CN113458400B - Ti-Al 3 Preparation method of Ti intermetallic compound laminated composite board - Google Patents
Ti-Al 3 Preparation method of Ti intermetallic compound laminated composite board Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/006—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of flat products, e.g. sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
- B22F2007/042—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention relates to a laminated composite board, in particular to a Ti-Al composite board 3 Ti intermetallic compound laminated composite board, in particular to a Ti-Al 3 A method for preparing Ti intermetallic compound laminated composite board. The invention aims to solve the problems of the prior Ti-Al 3 The problem of abrupt change of mechanical properties of the Ti intermetallic compound laminated composite board at the interface is solved, and a new Ti-Al is provided 3 Ti intermetallic compound laminated composite board preparation method, ti is used for preparing 3 AlC 2 Introducing conventional Ti-Al 3 Interface layer of Ti intermetallic compound laminated composite board is sintered by hot pressing, and Ti and Al are mutually diffused, and finally Ti and Al are formed 3 Ti interface formation contains Ti 3 AlC 2 /Al 3 The transition interface layer of Ti phase solves the problem of abrupt change of mechanical property at the interface, and the preparation process is simple and feasible and is suitable for commercial production.
Description
Technical Field
The invention relates to a laminated composite board, in particular to a Ti-Al composite board 3 Ti intermetallic compound laminated composite board, in particular to a Ti-Al 3 A method for preparing Ti intermetallic compound laminated composite board.
Background
Intermetallic compound laminated composite board is made of ductile goldThe composition is formed by alternately superposing brittle intermetallic compounds. The last nineties of the century, the American scientist developed Ti-Al 3 Ti intermetallic compound laminated composite panel in which intermetallic compound Al 3 Ti is alternately laminated with a ductile metal layer Ti due to the characteristics of high hardness, large modulus, small density and the like, and the structure of the alternately laminated brittle-ductile material imitates a natural shell organic-inorganic material, when being impacted, the Ti can better absorb impact kinetic energy due to the unique failure modes of crack deflection, layer-by-layer failure and the like of an interface, so that the Ti-based alloy composite material is widely applied to the armor protection and industrial production fields, however, the Ti-based alloy composite material is also used for the protection of the armor and the industrial production field due to the fact that the Ti-based alloy composite material is composed of Ti and Al 3 The difference of mechanical properties of Ti is large, for example, the Vickers hardness of Ti is about 310HV, al 3 The Vickers hardness of Ti reaches about 660HV to 750HV, and the Ti and Al 3 The abrupt change of mechanical properties at the Ti interface is extremely easy to cause the concentration of interface stress, so that the laminated composite board generates cracks at the interface, and finally the laminated composite board cracks at the interface.
Disclosure of Invention
The invention aims to solve the problems of the prior Ti-Al 3 The problem of abrupt change of mechanical properties of the Ti intermetallic compound laminated composite board at the interface is solved, and a new Ti-Al is provided 3 A method for preparing Ti intermetallic compound laminated composite board.
