CN109319785B - Method for preparing superfine tungsten carbide powder by mechanochemical method - Google Patents
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Abstract
The invention discloses a method for preparing superfine tungsten carbide powder by a mechanochemical method, which comprises the following steps: the method comprises the following steps of mixing tungsten trioxide powder and carbon black in a mass ratio of 1: 3-5, mixing to prepare a mixed raw material; putting the mixed raw materials into a ball milling tank of a ball mill, adding grinding balls, and then performing inert gas protection or vacuum pumping treatment on the ball milling tank; placing the ball milling tank into a hearth of the ball mill, and then carrying out ball milling on the mixed raw materials through the ball mill; in the ball milling process, after the temperature of the hearth is raised to 850-950 ℃, the hearth is kept warm for 70-90 h; and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the ultrafine tungsten carbide powder with uniform granularity. The invention has the advantages of simple process, low energy consumption and low cost, can shorten the reaction time and has high industrial value.
Description
Technical Field
The invention belongs to the technical field of tungsten carbide-based hard alloy, and particularly relates to a method for preparing superfine tungsten carbide powder by a mechanochemical method.
Background
With the rapid development of science and technology, the demand of industrial production and daily life of people on hard alloy is increasing day by day. The superfine tungsten carbide (WC) is used as the most widely applied hard alloy material at present, has high hardness, good wear resistance, high strength and toughness, and is widely applied to the field of difficult-to-cut processing. And in fact, under the condition that all other conditions are equal, each property of the tungsten carbide-based hard alloy, such as hardness, modulus, wear resistance, compressive strength and the like, is enhanced along with the reduction of the average particle size of the tungsten carbide powder, so that the method has far-reaching significance for preparing the superfine tungsten carbide powder.
At present, the preparation process of the ultrafine tungsten carbide powder with wider industrial application mainly comprises a tungsten oxide hydrogen reduction carbonization method and a high-energy ball milling method; the tungsten oxide hydrogen reduction carbonization method needs to introduce hydrogen into a high-temperature furnace to reduce tungsten trioxide into tungsten powder, then the tungsten powder and carbon black are mixed according to an equal molar ratio, carbonization is carried out in a hydrogen atmosphere, and the carbonization temperature is 1400-1600 ℃, so that the method is complex in process flow, high in energy consumption and high in cost; the high-energy ball milling method needs to mix tungsten powder and carbon powder uniformly and then put the mixture into a high-energy ball mill with the rotating speed as high as 800r/min for ball milling for a long time, and the method has higher requirement on the rotating speed of the ball mill, and the efficiency of the ball mill for crushing WC powder is lower, so that quite long crushing time is needed, the particle size distribution of the product is difficult to control, and the powder performance is influenced.
In summary, there are some technical difficulties in the tungsten oxide hydrogen reduction carbonization method and the high energy ball milling method for producing the ultrafine tungsten carbide powder, and therefore, a process method suitable for producing the ultrafine tungsten carbide powder at a process level is required.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing superfine tungsten carbide powder by a mechanochemical method.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for preparing superfine tungsten carbide powder by a mechanochemical method comprises the following steps:
the method comprises the following steps of mixing tungsten trioxide powder and carbon black in a mass ratio of 1: 3-5, mixing to prepare a mixed raw material;
putting the mixed raw materials into a ball milling tank of a ball mill, adding grinding balls, and then performing inert gas protection or vacuum pumping treatment on the ball milling tank;
placing the ball milling tank into a hearth of the ball mill, and then carrying out ball milling on the mixed raw materials through the ball mill; in the ball milling process, after the temperature of the hearth is raised to 850-950 ℃, the hearth is kept warm for 70-90 h;
and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the ultrafine tungsten carbide powder with uniform granularity.
Further, the preparation method of the tungsten trioxide powder comprises the following steps:
dropwise adding concentrated hydrochloric acid into a sodium tungstate solution in a stirring state to prepare tungstic acid colloid;
and drying the tungstic acid colloid, and calcining to obtain the tungsten trioxide powder.
