CN102731096A - Textured boride base ultra-high temperature ceramic material and its preparation method - Google Patents
Textured boride base ultra-high temperature ceramic material and its preparation method Download PDFInfo
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Abstract
The invention discloses a textured boride base ultra-high temperature ceramic material and its preparation method. The ceramic material is a boride-silicide base composite material and is prepared from raw materials of group IVB metal, boron, silicon and transition metal. In addition, the microstructure of the composite material contains boride crystal grains of anisotropic grain growth and directional arrangement. The ceramic material is prepared by the following steps of: firstly performing reactive hot-pressing sintering to prepare densified boride base ceramic with the anisotropy crystal grain microstructure, and carrying out microstructure modulation on the ceramic which has undergone reactive hot-pressing sintering by a hot forging method to realize directional arrangement of the crystal grains of anisotropic grain growth. Therefore, the textured boride base ultra-high temperature ceramic material with the anisotropic grain growth crystal grain microstructure is obtained. According to the invention, relative density of the obtained ceramic material is greater than 98%; Lotgering orientation factor f (001) can reach up to 0.91; and its oxidation resistance, thermal conductivity and other properties all show obvious anisotropy.
Description
Technical field
The present invention relates to a kind of texturing boride-based superhigh temperature ceramic material and preparation method thereof; Specifically; Relate to a kind of texturing boride-based superhigh temperature ceramic material and preparation method thereof, belong to the boride base ceramic materials technical field with anisotropic grain pattern.
Background technology
The ultrahigh-temperature pottery is meant that those can use more than 1800 ℃ He in the reaction atmosphere, and has transition metal boride, carbide and the nitride material of excellent high-temperature oxidation-resistance and heat-shock resistance.Transition metal boride MB
2(M=Ti, Zr is Hf) owing to have HMP (＞3000 ℃), high firmness and good thermal conductivity; Become at present the important candidate material of ultrahigh-temperature pottery; Be expected to use (J.Am.Ceram.Soc., 90 [5] 1347～1364,2007) as high-temperature heat-resistance parts in the industrial circle.But single-phase boride ceramics is difficult to densification, and at high temperature the resistance of oxidation of (＞1100 ℃) is relatively poor simultaneously.Research shows through adding molybdenum disilicide (MoSi
2) wait silicide can promote the densification of boride ceramics, also can significantly improve its high-temperature oxidation resistance (J.Am.Ceram.Soc., 89 [7] 2320～2322,2006) simultaneously.Therefore, boride-silicide sill becomes the research focus of ultrahigh-temperature pottery.
Be to improve the performance of boride base ceramic materials, most studies concentrates on the design of components of material at present, promptly through selecting component that different additives changes material to improve the performance of material.Different with design of components, as to adopt microstructure to regulate and control means, preparation crystal grain have the texturing pottery of certain orientation, and the designing material microstructure is to improve another effective way of its performance.Crystal grain align the formation that not only can prevent some defectives in the material, increase the possibility that forms crackle bridging and crack deflection, thus in the mechanical property of the direction raising material of arranging perpendicular to crystal grain; And the anisotropy that can also utilize material property realizes the optimization (J.Am.Ceram.Soc., 81 [3] 713～716,1998) of material at some directional performance.
In the at present relevant boride-based ceramics texturing report, employing be the high-intensity magnetic field method, this method is in the forming and hardening process of ceramic body, utilizes magnetic field to make ceramic particle align (Scripta Mater., 60 [8] 615～618,2009).Though boride ceramics is a hexagonal system, adopt the boride ceramics of high-intensity magnetic field preparation, it still is equi-axed crystal on microscopic appearance, and its mechanical property more not textured ceramic be not significantly improved.
Summary of the invention
The present invention provides a kind of texturing boride-based superhigh temperature ceramic material with anisotropic grain pattern and preparation method thereof in order to solve the not high difficult problem of boride-based ceramics mechanical property in the prior art, to fill up the blank of prior art.
