CN107117981B - Layered Ti/B4C composite material and preparation method thereof - Google Patents
Layered Ti/B4C composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a layered Ti/B4C composite material and preparation thereofThe method belongs to the technical field of metal reinforced ceramic composite materials. The composite material consists of a Ti layer and a B layer4The C layers are sequentially and alternately superposed, and Ti and B4C has different thermal expansion coefficients and elastic moduli, so that the crack deflects when the crack expands in the composite material and gradually consumes the fracture energy, which is beneficial to improving the fracture toughness of the composite material; in addition, the interface strength can be improved by adding a small amount of Al, so that the mechanical property of the material is improved; further, use of Ti layer and B4Reducing the contact between the Ti layer and the B layer by the mode of grain surface between C layers4Degree of interfacial reaction between layers C. The method has simple process, easy operation and good industrial application prospect; and the prepared layered Ti/B4The C composite material has good microstructure, low porosity and good mechanical property.
Description
Technical Field
The invention relates to a layered Ti/B4A C composite material and a preparation method thereof, belonging to the technical field of metal reinforced ceramic composite materials.
Background
B4The C ceramic has low density (2.52 g/cm)3) High hardness (27.5-49.5 GPa), high wear resistance, strong chemical stability, excellent neutron absorptivity and the like, and is widely researched and gradually applied to the fields of protective armor, engineering structural parts, nuclear industry and the like in recent years. However, since B4The content of covalent bonds in C reaches 93.94%, so that the boron carbide ceramic has higher sintering temperature and poorer fracture toughness compared with other ceramic materials, thereby seriously limiting the wide application of the boron carbide ceramic in the engineering field and the military field.
The first proposal of the laminated ceramic matrix composite material is in the journal of Nature (Clegg W J, Kendall K, Alford N M, et al.A. simple way to make tough ceramics [ J ]. Nature,1990, 347(4):455-457.) in 1990), and a method for toughening SiC ceramic by taking a graphite layer as a toughness layer. With the development of research, a plurality of layered ceramic composite materials are appeared, wherein most of the layered ceramic composite materials are ceramic-ceramic layered composite materials, but the toughening effect is not obvious due to the fact that all layers of the layered ceramic composite materials are brittle materials. The metal-ceramic layered composite material is proposed based on the fact that the strength ceramic layer and the toughness metal layer are mutually overlapped and complement each other, but the layered metal-ceramic composite material is still under research because the stability between the layers is affected by the uncontrollable interface reaction between the metal and the ceramic during the sintering process.
Metal Ti is a light and stable transition metal, and is often used in the field of aviation and in severe service environments. In recent years, metallic Ti has been used as a reinforcing and toughening phase of ceramic materials, but since it has strong reducibility, it is very likely to react with the ceramic to generate a large amount of Ti compounds, thereby affecting the overall performance of the composite material.
Disclosure of Invention
Aiming at the problem that Ti is easy to react with a ceramic material in the prior art so as to influence the performance of a Ti-reinforced ceramic composite material, the invention aims to provide a layered Ti/B4C composite material consisting of a Ti toughening layer and B4C strength layers, Ti layers and B layers4The C-layer causes crack deflection in the fracture, so that the composite material has excellent fracture toughness.
It is another object of the present invention to provide a layered Ti/B4Method for preparing C composite material by using Ti layer and B4The mode of particle surface contact between C layers replaces the mode of integral contact of the traditional uniform massive materials, so that Ti and B are enabled to be in contact with each other4The degree of interfacial reaction between C is reduced, and the interfacial diffusion behavior between the layers is such that the Ti layer and B4The layer C is tightly combined, so that the mechanical property of the composite material is improved; moreover, the method has simple process, easy operation and good industrial application prospect.
The purpose of the invention is realized by the following technical scheme.
Layered Ti/B4C composite material consisting of a Ti layer and B4The C layers are sequentially and alternately superposed; wherein each Ti layer has a thickness of 0.2-0.4 mm, and each B layer has a thickness of 0.2-0.4 mm4The thickness of the C layer is 0.4 mm-0.8 mm.
