CN112442643B - Layered fiber toughened tungsten-based composite material and preparation method thereof - Google Patents
Layered fiber toughened tungsten-based composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a layered fiber toughening tungsten-based composite material and a preparation method thereof, wherein the layered fiber toughening tungsten-based composite material comprises a substrate layer and a toughening layer which are alternately stacked, wherein the substrate layer comprises a tungsten layer; the toughening layer comprises titanium foil and a tungsten fiber net; compared with pure tungsten, the layered fiber toughened tungsten-based composite material prepared according to the technical scheme provided by the invention has the toughness improved by 60-80%; the layered fiber toughened tungsten-based composite material has important practical significance on a first wall structure in a fusion reactor device.
Description
Technical Field
The invention relates to the technical field of composite material preparation, in particular to a layered fiber toughening tungsten-based composite material and a preparation method thereof.
Background
Tungsten and its alloy have high melting point, high hardness, high thermal conductivity, low sputtering corrosion rate, high self-sputtering threshold value, low vapor pressure, corrosion resistance and other excellent performances, and are widely applied to the fields of aerospace, energy and power, microelectronics, biomedicine, machining, medical equipment, illumination, glass fiber, national defense construction and the like. Particularly in the field of high-temperature energy equipment, such as first wall materials in nuclear fusion generation devices, reactor shunts, beam collectors of accelerators and magnetic fluids (MHD), and crucible materials with certain requirements on high-temperature performance.
Places where tungsten (W) and its alloys are typically used, such as aircraft rockets, machining equipment cutters, high-temperature pressure vessels, nuclear fusion reactors, all have very high requirements on the comprehensive mechanical properties of the materials. However, the Ductile-to-Brittle Transition Temperature (DBTT) is higher and reaches about 400 ℃; the recrystallization temperature is low, about 1200 ℃; the low-temperature brittleness and the recrystallization brittleness of tungsten are obvious, and the tungsten material with the performance defect can not be further applied in engineering.
In view of the above-mentioned drawbacks, the inventors of the present invention have finally obtained the present invention through a long period of research and practice.
Disclosure of Invention
In order to solve the technical defects, the invention adopts the technical scheme that a layered fiber toughening tungsten-based composite material is provided, which comprises a substrate layer and a toughening layer which are alternately stacked, wherein the substrate layer comprises a tungsten layer; the toughening layer comprises titanium foil and a tungsten fiber net.
Preferably, the thickness of the tungsten layer is 100-300 μm; the thickness of the titanium foil is 50-80 μm; the filament diameter of the tungsten fiber net is 30-100 mu m, and the pore diameter is 100-600 mu m.
Preferably, the thickness of the tungsten layer is 100-150 μm, the thickness of the titanium foil is 50 μm, the filament diameter of the tungsten fiber mesh is 50 μm, and the pore diameter is 600 μm.
Preferably, the preparation method of the layered fiber toughened tungsten-based composite material comprises the following steps:
s1: carrying out high-energy ball milling treatment on tungsten powder under the protection of inert gas;
s2: carrying out surface treatment on the tungsten fiber mesh and the titanium foil;
s3: loading the tungsten powder subjected to the high-energy ball milling treatment in the step S1, the tungsten fiber mesh and the titanium foil into a mold in an alternating and laminated manner to obtain a body to be sintered, wherein the titanium foil is placed on the upper side and the lower side of the tungsten fiber mesh;
s4: and performing discharge plasma sintering on the body to be sintered under a vacuum condition, wherein the sintering process is divided into three stages, the temperature of each stage is gradually increased, and the pressure is kept unchanged.
Preferably, in the step S1, the tungsten powder is subjected to high-energy ball milling under the protection of inert gas, dry milling is performed for 3h to 15h, and then anhydrous ethanol is added for wet milling for 3h to 8 h.
Preferably, the ball-material ratio of the high-energy ball mill is 8: 1-20: 1, and the rotating speed of the ball mill tank is 200 r/min-400 r/min.
