阅读说明：本技术 一种纳米氮化钒粉体的粒径分级可控制备方法 (Particle size grading controllable preparation method of nano vanadium nitride powder ) 是由 王开新 吴斌 孙虹 杨得全 谢劲松 韩成良 于 2020-06-09 设计创作，主要内容包括：一种纳米氮化钒粉体的粒径分级可控制备方法,涉及高熔点氮化物粉体制备技术领域。首先通过分散研磨设备对金属钒粉进行表面处理,然后通过化学气相沉积法制备得到氮化钒团聚体,最后再次通过分散研磨设备进行研磨处理,得到纳米氮化钒粉体成品。金属钒粉的改性是在分散研磨设备中进行的,这样可以显著提高改性效果,使表面涂覆均匀,更有利于后续化学气相沉积反应的进行。在制备氮化钒团聚体后利用分散研磨设备再次进行处理,通过这种结构设计合理的研磨设备,可以制备出产物粒径分布均匀的纳米氮化钒产品,产物品质高。(A grain size grading controllable preparation method of nano vanadium nitride powder relates to the technical field of high-melting-point nitride powder preparation. Firstly, carrying out surface treatment on metal vanadium powder by using dispersion grinding equipment, then preparing vanadium nitride aggregates by using a chemical vapor deposition method, and finally carrying out grinding treatment by using dispersion grinding equipment to obtain a nano vanadium nitride powder finished product. The modification of the metal vanadium powder is carried out in the dispersing and grinding equipment, so that the modification effect can be obviously improved, the surface coating is uniform, and the subsequent chemical vapor deposition reaction is more favorably carried out. After the vanadium nitride aggregate is prepared, the dispersion grinding equipment is used for processing again, and the grinding equipment with reasonable structural design can be used for preparing the nano vanadium nitride product with uniform product particle size distribution and high product quality.)

1. A controllable preparation method of nanometer vanadium nitride powder in particle size grading is characterized in that metal vanadium powder is subjected to surface treatment through dispersion grinding equipment, vanadium nitride aggregates are prepared through a chemical vapor deposition method, and finally grinding is performed through the dispersion grinding equipment again to obtain a finished product of the nanometer vanadium nitride powder.

2. The method of claim 1, wherein the dispersion mill apparatus is mainly composed of a base plate, a U-shaped block, a movable box, a feed box, a motor; the bottom of the U-shaped block is fixed at the top of the bottom plate; the grinding structure is arranged in the U-shaped block and consists of a grinding groove, a rotating shaft, a grinding wheel, a filter plate and a discharge pipe; the two sides of the grinding groove are respectively fixed on the two sides of the inner wall of the U-shaped block, a rotating shaft is rotatably connected between the two sides of the inner wall of the grinding groove, a grinding wheel is fixedly connected to the outer surface of the rotating shaft, a filter plate is fixedly connected between the two sides of the inner wall of the grinding groove, the grinding wheel is arranged above the filter plate, and the distance between the filter plate and the grinding wheel is adjustable; the bottom of the inner wall of the grinding groove is communicated with a discharge pipe, and the bottom end of the discharge pipe penetrates through the grinding groove and extends to the bottom of the grinding groove; a material receiving groove is slidably connected with the inner part of the U-shaped block below the grinding groove, and a discharge pipe is used for discharging the ground material to the inner part of the material receiving groove;

the motor is fixed on one side of the U-shaped block, an output shaft of the motor is fixedly connected with a rotating shaft, the outer surface of one end, close to the motor, of the rotating shaft is fixedly connected with a first bevel gear, one end, penetrating through the side face of the U-shaped block and extending to the outside of the U-shaped block, of the rotating shaft is fixedly connected with a second bevel gear, and the outer surface of the second bevel gear is meshed with the outer surface of the first bevel gear; through the rotation of the first bevel gear, the second bevel gear can be driven to rotate through meshing, so that the rotating shaft is driven to rotate, the grinding wheel is driven to rotate, and materials on the filter plate are ground and processed through the rotation of the grinding wheel;

the two sides of the movable box are respectively fixed on the top of the U-shaped block, a threaded rod is rotatably connected between the two sides of the inner wall of the movable box, a threaded block is in threaded connection with the outer surface of the threaded rod, the top of the threaded block is slidably connected to the top of the inner wall of the movable box, a T-shaped plate is fixedly connected to the bottom of the threaded block, the bottom of the T-shaped plate penetrates through the bottom of the movable box and extends into the grinding groove, and a sliding rail matched with the T-shaped plate for sliding is arranged at the position where the T; one end of the threaded rod penetrates through the side face of the movable box and extends to the outside of the movable box, and the outer surface of one end of the threaded rod extending to the outside of the movable box is fixedly connected with a worm wheel;