A kind of texturing boride-based superhigh temperature ceramic material provided by the invention; Be a kind of boride-silicide based composites, by IVB family metal, boron; Silicon and transition metal are that raw material is processed, and the boride crystal grain that has anisotropic growth in the microstructure of matrix material and align.
As preferred version, described texturing boride-based superhigh temperature ceramic material is by IVB family metal, and boron, silicon and transition metal are 1: 2 in molar ratio: (0.10～1.00): process for raw material (0.05～0.50).
Described IVB family metal is preferably Ti, Zr or Hf, and described transition metal is preferably Mo, W, V, Ta or Ni.
Described boride crystal grain is tabular.
The diameter of described tabular boride crystal grain is 2～10 μ m, and thickness is 0.2～1.2 μ m, and length-to-diameter ratio is 5～20.
The preparation method of texturing boride-based superhigh temperature ceramic material of the present invention comprises the steps:
A) IVB family metal simple-substance, amorphous boron powder, silica flour are mixed with transition metal, ball milling, drying obtains mixed powder;
B) will go up the mixed powder that makes of step and place mould, in vacuum or inert atmosphere, carry out the reaction hot-pressing sintering;
C) material behind the above-mentioned hot pressed sintering is placed hot forged mould again, in vacuum or inert atmosphere, carry out forge hot.
As preferred version, the IVB family metal simple-substance in the step a) is a purity greater than 98%, particle diameter is Ti, Zr or the Hf powder of 0.5～80 μ m; Amorphous boron powder be purity greater than 95%, particle diameter is the powder of 0.1～10 μ m; Silica flour be purity greater than 98%, particle diameter is the powder of 0.5～100 μ m; Transition metal is a purity greater than 98%, particle diameter is Mo, W, V, Ta or the Ni powder of 0.5～100 μ m; And IVB family metal simple-substance and amorphous boron powder, the mol ratio of silica flour and transition metal are 1: 2: (0.10～1.00): (0.05～0.50).
Ball-milling medium in the step a) is an acetone, and abrading-ball is ZrO
2, rotating speed is 100～600 rev/mins.
Drying temperature in the step a) is 50～100 ℃.
Mould in the step b) is the graphite jig that inner wall surface applies BN.
Hot pressed sintering temperature in the step b) is 1600～2000 ℃, and pressure is 5～50MPa.
Hot forged mould in the step c) is a graphite jig, and the length of mould * wide size is greater than the length * wide size of sample.
The length of hot forged mould * wide size=2a * 2bmm
2, wherein a and b are the length of sample and wide size.
Hot forging temperature in the step c) is 1600～2000 ℃, and pressure is 10～100MPa.
Bi-directional compression forge hot pattern or unidirectional heat of compression forging die formula are adopted in forge hot in the step c).
Forge hot pressure in the step c) adopts once pressurization or repeatedly pressuring method.
Described repeatedly pressuring method is meant after temperature rises to hot forging temperature, at first adds certain pressure, along with the distortion of sample and the increase of the area that is stressed; Intensified pressure again, sample continues distortion, and pressure continues to increase; So repeatedly, level off to zero until the sample rate of deformation.
Described inert atmosphere is an argon gas atmosphere.
The present invention adopts IVB family metal simple-substance (Ti, Zr, Hf) powder; Amorphous boron powder, silica flour and other transition metal (Mo, W; V, Ta, Ni etc.) powder is raw material; The densification boride-based ceramics that at first has the anisotropic grain microscopic appearance through the preparation of reaction hot-pressing sintering; The pottery of method through forge hot after to the reaction hot-pressing sintering carries out the microstructure regulation and control then, makes the crystal grain of anisotropic growth realize aligning, thereby obtains to have the texturing boride-based superhigh temperature ceramic material of anisotropic grain pattern.The texturing boride-based superhigh temperature ceramic material with anisotropic grain pattern of the present invention preparation is the practical application of performance ultrahigh-temperature pottery, realize material property raising and the optimization of some direction provide a kind of maybe.
