CN113880583A - Preparation method of high-performance zirconium boride-silicon carbide composite ceramic electrode - Google Patents
Preparation method of high-performance zirconium boride-silicon carbide composite ceramic electrode Download PDFInfo
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 40
- 239000000919 ceramic Substances 0.000 title claims abstract description 36
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title description 7
- 239000000843 powder Substances 0.000 claims abstract description 65
- 238000000498 ball milling Methods 0.000 claims abstract description 40
- 238000000227 grinding Methods 0.000 claims abstract description 34
- 239000000203 mixture Substances 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000005303 weighing Methods 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 230000001965 increasing effect Effects 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 9
- 239000004014 plasticizer Substances 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 230000007613 environmental effect Effects 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000002490 spark plasma sintering Methods 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 8
- 241001391944 Commicarpus scandens Species 0.000 abstract description 4
- 239000011215 ultra-high-temperature ceramic Substances 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 description 11
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910007948 ZrB2 Inorganic materials 0.000 description 3
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000011819 refractory material Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- -1 metalloid structure compound Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of ultra-high temperature ceramic materials, and particularly relates to a preparation method of a high-performance zirconium boride-silicon carbide complex phase ceramic electrode, which comprises the following specific steps: taking materials: weighing silicon carbide powder and zirconium boride powder in certain weight, pouring the two kinds of powder into a grinding device, continuously grinding the two kinds of powder by using the grinding device, fully stirring the powder for 8-10 minutes by using a stirring device after the powder is completely ground, adding excessive ethanol solution into the powder until the powder is completely mixed, and continuously and fully stirring the powder for 5-7 minutes; constant temperature ball milling: pouring the two mixtures into a grinding device, keeping the temperature at 30-40 ℃, continuously ball-milling the mixture at constant temperature for 2-4 hours, and after ball-milling at constant temperature, effectively improving the toughness of the produced zirconium boride-silicon carbide complex phase ceramic electrode, and being not easy to break in the later use process, thereby improving the quality of the ceramic electrode.
Description
Technical Field
The invention relates to the technical field of ultra-high temperature ceramic materials, in particular to a preparation method of a high-performance zirconium boride-silicon carbide complex phase ceramic electrode.
Background
The ZrB2-SiC composite material has the characteristics of melting point, good electrical conductivity, good neutron control capability and the like, and is generally used in various fields such as high-temperature structural ceramic materials, refractory materials, electrode materials, aerospace and the like. Particularly, the demand of ZrB2-SiC is more urgent due to the high-speed development of the existing rocket and missile technologies, the performance requirements of the fields on ZrB2-SiC composite materials are high, and the ultrahigh-temperature ceramic material is a special ceramic material capable of keeping physical and chemical stability in a high-temperature environment and a reaction atmosphere. Such materials include mainly transition metal borides, carbides and nitrides, all with melting points in excess of 3000 ℃. The transition metal boride is a most advantageous high-temperature structural ceramic material by virtue of high melting point, high thermal conductivity, high electrical conductivity, good chemical stability and thermal shock resistance, and has wide application prospects in extreme environments such as hypersonic flight, atmosphere reentry, cross-atmosphere flight, rocket propulsion systems and the like.
However, the existing preparation method of the zirconium boride-silicon carbide complex phase ceramic electrode is relatively backward, and the prepared zirconium boride-silicon carbide complex phase ceramic electrode has relatively poor toughness, so that the zirconium boride-silicon carbide complex phase ceramic electrode is easy to break in the later use process, thereby influencing the use.
