CN113429208A - Rapid preparation method of pure tungsten carbide - Google Patents
Rapid preparation method of pure tungsten carbide Download PDFInfo
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- CN113429208A CN113429208A CN202110657388.2A CN202110657388A CN113429208A CN 113429208 A CN113429208 A CN 113429208A CN 202110657388 A CN202110657388 A CN 202110657388A CN 113429208 A CN113429208 A CN 113429208A
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Abstract
本发明公开了一种纯碳化钨的快速制备方法，包括步骤：(1)将碳化钨粉末填入模具，在绝对真空的环境下装炉烧结；(2)预设段：压力为50‑65Mpa、时间为10‑60秒；(3)初步升温段：在速度110‑130℃/min下升温，至塑化状态；(4)二次升温段：在压力80‑100Mpa、升温速度60‑85℃/min下，温度升温至1850‑1950℃；(5)保持段：在压力120Mpa下，保压10‑25min；(6)冷却段：冷却2‑4小时。实现快速成型、烧结，制得致密性好、硬度高、强度高、更贴合理论值的碳化钨。The invention discloses a rapid preparation method of pure tungsten carbide, comprising the steps of: (1) filling tungsten carbide powder into a mold, and sintering in a furnace under an absolute vacuum environment; (2) preset section: the pressure is 50-65Mpa , the time is 10-60 seconds; (3) Preliminary heating section: heating at a speed of 110-130 ℃/min, to a plasticized state; (4) Secondary heating section: at a pressure of 80-100Mpa and a heating rate of 60-85 Under ℃/min, the temperature is raised to 1850-1950 ℃; (5) Hold section: under pressure of 120Mpa, maintain pressure for 10-25min; (6) Cooling section: cool for 2-4 hours. Realize rapid prototyping and sintering, and obtain tungsten carbide with good compactness, high hardness, high strength, and more in line with the theoretical value.
Description
Technical Field
The invention relates to the technical field of workpiece forming, in particular to a rapid preparation method of pure tungsten carbide.
Background
Tungsten carbide is a compound consisting of tungsten and carbon, has stable chemical properties, hardness similar to that of diamond, is a good conductor of electricity and heat, is classified in the category of hard alloy, has the density as high as 15.63 and the melting point as high as 2870 ℃, and belongs to the category of extremely difficult processing.
However, the process for preparing tungsten carbide in the prior art is immature, and the quality of the produced tungsten carbide still has certain difference from a theoretical value.
On the basis of the above, manufacturers also add other metals to improve the quality of tungsten carbide, for example, add titanium, cobalt, titanium carbide, tantalum carbide to improve the brittleness and the anti-explosion capability of tungsten carbide alloy.
Pure tungsten carbide belongs to cermet which is extremely difficult to form in actual production, a good tungsten carbide product cannot be prepared by the traditional process, the isostatic pressing process is very high in cost, and the pure tungsten carbide product is expensive and limited in size, so that the application cannot be popularized, and batch production cannot be realized.
Disclosure of Invention
The invention provides a rapid preparation method of pure tungsten carbide, which realizes rapid molding and sintering and prepares tungsten carbide with good compactness, high hardness, high strength and more fit with theoretical value.
The invention provides a rapid preparation method of pure tungsten carbide, which comprises the following steps:
(1) filling tungsten carbide powder into a mould, charging and sintering, and performing absolute vacuum environment;
(2) a preset section: the pressure is 50-65Mpa, and the time is 10-60 seconds;
(3) the initial temperature rise section: heating at a speed of 110-;
(4) a secondary temperature rising section: heating to 1850 ℃ and 1950 ℃ under the pressure of 80-100Mpa and the heating speed of 60-85 ℃/min;
(5) a holding section: maintaining the pressure at 120Mpa for 10-25 min;
(6) a cooling section: cooling for 2-4 hours.
Preferably, the step (4) is specifically:
a secondary temperature rising section:
heating to 1850 ℃ and 1950 ℃ at the pressure of 80-100Mpa and the heating speed of 78-85 ℃/min;
continuously observing the plasticizing state of the tungsten carbide in the temperature rising process;
when the plasticizing is finished, entering the step (5);
when the tungsten carbide is not plasticized completely, adjusting the pressure to 120Mpa, and entering the step (5) if the tungsten carbide is plasticized completely; if the plasticization is not finished, adjusting the heating speed to 60 ℃/min, heating to the maximum 1950 ℃, and entering the step (5).
Preferably, the pressure increase of step (4) is increased by 5Mpa at a time.
