CN115196968B - High-entropy boride ceramic powder and preparation method and application thereof - Google Patents
High-entropy boride ceramic powder and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses high-entropy boride ceramic powder and a preparation method and application thereof. The preparation method of the high-entropy boride ceramic powder comprises the following steps: 1) Mixing metal oxide powder and boron powder, and grinding to obtain mixed powder; 2) And adding the mixed powder into a tungsten ark, and then placing the tungsten ark in a protective atmosphere for electric field sintering to obtain the high-entropy boride ceramic powder. The high-entropy boride ceramic powder has the advantages of huge component space, high purity, uniform distribution of metal elements, low oxygen impurity content and the like, and the preparation method has the advantages of simple operation, high temperature rise and fall speed, extremely short reaction time, low equipment requirement, simple process flow, low synthesis cost, no pollution to the environment and the like, and is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of high-entropy ceramic powder materials, in particular to high-entropy boride ceramic powder and a preparation method and application thereof.
Background
High entropy ceramic materials generally refer to single phase solid solutions formed from four or more ceramic components, each component being present in an amount ranging from 5at.% to 35 at.%. The high-entropy ceramic material has a unique microstructure and adjustable and controllable performance, becomes a research hotspot in the field of ceramics in recent years, and the high-entropy ceramic material reported at present mainly comprises high-entropy oxide, high-entropy boride, high-entropy carbide, high-entropy nitride and the like.
The high-entropy boride ceramic is a novel ultrahigh-temperature ceramic material, not only has the properties of extremely high melting point, higher hardness, strength, wear resistance, good high-temperature physical and chemical stability and the like of the traditional boride, but also has the properties of hardness, modulus, high-temperature physical and chemical stability and the like which are greatly improved under the high-entropy action of multiple main elements, so that the high-entropy boride ceramic becomes one of powerful alternative materials in extreme fields of aerospace, national defense and military industry and the like. However, the existing high-entropy boride ceramic material generally has the problems of large grains, low density, non-uniform element distribution, high oxygen impurity content and the like, so that the popularization and application of the material are severely limited, and the synthesis of a high-quality powder raw material is a well-known fundamental way for solving the problems.
At present, the method for synthesizing the high-entropy boride ceramic powder mainly comprises a borothermic reduction method, a carbon/borothermic reduction method, a molten salt synthesis method and the like, and the synthesis methods generally have a series of problems of complex operation, long synthesis period, high energy consumption, large environmental pollution, small synthesized powder component space and the like, and are difficult to meet the requirements of practical application.
Therefore, the development of a rapid preparation method of the high-entropy boride ceramic powder and the preparation of the high-entropy boride ceramic powder with the advantages of large component space, high purity, uniform distribution of metal elements, low content of oxygen impurities and the like have very important significance.
Disclosure of Invention
The invention aims to provide high-entropy boride ceramic powder and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
the preparation method of the high-entropy boride ceramic powder comprises the following steps:
1) Mixing metal oxide powder and boron powder, and grinding to obtain mixed powder; the metal oxide powder is made of HfO 2 Powder, zrO 2 Powder, tiO 2 Powder, ta 2 O 5 Powder and Nb 2 O 5 Powder, cr 2 O 3 Powder, moO 3 Powder of V 2 O 5 Powder and WO 3 At least four components of the powder;
2) And adding the mixed powder into a tungsten ark, and then placing the tungsten ark in a protective atmosphere for electric field sintering to obtain the high-entropy boride ceramic powder.
Preferably, the metal oxide powder in step 1) is made of HfO 2 Powder, zrO 2 Powder, tiO 2 Powder, ta 2 O 5 Powder and Nb 2 O 5 Powder, cr 2 O 3 Powder, moO 3 Powder, V 2 O 5 Powder and WO 3 At least four kinds of the powder are mixed according to the equal molar ratio of metal elements.
Preferably, the ratio of the total mass of metal atoms in the metal oxide powder in step 1) to the mass of boron powder is 1.
Preferably, the HfO of step 1) 2 Powder, zrO 2 Powder, tiO 2 Powder, ta 2 O 5 Powder and Nb 2 O 5 Powder, cr 2 O 3 Powder, moO 3 Powder, V 2 O 5 Powder and WO 3 The particle size of the powder is 1-3 μm, and the purity is more than or equal to 99.9%.