Disclosure of Invention
The invention aims to provide a preparation method of a high-performance zirconium boride-silicon carbide complex phase ceramic electrode, and aims to solve the problem that the zirconium boride-silicon carbide complex phase ceramic electrode prepared by the existing preparation method in the background technology has poor toughness, so that the zirconium boride-silicon carbide complex phase ceramic electrode is easy to break in the later use process, and the use is influenced.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a high-performance zirconium boride-silicon carbide complex phase ceramic electrode comprises the following specific steps of:
taking materials: weighing silicon carbide powder and zirconium boride powder in certain weight, pouring the two kinds of powder into a grinding device, continuously grinding the two kinds of powder by using the grinding device, fully stirring the powder for 8-10 minutes by using a stirring device after the powder is completely ground, adding excessive ethanol solution into the powder until the powder is completely mixed, and continuously and fully stirring the powder for 5-7 minutes;
constant temperature ball milling: pouring the two mixtures into a grinding device, keeping the temperature at 30-40 ℃, carrying out continuous constant-temperature ball milling on the mixture for 2-4 hours, and after the ball milling at the constant temperature, placing the mixture at the rotating speed of 30-60r/min and continuously drying the mixture for 30-40 minutes;
spark plasma sintering: and (2) putting the powder obtained in the step into a graphite die, placing the graphite die in a vacuum environment, uniformly pressurizing to perform discharge plasma sintering, stably and uniformly increasing the environmental pressure to 30-40 MPa in the process of increasing the temperature from room temperature to 1600-1700℃, then keeping the temperature for 8-10min under the conditions of 1700 ℃ and 40MPa, and then cutting off the power and naturally cooling to the room temperature to obtain the high-performance zirconium boride-silicon carbide complex phase ceramic electrode.
Preferably, in the material taking and constant-temperature ball milling steps, all grinding devices required are agate ball milling tanks.
Preferably, in the constant-temperature ball milling step, the ball milling method is wet planetary ball milling.
Preferably, in the step of constant-temperature ball milling, a binder and a plasticizer are required to be added, the ratio of the binder to the plasticizer is 1: 2, the binder is polyvinyl butyral, and the plasticizer is polyethylene glycol.
Preferably, in the material taking step, the particles obtained by grinding the silicon carbide powder and the zirconium boride powder need to be sieved by a 200-mesh sieve.
Compared with the prior art, the invention has the beneficial effects that:
through the common cooperation of material taking, constant-temperature ball milling and discharge plasma sintering, the toughness of the produced zirconium boride-silicon carbide complex phase ceramic electrode is effectively improved, and the zirconium boride-silicon carbide complex phase ceramic electrode is not easy to break in the later use process, so that the quality of the ceramic electrode is improved.
Drawings
FIG. 1 is a flow chart of the steps of the preparation method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a high-performance zirconium boride-silicon carbide complex phase ceramic electrode comprises the following specific steps of:
taking materials: weighing silicon carbide powder and zirconium boride powder in certain weight, pouring the two kinds of powder into a grinding device, continuously grinding the two kinds of powder by using the grinding device, fully stirring the powder for 8-10 minutes by using a stirring device after the powder is completely ground, adding excessive ethanol solution into the powder until the powder is completely mixed, and continuously and fully stirring the powder for 5-7 minutes;
constant temperature ball milling: pouring the two mixtures into a grinding device, keeping the temperature at 30-40 ℃, carrying out continuous constant-temperature ball milling on the mixture for 2-4 hours, and after the ball milling at the constant temperature, placing the mixture at the rotating speed of 30-60r/min and continuously drying the mixture for 30-40 minutes;
spark plasma sintering: and (2) putting the powder obtained in the step into a graphite die, placing the graphite die in a vacuum environment, uniformly pressurizing to perform discharge plasma sintering, stably and uniformly increasing the environmental pressure to 30-40 MPa in the process of increasing the temperature from room temperature to 1600-1700℃, then keeping the temperature for 8-10min under the conditions of 1700 ℃ and 40MPa, and then cutting off the power and naturally cooling to the room temperature to obtain the high-performance zirconium boride-silicon carbide complex phase ceramic electrode.
In the material taking and constant-temperature ball milling steps, the grinding devices required to be used are agate ball milling tanks.
In the step of constant temperature ball milling, the ball milling method is wet planetary ball milling.
In the step of constant-temperature ball milling, a binder and a plasticizer are required to be added, the ratio of the binder to the plasticizer is 1: 2, the binder adopts polyvinyl butyral, and the plasticizer adopts polyethylene glycol.
In the material taking step, the particles obtained by grinding the silicon carbide powder and the zirconium boride powder need to be sieved by a 200-mesh sieve.
ZrB2 is a hexagonal C32 metalloid structure compound, has high melting point, high hardness, high stability, and good electrical conductivity, thermal conductivity and chemical corrosion resistance, so that the ZrB2 has a great development prospect in the industries of refractory materials, nozzles, cutting tools and bearings, and ZrB2 has good neutron control capability and can be used in the nuclear industry.