Compared with prior art, the present invention has following beneficial effect:
1, the texturing boride-based superhigh temperature ceramic material for preparing gained through the inventive method: specific density is greater than 98%; The boride crystal grain that has anisotropic growth in the microstructure and align has higher texturing degree, and the Lotgering orientation factor f (00l) of material can be up to 0.91;
2, the texturing boride-based superhigh temperature ceramic material for preparing gained through the inventive method: its mechanical property, antioxidant property, thermal conductivity and all other performances all show tangible anisotropy; Simultaneously because the reinforcing effect of anisotropic grain, this pottery on the direction of vertical heat forging force each item performance than the microstructure regulation and control before the performance of sample have a more substantial increase.
Description of drawings
Fig. 1 is two kinds of forge hot pattern diagram that relate among the preparation method of the present invention.
Fig. 2 is the X-ray diffractogram through samples vertical hot-pressed surface before and after the microstructure regulation and control of the present invention: (a) be ZrB
2JCPDS card 34-0423; (b) be through the preceding vertically X-ray diffractogram of hot-pressed surface of the sample microstructure regulation and control of the present invention's preparation; (c) be the X-ray diffractogram of regulating and control the vertical hot-pressed surface in back through the sample microstructure of the present invention's preparation.Can find out before the Lotgering orientation factor of microstructure regulation and control back sample is regulated and control than microstructure raising is by a relatively large margin arranged.
Fig. 3 is that the polished surface and the fracture apperance of sample compares before and after regulating and control through microstructure of the present invention: (a) be sample polished surface SEM photo before the microstructure regulation and control; (b) be microstructure regulation and control back sample polished surface SEM photo; (c) be sample fracture SEM photo before the microstructure regulation and control; (d) be microstructure regulation and control back sample fracture SEM photo.Can find out that in the texturing sample after the microstructure regulation and control, the arrangement of boride lath is rule comparatively, form certain texture orientation.
The practical implementation method
Below in conjunction with embodiment the present invention is done further in detail, intactly explains, but do not limit content of the present invention.
Embodiment 1
Be preparation ZrB
2-5mol%MoSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, Mo powder 2.399 grams and Si powder 1.404 grams.
With acetone is solvent, with 560 rev/mins speed, uses ZrO
2The powder that ball planetary ball mill 8 hours, gained slurry obtain mixing after drying through rotary evaporation.
The powder that mixes is placed on the graphite jig that inner wall surface applies BN (among the 37mm * 30mm); Carry out the reaction hot-pressing sintering in a vacuum: temperature rise rate is 10 ℃/min during sintering; Be warming up to 1550 ℃ and be incubated 30 minutes; Apply 20MPa pressure then, simultaneously temperature is risen to 1800 ℃ and be incubated 1 hour with 10 ℃/minute heat-up rate.
(before the cutting is 40mm * 30mm * 9.8mm after the sample cutting with the preparation of reaction hot-pressing sintering; Cut then is 20mm * 15mm * 9.8mm); (40mm * 30mm) carries out forge hot: be warming up to 1550 ℃ and be incubated 30 minutes with 10 ℃/minute heat-up rates to place graphite jig again; And then be warming up to 1800 ℃ with 10 ℃/minute heat-up rate, apply 60MPa pressure, and be incubated 1 hour.
The specific density of sample is 98.4% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.09 (before the forge hot) and 0.50 (bi-directional compression forge hot), 0.52 (unidirectional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 555MPa; Parallel forge hot direction, 495MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 785MPa; Parallel forge hot direction, 622MPa.The flexural strength of sample after the unidirectional compression forge hot: vertical forge hot direction, 703MPa; Parallel forge hot direction, 625MPa.