Furthermore, the composite material also contains Al which can generate liquid phase in the sintering process as a sintering aid, so that the interface bonding strength of the ceramic layer and the metal layer is promoted; the mass ratio of the Al to the Ti is 4-8: 100, and the mass fraction of the Al in the composite material is not more than 3%.
The layered Ti/B of the invention4The preparation method of the composite material comprises the following steps:
(1) preparation of layered Ti/B4C composite green body
(a) When no Al is added: respectively mixing titanium powder and B with polyvinyl alcohol as binder4Dry pressing the C powder to obtain Ti sheets with thickness of 0.2-0.4 mm and B sheets with thickness of 0.4-0.8 mm4C thin slice, then Ti thin slice and B thin slice4C sheets are sequentially and alternately superposed to obtain layered Ti/B4C, green bodies of the composite material;
(b) when Al is added: carrying out wet ball milling mixing on titanium powder, aluminum powder, absolute ethyl alcohol and polyethylene glycol, and drying the slurry subjected to ball milling under a vacuum condition to obtain Al/Ti mixed powder; respectively mixing Al/Ti mixed powder and B with polyvinyl alcohol as binder4Dry pressing the C powder to obtain Ti sheet with thickness of 0.2-0.4 mm and doped Al and B sheet with thickness of 0.4-0.8 mm4C thin slice, then Ti thin slice and B thin slice4C sheets are sequentially and alternately superposed to obtain layered Ti/B4C, green bodies of the composite material;
(2) vacuum hot pressing sintering
Laminating Ti/B4Placing the green body of the C composite material in a vacuum hot-pressing sintering furnace for vacuum hot-pressing sintering, and cooling to obtain the layered Ti/B4C, a composite material;
the pressure of dry pressing is 10MPa to 30MPa, and the pressure maintaining time is 5min to 10 min;
the vacuum degree in the vacuum hot-pressing sintering furnace is not lower than 6.63 × 10-3Pa, sintering temperature of 1700-1800 ℃, sintering pressure of 20-30 MPa, and sintering time of 1-2 h.
The average particle diameter of the titanium powder is preferably 5 to 10 μm, the average particle diameter of the aluminum powder is preferably 1 to 3 μm, B4The average particle diameter of the C powder is preferably 3 to 5 μm.
Has the advantages that:
(1) the invention proposes to use metal Ti as toughening layer and ceramic B4C as a strength layer, a Ti layer and B4The C layers are sequentially and alternately superposed and sintered to form layered Ti/B4C composite material, high-toughness Ti layer and high-strength B4The C layers are alternately arranged, and Ti and B4C has different thermal expansion coefficients and elastic moduli, thereby leading the crack to deflect and gradually consume the fracture energy when the layered material expands, prolonging the crack expansion length and being beneficial to the layered Ti/B4C, improving the fracture toughness of the composite material;
(2) in the preparation process of the invention, the Ti layer and the B layer are utilized4The mode of particle surface contact between C layers replaces the mode of integral contact of the traditional uniform massive materials, thereby reducing the Ti layer and B layer4Degree of interfacial reaction between layers C; in addition, since Ti and Al have strong reducibility, this makes Ti/B4Diffusion of elements at the C layer interface and formation of e.g. TiB2TiAlX and Al8B4C7The interface reaction product enables the combination between the metal and the ceramic to be changed into metallurgical combination from physical combination before sintering, and the interface combination strength is improved, thereby improving the mechanical property of the composite material;
(3) the method has simple process, easy operation and good industrial application prospect; and the prepared layered Ti/B4The C composite material has good microstructure, low porosity and good mechanical property.
Drawings
FIG. 1 is a Ti/B layer in the examples4X-ray diffraction (XRD) pattern of the C composite.
FIG. 2 shows the layered Ti/B of the example4Scanning Electron Microscope (SEM) images of low power sections of the C composite.
FIG. 3 is a layered Ti/B of example 14High power cross-section SEM image of C composite.
FIG. 4 is a layered Ti/B of example 14C picture of crack propagation of composite material.
Detailed Description
The present invention will be further described with reference to the following embodiments.
