CN113896553B - Fiber monolithic structure ultrahigh-temperature ceramic composite material and preparation method thereof - Google Patents
Fiber monolithic structure ultrahigh-temperature ceramic composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a fiber monolithic structure ultra-high temperature ceramic composite material and a preparation method thereof, wherein the ceramic composite material is of a fiber monolithic structure and comprises a fiber cell body and a cell body interface; the cellule is carbon, and the cellule interface is one of TiC ceramic, zrC ceramic, hfC ceramic and TaC ceramic. The preparation method mainly comprises two steps: firstly, carbon fiber is used as a template to synthesize skin-core structure fiber with an ultrahigh-temperature ceramic outer layer and carbon core part by a molten salt disproportionation method, then the skin-core structure fiber is laid out and then is subjected to discharge plasma sintering, and finally the ultrahigh-temperature ceramic composite material with the fiber monolithic structure is obtained. The fiber monolithic structure ultrahigh-temperature ceramic composite material has the characteristics of uniform tissue structure, good mechanical property and the like; the preparation method has the advantages of simple and controllable process, short production period, low cost and the like.
Description
Technical Field
The invention relates to the technical field of ceramic matrix composite materials, in particular to a fiber monolithic ultra-high temperature ceramic composite material and a preparation method thereof.
Background
The ultrahigh-temperature ceramic has excellent characteristics of high melting point, oxidation resistance, ablation resistance, high strength and the like, and is an excellent candidate high-temperature resistant material for hot end parts in the fields of high-speed aircrafts, rocket engines, aeroengines and the like. However, the ultrahigh-temperature ceramic has the intrinsic brittleness of a ceramic material, and is very easy to cause catastrophic damage in the using process. The bionic fiber monolithic structure is one of feasible ways for improving the brittleness of the ultrahigh-temperature ceramic, and the high-strength and high-toughness synergistic effect can be achieved by using the fibrous cell body and cell body interface structure of the bamboo fiber in the natural bamboo material for reference. Therefore, the ultra-high temperature ceramic composite material with the fiber monolithic structure becomes a research hotspot which is concerned by researchers at home and abroad.
The existing fiber monolithic structure ultrahigh-temperature ceramic composite material has the problems of difficult molding, poor mechanical property and the like.
Disclosure of Invention
The invention provides an ultrahigh-temperature ceramic composite material with a fiber monolithic structure and a preparation method thereof, which are used for overcoming the defects of difficult molding, poor mechanical property and the like of the ultrahigh-temperature ceramic composite material with the fiber monolithic structure in the prior art.
In order to achieve the purpose, the invention provides an ultrahigh-temperature ceramic composite material with a fiber monolithic structure, wherein the ceramic composite material is of a fiber monolithic structure and comprises a fiber cell body and a cell body interface; the cellule is carbon, and the cellule interface is one of TiC ceramic, zrC ceramic, hfC ceramic and TaC ceramic.
In order to realize the purpose, the invention also provides a preparation method of the fiber monolithic structure ultrahigh-temperature ceramic composite material, which comprises the following steps:
s1: the method comprises the following steps of (1) preparing a skin-core structure fiber with an outer layer made of ceramic and a core made of carbon by using a carbon fiber as a starting core fiber, using a transition metal, a transition metal fluoride and a molten salt medium as raw materials and adopting a molten salt disproportionation method;
s2: and (3) paving the skin-core structure fibers, and sintering by using discharge plasma to obtain the fiber monolithic structure ultrahigh-temperature ceramic composite material.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides an ultra-high temperature ceramic composite material with a fiber monolithic structure, which is of a fiber monolithic structure and comprises a fiber cell body and a cell body interface; the cellule is carbon, and the cellule interface is one of TiC ceramic, zrC ceramic, hfC ceramic and TaC ceramic. Compared with the traditional ultra-high temperature ceramic composite material with a fiber monolithic structure, the ultra-high temperature ceramic composite material takes the ultra-high temperature ceramic as the cellula body, and the carbon is taken as the cellula body, so that the quality of the ceramic composite material can be obviously reduced (the density of the ultra-high temperature ceramic is about 4-14 g/cm) 3 And the density of the carbon is about 1.5 to 1.8g/cm 3 ). In addition, the carbon fiber cell body keeps the excellent mechanical property of the original carbon fiber, so that the ceramic composite material has higher strength and toughness; meanwhile, the ceramic cell body interface has better oxidation resistance, can protect the ceramic cell body and the carbon fiber cell body from being oxidized, and finally enables the ceramic composite material to have good oxidation resistance.