Preferably, in step S4, the sintering process includes three stages:
in the first stage, the temperature is kept for 4-6 min under the conditions of 600-700 ℃ and 8-12 KN of pressure;
in the second stage, the temperature is kept for 15-20 min under the conditions of 1200-1400 ℃ and 8-12 KN of pressure;
and in the third stage, the temperature is kept for 2-4 min under the conditions of 1600-1800 ℃ and 8-12 KN of pressure.
Preferably, in the step S4, the temperature increase rate of spark plasma sintering is 50 ℃/min to 100 ℃/min.
Compared with the prior art, the invention has the beneficial effects that: compared with pure tungsten, the layered fiber toughness-increased tungsten-based composite material prepared according to the technical scheme provided by the invention has the toughness improved by 60-80%; the layered fiber toughened tungsten-based composite material has important practical significance for a first wall structure in a fusion reactor device.
Drawings
FIG. 1 is a schematic diagram of a sample of the layered fiber toughened tungsten-based composite;
FIG. 2 is a schematic diagram of the layered fiber toughened tungsten-based composite material SPS sintering process;
FIG. 3 is a diagram of the gold phase of the laminated fiber toughened tungsten-based composite material after corrosion according to the first embodiment;
FIG. 4 is a scanning electron microscope image of the fracture morphology of the tensile front surface of the layered fiber toughened tungsten-based composite material in the first embodiment;
FIG. 5 is a diagram of the gold phase of the laminated fiber-toughened tungsten-based composite material of example two after etching;
FIG. 6 is a scanning electron microscope image of the fracture morphology on the stretching front surface of the layered fiber toughened tungsten-based composite material according to the second embodiment.
Detailed Description
The above and further features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
The layered fiber toughening tungsten-based composite material comprises a substrate layer and a toughening layer which are alternately stacked, wherein the substrate layer comprises a tungsten layer; the toughening layer comprises titanium foil and a tungsten fiber net.
Further, the thickness of the tungsten layer is 100-300 μm; the thickness of the titanium foil is 50-80 μm; the filament diameter of the tungsten fiber net is 30-100 mu m, and the pore diameter is 100-600 mu m.
Preferably, when the thickness of the tungsten layer is 100 μm to 150 μm, the thickness of the titanium foil is 50 μm, the filament diameter of the tungsten fiber mesh is 50 μm, and the pore diameter is 600 μm, the layered fiber toughened tungsten-based composite material has good comprehensive performance.
A method for preparing the layered fiber toughened tungsten-based composite material comprises the following steps:
s1: carrying out high-energy ball milling on tungsten powder under the protection of inert gas;
s2: carrying out surface treatment on the tungsten fiber mesh and the titanium foil;
s3: loading the tungsten powder obtained in the step S1, and a tungsten fiber mesh and a titanium foil serving as toughening layers into a mold in an alternating and laminated manner to obtain a body to be sintered, wherein the titanium foil is placed on the upper side and the lower side of the tungsten fiber mesh;
s4: and (3) performing discharge plasma sintering on the to-be-sintered body obtained in the step (S3) under vacuum conditions, wherein the sintering process is divided into three stages, the temperature is gradually increased in each stage, and the pressure is kept constant.
Specifically, in step S1, the tungsten powder is subjected to high-energy ball milling under the protection of inert gas, dry milling is performed to refine the powder for 3 to 15 hours, and then anhydrous ethanol is added to wet milling to prevent the refined powder from agglomerating for 3 to 8 hours.
The ball-material ratio of the high-energy ball mill is 8: 1-20: 1, and the rotating speed of the ball mill tank is 200 r/min-400 r/min.
Specifically, in step S4, the sintering process includes three stages:
in the first stage, the temperature is kept for 4-6 min under the conditions of 600-700 ℃ and 8-12 KN of pressure;
in the second stage, the temperature is kept for 15-20 min under the conditions of 1200-1400 ℃ and 8-12 KN of pressure;
and in the third stage, the temperature is kept for 2-4 min under the conditions of 1600-1800 ℃ and 8-12 KN of pressure.