Preferably, the particle size of the boron powder in the step 1) is 10-20 μm, and the purity is more than or equal to 99.0%.
Preferably, the tungsten ark in the step 2) has the size specification of 115 mm-135 mm in length, 15 mm-20 mm in width, 5 mm-15 mm in height and 2 mm-6 mm in thickness (thickness of the bottom surface). The tungsten ark cannot be too large in size, otherwise it is difficult to quickly form a uniform sintering environment of about 3000 ℃.
Preferably, the purity of the tungsten ark in the step 2) is more than or equal to 99.99%.
Preferably, the protective atmosphere in step 2) is an argon atmosphere.
Preferably, the specific operation of the electric field sintering in the step 2) is as follows: and (3) connecting alternating current with the fixed power of 2.0-2.5 kW at two ends of the tungsten square boat, and electrifying for 1-30 s.
A high-entropy boride ceramic powder is prepared by the preparation method.
The preparation raw materials of the high-entropy ceramic comprise the high-entropy boride ceramic powder.
The beneficial effects of the invention are: the high-entropy boride ceramic powder has the advantages of huge component space, high purity, uniform distribution of metal elements, low oxygen impurity content and the like, and the preparation method has the advantages of simple operation, high temperature rise and fall speed, extremely short reaction time, low equipment requirement, simple process flow, low synthesis cost, no pollution to the environment and the like, and is suitable for large-scale industrial production.
Specifically, the method comprises the following steps:
1) The method can prepare the high-entropy boride ceramic powder with any four or more (at most nine) element components in Hf, zr, ti, ta, nb, cr, mo, V and W elements, the element composition of the high-entropy boride ceramic powder can regulate and control the space greatly, the problem that the high-entropy boride ceramic powder with huge component space cannot be prepared by the traditional method is solved (for a high-entropy ceramic material, the more the element components are, the greater the synthesis difficulty is), and the synthesized high-entropy boride ceramic powder has the advantages of high purity, uniform distribution of metal elements, low oxygen impurity content (2.18 wt% -2.30 wt%), and the like;
2) The preparation method of the high-entropy boride ceramic powder has the advantages of simple operation, high temperature rise and drop speed (the temperature can be raised to about 3000 ℃ at the moment of electrifying), extremely short reaction time (1-30 s), low equipment requirement, simple process flow, low synthesis cost, no environmental pollution and the like, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is an XRD pattern of high-entropy boride ceramic powders of examples 1 to 3.
FIG. 2 is an SEM photograph and an EDS elemental surface distribution chart of the high-entropy boride ceramic powder of example 1.
Fig. 3 is an XRD pattern of the high-entropy boride ceramic powders of comparative example 1 and comparative example 2.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
HfO in examples 1 to 3 and comparative examples 1 to 2 2 Powder, zrO 2 Powder, tiO 2 Powder, ta 2 O 5 Powder and Nb 2 O 5 Powder, cr 2 O 3 Powder, moO 3 Powder, V 2 O 5 Powder and WO 3 The particle size of the powder is 1-3 μm, and the purity is more than or equal to 99.9%.
The boron powder in examples 1-3 and comparative examples 1-2 has a particle size of 10-20 μm (which can pass through a 500 mesh sieve), and a purity of not less than 99.0%.
Example 1:
a preparation method of high-entropy boride ceramic powder comprises the following steps:
1) 0.73g of HfO 2 Powder, 0.43g of ZrO 2 Powder, 0.77g of Ta 2 O 5 Powder, 0.46g of Nb 2 O 5 Powder, 0.28g TiO 2 Adding the powder and 0.89g of boron powder into an agate mortar, and manually grinding for 60min to obtain mixed powder;
2) Adding the mixed powder into a tungsten ark, wherein the tungsten ark has the size specification of 115m in lengthm, width 15mm, height 5mm and thickness 2mm, the purity of the tungsten square boat is more than or equal to 99.99%, then the tungsten square boat is placed in a self-made combustion reaction kettle and clamped in the middle of an electrode, firstly, a mechanical pump is used for carrying out vacuum pumping treatment on the combustion reaction kettle to enable the value of a vacuum pressure gauge to reach 10Pa, then, a molecular pump is replaced for continuing vacuum pumping treatment until the vacuum pressure count value reaches 1 multiplied by 10 -4 Pa, introducing argon to normal pressure, pre-adjusting the power of two ends of the electrode to be 2.0kW and keeping the power unchanged, turning on a power switch to supply alternating current to the tungsten ark for 15s, then turning off the switch, and naturally cooling to room temperature to obtain high-entropy boride ceramic powder (five-element high-entropy boride (Hf) 1/5 Zr 1/5 Ta 1/5 Nb 1/5 Ti 1/5 )B 2 And noted as 5 HEB).
