CN108358645B - Method for preparing high-density hafnium diboride ceramic - Google Patents
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Abstract
The invention discloses a method for preparing high-density hafnium diboride ceramic, which comprises the steps of carrying out high-energy ball milling, acid washing, vacuum treatment and packaging and prepressing on hafnium diboride powder and high-melting-point packaging material, and directly sintering the hafnium diboride powder into the high-density hafnium diboride ceramic under the conditions of 3-15 GPa and 600-2000 ℃. The high-temperature high-pressure method is utilized for the first time to prepare the high-density pure-phase hafnium diboride bulk material with good crystal morphology and microstructure, and the high-density pure-phase hafnium diboride bulk material has the characteristics of small crystal grain size, high crystallinity, high density, stable structure, higher hardness and excellent fracture toughness. The high-temperature-resistant ceramic material is a novel high-temperature-structure ceramic material, can be used as a candidate material of a high-temperature-resistant part of an aircraft engine, can also be developed into a novel hard alloy, can replace a tungsten carbide hard alloy cutter, and is widely applied to the field of mechanical cutting.
Description
Technical Field
The invention relates to a high-density hafnium diboride ceramic, belongs to the field of high-temperature structural ceramics and hard alloys thereof, and particularly relates to a method for preparing the high-density hafnium diboride ceramic.
Background
Ultra-high Temperature structural materials (UHTCs) are a class of materials that can maintain chemical stability in high Temperature environments (above 2000 ℃) and in reactive atmospheres (such as atomic oxygen environments), and generally include high melting point transition metal compounds including borides, carbides, and oxides. Of these high melting point transition metal compounds, HfB2The melting points of HfC, TaC, etc. exceed 3000 c, making them potentially useful in extreme conditions. The transition metals have high electron concentration, so that the transition metals have large bulk modulus and elastic deformation resistance, but because the generation and movement of dislocation cannot be effectively prevented by forming metal bonds among metal atoms, the transition metals tend to have low hardness values, but the incorporation of light elements can effectively improve the hardness. For example, tungsten has hardness changed from 8.63 GPa to 24 GPa due to the doping of boron. High hardness imparting transition metal compounds in cemented carbidesThe product can be used as cutting tool. But due to HfB2Sintering is difficult, densification is difficult, and application of the method is limited.
Sintering of bulk 5d transition metal borides and carbides has been a significant challenge. Hafnium diboride, a typical 5d transition metal boride, can be widely applied to the field of high-temperature structural ceramics and hard alloys thereof due to excellent physical and chemical properties, but the problem of bulk sintering is troubling people. In order to obtain a hafnium diboride bulk sintered body, a domestic hinge type cubic press is utilized, and a pure phase sintering method without adding a binder is adopted under the conditions of high temperature and high pressure to prepare the pure phase bulk sintered body with excellent performance and application value for the first time. It was again experimentally verified that the introduction of light elements into the transition metal lattice produces strongly directional covalent bonds, thereby improving its feasibility to resist plastic and elastic deformation. The invention has simple preparation process, is beneficial to industrial production, has high melting point, high strength, high hardness, high toughness and high oxidation resistance, is developing into a novel high-temperature structure ceramic material, can be used as a candidate material of a high-temperature resistant part of an aircraft engine, has great application potential under extreme conditions, and can be developed into a novel hard alloy due to the hardness of the high-temperature structure ceramic material compared with that of commercial tungsten carbide.
Disclosure of Invention
The invention aims to provide a method for preparing high-density hafnium diboride ceramic, which solves the problems that the traditional hafnium diboride ceramic is difficult to densify, pure phase is difficult to prepare into blocks and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for preparing high-density hafnium diboride ceramic comprises the following steps:
(1): adopting hafnium diboride as a raw material;
(2): carrying out high-energy ball milling on the raw material obtained in the step (1);
(3): pickling the raw material subjected to ball milling in the step (2);
(4): performing high-temperature vacuum treatment on the raw material subjected to acid cleaning in the step (3), then performing sealing wrapping by adopting a high-melting-point material, and performing pre-pressing forming to obtain a sealing wrapping body;
(5): putting the seal inclusion formed by prepressing in the step (4) into a high-pressure synthesis assembly part for assembling to obtain an assembly body;
(6): placing the assembly obtained in the step (5) in a synthesis cavity of high-temperature high-pressure equipment for high-temperature high-pressure sintering, wherein the sintering conditions are 3-15 GPa, 600-2000 ℃, and the heat preservation time is 5-100 minutes;
(7): and (6) after the high-temperature high-pressure sintering is finished, cooling and depressurizing to normal temperature and normal pressure, taking out the assembly body, and removing the assembly part and the inclusion on the assembly body to obtain the high-density hafnium diboride ceramic.