In the following examples:
titanium powder: the average grain diameter is 5 mu m, and the method is applied to the sea water field;
aluminum powder: the average grain diameter is 1 mu m, and the method is applied to the sea water field;
B4c, powder body: the average grain diameter is 3 mu m, and the method is applied to the sea water field;
polyvinyl alcohol: PVAl7-92 (molecular weight 17 ten thousand) with high polymerization degree, and Chengjin Co., Ltd.
Relative density: testing by adopting a drainage method;
and (3) testing mechanical properties: testing the bending strength and the fracture toughness according to the standard GB/T4741-1999, GB/T GB/T23806-2009;
XRD characterization: the type of the X-ray diffractometer used was D8-ADVANCE, manufacturer: germany bloke electrons;
and (3) SEM appearance characterization: the model of the scanning electron microscope used is S-4800, manufacturer: hitachi, Japan.
Example 1
(1) 50g of titanium powder, 3g of aluminum powder, 400mL of absolute ethyl alcohol and 0.5g of polyethylene glycol (molecular weight 4000) are added into a ball milling tank, and ZrO is added according to the ball-to-material ratio of 10:12Ball-milling for 12h at the rotating speed of 150r/min, and drying the slurry which is uniformly mixed after ball-milling in a vacuum drying oven at the temperature of 80 ℃ for 8h to obtain Al/Ti mixed powder;
(2) respectively processing Al/Ti mixed powder and B under the pressure of 30MPa by using polyvinyl alcohol as a binder4Dry pressing the C powder for 10min to obtain the product with thickness of 0.2mm Al-doped Ti flakes and B with a thickness of 0.4mm4C thin slice, then Ti thin slice and B thin slice4C sheets are sequentially and alternately superposed to obtain layered Ti/B4C, green bodies of the composite material;
(3) laminating Ti/B4Placing the green body of the C composite material in a vacuum hot-pressing sintering furnace until the vacuum degree reaches 6.63 × 10-3At the temperature of 1800 ℃ under the sintering pressure of 30MPa for 2h under Pa, and cooling along with the furnace to obtain the layered Ti/B4C, a composite material; wherein the prepared layered Ti/B4The C composite material contains 3 mass percent of Al.
The composite material prepared in this example was characterized: the relative density was found to be 98.2%, the bending strength was 622.3MPa, and the fracture toughness was 7.88MPa · m1/2. As can be seen from FIG. 1, the main phase in the composite material prepared is B4C. Ti and TiB2In addition, intermetallic compounds TiAlXAnd Al-B-C solid solution Al8B4C7It can be seen that the Ti layer and B layer are formed during the sintering process4The C layer has an interface reaction to generate TiB2And Al in the Ti layer is simultaneously with B4C reacts to form Al8B4C7The presence of the interface product greatly enhances the Ti layer and B4The bonding force between the C layers improves the bonding strength. In the SEM images of FIGS. 2 and 3, the darker color is B4The layer C is a Ti layer with lighter color, so that the prepared composite material has a tough metal Ti layer and a high-strength ceramic B layer4The C layers are mutually overlapped to form a strong and tough alternating laminated structure, and the interfaces are clear and tightly combined. The results of combining XRD and SEM images can be judged: ti layer and B4The bonding between the C layers is changed from physical bonding before sintering into metallurgical bonding, so that the interface bonding strength is improved. The white dotted line in FIG. 4 indicates that the cracks are in the layered Ti/B4C the propagation path of the composite material, the visible crack deflection basically occurs in the Ti layer and the B4At the interface of the C layer, this is due to Ti and B4C has different thermal expansion coefficient and elastic modulus, so that the crack can deflect and gradually consume the fracture when the crack propagates among the layered materialsCan extend the crack propagation length and further make the layered Ti/B4The fracture toughness of the C composite material is improved.