Further, in the step S4, the temperature increase rate in the spark plasma sintering is 50 to 100 ℃/min.
Compared with the conventional composite material for preparing a commonly used fiber composite material and a layered composite material, the layered fiber toughened tungsten-based composite material simultaneously introduces tungsten fibers and a metal titanium layer with good plasticity into the composite material, and sinters a hard-phase tungsten layer, a soft-phase titanium foil and a tungsten fiber net together to obtain the composite material with alternately superposed hard phases and soft phases, wherein the soft-phase titanium foil and the soft-phase tungsten fiber net are used as the toughened layers, and the tungsten fiber net cannot be directly contacted with a tungsten matrix in the sintering process due to the wrapping of the titanium metal layer, so that the surface of the tungsten fiber net does not need to be subjected to special film coating treatment.
After the composite material is acted by external force, the metal titanium and tungsten fibers in the toughening layer can generate plastic deformation to a greater degree so as to absorb a large amount of energy, the existence of the fibers can more effectively transmit and bear the external force, and a large amount of energy is consumed in the processes of fiber pulling-out, fiber and titanium foil interface debonding and interface crack expansion between the matrix layer and the titanium layer, so that the tip of a crack can be passivated to a certain degree, the crack can be bent and deflected, and the crack expansion path is prolonged; meanwhile, when the substrate layer of the hard phase is broken, the titanium foil and the fibers of the soft phase can play a role in bridging, so that further expansion of cracks is prevented, and the toughening effect is achieved; in addition, the titanium foil wraps and protects the fibers, so that toughening measures such as pulling-out of the tungsten fibers and the like caused by the fact that the tungsten of the matrix is tightly combined with the fibers in the sintering process are avoided.
The sintering method adopted by the invention is spark plasma sintering, has the advantages of high heating rate, uniform heating, low sintering temperature, short sintering time, high production efficiency and the like, can enable the matrix powder to generate solid phase sintering by controlling the sintering temperature, respectively generates metal recovery, recrystallization and densification at a low temperature stage, a medium temperature stage and a high temperature stage, and can effectively promote the densification of a sintered body and the firm combination of the matrix layer and the toughening layer interface by applying certain pressure.
Compared with pure tungsten, the layered fiber toughness-increased tungsten-based composite material prepared according to the technical scheme provided by the invention has the toughness improved by 60-80%. The layered fiber toughened tungsten-based composite material has important practical significance for a first wall structure in a fusion reactor device.
Example one
The embodiment is used for preparing the layered fiber toughened tungsten-based composite material, and the layered fiber toughened tungsten-based composite material comprises tungsten layers and toughening layers which are alternately stacked, wherein the thickness of each tungsten layer is about 150 micrometers, the thickness of each toughening layer is about 100 micrometers, and the toughening layers comprise tungsten fiber nets with the wire diameter of 30 micrometers and two layers of titanium foils with the thickness of 50 micrometers. The method comprises the following specific steps:
s1: and carrying out high-energy ball milling on the tungsten powder under the protection of argon to prepare tungsten-based powder.
The high-energy ball milling is carried out by dry milling for 8h, and then the dry milling is carried out by adding absolute ethyl alcohol for wet milling for 5 h. The ball-material ratio in the high-energy ball milling is 10: 1, and the rotating speed of a ball milling tank is 300 r/min.
S2: cutting titanium foil with thickness of 50 μm into pieces
And impregnating titanium with a cotton swab soaked in absolute ethanol
The foil surface was wiped clean. Cutting tungsten fiber net with wire diameter of 30 μm and pore diameter of 600 μm into pieces
The wafer is electropolished for 10s by taking 2 percent sodium hydroxide solution as polishing solution, and the aim is to removeAnd removing the oxide on the surface of the tungsten filament.