SiC can form different crystal structures under different physical and chemical environments, the crystals with the same components, different shapes, different structures and different physical characteristics are called homogeneous multi-image variants, the toughening application of SiC in engineering mainly comprises SiCp and SiCw, the SiCp toughening ceramic composite base material belongs to a dispersed particle reinforced composite material, the composite material is isotropic, and the preparation and processing method is simple; the SiCp toughening mechanism comprises residual stress field toughening, microcrack toughening, crack deflection, crack bifurcation, crack bridging, crack pinning and the like; the toughening mechanism of SiCp is mainly that an inner crystal structure is formed in the composite material, the grain refinement of nano composite ceramic with the inner crystal structure generates a secondary crystal boundary at the same time, so that the number of the crystal boundaries is greatly increased, the strength and the toughness of the material are also greatly improved, some ceramics even show super toughness, and the nano composite ceramic material with the inner crystal structure is mainly used for enhancing the ceramic material through the following effects: firstly, the introduction of disperse phase effectively inhibits the growth of matrix grains and lightens the abnormal growth of the grains; local stress exists around the dispersed phase or the dispersed phase, the stress is generated by thermal expansion mismatch between the matrix and the dispersed phase, dislocation is generated in the cooling stage, and nano particles are pinned or enter a dislocation region to generate a latent crystal boundary in basic crystal grains, so that the crystal grains are refined to weaken the action of the main crystal boundary; inducing transgranular fracture by local tensile stress around the nano particles, and toughening the hard particles due to the reflection effect of the hard particles on the crack tips; fourthly, the dislocation motion is controlled by the nano particles at high temperature, so that the high-temperature mechanical properties such as hardness, strength and creep resistance are improved.
Example 1:
the preparation method of the high-performance zirconium boride-silicon carbide complex phase ceramic electrode comprises the following specific steps of:
taking materials: weighing silicon carbide powder and zirconium boride powder in certain weight, pouring the two kinds of powder into a grinding device, continuously grinding the two kinds of powder by using the grinding device, fully stirring the powder for 8 minutes by using a stirring device after the powder is completely ground, adding excessive ethanol solution into the powder after the powder is completely mixed, and continuously and fully stirring the powder for 5 minutes;
constant temperature ball milling: pouring the two mixtures into a grinding device, keeping the temperature at 30 ℃, carrying out continuous constant-temperature ball milling on the mixture for 2 hours, and after carrying out constant-temperature ball milling, placing the mixture at a rotating speed of 30-60r/min and continuously drying the mixture for 30 minutes;
spark plasma sintering: putting the powder obtained in the step into a graphite die, placing the graphite die in a vacuum environment, uniformly pressurizing to perform discharge plasma sintering, wherein during sintering, in the process of rising from room temperature to 1600 ℃, the environmental pressure is stably and uniformly increased to 30MPa, then, the temperature is kept for 8min under the conditions that the temperature is 1700 ℃ and the pressure is 40MPa, and then, the power is cut off and the ceramic electrode is naturally cooled to the room temperature to obtain the high-performance zirconium boride-silicon carbide complex phase ceramic electrode;
example 2:
the preparation method of the high-performance zirconium boride-silicon carbide complex phase ceramic electrode comprises the following specific steps of:
taking materials: weighing silicon carbide powder and zirconium boride powder in certain weight, pouring the two kinds of powder into a grinding device, continuously grinding the two kinds of powder by using the grinding device, fully stirring the powder for 9 minutes by using a stirring device after the powder is completely ground, adding excessive ethanol solution into the powder after the powder is completely mixed, and continuously and fully stirring the powder for 6 minutes;
constant temperature ball milling: pouring the two mixtures into a grinding device, keeping the temperature at 35 ℃, carrying out continuous constant-temperature ball milling on the mixture for 3 hours, and after carrying out constant-temperature ball milling, placing the mixture at a rotating speed of 45r/min and continuously drying the mixture for 35 minutes;
spark plasma sintering: putting the powder obtained in the step into a graphite die, placing the graphite die in a vacuum environment, uniformly pressurizing to perform discharge plasma sintering, stably and uniformly increasing the environmental pressure to 35MPa in the process of increasing the room temperature to 1650 ℃, then keeping the temperature for 9min under the conditions that the temperature is 1700 ℃ and the pressure is 40MPa, and then naturally cooling to the room temperature after power failure to obtain the high-performance zirconium boride-silicon carbide complex phase ceramic electrode;