2. The preparation method of the fiber monolithic structure ultrahigh-temperature ceramic composite material comprises two steps of preparing a skin-core structure fiber by a molten salt disproportionation method and sintering by discharge plasma. The outer layer prepared by the molten salt disproportionation method is ceramic, and the core part is the skin-core structure fiber of carbon, so that on one hand, the continuity of the skin-core structure fiber can be realized by using the carbon fiber as a template, on the other hand, the high requirement of the traditional extrusion molding of a cellula body on equipment is avoided, the advantages of simple equipment requirement, low reaction temperature and the like are achieved, and the integrated molding of the interface of the ultrafine cellula body and the cellula body can be realized. The spark plasma sintering process belongs to a mature process, has no special condition requirement, and has simple whole preparation process and short period. In addition, the raw materials such as carbon fiber and metal source are wide in source and easy to obtain, and can be popularized to industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is an SEM photograph of a core-sheath structured fiber prepared in example 1;
FIG. 2 is an SEM photograph of the fibrous monolithic ultra-high temperature ceramic composite prepared in example 1;
FIG. 3 is an SEM photograph of a core-sheath structured fiber prepared in example 2;
fig. 4 is an SEM photograph of the fibrous monolith structure ultra-high temperature ceramic composite prepared in example 2.
The implementation, functional features and advantages of the present invention will be further described with reference to the accompanying drawings.
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 addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
The drugs/reagents used are all commercially available without specific mention.
The invention provides an ultrahigh-temperature ceramic composite material with a fiber monolithic structure, which is of a fiber monolithic structure and comprises a fiber cell body and a cell body interface; the cellule is carbon, and the interface of the cellule is one of TiC ceramic, zrC ceramic, hfC ceramic and TaC ceramic.
Preferably, the volume content of the cell body interface in the ceramic composite material is 20-60%. The interface content of the cell body of the ultra-high temperature ceramic can achieve the effects of high temperature resistance, oxidation resistance and the like of the ultra-high temperature ceramic, and can fully play the effects of light weight, toughness and the like of the carbon fiber, so that the ceramic composite material has the synergistic properties of high temperature resistance, oxidation resistance, light weight, high toughness and the like.
The invention also provides a preparation method of the fiber monolithic structure ultrahigh-temperature ceramic composite material, which is characterized by comprising the following steps of:
s1: the method comprises the following steps of (1) preparing a skin-core structure fiber with a ceramic outer layer and carbon core part by using a carbon fiber as an initial core material fiber and using transition metal, transition metal fluoate and a molten salt medium as raw materials through a molten salt disproportionation method;
the purpose of adopting the molten salt disproportionation method is to grow the ultrahigh-temperature ceramic on the surface of the carbon fiber in situ, thereby forming a skin-core structure fiber with an outer layer of the ultrahigh-temperature ceramic and a core part of the carbon, realizing the integrated molding of a fiber cell body and a cell body interface, and laying a foundation for forming a fiber monolithic structure for a subsequent ultrahigh-temperature ceramic composite material; meanwhile, the molten salt disproportionation method has low process temperature and short reaction time, can reduce the damage of the carbon fiber and finally enables the composite material to have good mechanical property.