S3: alternately laminating the tungsten powder obtained in the step S1, the titanium foil obtained in the step S2 and the tungsten fiber net and filling the tungsten powder and the titanium foil into a graphite mold to obtain a body to be sintered, wherein the size of a cavity of the graphite mold is equal to that of the graphite mold
The wall thickness is 15 mm. The die filling is carried out according to the following sequence: firstly, a layer of tungsten powder is paved, then a layer of titanium foil is paved, a layer of tungsten fiber net is paved on the titanium foil, then a layer of titanium foil is paved, then a layer of tungsten powder is paved, and in this way, four toughening layers and five substrate layers are repeatedly filled. The thickness of the matrix layer is controlled by the quality of the tungsten powder, and when a sintered body with larger thickness needs to be prepared, the tungsten powder can be added. Since the tungsten powder has no loss or very little loss in the sintering process, which can be ignored, the mass of the tungsten layer in the sintered body is equal to that of the tungsten powder.
As shown in fig. 1, fig. 1 is a sample schematic diagram of the laminated fiber toughened tungsten-based composite material after specific sintering.
S4: the body to be sintered obtained in step S3 is subjected to spark plasma sintering under vacuum conditions, the sintering process being divided into three stages: in the first stage, the temperature is kept for 5min at 700 ℃ and under the pressure of 9.2 KN; in the second stage, the temperature is kept for 20min at 1300 ℃ under the pressure of 9.2 KN; the third stage is carried out at 1600 deg.C under 9.2KN for 2 min. Furthermore, the heating rate of the spark plasma sintering in the step is 13 ℃/min except before the first stage, and the rest heating and cooling rates are both 100 ℃/min.
As shown in fig. 2, fig. 2 is a schematic diagram of an SPS sintering process of the laminated fiber-toughened tungsten-based composite material.
And (3) taking out the graphite mold after sintering is finished, air-cooling to room temperature, and demolding the prepared sample to obtain the layered fiber toughness-enhanced tungsten-based composite material.
As shown in fig. 3, fig. 3 is a gold phase diagram of the laminated fiber toughened tungsten-based composite material (tungsten fiber mesh with a wire diameter of 30 μm) of the first embodiment after corrosion, a dark-colored tungsten matrix layer and a light-colored titanium layer are stacked on each other, and a dark-colored stripe-shaped texture, which is a tungsten fiber mesh, is clearly visible in the titanium layer. Meanwhile, the tungsten substrate layer, the toughening layer, the tungsten fiber net and the titanium foil are combined very tightly, and no obvious crack and other defects exist at the interface.
As shown in fig. 4, fig. 4 is a scanning electron microscope image of the fracture morphology on the tensile front surface of the laminated fiber toughened tungsten-based composite material in the embodiment.
The engineering stress-strain curve of the layered fiber toughened tungsten-based composite material and pure tungsten is obtained by performing uniaxial tensile test on the layered fiber toughened tungsten-based composite material and the pure tungsten, the total elongation after fracture of the material is used for representing the plastic deformation resistance of the material, the toughness of the material can be reacted, the higher the elongation is, the better the toughness is, and the total elongation after fracture is 4.1%, so that the toughness of the layered fiber toughened tungsten-based composite material is improved by 60.5% compared with that of the pure tungsten.
Example two
The main difference between this embodiment and the second embodiment is mainly the filament diameter of the tungsten fiber web.
The embodiment is used for preparing the layered fiber toughened tungsten-based composite material, and the layered fiber toughened tungsten-based composite material comprises tungsten layers and toughening layers which are alternately stacked, wherein the thickness of each tungsten layer is about 150 micrometers, the thickness of each toughening layer is about 100 micrometers, and the toughening layers comprise tungsten fiber nets with the wire diameter of 50 micrometers and two layers of titanium foils with the thickness of 50 micrometers. The method comprises the following specific steps:
s1: and carrying out high-energy ball milling on the tungsten powder under the protection of argon to prepare tungsten-based powder.
