heating the high-temperature carbonization furnace to 1300 ℃ at the speed of 20 ℃/min under the argon atmosphere condition, preserving the heat for 3 hours, and then naturally cooling to room temperature to obtain the tantalum disilicide nano powder, wherein the particle size of the tantalum disilicide nano powder is 130-180 nm.
The tantalum disilicide nano powder sample prepared in the embodiment is detected by XRD, and the detection result shows that the product is single-phase tantalum disilicide powder.
Example 4
A preparation method of tantalum disilicide nano powder sequentially comprises the following steps:
(1) respectively weighing silicon powder and tantalum carbide powder with the particle sizes of 500 meshes according to the molar ratio of 2: 1, and then 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 in a ceramic crucible, then placing the ceramic crucible in a high-temperature carbonization furnace, vacuumizing to 20Pa, and then introducing argon to normal pressure;
(3) heating the high-temperature carbonization furnace to 1400 ℃ at the speed of 20 ℃/min under the argon atmosphere condition, preserving the heat for 4 hours, and then naturally cooling to room temperature to obtain the tantalum disilicide nano powder, wherein the particle size of the tantalum disilicide nano powder is 150-200 nm.
The tantalum disilicide nano powder sample prepared in the embodiment is detected by XRD, and the detection result shows that the product is single-phase tantalum disilicide powder.
Claims (3)
1. A preparation method of tantalum disilicide nano powder is characterized by sequentially comprising the following steps:
(1) respectively weighing silicon powder and tantalum carbide powder with the particle sizes of 500 meshes according to the molar ratio of 2: 1, and 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 introducing argon to normal pressure;
(3) under the condition of argon atmosphere, heating the high-temperature carbonization furnace to 900-1400 ℃ at the speed of 10-20 ℃/min, preserving the heat for 1-4 h, and then naturally cooling to room temperature.
2. The method of preparing tantalum disilicide nanopowder according to claim 1, wherein: the particle size of the tantalum disilicide nano powder is 100-200 nm.
3. The method of preparing tantalum disilicide nanopowder according to claim 1 or 2, wherein: the surface of the tantalum disilicide nano powder particles is coated by the amorphous carbon layer.
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| CN114260449A (en) * | 2021-11-06 | 2022-04-01 | 广东省粤钢新材料科技有限公司 | High-hardness stainless steel wire |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114260449A (en) * | 2021-11-06 | 2022-04-01 | 广东省粤钢新材料科技有限公司 | High-hardness stainless steel wire |
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