Further, when tungstic acid colloid is prepared by dropwise adding concentrated hydrochloric acid into a sodium tungstate solution in a stirring state, the sodium tungstate solution is a sodium tungstate aqueous solution with a concentration of 0.36mol/L prepared by sodium tungstate crystals.
Further, when tungstic acid colloid is prepared by dropwise adding concentrated hydrochloric acid to a sodium tungstate solution in a stirred state, the concentration of the dropwise added concentrated hydrochloric acid is 12 mol/L.
Further, when tungstic acid colloid is prepared by dropwise adding concentrated hydrochloric acid into a sodium tungstate solution in a stirring state, dropwise adding concentrated hydrochloric acid into the sodium tungstate solution at a temperature of 80 ℃ to make the pH value of the mixed solution 1, and then stopping dropwise adding the concentrated hydrochloric acid into the sodium tungstate solution.
Further, when the mixed raw material and the grinding balls are loaded into the ball milling tank, the ball material ratio of the grinding balls to the mixed raw material is 15-30: 1, wherein the grinding balls are stainless steel or tungsten carbide grinding balls with the diameter of 12 mm.
Further, when the mixed raw material is ball-milled by the ball mill, the rotation speed of the ball mill motor is 450 to 500 rpm.
Further, in the process of heating the hearth to 850-950 ℃, the heating rate of the hearth is 4-6 ℃/min.
According to the method for preparing the superfine tungsten carbide powder by the mechanochemical method, provided by the invention, the tungsten trioxide powder and the carbon black are subjected to one-step reaction by using the high-temperature mechanochemical method, so that the superfine tungsten carbide powder with uniform granularity can be obtained, and the tungsten powder is prepared without pretreating tungsten oxide; in addition, the carbonization temperature of the conventional tungsten oxide hydrogen reduction carbonization method is greatly reduced from 1400-1600 ℃ to 850-950 ℃; meanwhile, the superfine WC powder with the average grain diameter of 0.225 mu m can be successfully prepared at a very low rotating speed without using a high-rotating-speed ball mill. Therefore, the method has the advantages of simple process, less energy consumption and low cost, can shorten the reaction time, and has high industrial value.
Drawings
FIG. 1 is a flowchart of a mechanochemical method of producing ultra-fine tungsten carbide powder in accordance with an exemplary embodiment of the present invention;
FIG. 2 is a flowchart of yet another mechanochemical method of producing ultra-fine tungsten carbide powder in accordance with an exemplary embodiment of the present invention;
FIG. 3 is a flowchart of yet another mechanochemical method of producing ultra-fine tungsten carbide powder in accordance with an exemplary embodiment of the present invention;
FIG. 4 is a diffraction pattern of XRD of the ultra fine tungsten carbide powder prepared in exemplary example 1 of the present invention;
FIG. 5 is a detection spectrum of a laser particle sizer of the ultra-fine tungsten carbide powder prepared in exemplary embodiment 1 of the present invention;
fig. 6 is a scanning electron microscope analysis picture of the ultra-fine tungsten carbide powder prepared in exemplary example 1 of the present invention.
Detailed Description
In order to overcome the defects in the prior art, the invention provides a method for preparing superfine tungsten carbide powder by a mechanochemical method. In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be described in more detail below with reference to the accompanying drawings in the preferred embodiments of the present invention. The described embodiments are only some, but not all embodiments of the invention. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
As shown in fig. 1, a mechanochemical method for preparing ultrafine tungsten carbide powder includes:
s100, mixing tungsten trioxide powder and carbon black according to a mass ratio of 1: 3-5, mixing to prepare a mixed raw material;
s200, filling the mixed raw materials into a ball milling tank of a ball mill, adding stainless steel or tungsten carbide grinding balls with the diameter of 12mm, wherein the ball-material ratio of the grinding balls to the mixed raw materials is 15-30: 1, and performing inert gas protection or vacuum pumping treatment on the ball milling tank;
s300, placing the ball milling tank into a hearth of a ball mill, and setting the rotating speed of the ball mill to be 450-500 rpm to perform ball milling on the mixed raw materials; in the ball milling process, heating the hearth to 850-950 ℃ at a heating rate of 4-6 ℃/min, and then preserving the heat of the hearth for 70-90 h;
s400, closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the ultrafine tungsten carbide powder with uniform particle size.