The high-energy ball milling is carried out by dry milling for 8h, and then the dry milling is carried out by adding absolute ethyl alcohol for wet milling for 5 h. The ball-material ratio in the high-energy ball milling is 10: 1, and the rotating speed of a ball milling tank is 300 r/min.
S2: cutting titanium foil with thickness of 50 μm into pieces
And wiping the surface of the titanium foil clean by using a cotton swab soaked in absolute ethyl alcohol. Cutting tungsten fiber net with filament diameter of 50 μm and pore diameter of 600 μm into pieces
Of wafers ofAnd 2% sodium hydroxide solution is used as polishing solution for electrolytic polishing for 10s, so as to remove oxides on the surface of the tungsten wire.
S3: alternately laminating the tungsten powder obtained in the step S1, the titanium foil obtained in the step S2 and the tungsten fiber net and filling the tungsten powder and the titanium foil into a graphite mold to obtain a body to be sintered, wherein the size of a cavity of the graphite mold is equal to that of the graphite mold
The wall thickness is 15 mm. The die filling is carried out according to the following sequence: firstly, a layer of tungsten powder is paved, then a layer of titanium foil is paved, a layer of tungsten fiber net is paved on the titanium foil, then a layer of titanium foil is paved, then a layer of tungsten powder is paved, and in this way, four toughening layers and five substrate layers are repeatedly filled. The thickness of the matrix layer is controlled by the quality of the tungsten powder, and when a sintered body with larger thickness needs to be prepared, the tungsten powder can be added. Since the tungsten powder has no loss or very little loss in the sintering process, which can be ignored, the mass of the tungsten layer in the sintered body is equal to that of the tungsten powder.
S4: the body to be sintered obtained in step S3 is subjected to spark plasma sintering under vacuum conditions, the sintering process being divided into three stages: in the first stage, the temperature is kept for 5min at 700 ℃ and under the pressure of 9.2 KN; in the second stage, the temperature is kept for 20min at 1300 ℃ under the pressure of 9.2 KN; the third stage is carried out at 1600 deg.C under 9.2KN for 2 min. Furthermore, the heating rate of the spark plasma sintering in the step is 13 ℃/min except before the first stage, and the rest heating and cooling rates are both 100 ℃/min.
And (3) taking out the graphite mold after sintering is finished, air-cooling to room temperature, and demolding the prepared sample to obtain the layered fiber toughness-enhanced tungsten-based composite material.
As shown in FIG. 5, FIG. 5 is a gold phase diagram of the corroded tungsten-based composite material (tungsten fiber mesh diameter 50 μm) toughened by the second layered fiber of the example, and it can be seen that a tungsten matrix layer with dark color and a titanium layer with light color are stacked. The tungsten substrate layer, the toughening layer, the tungsten fiber net and the titanium foil are combined very tightly, and no obvious defects such as cracks, gaps and the like exist at the interface. The tungsten fibers in the titanium layer in the second embodiment are more complete in shape due to the increase of the fiber diameter, and have better reinforcing and toughening effects on the composite material.
As shown in fig. 6, fig. 6 is a scanning electron microscope image of the fracture morphology on the tensile front surface of the second lamellar fiber-toughened tungsten-based composite material in the embodiment.
The engineering stress-strain curve of the layered fiber toughened tungsten-based composite material and pure tungsten is obtained by performing uniaxial tensile test on the layered fiber toughened tungsten-based composite material and the pure tungsten, the total elongation after fracture of the material is used for representing the plastic deformation resistance of the material, the toughness of the material can be reacted, the higher the elongation is, the better the toughness is, and the total elongation after fracture is 4.6%, so that the toughness of the layered fiber toughened tungsten-based composite material is improved by 78% compared with that of the pure tungsten.
