Preparation method of superfine tantalum pentachloride powder

Abstract

The invention provides a preparation method of superfine tantalum pentachloride powder, which comprises the following steps of: firstly, putting metallurgical-grade tantalum powder into a reaction container, and heating and reacting in a chlorine environment to generate tantalum pentachloride steam; then, the steam is condensed into primary powder through a condensing device; then, heating and purifying the primary powder, and separating according to the boiling point difference of tantalum pentachloride and impurities to obtain high-purity tantalum pentachloride powder; and finally, grinding the high-purity powder and a grinding medium in an oxygen-free environment to obtain the nanoscale tantalum pentachloride powder with the particle size of less than 500nm. According to the method, by accurately controlling the chlorination reaction temperature, the condensation temperature and the grinding conditions, the particle size of the powder is effectively reduced, the solubility and the reaction activity of tantalum pentachloride in a solvent are remarkably improved, and the problems that in the prior art, the particle size of the powder is large, and the dissolution rate is low are solved. The nanoscale tantalum pentachloride powder prepared by the method has wide application potential in the high-tech fields of semiconductors, catalysts, alloys and the like.

Description

Technical Field

[0001] The invention relates to the technical field of powder material preparation, and in particular to a method for preparing ultrafine tantalum pentachloride powder. Background Art

[0002] Tantalum pentachloride (TaCl5), as an important metal halide, has shown wide application potential in high-tech fields such as semiconductors, catalysts, alloys, biomaterials, and military defense due to its unique physical and chemical properties. In particular, the demand for tantalum pentachloride is growing as an intermediate material for the preparation of high-purity tantalum products or high-precision and cutting-edge technologies such as vapor deposition. However, the chemical properties of tantalum pentachloride are extremely unstable, easy to reduce, easy to hydrolyze, and easy to react with the environment, which poses great challenges to its preparation and storage.

[0003] At present, the preparation methods of tantalum pentachloride mainly include direct chlorination and carbon addition chlorination. The direct chlorination method is to place tantalum powder or tantalum block in a quartz furnace and heat it to 500-700℃, then introduce chlorine gas for chemical reaction to generate tantalum pentachloride gas product, and then condense and collect the product. The carbon addition chlorination method is to mix tantalum pentoxide and carbon powder and place them in a quartz furnace and heat them to 800-1000℃, and also introduce chlorine gas for reaction to generate tantalum pentachloride and gas by-products (such as CO, CO2), and finally condense and collect the tantalum pentachloride product.

[0004] However, both preparation methods have some problems. First, due to the limitations of raw material purity and equipment materials, the purity of the produced tantalum pentachloride is not high, which is difficult to meet the demand for high-purity tantalum pentachloride in the high-tech field. In order to improve the purity, it is necessary to use the difference in boiling points between tantalum pentachloride and impurities to purify the product and separate the impurities. However, this process is complicated and costly.

[0005] Secondly, the particle size of tantalum pentachloride powder prepared by the prior art is relatively coarse, generally between 2600-5000nm. When such coarse-grained tantalum pentachloride is used as an intermediate for dissolving in a solvent or vapor deposition, it exhibits problems of slow reaction and low yield. This not only affects the application effect of tantalum pentachloride, but also limits its application scope in the field of high technology.

[0006] Therefore, in view of the problems existing in the prior art, it is particularly important to develop a new method for preparing nano-scale tantalum pentachloride. By preparing nano-scale tantalum pentachloride, its solubility and reactivity in solvents can be significantly improved, thereby solving the problems of slow reaction and low yield when tantalum pentachloride is used as an intermediate. At the same time, the preparation of nano-scale tantalum pentachloride will also provide a broader space for the application of tantalum pentachloride in the field of high technology. Summary of the invention

[0007] In view of the fact that the tantalum pentachloride powder prepared by the prior art has a relatively coarse particle size (2600-5000nm), slow reaction and low yield when used as an intermediate for solvent dissolution or vapor deposition, and the limitation that the prior art cannot prepare nano-scale tantalum pentachloride powder, the purpose of the present invention is to provide an innovative method for preparing ultrafine tantalum pentachloride powder. By precisely controlling key processes such as chlorination, condensation, purification, and crushing, the present invention aims to prepare tantalum pentachloride powder with a particle size of less than 500nm.

[0008] The preparation method of the present invention comprises the following steps:

[0009] A method for preparing ultrafine tantalum pentachloride powder comprises the following steps:

[0010] (1) Chlorination: Add metallurgical grade tantalum powder into a reaction vessel, introduce inert gas to exclude air, heat to a suitable temperature, and then introduce chlorine gas to carry out a chlorination reaction, which generates tantalum pentachloride vapor. In this step, the amount of tantalum powder added and the temperature of the chlorination reaction are controlled to ensure the smooth progress of the chlorination reaction and the generation of tantalum pentachloride vapor.