Further, to better explain the preparation method of the ultrafine tungsten carbide powder, as a refinement and extension of the above example, an embodiment of the present invention provides a preparation method of a tungsten trioxide powder, as shown in fig. 2, the method including:
s101, preparing sodium tungstate crystals into a sodium tungstate aqueous solution with the concentration of 0.36mol/L, heating the temperature of the sodium tungstate aqueous solution to 80 ℃, dropwise adding concentrated hydrochloric acid with the concentration of 12mol/L into the sodium tungstate aqueous solution in a stirring state to enable the pH value of the mixed solution to be 1, and stopping dropwise adding the concentrated hydrochloric acid into the sodium tungstate aqueous solution to obtain tungstic acid colloid;
s102, drying tungstic acid colloid, and calcining to obtain tungsten trioxide powder.
According to the method for preparing the ultrafine tungsten carbide powder by the mechanochemical method, the tungsten trioxide and the carbon black are reacted by using a high-temperature mechanochemical method, the pressure of the reaction is not changed, the powder is further refined and dispersed more uniformly by the mechanical force of ball milling, a reactant and a product are continuously refined along with the reaction, the ultrafine tungsten trioxide as the reactant is reduced into an oxide of low-valent tungsten in the process of heating and ball milling, the oxide of the low-valent tungsten is gradually reduced by carbon powder along with the extension of time, meanwhile, the unreacted reaction surface is timely exposed due to the uninterrupted ball milling, the carbon can more easily enter the crystal lattice of the tungsten oxide, and the combination reaction of the carbon powder and the tungsten oxide powder is promoted. In addition, the proper ball milling refines crystal grains and increases the specific surface area, thereby improving the kinetic condition, leading the reaction to be more complete at high temperature and also being realized at lower temperature, and reducing the occurrence of agglomeration phenomenon due to the existence of the ball milling.
The method for preparing ultrafine tungsten carbide powder by mechanochemical method according to the present invention will be described in detail with reference to the following examples.
Example 1
As shown in fig. 3, a mechanochemical method for preparing ultrafine tungsten carbide powder includes:
(1) preparing 120g of sodium tungstate crystal into 0.36mol/L sodium tungstate aqueous solution, heating 500ml of sodium tungstate aqueous solution to 80 ℃, dropwise adding 50ml of 12mol/L concentrated hydrochloric acid while stirring to enable the pH value of the mixed solution to be 1, stopping dropwise adding concentrated hydrochloric acid into the sodium tungstate aqueous solution, and stirring for 1.5 hours to obtain tungstic acid colloid;
(2) drying tungstic acid colloid, placing the tungstic acid colloid in a resistance furnace, heating to 600 ℃, calcining, and keeping the temperature for 2 hours to prepare superfine tungsten trioxide powder with the average particle size of 0.202 mu m;
(3) preparing a mixed raw material by mixing 80g of tungsten trioxide powder and 39g of carbon black;
(4) putting the mixed raw materials into a ball milling tank of a ball mill, adding stainless steel or tungsten carbide grinding balls with the diameter of 12mm, wherein the ball-material ratio of the grinding balls to the mixed raw materials is 15:1, and performing inert gas protection or vacuum pumping treatment on the ball milling tank;
(5) after the ball milling tank is placed in a hearth of a ball mill, the mixed raw materials are ball milled by setting the rotating speed of the ball mill to 450 rpm; in the ball milling process, heating the hearth to 850 ℃ at the heating rate of 4 ℃/min, and then preserving the heat of the hearth for 70 h;
(6) and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the ultrafine tungsten carbide powder with uniform granularity.