the feeding box is fixed at the upper part of the movable box, the top of the feeding box is provided with a feeding nozzle, the bottom of the inner wall of the feeding box is communicated with two connecting pipes, and one end of each connecting pipe is connected with one end of the T-shaped plate extending to the inside of the grinding groove;

one end of the outer surface of the end part of the rotating shaft is fixedly connected with a worm, and the worm is meshed with the outer surface of the worm wheel; through the rotation of threaded rod, can drive the screw thread piece side-to-side motion, and the motion about the screw thread piece can drive the bottom of two connecting pipes through the T template and carry out the side-to-side motion to the inside of grinding groove is arranged through two connecting pipes to the material of feeding incasement portion, through the motion about the connecting pipe moreover, can be with the even dispersion of material in the inside of grinding groove.

3. The manufacturing method of claim 2, wherein the vibrating machine is provided on both sides of the top of the inner wall of the feeding box, and the vibrating rod is provided on the bottom of the vibrating machine.

4. The method of claim 2, wherein the bottom of the inner wall of the feed box is provided at both sides with inclined blocks to facilitate the collection of the materials inside the feed box and the discharge of the materials to the inside of the grinding tank through two connecting pipes.

5. The method for preparing the rubber material as claimed in claim 2, wherein the connecting pipes are flexible pipes, so that the T-shaped plates can drive the two connecting pipes to move left and right to disperse the material.

6. The method of claim 2, 3, 4 or 5, wherein the step of surface-treating the metal vanadium powder comprises: adding metal vanadium powder into a feeding box of dispersing and grinding equipment, and then adding ethanol, sodium fatty acid and 2-ethylhexyl phosphate mono-2-ethylhexyl as a solvent, a surface treatment agent and a chelating agent respectively; the weight ratio of the metal vanadium powder, the ethanol, the sodium fatty acid and the 2-ethylhexyl phosphate mono-2-ethylhexyl ester is 1: 1-3: 0.1-0.5: 0.1 to 0.5; and processing the vanadium powder by using dispersion grinding equipment to obtain the modified metal vanadium powder wrapped by the surface treating agent.

7. The method of claim 6, wherein the vanadium nitride agglomerates are prepared by a chemical vapor deposition method comprising: the chemical vapor deposition reactor is divided into an elevated temperature area, a high temperature area and a cooling area, wherein the temperatures of the elevated temperature area and the high temperature area are respectively as follows: 200-300 ℃ and 600-800 ℃; continuously introducing argon and nitrogen into the heating area, the high-temperature area and the cooling area, and simultaneously continuously introducing ammonia into the high-temperature area; enabling the vanadium powder subjected to surface treatment to enter a heating area of a reactor through automatic feeding equipment, staying for 1-5 minutes, then continuing to advance to a high-temperature area, staying for 10-30 minutes, and then leaving the high-temperature area to enter a cooling area for cooling; and after the temperature is reduced to room temperature, the mixture enters a finished product box to obtain the vanadium nitride aggregate.

8. The preparation method of claim 7, wherein the grinding treatment is carried out again by a dispersion grinding device, and the method for obtaining the finished product of the nano vanadium nitride powder comprises the following steps: adding vanadium nitride aggregates and a grinding aid into a feed box of dispersing and grinding equipment respectively, wherein the grinding aid is quartz sand, and the weight ratio of the vanadium nitride aggregates to the quartz sand is controlled to be 1: and 3, grinding for 1-3 h, processing by using dispersing and grinding equipment, and separating quartz sand to obtain a finished product of the nano vanadium nitride powder.

Technical Field

The invention relates to the technical field of preparation of high-melting-point nitride powder, in particular to a particle size grading controllable preparation method of nano vanadium nitride powder.

Background

Nitride powders having high melting points, high hardness, high chemical stability, and excellent electrical and optical properties have attracted general attention. The unique physical and chemical properties make the nitride have wide application in the fields of semiconductor devices, microelectronics, porous ceramics and the like.

The vanadium-nitrogen alloy is a novel alloy additive, and can replace ferrovanadium to be used for producing microalloyed steel. The vanadium nitride added into the steel can improve the comprehensive mechanical properties of the steel, such as strength, toughness, ductility, thermal fatigue resistance and the like, and enables the steel to have good weldability. Under the condition of achieving the same strength, the vanadium nitride is added, so that the adding amount of vanadium is saved by 30-40%, and the cost is further reduced.