[0011] (2) Condensation: introducing tantalum pentachloride vapor into a condensation device to condense it into primary tantalum pentachloride powder;

[0012] (3) Purification: heating the primary tantalum pentachloride powder to volatilize it, and then condensing it to obtain high-purity tantalum pentachloride powder;

[0013] (4) Preparation of nano-scale powder: High-purity tantalum pentachloride powder and grinding media are added into a grinding device for grinding to finally obtain nano-scale tantalum pentachloride powder.

[0014] The temperature range of the chlorination reaction is 200°C to 700°C, preferably, the temperature range of the chlorination reaction is 500±10°C.

[0015] The condensation temperature is controlled between 100℃ and 150℃. The precise control of the condensation temperature ensures the effective condensation and collection of the powder.

[0016] In the purification step, the heating temperature is controlled at 180-210°C. At this temperature, the tantalum pentachloride powder melts and volatilizes, and then the steam is condensed to obtain high-purity tantalum pentachloride powder. At the same time, low-boiling point substances are discharged into the alkali liquid absorption device through the flue, and high-boiling point substances are retained in the evaporation kettle, which realizes the separation of the product and impurities and improves the purity of the tantalum pentachloride powder.

[0017] In the grinding step, the mass ratio of grinding balls to tantalum pentachloride powder is 1:1, and an oxygen-free environment is maintained during the grinding process to prevent oxidation of the powder. Preferably, the grinding medium is a mixture of zirconium oxide grinding balls with diameters of 2 mm and 1 mm, respectively, in a mass ratio of 1:9. The amount of ball material does not exceed two-thirds of the tank body, the ball mill speed is set to 160-300 r / min, and the grinding time is set to 300-500 min.

[0018] Beneficial effects of the present invention:

[0019] The present invention aims to solve the problems of coarse particle size, slow dissolution rate and low solubility of tantalum pentachloride powder in the prior art, and proposes an innovative method for preparing fine-grained high-purity tantalum pentachloride powder. The method successfully prepares tantalum pentachloride powder with a particle size of less than 500nm by precisely controlling key steps such as chlorination, condensation, purification and grinding, which significantly improves the performance and application effect of the product.

[0020] Specifically, the beneficial effects of the present invention are mainly reflected in the following aspects:

[0021] Improved reactivity and solubility: By preparing nano-scale tantalum pentachloride powder, its solubility and reactivity in solvents are significantly improved. This enables tantalum pentachloride to exhibit faster reaction speed and higher yield when used as an intermediate for solvent dissolution or vapor deposition, thereby improving its application effect in related fields.

[0022] Optimized preparation process: The present invention optimizes the steps of chlorination, condensation and purification to ensure the high purity and fine grain characteristics of tantalum pentachloride powder. At the same time, by introducing the grinding step, the particle size of the powder is further refined to the nanometer level, meeting the demand for nanomaterials in the high-tech field.

[0023] Solve the existing technical problems: the tantalum pentachloride powder prepared by the existing technology has coarse particle size, slow reaction and low yield. The present invention successfully solves this problem through an innovative preparation method, providing a better material foundation for the application of tantalum pentachloride in the high-tech field.

[0024] Expanding application areas: The successful preparation of nano-scale tantalum pentachloride powder will provide a broader space for its application in high-tech fields such as semiconductors, catalysts, alloys, biomaterials, and military defense. This will not only help promote the innovation and development of related technologies, but also help enhance my country's international competitiveness in these fields.

[0025] In summary, the method for preparing fine-grained high-purity tantalum pentachloride powder proposed in the present invention has significant beneficial effects and application prospects, and is of great significance for promoting the development of tantalum pentachloride and related technologies. DETAILED DESCRIPTION

[0026] Preferred embodiments of the present invention are given below to illustrate the technical solutions of the present invention in detail.

[0027] Embodiment 1:

[0028] (1) Add 8 kg of tantalum powder into a quartz tank, evacuate and deoxidize for 30 minutes, then heat to 500°C and introduce chlorine gas at a flow rate of 5 L / min. The chlorine gas and tantalum powder react chemically to generate tantalum pentachloride vapor.

[0029] (2) The generated tantalum pentachloride vapor is passed into a condenser, and the condenser starts to be heated. The heating temperature is set to 100° C., and the tantalum pentachloride vapor generates tantalum pentachloride primary powder.

[0030] (3) Add the primary tantalum pentachloride powder into the evaporator of the distillation equipment, and set the heating temperature to 210°C. When the temperature in the evaporator reaches 210°C, the tantalum pentachloride powder melts into liquid and volatilizes tantalum pentachloride vapor. The tantalum pentachloride vapor enters the condenser and is naturally cooled to become high-purity tantalum pentachloride powder and enters the receiving bottle.

[0031] (4) High-purity tantalum pentachloride powder and zirconium oxide grinding balls were added to a vacuum grinding tank for grinding with a ball-to-material ratio of 1:1 and a grinding ball ratio of 2 mm:1 mm = 1:9. The amount of ball material did not exceed two-thirds of the tank. The ball mill speed was set to 300 r / min and the grinding time was set to 300 min. After the grinding was completed, the ball material was separated in a glove box to obtain nano-scale tantalum pentachloride powder. The particle size distribution is shown in Table 1.