Embodiment 2
Be preparation ZrB
2-19mol%MoSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, Mo powder 9.114 grams and Si powder 5.336 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 98.9% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.12 (before the forge hot) and 0.59 (bi-directional compression forge hot), 0.64 (unidirectional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 595MPa; Parallel forge hot direction, 531MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 845MPa; Parallel forge hot direction, 691MPa.The flexural strength of sample after the unidirectional compression forge hot: vertical forge hot direction, 734MPa; Parallel forge hot direction, 682MPa.
Embodiment 3
Be preparation ZrB
2-50mol%MoSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, Mo powder 23.985 grams and Si powder 14.043 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 99.5% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.16 (before the forge hot) and 0.70 (bi-directional compression forge hot), 0.73 (unidirectional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 520MPa; Parallel forge hot direction, 467MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 789MPa; Parallel forge hot direction, 659MPa.The flexural strength of sample after the unidirectional compression forge hot: vertical forge hot direction, 680MPa; Parallel forge hot direction, 607MPa.
Embodiment 4
Be preparation ZrB
2-5mol%WSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, W powder 4.596 grams and Si powder 1.404 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 98.5% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.10 (before the forge hot) and 0.56 (bi-directional compression forge hot), 0.60 (unidirectional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 560MPa; Parallel forge hot direction, 508MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 812MPa; Parallel forge hot direction, 640MPa.The flexural strength of sample after the unidirectional compression forge hot: vertical forge hot direction, 720MPa; Parallel forge hot direction, 632MPa.
Embodiment 5
Be preparation ZrB
2-50mol%WSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, W powder 45.960 grams and Si powder 14.043 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 99.2% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.14 (before the forge hot) and 0.61 (bi-directional compression forge hot), 0.68 (unidirectional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 581MPa; Parallel forge hot direction, 546MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 905MPa; Parallel forge hot direction, 715MPa.The flexural strength of sample after the unidirectional compression forge hot: vertical forge hot direction, 730MPa; Parallel forge hot direction, 693MPa.
Embodiment 6
Be preparation ZrB
2-20mol%VSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, V powder 5.094 grams and Si powder 5.617 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 99.0% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.11 (before the forge hot) and 0.70 (bi-directional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 589MPa; Parallel forge hot direction, 534MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 786MPa; Parallel forge hot direction, 621MPa.
Embodiment 7
Be preparation ZrB
2-20mol%TaSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, Ta powder 18.095 grams and Si powder 5.617 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 99.5% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.17 (before the forge hot) and 0.63 (bi-directional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 525MPa; Parallel forge hot direction, 499MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 734MPa; Parallel forge hot direction, 605MPa.
Embodiment 8
Be preparation ZrB
2-20mol%NiSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, Ni powder 5.869 grams and Si powder 5.617 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 98.1% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.11 (before the forge hot) and 0.51 (bi-directional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 625MPa; Parallel forge hot direction, 608MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 925MPa; Parallel forge hot direction, 801MPa.
Embodiment 9
Be preparation TiB
2-20mol%MoSi
2Complex phase ceramic, weighing Ti powder 23.934 grams, B powder 10.811 grams, Mo powder 9.594 grams and Si powder 5.617 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 99.1% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.13 (before the forge hot) and 0.61 (bi-directional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 556MPa; Parallel forge hot direction, 520MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 803MPa; Parallel forge hot direction, 656MPa.
Embodiment 10
Be preparation TiB
2-20mol%WSi
2Complex phase ceramic, weighing Ti powder 23.934 grams, B powder 10.811 grams, W powder 18.384 grams and Si powder 5.617 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 99.0% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.15 (before the forge hot) and 0.64 (bi-directional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 585MPa; Parallel forge hot direction, 546MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 871MPa; Parallel forge hot direction, 680MPa.