Preferably, the dwell time of step (5) is the weight-to-time ratio of the tungsten carbide powder: 10-15kg of tungsten carbide powder: for 10 min.
Preferably, the tungsten carbide powder has a particle size of 20-400 mesh.
Preferably, the production time of the steps (1) to (5) is 1.5 to 2.5 hours.
Preferably, the requirement of filling the tungsten carbide powder into the die in the step (1) is uniform powder filling.
Preferably, the charging sintering in the charging of the step (1) is to keep the balance and consistency of the upper and lower pressing heads of the die.
Compared with the prior art, the invention has the beneficial effects that: the preparation method is simple, the tungsten carbide is prepared from the preset section, the temperature rising section, the maintaining section and the cooling section in an absolute vacuum environment, the generated tungsten carbide has good compactness, high hardness and high strength, and the whole preparation process has high efficiency and low cost.
Tungsten carbide can be rapidly molded in place under the high-pressure condition, is completely compact, and has lower and more uniform temperature compared with the common process in the absolute vacuum state and different heating modes, so that the tungsten carbide has short sintering time and high continuity, the process efficiency is promoted, and the prepared product has better performance and more uniform material.
Detailed Description
The following examples further describe embodiments of the present invention in detail. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The tungsten carbide has stable chemical property and hardness similar to that of diamond, belongs to hard alloy, and is wear-resistant and high in hardness. Pure tungsten carbide is applied more and more in the market, and products comprise tungsten carbide water jet and tungsten carbide nozzles. Density value of common tungsten carbide: 15.63g/cm3。
The invention discloses a rapid preparation method of pure tungsten carbide, which comprises the following steps:
(1) filling tungsten carbide powder into a mould, and loading and sintering in a furnace in an absolute vacuum environment;
(2) a preset section: the pressure is 50-65Mpa, and the time is 10-60 seconds;
(3) the initial temperature rise section: heating at a speed of 110-;
(4) a secondary temperature rising section: heating to 1850 ℃ and 1950 ℃ under the pressure of 80-100Mpa and the heating speed of 60-85 ℃/min;
(5) a holding section: maintaining the pressure at 120Mpa for 10-25 min;
(6) a cooling section: cooling for 2-4 hours.
Preferably, the step (4) is specifically:
a secondary temperature rising section:
heating to 1850 ℃ and 1950 ℃ at the pressure of 80-100Mpa and the heating speed of 78-85 ℃/min;
continuously observing the plasticizing state of the tungsten carbide in the temperature rising process;
when the plasticizing is finished, entering the step (5);
when the tungsten carbide is not plasticized completely, adjusting the pressure to 120Mpa, and entering the step (5) if the tungsten carbide is plasticized completely; if the plasticization is not finished, adjusting the heating speed to 60 ℃/min, heating to the maximum 1950 ℃, and entering the step (5).
The plasticizing completion means that the tungsten carbide powder achieves a plasticizing effect of 20-60%, preferably 50-60%, which is judged by those skilled in the art.
Under the treatment of the primary heating section and the secondary heating section, the tungsten carbide powder can quickly reach 20-60% plasticizing conditions, and can be quickly molded in place under the pressure of 80-100Mpa, and is completely compact.
Preferably, the pressure increase of step (4) is increased by 5Mpa at a time.
Preferably, the dwell time of step (5) is the weight-to-time ratio of the tungsten carbide powder: 10-15kg of tungsten carbide powder: for 10 min.
Preferably, the tungsten carbide powder has a particle size of 20-400 mesh.
Preferably, the production time of the steps (1) to (5) is 1.5 to 2.5 hours.
Preferably, the requirement of filling the tungsten carbide powder into the die in the step (1) is uniform powder filling.
The preparation method can be used on an alternating-current high-power vacuum hot-pressing sintering furnace.
The term "absolute vacuum" as used herein means the use on the sintering furnace.
The preparation method controls the heating speed with the large pressure approximate to isostatic pressure, reduces the vacuum sintering time, reduces the production time, and makes the material more uniform in a special heating mode.
The process has short production time and can be quickly molded, and the sintering time is short, so that the process is suitable for split sintering of various particle sizes, crystal grains are not easy to grow, the product strength caused by uneven crystal grains is avoided, the product can be quickly molded under high pressure, and the temperature is more uniform.
The process is produced in a vacuum state, can effectively reduce the sintering temperature, can also solve the problem of residual gas (such as closed pores) in tungsten carbide, thoroughly solves the problem under the coordination of high pressure, vacuum and high temperature, can also prevent the oxidation problem of a mold, and can also ensure that heat is uniform, so that the combination density and the efficiency among crystal grains in the product are greatly improved.