Preferably, in step S1, the molten salt disproportionation method is specifically: mixing carbon fiber, transition metal fluoride and molten salt medium in proportion, carrying out high-temperature reaction, cooling, and washing to obtain the skin-core structure fiber.
Preferably, the molar ratio of the carbon fiber to the transition metal powder to the transition metal fluoride to the molten salt medium is 1 (0.3-1) to (0.1-3) to (10-30). The type and proportion of the raw materials are controlled to ensure that an ultrahigh-temperature ceramic layer with a certain thickness grows on the surface of carbon fibers in a liquid molten salt medium and ensure that the carbon fibers do not react completely.
Preferably, the carbon fiber is a polyacrylonitrile-based carbon fiber.
Preferably, the transition metal is one of Ti, zr, hf and Ta; the transition metal fluoride salt is K 2 TiF 6 、K 2 ZrF 6 、K 2 HfF 6 And K 2 TaF 7 One kind of (1).
Preferably, the molten salt medium is LiCl-KCl eutectic salt or NaCl-KCl eutectic salt.
Preferably, the high-temperature reaction is carried out at 800-1200 ℃ for 1-5 h in argon atmosphere. The high temperature reaction process condition is controlled, and the aim is to control the growth of the ultrahigh temperature ceramic on the surface of the carbon fiber and reduce the damage of the carbon fiber by adjusting the reaction rate of the transition metal and the carbon and the nucleation growth speed of a reaction product.
S2: and (3) paving the skin-core structure fibers, and sintering by using discharge plasma to obtain the fiber monolithic structure ultrahigh-temperature ceramic composite material.
The spark plasma sintering is used for promoting the rapid sintering densification among the fibers with the skin-core structure, and finally obtaining the compact fiber monolithic structure ultrahigh-temperature ceramic composite material.
Preferably, in step S2, the temperature of the spark plasma sintering is 1600-2000 ℃, the pressure is 30-70 MPa, the time is 10-30 min, and the atmosphere is vacuum. The control of the spark plasma sintering process condition is to promote the sintering densification of the skin-core structure fiber, and finally obtain the fiber monolithic structure ultra-high temperature ceramic composite material.
Example 1
The embodiment provides a preparation method of a TaC ultra-high temperature ceramic composite material with a fiber monolithic structure, which comprises the following steps:
(1) Weighing 1.00g of carbon fiber, 4.52g of Ta powder 2 TaF 7 9.79g of powder and 55.41g of NaCl-KCl eutectic salt powder, uniformly mixing the four materials, pouring the mixture into a crucible, then placing the crucible into a high-temperature furnace for high-temperature reaction at 800 ℃ for 1h in argon gas as reaction atmosphere, and washing the product after cooling to obtain the skin-core structure TaC @ C fiber. Fig. 1 shows a sheath-core structured fiber prepared in this example. As can be seen from the figure, the fiber prepared in this example has an obvious skin-core structure, in which the outer ultra-high temperature ceramic layer is uniformly coated on the surface of the carbon fiber, and the core is unreacted carbon fiber.
(2) Placing the skin-core structure TaC @ C fiber in a graphite mould for unidirectional paving, then placing the graphite mould in a discharge plasma sintering furnace for sintering, setting the sintering temperature to be 1600 ℃, the pressure to be 30MPa, the time to be 10min and the atmosphere to be vacuum. And then cooling along with the furnace to obtain the TaC ultra-high temperature ceramic composite material with the fiber monolithic structure. Fig. 2 shows the ultra-high temperature ceramic composite material with the fibrous monolithic structure prepared in the embodiment. As can be seen from the figure, the fibrous cell body in the ultra-high temperature ceramic composite material with the fibrous monolithic structure is carbon, the cell body interface is TaC, and the two are uniformly distributed.