The invention is realized by adopting the following technical scheme: ti-Al 3 The preparation method of the Ti intermetallic compound laminated composite board comprises the following steps:
1) Preparing Al and Ti which are uniformly mixed 3 AlC 2 Composite powder: filling Al powder with the granularity of 10 mu m into a high-energy ball mill for ball milling, wherein the ball-material ratio is 10:1, the rotating speed is 100-200 r/min, the ball milling time is 8-15h, and then the ball-milled Al powder and Ti with the granularity of 1 mu m are subjected to ball milling according to the mass ratio of 1:5-1:9 3 AlC 2 Proportioning the powder, and mixing the Al powder and Ti 3 AlC 2 The powder is put into a ball milling tank for ball milling, the ball milling time is 8-15h, argon is introduced for protection during the ball milling process, and ethanol with the concentration of 1% is added as a process control agent, so that composite powder is formed;
2) Acid-base cleaning Ti plate and Al plate: treating a Ti plate with the thickness of 0.5 and mm by using a hydrofluoric acid solution with the concentration of 5%, taking out and cleaning by using clear water, placing the Ti plate cleaned by the clear water into an ultrasonic cleaner for ultrasonic cleaning, and finally drying the Ti plate cleaned by using a blower; treating an Al plate with the thickness of 0.5 and mm by using a sodium hydroxide solution with the concentration of 5%, taking out and cleaning by using clear water, placing the Al plate cleaned by the clear water into an ultrasonic cleaner for ultrasonic cleaning, and finally drying the Al plate cleaned by the ultrasonic cleaner by using a blower;
3) And (3) laminating and packaging: alternately laminating the Ti plates and the Al plates subjected to acid-base cleaning, wherein composite powder with the powder thickness of 0.1-0.15mm is laminated between the Ti plates and the Al plates, and the outermost layers are ensured to be Ti plates, so that laminated plates are formed, and the laminated plates are packaged by adopting Ti foil with the thickness of 20 mu m, so that a package body is formed; (the composite powder cannot be too thick or too thin, which results in too low hardness gradient and failure to exert Ti-Al 3 The Ti intermetallic compound laminated composite board has the advantages of being overlapped by heterogeneous materials and bringing about mechanical properties, the composite powder is too thin to be paved, and the interface hardness gradient cannot be effectively reduced
4) Vacuum hot pressing sintering: placing the packaging body in a vacuum hot-pressing sintering furnace, and then performing vacuum hot-pressing sintering on the packaging body according to the following steps:
applying 20-30 MPa pressure to the obtained package, increasing sintering temperature to 600deg.C at 5-15deg.C/min, and maintaining for 120 min at 3-5 MPa (in this step, ti plate reacts with Al powder and Al plate in the composite powder to form transition interface layer Ti 3 AlC 2 /Al 3 Ti）；/>
Raising the sintering temperature to 660 ℃ at a speed of 5 ℃/min, and preserving heat for 90 min, wherein the pressure is 0.5-1MPa during the heat preservation period; />
Raising sintering temperature to 665 deg.c at 5 deg.c/min and maintaining the temperature for 210min at 0.5 MPa to form Al 3 A Ti layer); />
Reducing the temperature to 550 ℃ at a speed of 5 ℃/min, and preserving the heat for 180min, wherein the pressure is 0.5-1 MPa; />
Reducing the temperature to 200 ℃ at a rate of 5 ℃/min, and keeping the pressure at 0.5-1 MPa; />
And (3) closing a heating device of the vacuum hot-pressing sintering furnace, and cooling the packaging body along with the furnace to room temperature to finish the preparation, wherein the pressure is 0.5-1MPa during the cooling period.
Principle analysis:
1) Between Ti plate and Al plate Ti 3 AlC 2 The composite powder composed of the powder and the Al powder has the function of generating a transition interface layer Ti 3 AlC 2 /Al 3 Ti. In the preparation process Ti 3 AlC 2 The powder is mixed and divided into Al powder, and Ti plate and Ti are mixed and divided into 3 AlC 2 The Al powder around the powder is directly contacted; throughout the preparation process, ti 3 AlC 2 The powder does not react with Al powder in the Al plate, the Ti plate and the composite powder, ti 3 AlC 2 Exists as a second phase in newly formed Al 3 In the Ti layer, to Al 3 The Ti layer has toughening effect, namely, a thin transition interface layer Ti is generated between Ti and Al plates 3 AlC 2 /Al 3 Ti. As the reaction proceeds, the Ti and Al plates form Al 3 And a Ti layer. Transition interface layer Ti 3 AlC 2 /Al 3 The hardness of Ti is between the hardness of Ti and Al 3 Between the hardness of Ti, between the Ti plate and Al 3 The Ti interface plays a transitional role to avoid Ti and Al 3 The mechanical property of the Ti interface is suddenly changed, and the stress concentration is greatly relaxed when the Ti interface is impacted;
2) According to the user's relation between Ti plate and Al 3 The hardness gradient at the Ti interface has different requirements, and the preparation can be carried out by adjusting the Al powder and Ti in the composite powder 3 AlC 2 The ratio of the powder (adjusted in the ratio interval) and the thickness of the composite powder layer (adjusted in the thickness interval) are used for realizing Ti plates and Al with different sizes 3 The hardness gradient at the interface between Ti and Ti meets the requirements of different users by adopting the same preparation principle.