The chemical vapor deposition method has incomparable advantages and advantages in the preparation process of the high-melting-point nitride. However, the existing chemical vapor deposition method has the defects of serious agglomeration of prepared products, uneven particle size distribution and the like.

Disclosure of Invention

Aiming at the technical problems of the preparation of vanadium nitride powder, the invention provides a particle size grading controllable preparation method of nano vanadium nitride powder, which has the advantages of simple and convenient operation, high purity and the like, and overcomes the defect of uneven particle size distribution of the existing preparation method.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a controllable preparation method of nanometer vanadium nitride powder by particle size grading comprises the steps of firstly carrying out surface treatment on metal vanadium powder through dispersion grinding equipment, then preparing vanadium nitride aggregates through a chemical vapor deposition method, and finally carrying out grinding treatment through the dispersion grinding equipment again to obtain a finished product of the nanometer vanadium nitride powder.

As the preferred technical scheme of the invention, the dispersing and grinding equipment mainly comprises a bottom plate, a U-shaped block, a movable box, a feeding box and a motor; the bottom of the U-shaped block is fixed at the top of the bottom plate; the grinding structure is arranged in the U-shaped block and consists of a grinding groove, a rotating shaft, a grinding wheel, a filter plate and a discharge pipe; the two sides of the grinding groove are respectively fixed on the two sides of the inner wall of the U-shaped block, a rotating shaft is rotatably connected between the two sides of the inner wall of the grinding groove, a grinding wheel is fixedly connected to the outer surface of the rotating shaft, a filter plate is fixedly connected between the two sides of the inner wall of the grinding groove, the grinding wheel is arranged above the filter plate, and the distance between the filter plate and the grinding wheel is adjustable; the bottom of the inner wall of the grinding groove is communicated with a discharge pipe, and the bottom end of the discharge pipe penetrates through the grinding groove and extends to the bottom of the grinding groove; a material receiving groove is slidably connected with the inner part of the U-shaped block below the grinding groove, and a discharge pipe is used for discharging the ground material to the inner part of the material receiving groove;

the motor is fixed on one side of the U-shaped block, an output shaft of the motor is fixedly connected with a rotating shaft, the outer surface of one end, close to the motor, of the rotating shaft is fixedly connected with a first bevel gear, one end, penetrating through the side face of the U-shaped block and extending to the outside of the U-shaped block, of the rotating shaft is fixedly connected with a second bevel gear, and the outer surface of the second bevel gear is meshed with the outer surface of the first bevel gear; through the rotation of the first bevel gear, the second bevel gear can be driven to rotate through meshing, so that the rotating shaft is driven to rotate, the grinding wheel is driven to rotate, and materials on the filter plate are ground and processed through the rotation of the grinding wheel;

the two sides of the movable box are respectively fixed on the top of the U-shaped block, a threaded rod is rotatably connected between the two sides of the inner wall of the movable box, a threaded block is in threaded connection with the outer surface of the threaded rod, the top of the threaded block is slidably connected to the top of the inner wall of the movable box, a T-shaped plate is fixedly connected to the bottom of the threaded block, the bottom of the T-shaped plate penetrates through the bottom of the movable box and extends into the grinding groove, and a sliding rail matched with the T-shaped plate for sliding is arranged at the position where the T; one end of the threaded rod penetrates through the side face of the movable box and extends to the outside of the movable box, and the outer surface of one end of the threaded rod extending to the outside of the movable box is fixedly connected with a worm wheel;

the feeding box is fixed at the upper part of the movable box, the top of the feeding box is provided with a feeding nozzle, the bottom of the inner wall of the feeding box is communicated with two connecting pipes, and one end of each connecting pipe is connected with one end of the T-shaped plate extending to the inside of the grinding groove;

one end of the outer surface of the end part of the rotating shaft is fixedly connected with a worm, and the worm is meshed with the outer surface of the worm wheel; through the rotation of threaded rod, can drive the screw thread piece side-to-side motion, and the motion about the screw thread piece can drive the bottom of two connecting pipes through the T template and carry out the side-to-side motion to the inside of grinding groove is arranged through two connecting pipes to the material of feeding incasement portion, through the motion about the connecting pipe moreover, can be with the even dispersion of material in the inside of grinding groove.

As a preferable technical scheme of the invention, the two sides of the top of the inner wall of the feeding box are respectively provided with a vibrating machine, and the bottom of the vibrating machine is provided with a vibrating rod.