In the invention, the numerical values of the ball-to-material ratio, the rotation speed of the ball-milling tank, the ball-milling time, the thickness of the tungsten layer during die filling, the sintering temperature, the heating rate, the sintering pressure, the heat preservation time and the like during the spark plasma sintering process are not specifically limited to the parameters in the above embodiments, nor are the numerical combinations of the above embodiments, but the adjustment of the parameters may have a certain influence on the preparation process and the toughening effect of the tungsten-based composite material for toughening the layer fibers.
The foregoing is merely a preferred embodiment of the invention, which is intended to be illustrative and not limiting. It will be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. The layered fiber toughened tungsten-based composite material is characterized by comprising a substrate layer and a toughening layer which are alternately stacked, wherein the substrate layer comprises a tungsten layer; the toughening layer comprises titanium foils and tungsten fiber nets, wherein the titanium foils are arranged on the upper side and the lower side of the tungsten fiber nets;
the thickness of the tungsten layer is 100-300 mu m; the thickness of the titanium foil is 50-80 μm; the filament diameter of the tungsten fiber net is 30-100 mu m, and the pore diameter is 100-600 mu m.
2. The layered fiber-toughened tungsten-based composite material according to claim 1 wherein the tungsten layer has a thickness of 100 to 150 μm, the titanium foil has a thickness of 50 μm and the tungsten fiber mesh has a filament diameter of 50 μm and a pore diameter of 600 μm.
3. A method of preparing a layered fibre-toughened tungsten based composite material according to claim 1 or 2 comprising the steps of:
s1: carrying out high-energy ball milling treatment on tungsten powder under the protection of inert gas;
s2: carrying out surface treatment on the tungsten fiber mesh and the titanium foil;
s3: loading the tungsten powder subjected to the high-energy ball milling treatment in the step S1, the tungsten fiber mesh and the titanium foil into a mold in an alternating and laminated manner to obtain a body to be sintered, wherein the titanium foil is placed on the upper side and the lower side of the tungsten fiber mesh;
s4: and performing discharge plasma sintering on the body to be sintered under a vacuum condition, wherein the sintering process is divided into three stages, the temperature of each stage is gradually increased, and the pressure is kept unchanged.
4. The preparation method according to claim 3, wherein in the step S1, the tungsten powder is subjected to high-energy ball milling under the protection of inert gas, and is subjected to dry milling for 3 to 15 hours, and then is added with absolute ethyl alcohol to be subjected to wet milling for 3 to 8 hours.
5. The preparation method of claim 4, wherein the ball-to-material ratio of the high-energy ball mill is 8: 1-20: 1, and the rotation speed of the ball mill tank is 200 r/min-400 r/min.
6. The method of claim 3, wherein in the step S4, the sintering process includes three stages:
in the first stage, the temperature is kept for 4-6 min under the conditions of 600-700 ℃ and 8-12 kN;
in the second stage, the temperature is kept for 15-20 min under the conditions of 1200-1400 ℃ and 8-12 kN;
in the third stage, the temperature is kept for 2min to 4min under the conditions of 1600 ℃ to 1800 ℃ and the pressure of 8kN to 12 kN.
7. The method according to claim 6, wherein in step S4, the temperature rise rate in spark plasma sintering is 50 ℃/min to 100 ℃/min.
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| CN114959518B (en) * | 2022-05-30 | 2023-01-31 | 合肥工业大学智能制造技术研究院 | Tungsten fiber and oxide nanoparticle synergistic toughening tungsten-based composite material and preparation method thereof |
| CN115404419B (en) * | 2022-09-20 | 2023-09-01 | 厦门钨业股份有限公司 | Preparation method of tungsten wire reinforced tungsten-based composite material |
| CN116460295B (en) * | 2023-04-27 | 2024-04-12 | 江苏科融新材料有限公司 | Preparation method of tungsten-lanthanum alloy wire |
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| 钛箔的拉伸力学性能及其组织结构研究;牛龙;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20200215(第2期);第23和30页 * |
| 钨基材料层状复合强化研究;杜靖元等;《化学工程与装备》;20170831(第8期);第1-3页 * |
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