The beneficial effects of the invention are as follows: the preparation method is simple and feasible, and solves the problems of Ti-Al 3 Mechanical properties of the interface of the Ti intermetallic compound laminated composite board are suddenly changed, and meanwhile, the Ti board and the Al can be prepared according to the requirements of users 3 The intermetallic compound laminated composite board with different hardness gradients at the Ti interface is widely applied to commercial production.
Drawings
FIG. 1 is a schematic diagram of the distribution of a laminate prior to vacuum hot-pressed sintering;
FIG. 2 is Ti-Al 3 Schematic of the final product of the Ti intermetallic compound layered composite plate (the points in the figure represent Ti 3 AlC 2 A powder);
FIG. 3 is a graph showing the hardness distribution in the vicinity of the interface of the laminated composite sheet (the horizontal axis represents the hardness measurement points of the laminated composite sheet set in the thickness direction of the laminated sheet in this order, the vertical axis represents the hardness, and the circle represents Ti-Al 3 At the Ti interface).
In the figure: 1-Ti plate, 2-composite powder, 3-Al plate, 4-Al 3 Ti layer, 5-transition interface layer Ti 3 AlC 2 /Al 3 Ti。
Detailed Description
Ti-Al 3 The preparation method of the Ti intermetallic compound laminated composite board comprises the following steps:
1) Preparing Al and Ti which are uniformly mixed 3 AlC 2 Composite powder 2: loading Al powder with particle size of 10 μm into high-energy ball mill, ball milling at ball-material ratio of 10:1 and rotational speed of 100-200 r/min (such as 100 r/min,130 r/min,150 r/min,165 r/min,170 r/min,186 r/min,190 r/min,200 r/m)in), the ball milling time is 8-15h (for example, the ball milling time is 8h,9h,10h,11h,12h,13h,14h,15 h), and then the ball milled Al powder and Ti with granularity of 1 μm are subjected to ball milling according to the mass ratio of 1:9-1:5 (for example, 1:9,1:8,1:7,1:6 and 1:5) 3 AlC 2 Proportioning the powder, and mixing the Al powder and Ti 3 AlC 2 The powder is put into a ball milling tank for ball milling for 8-15h (such as 8h,9h,10h,11h,12h,13h,14h and 15 h) and argon is introduced for protection during ball milling, and ethanol with the concentration of 1% is added as a process control agent, so that composite powder is formed;
2) Acid-base cleaning Ti plate and Al plate: treating a Ti plate 1 with the thickness of 0.5mm with a hydrofluoric acid solution with the concentration of 5%, taking out and cleaning with clear water, putting the Ti plate 1 cleaned with clear water into an ultrasonic cleaner for ultrasonic cleaning, and finally drying the Ti plate 1 cleaned with ultrasonic waves by using a blower; treating an Al plate 3 with the thickness of 0.5mm by using a sodium hydroxide solution with the concentration of 5%, taking out and cleaning by using clear water, putting the Al plate 3 cleaned by the clear water into an ultrasonic cleaner for ultrasonic cleaning, and finally drying the Al plate 3 cleaned by the ultrasonic cleaner by using a blower;
3) And (3) laminating and packaging: alternately laminating the Ti plates 1 and the Al plates 3 subjected to acid-base cleaning, wherein composite powder 2 with the powder thickness of 0.1-0.15mm (0.1mm,0.11 mm,0.12 mm,0.13 mm,0.14 mm,0.15 mm) is laminated between the Ti plates 1 and the Al plates 3, and the outermost layers are all Ti plates 1, so that a laminated plate is formed, and the laminated plate is packaged by adopting a Ti foil with the thickness of 20 mu m, so that a package body is formed; (the composite powder 2 cannot be too thick or too thin, which results in too low hardness gradient and failure to exert Ti-Al 3 The Ti intermetallic compound laminated composite board has the advantages of heterogeneous material lamination on mechanical property, the composite powder is too thin, the lamination is difficult, and the final interface gradient hardness is still large