Preferably, the hafnium diboride used in the step (1) is solid particles or powder of hafnium diboride with a hexagonal structure, and the hafnium diboride is directly sintered together at high temperature and high pressure to form a high-density hafnium diboride bulk material, wherein the particle size of the hafnium diboride is further preferably 0.1-10 μm.
As optimization, the step of performing high-energy ball milling in the step (2) specifically comprises the following steps: at least one of normal hexane, ethanol and stearic acid is used as a process control agent, at least one of high-speed steel balls, zirconium dioxide balls and agate balls is used as grinding balls, and the process control agent, the grinding balls and the hafnium diboride raw materials are mixed and then placed in a high-energy ball mill for ball milling.
In the step (2), the process control agent, the grinding balls and the hafnium diboride raw materials are optimally mixed according to the weight ratio of 0.8-5: 8-10: 1, the ball milling speed is 250-500 r/min, and the ball milling time is 10-50 hours.
As optimization, aqua regia or hydrochloric acid aqueous solution is adopted for acid washing in the step (3), and the acid washing can remove impurities possibly carried in the production, transportation or storage process of the hafnium diboride raw material and impurities such as iron element possibly introduced by the high-energy ball milling in the step (2), so that the purity of the hafnium diboride raw material is improved.
As an optimization, the step (4) is carried outThe conditions for carrying out the high-temperature vacuum treatment are as follows: at a temperature of 400-1800 ℃ and a vacuum degree of 1 × 10-5And (3) preserving the heat for 10-300 minutes under the condition of-1 Pa, wherein the vacuum treatment is favorable for removing impurities which can be adsorbed in the hafnium diboride raw material and organic matters introduced by the high-energy ball milling in the step (2), so that the purity and the density of the hafnium diboride ceramic obtained by the high-temperature high-pressure treatment in the step (7) are improved.
Preferably, the high-melting-point wrapping material adopted in the step (4) is at least one of pure tantalum, platinum and molybdenum.
And (3) performing pre-pressing forming on the wrapped body in the step (4) under the pressure of 400-600 MPa to obtain the cylindrical sealed wrapped body.
And (3) as further optimization, placing the pre-pressed cylindrical sealed inclusion obtained in the step (4) in a salt pipe, sealing the upper end and the lower end of the salt pipe with salt sheets respectively to form a salt column assembly, then placing the salt column assembly in a graphite pipe, sealing the upper end and the lower end of the graphite pipe with graphite sheets respectively to form a graphite column assembly, finally placing the graphite column assembly in a pyrophyllite synthesis block, and sequentially arranging molybdenum sheets and conductive steel rings at the upper end and the lower end of the graphite column assembly respectively, wherein the assembly is an assembly structure commonly used by a domestic hinge type cubic press.
Preferably, the high-temperature and high-pressure equipment adopted in the step (6) is a two-sided press, a four-sided press or a cubic press, and a domestic hinge type cubic press is further preferably adopted.
Advantageous effects
(1) The method for preparing the high-density hafnium diboride ceramic provided by the invention takes solid hafnium diboride powder or particles obtained in the market as initial raw materials, obtains high-purity hafnium diboride ultrafine powder by grinding and acid washing, and then carries out high-temperature and high-pressure sintering, and the sintering process is pure-phase sintering without adding any binder, so that the method has the characteristics of low cost, environmental friendliness, simple sintering process, good product performance, high yield and the like.