And (3) performance testing:
the X-ray diffraction (XRD) pattern, the Scanning Electron Microscope (SEM) pattern and the EDS elemental surface distribution chart of the high-entropy boride ceramic powder (5 HEB) according to this example are shown in fig. 1, and fig. 2.
The test result shows that the high-entropy boride ceramic powder of the embodiment is pure phase, does not contain other impurity phases, has high purity, has the oxygen impurity content of only 2.18wt%, is granular in shape, and has the five components of Hf, zr, ta, nb and Ti which are uniformly distributed.
Example 2:
a preparation method of high-entropy boride ceramic powder comprises the following steps:
1) 0.47g of HfO 2 Powder, 0.28g of ZrO 2 Powder, 0.50g of Ta 2 O 5 Powder, 0.30g of Nb 2 O 5 Powder, 0.18g of TiO 2 Powder, 0.17g of Cr 2 O 3 Powder, 0.32g of MoO 3 Adding the powder and 0.76g of boron powder into an agate mortar, and manually grinding for 60min to obtain mixed powder;
2) Adding the mixed powder into a tungsten square boat, wherein the tungsten square boat has the size specification of 125mm in length, 18mm in width, 10mm in height and 4mm in thickness, the purity of the tungsten square boat is more than or equal to 99.99%, placing the tungsten square boat in a self-made combustion reaction kettle, clamping the tungsten square boat in the middle of an electrode, firstly carrying out vacuum-pumping treatment on the combustion reaction kettle by using a mechanical pump to enable the value of a vacuum pressure gauge to reach 10Pa, then replacing a molecular pump to continue vacuum-pumping treatment until the tungsten square boat is straightUntil the vacuum pressure gauge value reaches 1 × 10 -4 Pa, introducing argon to normal pressure, pre-adjusting the power of two ends of the electrode to be 2.0kW and keeping the power unchanged, turning on a power switch to supply alternating current to the tungsten ark for 30s, then turning off the switch, and naturally cooling to room temperature to obtain the high-entropy boride ceramic powder (seven-element high-entropy boride Hf) 1/7 Zr 1/7 Ta 1/7 Nb 1/7 Ti 1/7 Cr 1/7 Mo 1/7 )B 2 And is noted as 7 HEB).
And (3) performance testing:
the XRD pattern of the high-entropy boride ceramic powder (7 HEB) of this example is shown in FIG. 1.
The test result shows that the high-entropy boride ceramic powder of the embodiment is pure phase, does not contain other impurity phases, has high purity, has the oxygen impurity content of only 2.24wt%, is granular in shape, and is uniformly distributed by seven elements of Hf, zr, ta, nb, ti, cr and Mo.
Example 3:
a preparation method of high-entropy boride ceramic powder comprises the following steps:
1) 0.36g of HfO 2 Powder, 0.21g of ZrO 2 Powder, 0.38g of Ta 2 O 5 Powder, 0.23g of Nb 2 O 5 Powder, 0.14g TiO 2 Powder, 0.13g of Cr 2 O 3 Powder, 0.25g of MoO 3 Powder, 0.16g of V 2 O 5 Powder, 0.40g of WO 3 Adding the powder and 0.77g of boron powder into an agate mortar, and manually grinding for 60min to obtain mixed powder;
2) Adding the mixed powder into a tungsten square boat, wherein the tungsten square boat has the size specification of 135mm in length, 20mm in width, 15mm in height and 6mm in thickness, the purity of the tungsten square boat is more than or equal to 99.99%, placing the tungsten square boat in a self-made combustion reaction kettle, clamping the tungsten square boat in the middle of an electrode, firstly carrying out vacuum-pumping treatment on the combustion reaction kettle by using a mechanical pump to enable the value of a vacuum pressure gauge to reach 10Pa, then replacing a molecular pump to continue vacuum-pumping treatment until the vacuum pressure count value reaches 1 multiplied by 10 -4 Pa, introducing argon to normal pressure, adjusting the power of two ends of the electrode to be 2.5kW in advance, turning on a power switch to supply alternating current to the tungsten ark for 1s, then turning off the switch, naturally cooling to room temperature,obtaining the high-entropy boride ceramic powder (nine-element high-entropy boride (Hf) 1/9 Zr 1/9 Ta 1/9 Nb 1/9 Ti 1/9 Cr 1/9 Mo 1/9 V 1/9 W 1/9 )B 2 And 9 HEB).