Example 2
A method for preparing superfine tungsten carbide powder by a mechanochemical method comprises the following steps:
(1) preparing 120g of sodium tungstate crystal into 0.36mol/L sodium tungstate aqueous solution, heating 500ml of sodium tungstate aqueous solution to 80 ℃, dropwise adding 50ml of 12mol/L concentrated hydrochloric acid while stirring to enable the pH value of the mixed solution to be 1, stopping dropwise adding concentrated hydrochloric acid into the sodium tungstate aqueous solution, and stirring for 1.5 hours to obtain tungstic acid colloid;
(2) drying tungstic acid colloid, placing the tungstic acid colloid in a resistance furnace, heating to 600 ℃, calcining, and keeping the temperature for 2 hours to prepare superfine tungsten trioxide powder with the average particle size of 0.205 mu m;
(3) preparing a mixed raw material by mixing 80g of tungsten trioxide powder and 42g of carbon black;
(4) putting the mixed raw materials into a ball milling tank of a ball mill, adding stainless steel or tungsten carbide grinding balls with the diameter of 12mm, wherein the ball-material ratio of the grinding balls to the mixed raw materials is 25:1, and performing inert gas protection or vacuum pumping treatment on the ball milling tank;
(5) after the ball milling tank is placed in a hearth of a ball mill, the mixed raw materials are ball milled by setting the rotating speed of the ball mill to 480 rpm; in the ball milling process, heating the hearth to 900 ℃ at the heating rate of 5 ℃/min, and then preserving the heat of the hearth for 80 h;
(6) and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the ultrafine tungsten carbide powder with uniform granularity.
Example 3
A method for preparing superfine tungsten carbide powder by a mechanochemical method comprises the following steps:
(1) preparing 120g of sodium tungstate crystal into 0.36mol/L sodium tungstate aqueous solution, heating 500ml of sodium tungstate aqueous solution to 80 ℃, dropwise adding 50ml of 12mol/L concentrated hydrochloric acid while stirring to enable the pH value of the mixed solution to be 1, stopping dropwise adding concentrated hydrochloric acid into the sodium tungstate aqueous solution, and stirring for 1.5 hours to obtain tungstic acid colloid;
(2) drying the tungstic acid colloid, placing the tungstic acid colloid in a resistance furnace, heating to 600 ℃, calcining, and keeping the temperature for 2 hours to prepare superfine tungsten trioxide powder with the average particle size of 0.186 mu m;
(3) preparing a mixed raw material by mixing 80g of tungsten trioxide powder and 48g of carbon black;
(4) putting the mixed raw materials into a ball milling tank of a ball mill, adding stainless steel or tungsten carbide grinding balls with the diameter of 12mm, wherein the ball-material ratio of the grinding balls to the mixed raw materials is 30:1, and performing inert gas protection or vacuum pumping treatment on the ball milling tank;
(5) after the ball milling tank is placed in a hearth of a ball mill, the mixed raw materials are ball milled by setting the rotating speed of the ball mill to be 500 rpm; in the ball milling process, heating the hearth to 950 ℃ at the heating rate of 6 ℃/min, and then preserving the heat of the hearth for 90 hours;
(6) and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the ultrafine tungsten carbide powder with uniform granularity.
When the ultrafine tungsten carbide powder prepared in example 1 is subjected to XRD detection, laser granulometer detection, and scanning electron microscope analysis, the following conclusions can be drawn:
as shown in fig. 4, the XRD pattern shows sharp peaks of tungsten carbide, which correspond one-to-one to the standard peaks of tungsten carbide, and no excessive impurity peaks, thus indicating that the crystallinity of the tungsten carbide powder is good.
As shown in fig. 5, the volume of the product powder with a particle size of 0.2 μm is at most, approximately 20%, which can be analyzed by a spectrum of the particle size detected by a laser particle sizer, indicating that the particle size of the tungsten carbide powder is small.