As the preferable technical scheme of the invention, the two sides of the bottom of the inner wall of the feeding box are respectively provided with the inclined blocks, so that the materials in the feeding box can be conveniently collected and can be conveniently discharged to the inside of the grinding groove through the two connecting pipes.

As the preferred technical scheme of the invention, the connecting pipes adopt the telescopic hoses, so that the T-shaped plates can drive the two connecting pipes to move left and right conveniently, and the materials are dispersed.

As a preferred technical scheme of the invention, the step of carrying out surface treatment on the metal vanadium powder comprises the following steps: adding metal vanadium powder into a feeding box of dispersing and grinding equipment, and then adding ethanol, sodium fatty acid and 2-ethylhexyl phosphate mono-2-ethylhexyl as a solvent, a surface treatment agent and a chelating agent respectively; the weight ratio of the metal vanadium powder, the ethanol, the sodium fatty acid and the 2-ethylhexyl phosphate mono-2-ethylhexyl ester is 1: 1-3: 0.1-0.5: 0.1 to 0.5; and processing the vanadium powder by using dispersion grinding equipment to obtain the modified metal vanadium powder wrapped by the surface treating agent.

As a preferred technical scheme of the invention, the method for preparing the vanadium nitride aggregate by the chemical vapor deposition method comprises the following steps: the chemical vapor deposition reactor is divided into an elevated temperature area, a high temperature area and a cooling area, wherein the temperatures of the elevated temperature area and the high temperature area are respectively as follows: 200-300 ℃ and 600-800 ℃; continuously introducing argon and nitrogen into the heating area, the high-temperature area and the cooling area, and simultaneously continuously introducing ammonia into the high-temperature area; enabling the vanadium powder subjected to surface treatment to enter a heating area of a reactor through automatic feeding equipment, staying for 1-5 minutes, then continuing to advance to a high-temperature area, staying for 10-30 minutes, and then leaving the high-temperature area to enter a cooling area for cooling; and after the temperature is reduced to room temperature, the mixture enters a finished product box to obtain the vanadium nitride aggregate.

As a preferred technical scheme of the invention, the method for grinding again by using the dispersion grinding equipment to obtain the finished product of the nano vanadium nitride powder comprises the following steps: adding vanadium nitride aggregates and a grinding aid into a feed box of dispersing and grinding equipment respectively, wherein the grinding aid is quartz sand, and the weight ratio of the vanadium nitride aggregates to the quartz sand is controlled to be 1: and 3, grinding for 1-3 h, processing by using dispersing and grinding equipment, and separating quartz sand to obtain a finished product of the nano vanadium nitride powder.

Compared with the prior art, the invention has the beneficial effects that:

1) the method realizes the preparation of the high-purity nano vanadium nitride powder, has the advantages of simple and convenient process, low cost, high product purity and the like, and can be used for large-scale production.

2) The modified vanadium powder with the surface rich in active sites can be obtained by carrying out surface modification treatment on the vanadium powder before preparing vanadium nitride and adding a surface treating agent and a metal chelating agent for reaction, so that the subsequent generation of high-purity nano vanadium nitride powder is facilitated. The nitridation reduction reaction is completed in the inert atmosphere of argon and nitrogen, the influence of oxygen or air on the reaction process can be completely eliminated, and the sufficient ammonia gas enables the metal vanadium powder to be completely reacted.

3) The modification of the metal vanadium powder is carried out in the dispersion grinding equipment, so that the modification effect can be obviously improved, the surface coating is uniform, and the subsequent chemical vapor deposition reaction is more favorably carried out.

4) The nano vanadium nitride product with uniform product particle size distribution can be prepared by the grinding equipment with reasonable structural design, the product quality is high, and the particle size grading can be controlled.

5) The dispersing and grinding equipment drives the connecting pipe to move left and right through the T-shaped plate, the material can be uniformly dispersed in the grinding groove, the dispersing function is achieved, the grinding efficiency and the grinding effect are improved, the accumulation of nano titanium nitride slurry is avoided, the reduction of the grinding effect is caused, the damage of the grinding equipment is easily caused, and the service life of the grinding equipment is shortened.

Drawings

Fig. 1 is a schematic view of the internal structure of the dispersion grinding apparatus.

Fig. 2 is a schematic view of the external structure of the dispersion grinding apparatus.

Fig. 3 is a schematic structural view of a feed box.

FIG. 4 is an XRD pattern of the nano vanadium nitride powder prepared in examples 2-4.

FIG. 5 is an SEM image of nano vanadium nitride powder prepared in example 2.

Detailed Description