example 3:
the preparation method of the high-performance zirconium boride-silicon carbide complex phase ceramic electrode comprises the following specific steps of:
taking materials: weighing silicon carbide powder and zirconium boride powder in certain weight, pouring the two kinds of powder into a grinding device, continuously grinding the two kinds of powder by using the grinding device, fully stirring the powder for 10 minutes by using a stirring device after the powder is completely ground, adding excessive ethanol solution into the powder after the powder is completely mixed, and continuously fully stirring the powder for 7 minutes;
constant temperature ball milling: pouring the two mixtures into a grinding device, keeping the temperature at 40 ℃, carrying out continuous constant-temperature ball milling on the mixture for 4 hours, and after carrying out constant-temperature ball milling, placing the mixture at a rotating speed of 30-60r/min and continuously drying the mixture for 40 minutes;
spark plasma sintering: and (2) putting the powder obtained in the step into a graphite die, placing the graphite die in a vacuum environment, uniformly pressurizing to perform discharge plasma sintering, stably and uniformly increasing the environmental pressure to 40MPa in the process of increasing the temperature from room temperature to 1700 ℃, then preserving the temperature for 10min under the conditions of 1700 ℃ and 40MPa, and then powering off and naturally cooling to room temperature to obtain the high-performance zirconium boride-silicon carbide complex phase ceramic electrode.
While there have been shown and described the fundamental principles and essential features of the invention and advantages thereof, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof; the present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A preparation method of a high-performance zirconium boride-silicon carbide complex phase ceramic electrode is characterized by comprising the following steps: the preparation method of the high-performance zirconium boride-silicon carbide complex phase ceramic electrode comprises the following specific steps of:
taking materials: weighing silicon carbide powder and zirconium boride powder in certain weight, pouring the two kinds of powder into a grinding device, continuously grinding the two kinds of powder by using the grinding device, fully stirring the powder for 8-10 minutes by using a stirring device after the powder is completely ground, adding excessive ethanol solution into the powder until the powder is completely mixed, and continuously and fully stirring the powder for 5-7 minutes;
constant temperature ball milling: pouring the two mixtures into a grinding device, keeping the temperature at 30-40 ℃, carrying out continuous constant-temperature ball milling on the mixture for 2-4 hours, and after the ball milling at the constant temperature, placing the mixture at the rotating speed of 30-60r/min and continuously drying the mixture for 30-40 minutes;
spark plasma sintering: and (2) putting the powder obtained in the step into a graphite die, placing the graphite die in a vacuum environment, uniformly pressurizing to perform discharge plasma sintering, stably and uniformly increasing the environmental pressure to 30-40 MPa in the process of increasing the temperature from room temperature to 1600-1700℃, then keeping the temperature for 8-10min under the conditions of 1700 ℃ and 40MPa, and then cutting off the power and naturally cooling to the room temperature to obtain the high-performance zirconium boride-silicon carbide complex phase ceramic electrode.
2. The preparation method of the high-performance zirconium boride-silicon carbide complex phase ceramic electrode according to claim 1, characterized in that: in the material taking and constant-temperature ball milling steps, the grinding devices required to be used are agate ball milling tanks.
3. The preparation method of the high-performance zirconium boride-silicon carbide complex phase ceramic electrode according to claim 1, characterized in that: in the step of constant temperature ball milling, the ball milling method is wet planetary ball milling.
4. The preparation method of the high-performance zirconium boride-silicon carbide complex phase ceramic electrode according to claim 1, characterized in that: in the step of constant-temperature ball milling, a binder and a plasticizer are required to be added, the ratio of the binder to the plasticizer is 1: 2, the binder adopts polyvinyl butyral, and the plasticizer adopts polyethylene glycol.
5. The preparation method of the high-performance zirconium boride-silicon carbide complex phase ceramic electrode according to claim 1, characterized in that: in the material taking step, the particles obtained by grinding the silicon carbide powder and the zirconium boride powder need to be sieved by a 200-mesh sieve.
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