Example 2
The embodiment provides a preparation method of a TaC ultra-high temperature ceramic composite material with a fiber monolithic structure, which comprises the following steps:
(1) 1g of carbon fiber, 15.08g of Ta powder, K were weighed 2 TaF 7 32.67g of powder and 166.25g of NaCl-KCl eutectic salt powder, uniformly mixing the four materials, pouring the mixture into a crucible, then placing the crucible into a high-temperature furnace for high-temperature reaction at 1200 ℃ for 5 hours in argon gas as reaction atmosphere, and washing the product with water after cooling to obtain the skin-core structure TaC @ C fiber. Fig. 3 shows a sheath-core structured fiber prepared in this example. Can be seen from the figureThe fiber prepared by the embodiment has an obvious skin-core structure, wherein the outer ultrahigh-temperature ceramic layer is uniformly coated on the surface of the carbon fiber, and the core part is unreacted carbon fiber.
(2) Placing the skin-core structure TaC @ C fiber in a graphite mold for unidirectional laying, then placing the graphite mold in a discharge plasma sintering furnace for sintering, wherein the sintering temperature is 2000 ℃, the pressure is 50MPa, the time is 30min, and the atmosphere is vacuum. And then cooling along with the furnace to obtain the TaC ultra-high temperature ceramic composite material with the fiber monolithic structure. Fig. 4 shows the ultra-high temperature ceramic composite material with the fibrous monolithic structure prepared in the embodiment. As can be seen from the figure, the fibrous cell body in the ultra-high temperature ceramic composite material with the fibrous monolithic structure is carbon, the cell body interface is TaC, and the two are uniformly distributed.
Example 3
The embodiment provides a preparation method of a TiC ultrahigh-temperature ceramic composite material with a fiber monolithic structure, which comprises the following steps of:
(1) 1.0g carbon fiber, 2.0g Ti powder and K are weighed 2 TiF 6 30.0g of powder and 146.25g of LiCl-KCl eutectic salt powder, uniformly mixing the four, pouring the mixture into a crucible, then placing the crucible into a high-temperature furnace for high-temperature reaction at 1000 ℃ for 3 hours in argon atmosphere, cooling, and then washing the product with water to obtain the skin-core structure TiC @ C fiber;
(2) The skin-core structure TiC @ C fiber is placed in a graphite mold to be laid in a one-way mode, then the graphite mold is placed in a discharge plasma sintering furnace to be sintered, the sintering temperature is 1800 ℃, the pressure is 50MPa, the time is 10min, and the atmosphere is vacuum. And then cooling along with the furnace to obtain the TiC ultrahigh-temperature ceramic composite material with the fiber monolithic structure.
Example 4
The embodiment provides a preparation method of a fibrous monolithic ZrC ultrahigh temperature ceramic composite material, which comprises the following steps:
(1) 1g of carbon fiber, 2.28g of Zr powder 2 ZrF 6 21.27g of powder and 166.25g of NaCl-KCl eutectic salt powder, uniformly mixing the four, pouring the mixture into a crucible, placing the crucible into a high-temperature furnace for high-temperature reaction at 1000 ℃ for 1h in argon atmosphere, and coolingThen washing the product with water to obtain a skin-core structure ZrC @ C fiber;
(2) The skin-core structure ZrC @ C fiber is placed in a graphite mold for unidirectional laying, and then placed in a discharge plasma sintering furnace for sintering, wherein the sintering temperature is 1800 ℃, the pressure is 50MPa, the time is 10min, and the atmosphere is vacuum. And then cooling along with the furnace to obtain the fiber monolithic structure ZrC ultrahigh temperature ceramic composite material.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings, or any other related technical fields, which are directly or indirectly applied to the present invention, are included in the scope of the present invention.