(2) The high-density hafnium diboride ceramic obtained by the method provided by the invention has average crystal through XRD and scanning electron microscope analysisThe particle size is less than 0.1 mu m, a large number of nano-structure crystal grains exist at the same time, the porosity is low, the density is high, the hafnium diboride ceramic can be obtained by sintering under the condition of relatively low temperature and pressure by adopting the method, the hafnium diboride ceramic can be obtained by sintering at the lowest temperature of 600 ℃ and 3 GPa, the hardness of the sintered body is more than 18GPa, and the fracture toughness is 3.1MPa1/2The relative density is more than 90.2%, and the method has the advantages of easy popularization, large-scale production and the like.
(3) The high-density hafnium diboride ceramic obtained by the method has the remarkable characteristics of high density, small grain size, high hardness, high fracture toughness, high density and the like, can be developed into a novel high-temperature structure ceramic material, can be used as a candidate material of a high-temperature resistant part of an aircraft engine, has great application potential under extreme conditions, and can be developed into a novel hard alloy due to the fact that the high-temperature structure ceramic material has higher hardness than commercial tungsten carbide, can replace a tungsten carbide hard alloy cutter, and is widely applied to the field of mechanical cutting.
Drawings
FIG. 1 is a photograph of an actual implementation of the highly densified hafnium diboride ceramic prepared in example 18;
FIG. 2 is an XRD pattern of the highly densified hafnium diboride ceramic prepared in example 18;
FIG. 3 is a scanning electron micrograph of the highly densified hafnium diboride ceramic prepared in example 18;
FIG. 4 is a graph of hardness, fracture toughness and density measurements of the highly densified hafnium diboride ceramic prepared in example 18.
Detailed Description
Examples
A method for preparing high-density hafnium diboride ceramic comprises the following steps:
(1): adopting hafnium diboride powder with a hexagonal structure as a raw material;
(2): carrying out high-energy ball milling on the raw materials obtained in the step (1), taking normal hexane as a process control agent, taking a high-speed steel ball as a grinding ball, and mixing the process control agent, the grinding ball and the hafnium diboride raw materials according to a ratio of 4: 9: 1, placing the mixture in a high-energy ball mill for ball milling for 45 hours at the speed of 320 r/min;
(3): pickling the raw materials subjected to ball milling in the step (2), wherein the pickling adopts aqua regia;
(4): subjecting the pickled raw material in step (3) to vacuum degree of 1 × 10 at 800 deg.C-2Carrying out high-temperature vacuum treatment for 60 minutes under the condition of Pa, then carrying out sealing wrapping by adopting molybdenum, tantalum, niobium and platinum simple substances, and carrying out pre-pressing forming under the pressure of 520MPa to obtain a cylindrical sealing wrapping body;
(5): putting the cylindrical sealing inclusion subjected to pre-pressing forming in the step (4) into a high-pressure synthesis assembly part for assembling to obtain an assembly body, wherein the structure of the assembly body is commonly used for assembling a domestic hinge type cubic press: placing the cylindrical sealed inclusion in a salt tube, wherein the upper end and the lower end of the salt tube are respectively sealed by salt sheets to form a salt column assembly, then placing the salt column assembly in a graphite tube, the upper end and the lower end of the graphite tube are respectively sealed by graphite sheets to form a graphite column assembly, finally placing the graphite column assembly in a pyrophyllite synthesis block, and respectively and sequentially arranging molybdenum sheets and conductive steel rings at the upper end and the lower end of the graphite column assembly;
(6): placing the assembly obtained in the step (5) in a synthesis cavity of a domestic hinge type cubic press for high-temperature and high-pressure sintering, wherein the sintering conditions are 3-15 GPa, 600-2000 ℃, and the heat preservation time is 5-100 minutes;
(7): and (6) after the high-temperature high-pressure sintering is finished, cooling and depressurizing to normal temperature and normal pressure, taking out the assembly body, and removing the assembly part and the inclusion on the assembly body to obtain the high-density hafnium diboride ceramic.