The process is different from the traditional tungsten carbide preparation process, firstly, tungsten carbide powder is filled into a die and is required to be uniformly distributed, and the tungsten carbide powder is loaded and sintered to keep the balance of an upper pressure head and a lower pressure head of the loaded tungsten carbide powder.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The rapid preparation method of pure tungsten carbide comprises the following steps:
(1) filling tungsten carbide powder into a die, wherein the powder is required to be uniformly filled, and loading and sintering are carried out in an absolute vacuum environment, wherein the loading is required to keep the balance and consistency of an upper pressure head and a lower pressure head of the die;
(2) a preset section: the pressure is 50-65Mpa, and the time is 10-60 seconds;
(3) the initial temperature rise section: heating at a speed of 110-;
(4) a secondary temperature rising section:
heating to 1850 ℃ and 1950 ℃ at the pressure of 80-100Mpa and the heating speed of 78-85 ℃/min;
continuously observing the plasticizing state of the tungsten carbide in the temperature rising process;
when the plasticizing is finished, entering the step (5);
when the tungsten carbide is not plasticized completely, adjusting the pressure to 120Mpa, and entering the step (5) if the tungsten carbide is plasticized completely; if the plasticization is not finished, adjusting the heating speed to 60 ℃/min, heating to the maximum 1950 ℃, and entering the step (5);
wherein the pressure is increased by 5MPa each time;
(5) a holding section: maintaining the pressure at 120Mpa for 10-25 min;
wherein the dwell time is the weight-to-time ratio of the tungsten carbide powder: 10-15kg of tungsten carbide powder: 10 min;
(6) a cooling section: cooling for 2-4 hours.
The production time of steps (1) to (6) is 1.5 to 2.5 hours.
The invention is illustrated by the following specific examples:
example 1
The preparation method of the pure tungsten carbide comprises the following steps:
(1) taking 13kg of tungsten carbide powder with the same granularity, filling the tungsten carbide powder into a mould according to the principle of uniform distribution, and charging and sintering the tungsten carbide powder in an absolute vacuum environment;
(2) in the early preset stage: setting the pressure at 60MPa and maintaining pressure (i.e. prepressing) for 50 seconds;
a temperature rising section:
(3) the initial temperature rise section: heating at a speed of 120 ℃/min until the tungsten carbide begins to generate a plasticizing state;
(4) a secondary temperature rising section: raising the pressure to 90Mpa at a pressure raising rate of 5Mpa each time and at a temperature raising speed of 80 ℃/min, and raising the temperature to the maximum 1950 ℃;
during the temperature rise process, the plasticizing state of the tungsten carbide is continuously observed;
when the plasticizing is finished, entering the step (5);
when the plasticization is not finished, adjusting the pressure to 120Mpa, observing the plasticization condition of the tungsten carbide, and entering the step (5) if the plasticization is finished; if the plasticization is not finished, the temperature rising speed is adjusted to 60 ℃/min, the temperature is slowly raised to the maximum 1950 ℃, and the step (5) is carried out.
(5) A holding section: maintaining the pressure at 120MPa for 10 min;
the time from the step (1) to the step (5) is not more than 2.5 hours.
(6) A cooling section: cooling for 2-4 hours.
Obtaining the tungsten carbide.
Example 2
The preparation method of the pure tungsten carbide comprises the following steps:
(1) taking 13kg of tungsten carbide powder with the same granularity, filling the tungsten carbide powder into a mould according to the principle of uniform distribution, and charging and sintering the tungsten carbide powder in an absolute vacuum environment;
(2) in the early preset stage: setting the pressure at 60MPa and maintaining pressure (i.e. prepressing) for 60 seconds;
a temperature rising section:
(3) the initial temperature rise section: heating at a speed of 120 ℃/min until the tungsten carbide begins to generate a plasticizing state;
(4) a secondary temperature rising section: raising the pressure to 100Mpa at a pressure raising rate of 5Mpa each time and at a temperature raising speed of 78 ℃/min, and raising the temperature to 1920 ℃ at most;
during the temperature rise process, the plasticizing state of the tungsten carbide is continuously observed;
when the plasticizing is finished, entering the step (5);
when the plasticization is not finished, adjusting the pressure to 120Mpa, observing the plasticization condition of the tungsten carbide, and entering the step (5) if the plasticization is finished; if the plasticizing is not completed, adjusting the temperature rising speed to 60 ℃/min under the pressure of 120Mpa, slowly raising the temperature to the maximum 1920 ℃, and entering the step (5).