Embodiment 11
Be preparation HfB
2-20mol%MoSi
2Complex phase ceramic, weighing Hf powder 89.245 grams, B powder 10.811 grams, Mo powder 9.594 grams and Si powder 5.617 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 98.3% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.15 (before the forge hot) and 0.57 (bi-directional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 610MPa; Parallel forge hot direction, 592MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 889MPa; Parallel forge hot direction, 751MPa.
Embodiment 12
Be preparation HfB
2-20mol%WSi
2Complex phase ceramic, weighing Hf powder 89.245 grams, B powder 10.811 grams, W powder 18.384 grams and Si powder 5.617 grams.
According to preparing powder, reaction hot-pressing sintering and forge hot with embodiment 1 identical method.
The specific density of sample is 98.9% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.17 (before the forge hot) and 0.58 (bi-directional compression forge hot) before and after the forge hot.The flexural strength of sample before the forge hot: vertical forge hot direction, 603MPa; Parallel forge hot direction, 581MPa.The flexural strength of sample after the bi-directional compression forge hot: vertical forge hot direction, 852MPa; Parallel forge hot direction, 746MPa.
Embodiment 13
Be preparation ZrB
2-19mol%MoSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, Mo powder 9.114 grams and Si powder 5.336 grams.
With acetone is solvent, with 560 rev/mins speed, uses ZrO
2The powder that ball planetary ball mill 8 hours, gained slurry obtain mixing after drying through rotary evaporation.
The powder that mixes is placed on the graphite jig that inner wall surface applies BN, and (among the 37mm * 30mm), in argon gas atmosphere, carry out the reaction hot-pressing sintering: temperature rise rate is 10 ℃/min during sintering, is warming up to 1550 ℃ and be incubated 30 minutes; When insulation finishes, apply 20MPa pressure; Be warming up to 1800 ℃ and be incubated 1 hour with 10 ℃/minute heat-up rate again.
(before the cutting is 37mm * 30mm * 9.8mm after the sample cutting with the preparation of reaction hot-pressing sintering; Cutting back is 9mm * 9mm * 9mm), and (30mm * 30mm) carries out forge hot: be warming up to 1550 ℃ and be incubated 30 minutes with 10 ℃/minute heat-up rates to place the hot pressing furnace graphite jig again; When insulation finishes, be warming up to 1800 ℃ with 10 ℃/minute heat-up rate again; Heat up after the end, apply 60MPa pressure, and be incubated 1 hour.
The specific density of sample is 99.0% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.12 (before the forge hot) and 0.607 (bi-directional compression forge hot) before and after the forge hot.
Embodiment 14
Be preparation ZrB
2-19mol%MoSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, Mo powder 9.114 grams and Si powder 5.336 grams.
According to preparing powder, reaction hot-pressing sintering and cutting with embodiment 13 identical methods.But in hot forging process, when temperature is warming up to 1800 ℃, apply 60MPa pressure, be incubated 0.5 hour; Afterwards, apply corresponding 60MPa pressure, be incubated 0.5 hour again according to the physical size of gained forge hot sample among the embodiment 13.
The specific density of sample is 98.8% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.12 (before the forge hot) and 0.803 (bi-directional compression forge hot) before and after the forge hot.
Embodiment 15
Be preparation ZrB
2-19mol%MoSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, Mo powder 9.114 grams and Si powder 5.336 grams.
According to preparing powder, reaction hot-pressing sintering and cutting with embodiment 13 identical methods.But in hot forging process, when temperature is warming up to 1800 ℃, apply 60MPa pressure, be incubated 1/3 hour; Afterwards, apply corresponding 60MPa pressure, be incubated 1/3 hour (be sample state among the embodiment 14 this moment) according to the physical size of gained forge hot sample among the embodiment 13; Physical size according to gained forge hot sample among the embodiment 14 applies corresponding 60MPa pressure more again, is incubated 1/3 hour.
The specific density of sample is 99.0% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.12 (before the forge hot) and 0.857 (bi-directional compression forge hot) before and after the forge hot.