The method provided in the above embodiment is adopted to respectively perform 50 embodiments with different experimental parameters, for the sake of convenient comparison, the same ball milling, acid washing, vacuum treatment and assembly are performed in each embodiment, different temperature and pressure conditions are adopted in the high temperature and high pressure experimental process to test the influence of the different temperature and pressure conditions on the hardness, fracture toughness and relative density of the synthesized hafnium diboride ceramic, and the temperature, pressure and heat-preserving and pressure-maintaining time adopted in the high temperature and high pressure treatment process in each embodiment are as shown in the following table 1:
TABLE 1 high temperature and high pressure test conditions
The hardness, fracture toughness and relative density of the high density hafnium diboride ceramics obtained in the above examples 1 to 50 are measured as shown in table 2 below:
TABLE 2 test results
| Examples | hardness/GPa | Fracture toughness/MPa-1/2 | Relative density/%) | Examples | hardness/GPa | Fracture toughness/MPa-1/2 | Relative density/%) |
| 1 | 18.0 | 3.1 | 90.5 | 26 | 22.5 | 4.2 | 98.5 |
| 2 | 18.5 | 3.1 | 90.8 | 27 | 23.0 | 3.8 | 99.1 |
| 3 | 19.0 | 3.5 | 91.1 | 28 | 23.2 | 3.8 | 99.1 |
| 4 | 19.2 | 3.2 | 91.2 | 29 | 23.4 | 3.5 | 99.3 |
| 5 | 19.5 | 3.9 | 91.0 | 30 | 18.2 | 4.2 | 90.7 |
| 6 | 18.3 | 4.1 | 90.2 | 31 | 18.3 | 3.9 | 91.5 |
| 7 | 18.4 | 3.8 | 90.2 | 32 | 21.5 | 4.2 | 94.3 |
| 8 | 18.9 | 3.5 | 91.3 | 33 | 19.8 | 3.8 | 92.8 |
| 9 | 19.7 | 3.8 | 92.6 | 34 | 22.5 | 4.8 | 98.2 |
| 10 | 20.0 | 3.6 | 93.4 | 35 | 22.1 | 4.2 | 97.4 |
| 11 | 21.2 | 3.6 | 93.8 | 36 | 21.7 | 4.3 | 97.8 |
| 12 | 21.9 | 3.8 | 94.1 | 37 | 21.1 | 4.6 | 98.7 |
| 13 | 22.0 | 4.0 | 96.8 | 38 | 22.7 | 4.2 | 97.9 |
| 14 | 22.3 | 4.1 | 97.8 | 39 | 22.2 | 3.9 | 96.5 |
| 15 | 22.5 | 4.5 | 98.7 | 40 | 22.3 | 4.2 | 96.5 |
| 16 | 23.1 | 4.9 | 99.1 | 41 | 21.8 | 3.9 | 96.2 |
| 17 | 23.6 | 5.0 | 99.5 | 42 | 22.7 | 4.3 | 96.7 |
| 18 | 24.0 | 5.2 | 99.6 | 43 | 22.1 | 4.0 | 96.1 |
| 19 | 24.0 | 5.1 | 99.5 | 44 | 21.3 | 3.8 | 95.3 |
| 20 | 23.9 | 5.1 | 96.3 | 45 | 19.8 | 3.5 | 95.8 |
| 21 | 17.8 | 4.9 | 91.0 | 46 | 20.3 | 3.8 | 94.9 |
| 22 | 19.8 | 4.7 | 92.8 | 47 | 21.2 | 4.9 | 96.5 |
| 23 | 23.0 | 4.6 | 95.9 | 48 | 21.7 | 3.9 | 97.4 |
| 24 | 22.8 | 4.8 | 96.4 | 49 | 22.7 | 3.8 | 96.8 |
| 25 | 22.4 | 5.0 | 96.0 | 50 | 20.9 | 3.5 | 95.8 |
The high-density hafnium diboride ceramics obtained in examples 1 to 50 had hardness of 18GPa or more and fracture toughness of 3.1MPa1/2The relative density is more than 90.2%, wherein the highest performance of the high-density hafnium diboride ceramic obtained in the embodiment 18 is the best embodiment; wherein, fig. 1 to 4 respectively show a physical diagram, an XRD spectrum and an electron microscope scan of the high-density hafnium diboride ceramic obtained in example 18And hardness, fracture toughness and relative density test results.