As shown in fig. 6, by analyzing the scanning electron micrograph of the tungsten carbide powder, it can be observed that the powder is uniform, free from agglomeration, and granular.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (8)
1. A method for preparing superfine tungsten carbide powder by a mechanochemical method is characterized by comprising the following steps:
the method comprises the following steps of mixing tungsten trioxide powder and carbon black in a mass ratio of 1: 3-5, mixing to prepare a mixed raw material;
putting the mixed raw materials into a ball milling tank of a ball mill, adding grinding balls, and then performing inert gas protection or vacuum pumping treatment on the ball milling tank;
placing the ball milling tank into a hearth of the ball mill, and then carrying out ball milling on the mixed raw materials through the ball mill; in the ball milling process, after the temperature of the hearth is raised to 850-950 ℃, the hearth is kept warm for 70-90 h;
and closing the ball mill, cooling the hearth to room temperature, and taking out the ball milling tank to obtain the ultrafine tungsten carbide powder with uniform granularity.
2. The mechanochemical method for preparing ultrafine tungsten carbide powder according to claim 1, wherein the method for preparing tungsten trioxide powder comprises:
dropwise adding concentrated hydrochloric acid into a sodium tungstate solution in a stirring state to prepare tungstic acid colloid;
and drying the tungstic acid colloid, and calcining to obtain the tungsten trioxide powder.
3. The mechanochemical method for producing ultrafine tungsten carbide powder according to claim 2, wherein, in the production of the tungstic acid colloid by dropping concentrated hydrochloric acid into a sodium tungstate solution under stirring, the sodium tungstate solution used is an aqueous sodium tungstate solution in which sodium tungstate crystals are arranged at a concentration of 0.36 mol/L.
4. The mechanochemical method for producing ultrafine tungsten carbide powder according to claim 3 wherein, in the production of the tungstic acid colloid by dropping concentrated hydrochloric acid into the sodium tungstate solution under stirring, the concentration of the dropped concentrated hydrochloric acid is 12 mol/L.
5. The mechanochemical method for producing ultrafine tungsten carbide powder according to claim 4 wherein, in the production of a tungstic acid colloid by dropping concentrated hydrochloric acid into a sodium tungstate solution under stirring, dropping of concentrated hydrochloric acid into the sodium tungstate solution at a temperature of 80 ℃ is stopped after the pH of the mixed solution is set to 1.
6. The mechanochemical method for preparing ultrafine tungsten carbide powder according to claim 1, wherein the ball-to-material ratio of the grinding balls to the mixed raw material is 15-30: 1 when the mixed raw material and the grinding balls are loaded into the ball mill pot, wherein the grinding balls are stainless steel or tungsten carbide grinding balls with a diameter of 12 mm.
7. The mechanochemical method for preparing ultrafine tungsten carbide powder according to claim 1, wherein the rotation speed of the motor of the ball mill is 450 to 500rpm when the mixed raw materials are ball-milled by the ball mill.
8. The mechanochemical method for preparing ultrafine tungsten carbide powder according to any one of claims 1 to 7, wherein the heating rate of the hearth is 4-6 ℃/min during the heating of the hearth to 850-950 ℃.
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| CN110980735A (en) * | 2019-12-04 | 2020-04-10 | 北京科技大学 | Short flow path, low cost micron WO3Method for preparing high-performance nano WC powder |
| CN112226760B (en) * | 2020-10-14 | 2023-02-21 | 西安特种设备检验检测院 | Preparation method of wear-resistant coating of traction sheave of high-speed elevator |
| CN113816380B (en) * | 2021-10-19 | 2023-03-24 | 赣州有色冶金研究所有限公司 | Method for preparing ultrafine tungsten carbide powder by one-step carbonization of tungsten oxide |
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| CN101985356A (en) * | 2010-12-10 | 2011-03-16 | 中国科学院上海硅酸盐研究所 | Method for preparing tungsten carbide nano-powder |
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| KR20150000631A (en) * | 2013-06-25 | 2015-01-05 | 서울대학교산학협력단 | METHOD FOR PREPARING PLATELET WC POWDER AND WC-Co CEMENTED CARBIDE CONTAINING PLATELET WC |
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