Example 2
(1) 50g of titanium powder, 2g of aluminum powder, 400mL of absolute ethyl alcohol and 0.5g of polyethylene glycol (molecular weight 4000) are added into a ball milling tank, and ZrO is added according to the ball-to-material ratio of 10:12Ball-milling for 12h at the rotating speed of 150r/min, and drying the slurry which is uniformly mixed after ball-milling in a vacuum drying oven at the temperature of 80 ℃ for 8h to obtain Al/Ti mixed powder;
(2) respectively processing Al/Ti mixed powder and B under the pressure of 10MPa by using polyvinyl alcohol as a binder4Performing dry pressing on the C powder, and maintaining the pressure for 5min to correspondingly obtain Ti sheets with the thickness of 0.4mm and doped with Al and B with the thickness of 0.8mm4C thin slice, then Ti thin slice and B thin slice4C sheets are sequentially and alternately superposed to obtain layered Ti/B4C, green bodies of the composite material;
(3) laminating Ti/B4Placing the green body of the C composite material in a vacuum hot-pressing sintering furnace until the vacuum degree reaches 6.63 × 10-3At the temperature of 1800 ℃ under the sintering pressure of 30MPa for 2h under Pa, and cooling along with the furnace to obtain the layered Ti/B4C, a composite material; wherein the prepared layered Ti/B4The C composite material contains 2 mass percent of Al.
The composite material prepared in this example was characterized: the relative density was found to be 97.5%, the bending strength was found to be 601.3MPa, and the fracture toughness was found to be 7.22MPa · m1/2. According to the spectrum obtained by XRD characterization, the main phase in the prepared composite material is B4C. Ti and TiB2In addition, a small amount of intermetallic compound TiAlXAnd Al-B-C solid solution Al8B4C7The presence of these interface products greatly enhances the Ti layer and B4The bonding force between the C layers improves the bonding strength. According to the SEM image obtained by the morphology characterization, the prepared composite material has B with darker color4Layer C and a Ti layer with lighter color, which shows that the prepared composite material is a tough metal Ti layer and a high-strength ceramic B4The C layers are sequentially and alternately formedThe layered structure of (1). According to the characterization results of XRD and SEM, the following can be judged: ti layer and B4The bonding between the C layers is changed from physical bonding before sintering into metallurgical bonding, so that the interface bonding strength is improved. When the cracks are expanded in the composite material prepared in the embodiment, the phenomena of crack deflection and gradual consumption of fracture energy also occur, the crack expansion length is prolonged, and further the layered Ti/B4The fracture toughness of the C composite material is improved.
Example 3
(1) 50g of titanium powder, 3g of aluminum powder, 400mL of absolute ethyl alcohol and 0.5g of polyethylene glycol (molecular weight 4000) are added into a ball milling tank, and ZrO is added according to the ball-to-material ratio of 10:12Ball-milling for 12h at the rotating speed of 150r/min, and drying the slurry which is uniformly mixed after ball-milling in a vacuum drying oven at the temperature of 80 ℃ for 8h to obtain Al/Ti mixed powder;
(2) polyvinyl alcohol is used as a binder to respectively react the Al/Ti mixed powder and the B under the pressure of 20MPa4Performing dry pressing on the C powder, and maintaining the pressure for 8min to correspondingly obtain Ti sheets with the thickness of 0.4mm and doped with Al and B with the thickness of 0.8mm4C thin slice, then Ti thin slice and B thin slice4C sheets are sequentially and alternately superposed to obtain layered Ti/B4C, green bodies of the composite material;
(3) laminating Ti/B4Placing the green body of the C composite material in a vacuum hot-pressing sintering furnace until the vacuum degree reaches 6.63 × 10-3At the temperature of 1700 ℃ under the sintering pressure of 20MPa for 1 hour under Pa, and cooling along with the furnace to obtain the layered Ti/B4C, a composite material; wherein the prepared layered Ti/B4The C composite material contains 3 mass percent of Al.
The composite material prepared in this example was characterized: the relative density was found to be 96.4%, the bending strength was 589.7MPa, and the fracture toughness was 6.92MPa · m1/2. According to the spectrum obtained by XRD characterization, the main phase in the prepared composite material is B4C. Ti and TiB2In addition, a small amount of intermetallic compound TiAlXAnd Al-B-C solid solution Al8B4C7The presence of these interface products greatly enhances the Ti layer and B4The bonding force between the C layers improves the bonding strength. According to the SEM image obtained by the morphology characterization, the prepared composite material has B with darker color4Layer C and a Ti layer with lighter color, which shows that the prepared composite material is a tough metal Ti layer and a high-strength ceramic B4The C layers are sequentially and alternately formed into a layered structure. According to the characterization results of XRD and SEM, the following can be judged: ti layer and B4The bonding between the C layers is changed from physical bonding before sintering into metallurgical bonding, so that the interface bonding strength is improved. When the cracks are expanded in the composite material prepared in the embodiment, the phenomena of crack deflection and gradual consumption of fracture energy also occur, the crack expansion length is prolonged, and further the layered Ti/B4The fracture toughness of the C composite material is improved.