And (3) performance testing:
the XRD pattern of the high-entropy boride ceramic powder (9 HEB) of this example is shown in fig. 1.
The test result shows that the high-entropy boride ceramic powder of the embodiment is pure phase, does not contain other impurity phases, has high purity, has the oxygen impurity content of only 2.30wt%, is granular in shape, and has nine elements of Hf, zr, ta, nb, ti, cr, mo, V and W which are uniformly distributed.
Comparative example 1:
a high-entropy boride ceramic powder (7 HEB-1) was prepared in the same manner as in example 2 except that the tungsten ark was replaced with a domestic graphite felt (Tianjin carbon plant, model: SMZ 5 mm) having a size of 125mm in length, 18mm in width and 5mm in thickness.
And (3) performance testing:
the XRD pattern of the high-entropy boride ceramic powder (7 HEB-1) of this comparative example is shown in FIG. 3.
The test result shows that the actual multi-boride solid solution prepared by the comparative example is not single-phase high-entropy boride ceramic powder.
Comparative example 2:
a high-entropy boride ceramic powder (7 HEB-2) was prepared in the same manner as in example 2 except that the tungsten ark was changed to have a length of 200mm, a width of 30mm, a height of 10mm and a thickness of 4 mm.
And (3) performance testing:
the XRD pattern of the high-entropy boride ceramic powder (7 HEB-2) of this comparative example is shown in FIG. 3.
The test result shows that the actual multi-boride solid solution prepared by the comparative example is not single-phase high-entropy boride ceramic powder.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A preparation method of high-entropy boride ceramic powder is characterized by comprising the following steps:
1) Mixing metal oxide powder and boron powder, and grinding to obtain mixed powder; the metal oxide powder is made of HfO 2 Powder, zrO 2 Powder of TiO 2 Powder, ta 2 O 5 Powder and Nb 2 O 5 Powder, cr 2 O 3 Powder, moO 3 Powder of V 2 O 5 Powder and WO 3 At least four kinds of powder are mixed according to the equal molar ratio of metal elements;
2) Adding the mixed powder into a tungsten ark, and then placing the tungsten ark in a protective atmosphere for electric field sintering to obtain high-entropy boride ceramic powder; the ratio of the total mass of metal atoms in the metal oxide powder to the mass of boron powder in the step 1) is 1;
the tungsten ark in the step 2) has the size specifications of 115 mm-135 mm long, 15 mm-20 mm wide, 5 mm-15 mm high and 2 mm-6 mm thick;
the specific operation of the electric field sintering in the step 2) is as follows: and (3) connecting alternating current with the fixed power of 2.0-2.5 kW at two ends of the tungsten square boat, and electrifying for 1-30 s.
2. The preparation method of the high-entropy boride ceramic powder of claim 1, characterized in that: step 1) the HfO 2 Powder, zrO 2 Powder, tiO 2 Powder, ta 2 O 5 Powder and Nb 2 O 5 Powder, cr 2 O 3 Powder, moO 3 Powder of V 2 O 5 Powder and WO 3 The particle size of the powder is 1-3 μm, and the purity is more than or equal to 99.9%.
3. The preparation method of the high-entropy boride ceramic powder of claim 1, characterized in that: the particle size of the boron powder in the step 1) is 10-20 microns, and the purity is more than or equal to 99.0%.
4. The preparation method of the high-entropy boride ceramic powder of claim 1, characterized in that: and step 2), the purity of the tungsten ark is more than or equal to 99.99 percent.
5. A high-entropy boride ceramic powder characterized by being produced by the production method of any one of claims 1 to 4.
6. A high-entropy ceramic, characterized in that the preparation raw material comprises the high-entropy boride ceramic powder of claim 5.
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