(5) A holding section: maintaining the pressure at 120MPa for 10 min;
the time from the step (1) to the step (5) is not more than 2.5 hours.
(6) A cooling section: cooling for 2-4 hours.
Obtaining the tungsten carbide.
Example 3
The preparation method of the pure tungsten carbide comprises the following steps:
(1) taking 13kg of tungsten carbide powder with the same granularity, filling the tungsten carbide powder into a mould according to the principle of uniform distribution, and charging and sintering the tungsten carbide powder in an absolute vacuum environment;
(2) in the early preset stage: setting the pressure at 60MPa and maintaining pressure (i.e. prepressing) for 30 seconds;
a temperature rising section:
(3) the initial temperature rise section: heating at a speed of 120 ℃/min until the tungsten carbide begins to generate a plasticizing state;
(4) a secondary temperature rising section: raising the pressure to 80Mpa at a pressure raising rate of 5Mpa each time and at a temperature raising speed of 85 ℃/min, and raising the temperature to 1950 ℃ at most;
during the temperature rise process, the plasticizing state of the tungsten carbide is continuously observed;
when the plasticizing is finished, entering the step (5);
when the plasticization is not finished, adjusting the pressure to 120Mpa, observing the plasticization condition of the tungsten carbide, and entering the step (5) if the plasticization is finished; if the plasticization is not finished, the temperature rising speed is adjusted to 60 ℃/min, the temperature is slowly raised to the maximum 1950 ℃, and the step (5) is carried out.
(5) A holding section: maintaining the pressure at 120MPa for 10 min;
the time from the step (1) to the step (5) is not more than 2.5 hours.
(6) A cooling section: cooling for 2-4 hours.
Obtaining the tungsten carbide.
The tungsten carbide obtained in the above examples 1-3 was tested according to GB/T3850-2015, the sample was pure WC alloy, the testing equipment was a German Sartorius BSA224S full-automatic densimeter, and the test results were as follows:
it can be seen that the tungsten carbide products (alloys) of examples 1-3 have a high density.
The embodiments of the present invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiment was chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
Claims (8)
1. A rapid preparation method of pure tungsten carbide is characterized by comprising the following steps:
(1) filling tungsten carbide powder into a mould, and loading and sintering in a furnace in an absolute vacuum environment;
(2) a preset section: the pressure is 50-65Mpa, and the time is 10-60 seconds;
(3) the initial temperature rise section: heating at a speed of 110-;
(4) a secondary temperature rising section: heating to 1850 ℃ and 1950 ℃ under the pressure of 80-100Mpa and the heating speed of 60-85 ℃/min;
(5) a holding section: maintaining the pressure at 120Mpa for 10-25 min;
(6) a cooling section: cooling for 2-4 hours.
2. The rapid preparation method of pure tungsten carbide according to claim 1, wherein the step (4) is specifically:
a secondary temperature rising section:
heating to 1850 ℃ and 1950 ℃ at the pressure of 80-100Mpa and the heating speed of 78-85 ℃/min;
continuously observing the plasticizing state of the tungsten carbide in the temperature rising process;
when the plasticizing is finished, entering the step (5);
when the tungsten carbide is not plasticized completely, adjusting the pressure to 120Mpa, and entering the step (5) if the tungsten carbide is plasticized completely; if the plasticization is not finished, adjusting the heating speed to 60 ℃/min, heating to the maximum 1950 ℃, and entering the step (5).
3. The rapid preparation method of pure tungsten carbide according to claim 1, characterized in that the pressure increase of step (4) is increased by 5Mpa each time.
4. The method for rapidly preparing pure tungsten carbide according to claim 1, wherein the dwell time of the step (5) is that the weight-to-time ratio of the tungsten carbide powder is as follows: 10-15kg of tungsten carbide powder: for 10 min.
5. The method for rapidly preparing pure tungsten carbide according to claim 1, wherein the particle size of the tungsten carbide powder is 20-400 mesh.
6. The method for rapidly preparing pure tungsten carbide according to any one of claims 1 to 5, wherein the production time of the steps (1) to (5) is 1.5 to 2.5 hours.
7. The method for rapidly preparing pure tungsten carbide according to claim 1, wherein the requirement of filling the tungsten carbide powder in the step (1) into the die is uniform powder filling.
8. The rapid preparation method of pure tungsten carbide according to claim 1, wherein the charging sintering in step (1) is performed by maintaining the balance and consistency of the upper and lower pressure heads of the die.
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