Example 4
(1) Using polyvinyl alcohol as binder, respectively adding titanium powder and B powder under 20MPa4Dry pressing the C powder, maintaining the pressure for 5min to obtain Ti sheet with thickness of 0.2mm and B sheet with thickness of 0.4mm4C thin slice, then Ti thin slice and B thin slice4C sheets are sequentially and alternately superposed to obtain layered Ti/B4C, green bodies of the composite material;
(2) laminating Ti/B4Placing the green body of the C composite material in a vacuum hot-pressing sintering furnace until the vacuum degree reaches 6.63 × 10-3At the temperature of 1800 ℃ under the sintering pressure of 30MPa for 1.5h under Pa, and cooling along with the furnace to obtain the layered Ti/B4C, a composite material;
the composite material prepared in this example was characterized: the relative density was found to be 97.1%, the bending strength was 608.2MPa, and the fracture toughness was 7.14MPa · m1/2. According to the spectrum obtained by XRD characterization, the main phase in the prepared composite material is B4C. Ti and TiB2And a small amount of TiC. According to the SEM image obtained by the morphology characterization, the prepared composite material has B with darker color4Layer C and a Ti layer with lighter color, which shows that the prepared composite material is a tough metal Ti layer and a high-strength ceramic B4The C layers are sequentially and alternately formed into a layered structure. According to the characterization results of XRD and SEM, the method can be used for measuring the grain sizeAnd (3) judging: ti layer and B4The bonding between the C layers is changed from physical bonding before sintering into metallurgical bonding, so that the interface bonding strength is improved. When the cracks are expanded in the composite material prepared in the embodiment, the phenomena of crack deflection and gradual consumption of fracture energy also occur, the crack expansion length is prolonged, and further the layered Ti/B4The fracture toughness of the C composite material is improved.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. Layered Ti/B4C composite material, characterized in that: the composite material consists of a Ti layer and a B layer4The C layers are sequentially and alternately superposed; wherein each Ti layer has a thickness of 0.2-0.4 mm, and each B layer has a thickness of 0.2-0.4 mm4The thickness of the C layer is 0.4 mm-0.8 mm;
the composite material contains Al with the mass fraction not more than 3%, and the mass ratio of the mass of the Al to the mass of Ti is 4-8: 100;
the layered Ti/B4The preparation method of the C composite material comprises the following steps:
(1) carrying out wet ball milling mixing on titanium powder, aluminum powder, absolute ethyl alcohol and polyethylene glycol, and drying the slurry subjected to ball milling under a vacuum condition to obtain Al/Ti mixed powder; respectively mixing Al/Ti mixed powder and B with polyvinyl alcohol as binder4Dry pressing the C powder to obtain Ti sheet with thickness of 0.2-0.4 mm and doped Al and B sheet with thickness of 0.4-0.8 mm4C, thin slice; then, the Ti flakes and B are mixed4C sheets are sequentially and alternately superposed to obtain layered Ti/B4C, green bodies of the composite material;
(2) laminating Ti/B4Placing the green body of the C composite material in a vacuum hot-pressing sintering furnace for vacuum hot-pressing sintering, and cooling to obtain the layered Ti/B4C, a composite material;
in the step (1), the pressure of dry pressing is 10 MPa-30 MPa, and the pressure maintaining time is 5 min-10 min;
in the step (2), the vacuum degree in the vacuum hot-pressing sintering furnace is not lower than 6.63 × 10-3Pa, the sintering temperature is 1700-1800 ℃, the sintering pressure is 20-30 MPa, and the sintering time is 1-2 h;
the average grain diameter of the titanium powder is 5-10 mu m, the average grain diameter of the aluminum powder is 1-3 mu m, B4The average grain diameter of the C powder is 3-5 mu m.
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