[0032] Table 1 Tantalum pentachloride powder particle size distribution analysis report (implementation method 1)

[0033]

[0034]

[0035] Embodiment 2:

[0036] (1) Add 10 kg of tantalum powder into a quartz tank, evacuate and deoxidize for 30 minutes, then heat to 500°C and introduce chlorine gas at a flow rate of 5 L / min. The chlorine gas and tantalum powder react chemically to generate tantalum pentachloride vapor.

[0037] (2) The generated tantalum pentachloride vapor is passed into a condenser, and the condenser starts to be heated. The heating temperature is set to 150° C., and the tantalum pentachloride vapor generates tantalum pentachloride primary powder.

[0038] (3) Add the primary tantalum pentachloride powder into the evaporator of the distillation equipment, and set the heating temperature to 180°C. When the temperature in the evaporator reaches 180°C, the tantalum pentachloride powder melts into liquid and evaporates tantalum pentachloride vapor. The tantalum pentachloride vapor enters the condenser and is naturally cooled to become high-purity tantalum pentachloride powder and enters the receiving bottle.

[0039] (4) High-purity tantalum pentachloride powder and zirconium oxide grinding balls were added to a vacuum grinding tank for grinding with a ball-to-material ratio of 1:1 and a grinding ball ratio of 2 mm:1 mm = 1:9. The amount of ball material did not exceed two-thirds of the tank. The ball mill speed was set to 160 r / min and the grinding time was set to 500 min. After the grinding was completed, the ball material was separated in a glove box to obtain nano-scale tantalum pentachloride powder. The particle size distribution is shown in Table 2.

[0040] Table 2 Tantalum pentachloride powder particle size distribution analysis report (Example 2)

[0041]

[0042]

[0043] Comparative example: The experimental method of this comparative example was carried out according to patents (CN202310197752.0 and CN202310451548.7). The particle size distribution of the comparative example is shown in Table 3.

[0044] Table 3 Tantalum pentachloride powder particle size distribution analysis report (comparative example)

[0045]

[0046] According to the above examples and comparative examples, it can be seen that both Example 1 and Example 2 successfully prepared nano-scale tantalum pentachloride powder with a particle size of less than 500nm and with high purity. Example 2 can still prepare nano-scale tantalum pentachloride powder that meets the requirements when the chlorination reaction temperature is lowered, indicating that the preparation method has certain flexibility and stability. The particle size of the tantalum pentachloride powder prepared by the method used in the comparative example is much larger than 500nm, indicating that the method of the present invention has significant advantages in preparing nano-scale tantalum pentachloride powder.

[0047] The present invention successfully prepares nano-scale tantalum pentachloride powder with small particle size, high purity and high reaction activity by precisely controlling key steps such as chlorination, condensation, purification and grinding. The method solves the problems of coarse particle size, slow dissolution rate and low solubility of tantalum pentachloride powder in the prior art, and provides a better material basis for the application of tantalum pentachloride.

Claims

1. A method for preparing ultrafine tantalum pentachloride powder, characterized in that: The following steps are involved: (1) Chlorination: Add metallurgical grade tantalum powder into a reaction vessel, introduce inert gas to exclude air, heat to a suitable temperature, and then introduce chlorine gas to carry out chlorination reaction, which generates tantalum pentachloride vapor; (2) Condensation: introducing tantalum pentachloride vapor into a condensation device to condense it into primary tantalum pentachloride powder; (3) Purification: heating the primary tantalum pentachloride powder to volatilize it, and then condensing it to obtain high-purity tantalum pentachloride powder; (4) Preparation of nano-scale powder: High-purity tantalum pentachloride powder and grinding media are added into a grinding device for grinding to finally obtain nano-scale tantalum pentachloride powder.

2. The method according to claim 1, characterized in that The temperature range of the chlorination reaction is 200°C to 700°C.

3. The method according to claim 2, characterized in that The temperature range of the chlorination reaction is 500±10℃.

4. The method according to claim 1, characterized in that: The condensation temperature is controlled between 100°C and 150°C.

5. The method according to claim 1, characterized in that In the purification step, the heating temperature is controlled at 180-210°C, and the difference in boiling points between tantalum pentachloride and impurities is used for separation to improve the purity of the final product.

6. The method according to claim 1, characterized in that In the grinding step, the mass ratio of the grinding balls to the tantalum pentachloride powder is 1:1, and an oxygen-free environment is maintained during the grinding process to prevent oxidation of the powder.

7. The method according to claim 6, characterized in that The grinding media are zirconia grinding balls with diameters of 2 mm and 1 mm respectively, mixed in a mass ratio of 1:9, the amount of ball material does not exceed two-thirds of the tank body, the ball mill speed is set to 160-300 r / min, and the grinding time is set to 300-500 min.

Images