Claims (9)
1. The ultra-high temperature ceramic composite material with the fibrous monolithic structure is characterized in that the ceramic composite material is of the fibrous monolithic structure and comprises a fibrous cell body and a cell body interface; the cellule body is carbon, and the cellule body interface is one of TiC ceramic, zrC ceramic, hfC ceramic and TaC ceramic; the volume content of a cell body interface in the ceramic composite material is 20-60%;
the preparation method of the ceramic composite material comprises the following steps:
s1: the method comprises the following steps of (1) preparing a skin-core structure fiber with a ceramic outer layer and carbon core part by using a carbon fiber as an initial core material fiber and using transition metal, transition metal fluoate and a molten salt medium as raw materials through a molten salt disproportionation method;
s2: and (3) paving the skin-core structure fibers, and sintering by using discharge plasma to obtain the fiber monolithic structure ultrahigh-temperature ceramic composite material.
2. A method for preparing a fibrous monolithic structured ultra high temperature ceramic composite according to claim 1, comprising the steps of:
s1: the method comprises the following steps of (1) preparing a skin-core structure fiber with a ceramic outer layer and carbon core part by using a carbon fiber as an initial core material fiber and using transition metal, transition metal fluoate and a molten salt medium as raw materials through a molten salt disproportionation method;
s2: and (3) paving the skin-core structure fibers, and sintering by using discharge plasma to obtain the fiber monolithic structure ultrahigh-temperature ceramic composite material.
3. The method according to claim 2, wherein in step S1, the molten salt disproportionation method is specifically: mixing carbon fiber, transition metal fluoride and molten salt medium in proportion, carrying out high-temperature reaction, cooling, and washing to obtain the skin-core structure fiber.
4. The production method according to claim 2 or 3, wherein the molar ratio of the carbon fiber, the transition metal powder, the transition metal fluoride salt and the molten salt medium is 1 (0.3 to 1): 0.1 to 3 (10 to 30).
5. The production method according to claim 4, wherein the carbon fiber is a polyacrylonitrile-based carbon fiber.
6. The production method according to claim 2 or 3, wherein the transition metal is one of Ti, zr, hf and Ta; the transition metal fluoride salt is K 2 TiF 6 、K 2 ZrF 6 、K 2 HfF 6 And K 2 TaF 7 One kind of (1).
7. A production method according to claim 2 or 3, characterized in that the molten salt medium is LiCl-KCl eutectic salt or NaCl-KCl eutectic salt.
8. The preparation method according to claim 3, wherein the high-temperature reaction is carried out at a temperature of 800 to 1200 ℃ for 1 to 5 hours under an atmosphere of argon.
9. The method according to claim 2, wherein in step S2, the temperature of the spark plasma sintering is 1600 to 2000 ℃, the pressure is 30 to 70MPa, the time is 10 to 30min, and the atmosphere is vacuum.
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| JP2008285745A (en) * | 2007-04-17 | 2008-11-27 | Sumitomo Precision Prod Co Ltd | High thermal conductive composite material |
| CN108530110A (en) * | 2018-06-08 | 2018-09-14 | 中南大学 | A kind of superhigh temperature ceramics coating of C/C composite materials and preparation method thereof |
| CN108794033A (en) * | 2018-06-28 | 2018-11-13 | 中国科学院兰州化学物理研究所 | A kind of self toughening fibrous monolithic ceramic structural ceramics and preparation method thereof |
| CN111039291A (en) * | 2018-10-12 | 2020-04-21 | 中国科学院金属研究所 | Method for preparing NbC and/or TaC powder in situ by molten salt disproportionation reaction |
| CN111848167A (en) * | 2020-06-18 | 2020-10-30 | 山东理工大学 | Preparation of exoskeleton structure fiber monolithic zirconium carbide ceramic by wet spinning coextrusion |
| CN111848208A (en) * | 2020-06-18 | 2020-10-30 | 日照鼎源新材料有限公司 | Wet spinning coextrusion preparation of straight-through hole zirconia ceramic with compact hole wall |
| CN112279646A (en) * | 2020-12-24 | 2021-01-29 | 中南大学 | Preparation method of molten salt infiltration material, ceramic interface modified material and ultrahigh-temperature ceramic modified composite material |
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