Embodiment 16
Be preparation ZrB
2-19mol%MoSi
2Complex phase ceramic, weighing Zr powder 45.612 grams, B powder 10.811 grams, Mo powder 9.114 grams and Si powder 5.336 grams.
According to preparing powder, reaction hot-pressing sintering and cutting with embodiment 13 identical methods.But in hot forging process, when temperature is warming up to 1800 ℃, apply 60MPa pressure, be incubated 1/4 hour; Afterwards, apply corresponding 60MPa pressure, be incubated 1/4 hour (be sample state among the embodiment 14 this moment) according to the physical size of gained forge hot sample among the embodiment 13; Physical size according to gained forge hot sample among the embodiment 14 applies corresponding 60MPa pressure more again, is incubated 1/4 hour (be sample state among the embodiment 15 this moment); Physical size according to gained forge hot sample among the embodiment 15 applies corresponding 60MPa pressure more again, is incubated 1/4 hour.
The specific density of sample is 99.2% after the forge hot.The Lotgering orientation factor f (00l) of sample is respectively 0.12 (before the forge hot) and 0.912 (bi-directional compression forge hot) before and after the forge hot.
Claims (18)
1. texturing boride-based superhigh temperature ceramic material; It is characterized in that: be a kind of boride-silicide based composites, by IVB family metal, boron; Silicon and transition metal are that raw material is processed, and the boride crystal grain that has anisotropic growth in the microstructure of matrix material and align.
2. texturing boride-based superhigh temperature ceramic material according to claim 1 is characterized in that: described stupalith is by IVB family metal, and boron, silicon and transition metal are 1: 2 in molar ratio: (0.10～1.00): process for raw material (0.05～0.50).
3. texturing boride-based superhigh temperature ceramic material according to claim 1 and 2 is characterized in that: described IVB family metal is Ti, Zr or Hf, and described transition metal is Mo, W, V, Ta or Ni.
4. texturing boride-based superhigh temperature ceramic material according to claim 1 is characterized in that: described boride crystal grain is tabular.
5. texturing boride-based superhigh temperature ceramic material according to claim 4 is characterized in that: the diameter of tabular boride crystal grain is 2～10 μ m, and thickness is 0.2～1.2 μ m, and length-to-diameter ratio is 5～20.
6. the preparation method of the described texturing boride-based superhigh temperature ceramic material of claim 1 is characterized in that, comprises the steps:
A) IVB family metal simple-substance, amorphous boron powder, silica flour are mixed with transition metal, ball milling, drying obtains mixed powder;
B) will go up the mixed powder that makes of step and place mould, in vacuum or inert atmosphere, carry out the reaction hot-pressing sintering;
C) material behind the above-mentioned hot pressed sintering is placed hot forged mould again, in vacuum or inert atmosphere, carry out forge hot.
7. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 6 is characterized in that: the IVB family metal simple-substance in the step a) is a purity greater than 98%, particle diameter is Ti, Zr or the Hf powder of 0.5～80 μ m; Amorphous boron powder be purity greater than 95%, particle diameter is the powder of 0.1～10 μ m; Silica flour be purity greater than 98%, particle diameter is the powder of 0.5～100 μ m; Transition metal is a purity greater than 98%, particle diameter is Mo, W, V, Ta or the Ni powder of 0.5～100 μ m; And IVB family metal simple-substance and amorphous boron powder, the mol ratio of silica flour and transition metal are 1: 2: (0.10～1.00): (0.05～0.50).
8. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 6, it is characterized in that: the ball-milling medium in the step a) is an acetone, abrading-ball is ZrO
2, rotating speed is 100～600 rev/mins.
9. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 6, it is characterized in that: the drying temperature in the step a) is 50～100 ℃.
10. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 6 is characterized in that: the mould in the step b) is the graphite jig that inner wall surface applies BN.
11. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 6 is characterized in that: the hot pressed sintering temperature in the step b) is 1600～2000 ℃, and pressure is 5～50MPa.
12. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 6 is characterized in that: the hot forged mould in the step c) is a graphite jig, and the length of mould * wide size is greater than the length * wide size of sample.
13. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 12 is characterized in that: the length of mould * wide size=2a * 2b mm
2, wherein a and b are the length of sample and wide size.
14. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 6 is characterized in that: the hot forging temperature in the step c) is 1600～2000 ℃, and pressure is 10～100MPa.
15. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 6 is characterized in that: bi-directional compression forge hot pattern or unidirectional heat of compression forging die formula are adopted in the forge hot in the step c).
16. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 6 is characterized in that: the forge hot pressure in the step c) adopts once pressurization or repeatedly pressuring method.
17. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 16 is characterized in that: described repeatedly pressuring method is meant after temperature rises to hot forging temperature, at first adds certain pressure; Along with the distortion of sample and the increase of the area that is stressed; Intensified pressure again, sample continues distortion, and pressure continues to increase; So repeatedly, level off to zero until the sample rate of deformation.
18. the preparation method of texturing boride-based superhigh temperature ceramic material according to claim 6 is characterized in that: described inert atmosphere is an argon gas atmosphere.
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Cited By (6)
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| CN108341672A (en) * | 2018-04-04 | 2018-07-31 | 安徽工程大学 | A kind of hot forging method of low temperature preparation superhigh temperature ceramics |
| CN108424146A (en) * | 2018-04-28 | 2018-08-21 | 东北大学 | A kind of preparation method of four tungsten borides base ceramics |
| CN110483058A (en) * | 2019-08-07 | 2019-11-22 | 广东工业大学 | A kind of boride ceramics and its preparation method and application of superhard high intensity |
| CN110548829A (en) * | 2019-09-06 | 2019-12-10 | 哈尔滨工业大学 | forging method for controlling directional arrangement of aluminum matrix composite whiskers |
| CN110606749A (en) * | 2019-09-29 | 2019-12-24 | 石家庄铁道大学 | High-entropy boride ceramic material and preparation method thereof |
| CN112079645A (en) * | 2020-08-19 | 2020-12-15 | 广东工业大学 | Textured silicon carbide whisker toughened alumina-based ceramic and preparation method and application thereof |
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| CN108341672A (en) * | 2018-04-04 | 2018-07-31 | 安徽工程大学 | A kind of hot forging method of low temperature preparation superhigh temperature ceramics |
| CN108424146A (en) * | 2018-04-28 | 2018-08-21 | 东北大学 | A kind of preparation method of four tungsten borides base ceramics |
| CN108424146B (en) * | 2018-04-28 | 2020-06-16 | 东北大学 | Preparation method of tungsten tetraboride-based ceramic |
| CN110483058A (en) * | 2019-08-07 | 2019-11-22 | 广东工业大学 | A kind of boride ceramics and its preparation method and application of superhard high intensity |
| CN110483058B (en) * | 2019-08-07 | 2022-03-25 | 广东工业大学 | Superhard high-strength boride ceramic and preparation method and application thereof |
| CN110548829A (en) * | 2019-09-06 | 2019-12-10 | 哈尔滨工业大学 | forging method for controlling directional arrangement of aluminum matrix composite whiskers |
| CN110606749A (en) * | 2019-09-29 | 2019-12-24 | 石家庄铁道大学 | High-entropy boride ceramic material and preparation method thereof |
| CN112079645A (en) * | 2020-08-19 | 2020-12-15 | 广东工业大学 | Textured silicon carbide whisker toughened alumina-based ceramic and preparation method and application thereof |
| CN112079645B (en) * | 2020-08-19 | 2022-03-25 | 广东工业大学 | Textured silicon carbide whisker toughened alumina-based ceramic and preparation method and application thereof |
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