The above description is only for the preferred embodiment of the present invention, and the technical solutions of the present invention are not limited to the above description, and those skilled in the art can make various changes, substitutions and alterations without departing from the spirit and scope of the present invention, and thus the equivalent technical solutions also belong to the scope of the present invention.
Claims (10)
1. A method for preparing high-density hafnium diboride ceramic is characterized by comprising the following steps:
(1): adopting hafnium diboride as a raw material;
(2): carrying out high-energy ball milling on the raw material obtained in the step (1);
(3): pickling the raw material subjected to ball milling in the step (2);
(4): performing high-temperature vacuum treatment on the raw material subjected to acid cleaning in the step (3), then performing sealing wrapping by adopting a high-melting-point material, and performing pre-pressing forming to obtain a sealing wrapping body;
(5): putting the seal inclusion formed by prepressing in the step (4) into a high-pressure synthesis assembly part for assembling to obtain an assembly body;
(6): placing the assembly obtained in the step (5) in a synthesis cavity of high-temperature high-pressure equipment for high-temperature high-pressure sintering, wherein the sintering conditions are 3-15 GPa, 600-2000 ℃, and the heat preservation time is 5-100 minutes;
(7): and (6) after the high-temperature high-pressure sintering is finished, cooling and depressurizing to normal temperature and normal pressure, taking out the assembly body, and removing the assembly part and the inclusion on the assembly body to obtain the high-density hafnium diboride ceramic.
2. The method for preparing the high-density hafnium diboride ceramic according to claim 1, wherein the hafnium diboride raw material used in the step (1) is solid particles or powder of hafnium diboride with hexagonal structure.
3. The method for preparing the high-density hafnium diboride ceramic according to claim 1, wherein the step of performing high-energy ball milling in the step (2) is specifically as follows: at least one of normal hexane, ethanol and stearic acid is used as a process control agent, at least one of high-speed steel balls, zirconium dioxide balls and agate balls is used as grinding balls, and the process control agent, the grinding balls and the hafnium diboride raw materials are mixed and then placed in a high-energy ball mill for ball milling.
4. The method for preparing high-density hafnium diboride ceramic according to claim 3, wherein in the step (2), the process control agent, the grinding balls and the hafnium diboride raw materials are mixed according to the ratio of 0.8-5: 8-10: 1, the ball milling speed is 250-500 r/min, and the ball milling time is 10-50 hours.
5. The method for preparing the high-density hafnium diboride ceramic according to claim 1, wherein step (3) is performed by acid washing with aqua regia or hydrochloric acid aqueous solution.
6. The method for preparing the high-density hafnium diboride ceramic according to claim 1, wherein the conditions of the high-temperature vacuum treatment in the step (4) are as follows: at a temperature of 400-1800 ℃ and a vacuum degree of 1 × 10-5And keeping the temperature for 10-300 minutes under the condition of-1 Pa.
7. The method for preparing the high-density hafnium diboride ceramic according to claim 1, wherein the high-melting-point wrapping material adopted in the step (4) is at least one of molybdenum, tantalum, niobium and platinum.
8. The method for preparing the high-density hafnium diboride ceramic according to claim 1 or 7, wherein in the step (4), the sealed and wrapped inclusion is pre-pressed and formed under a pressure of 400-600 MPa to obtain a cylindrical sealed inclusion.
9. The method for preparing the high-density hafnium diboride ceramic according to claim 8, wherein the structure of the assembly in the step (5) is as follows: and (3) placing the pre-pressed cylindrical sealing inclusion obtained in the step (4) in a salt pipe, sealing the upper end and the lower end of the salt pipe with salt sheets respectively to form a salt column assembly, then placing the salt column assembly in a graphite pipe, sealing the upper end and the lower end of the graphite pipe with graphite sheets respectively to form a graphite column assembly, finally placing the graphite column assembly in a pyrophyllite synthesis block, and sequentially arranging a molybdenum sheet and a conductive steel ring above and below the graphite column assembly respectively.
10. The method for preparing the high-density hafnium diboride ceramic according to claim 1, wherein the high-temperature and high-pressure equipment adopted in the step (6) is a two-sided press, a four-sided press or a cubic press.
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