4) Vacuum hot pressing sintering: placing the packaging body in a vacuum hot-pressing sintering furnace, and then performing vacuum hot-pressing sintering on the packaging body according to the following steps:
applying 20-30 MPa (such as 20 MPa,21 MPa,23 MPa,25MPa,27 MPa,30MPa) pressure to the obtained package, increasing sintering temperature to 600deg.C at 5-15deg.C/min (such as 5deg.C/min, 7deg.C/min, 9deg.C/min, 10deg.C/min, 12deg.C/min, 15deg.C/min) rate, maintaining for 120 min, and maintaining the pressure at 3-5 MPa (such as 3 MPa,3.8 MPa,4 MPa,4.1 MPa,4.5 MPa,5 MPa) (in this step, the Ti plate 1 reacts with Al powder and Al plate 3 in the composite powder 2 to form transition interface layer Ti 3 AlC 2 /Al 3 Ti 5）；/>
Raising the sintering temperature to 660 ℃ at a speed of 5 ℃/min, and preserving the temperature for 90 min, wherein the pressure is 0.5-1MPa (0.5 MPa,0.6MPa,0.7 MPa,0.9MPa,1 MPa is adopted) during the heat preservation period; />
Raising sintering temperature to 665 deg.c at 5 deg.c/min and maintaining the temperature for 210min at 0.5 MPa (the Ti plate 1 and the Al powder in the composite powder 2 react completely to form Al 3 A Ti layer); />
Reducing the temperature to 550 ℃ at a speed of 5 ℃/min, and preserving the temperature for 180min under the pressure of 0.5-1MPa (0.5 MPa,0.7 MPa,0.8 MPa,0.9MPa,1 MPa is adopted if the temperature is reduced); />
Reducing the temperature to 200 ℃ at a rate of 5 ℃/min, and maintaining the pressure at 0.5-1MPa (as 0.5 MPa,0.7 MPa,0.8 MPa,0.9MPa,1 MPa); />
Closing the heating device of the vacuum hot-pressing sintering furnace, and cooling the package body to room temperature with the furnace, wherein the pressure is 0.5-1MPa (0.5 MPa,0.7 MPa,0.8 MPa,0.9MPa，1 MPa）。
Principle analysis: 1) Between Ti and Al plates Ti 3 AlC 2 The composite powder composed of the powder and the Al powder has the function of generating a transition interface layer Ti 3 AlC 2 /Al 3 Ti 5. In the preparation process Ti 3 AlC 2 The powder is mixed and divided into Al powder, and Ti plate and Ti are mixed and divided into 3 AlC 2 The Al powder around the powder is directly contacted; note that throughout the preparation process, ti 3 AlC 2 The powder does not react with Al powder in the Al plate, the Ti plate and the composite powder, ti 3 AlC 2 Exists as a second phase in newly formed Al 3 In the Ti layer, to Al 3 The Ti layer has toughening effect, namely, a thin transition interface layer Ti is generated between Ti and Al plates 3 AlC 2 /Al 3 Ti 5. As the reaction proceeds, the Ti and Al plates form Al 3 And a Ti layer. Transition interface layer Ti 3 AlC 2 /Al 3 The hardness of Ti 5 is between the hardness of Ti and Al 3 Between the hardness of Ti, between the Ti plate and Al 3 The Ti interface plays a transitional role to avoid Ti and Al 3 The mechanical property of the Ti interface is suddenly changed, and the stress concentration is greatly relaxed when the Ti interface is impacted;
2) According to the user's actions on Ti plate 1 and Al 3 The hardness gradient at the interface of the Ti layer 4 has different requirements, so that the preparation can be carried out by adjusting the Al powder and the Ti in the composite powder 3 AlC 2 The ratio of the powder (adjusted in the ratio interval) and the thickness of the composite powder layer (adjusted in the thickness interval) to realize different sizes of Ti plates 1 and Al 3 The hardness gradient at the interface between the Ti layers 4 meets the requirements of different users by adopting the same preparation principle.
Claims (1)
1. Ti-Al 3 The preparation method of the Ti intermetallic compound laminated composite board is characterized by comprising the following steps of:
1) Preparing Al and Ti which are uniformly mixed 3 AlC 2 Composite powder (2): al powder with the granularity of 10 mu m is put into a high-energy ball mill for ball milling, the ball-material ratio is 10:1, the rotating speed is 100-200 r/min, the ball milling time is 8-15h, and then the mass ratio is 1:5-1:9 ratio of Al powder after ball milling to Ti with particle size of 1 μm 3 AlC 2 Proportioning the powder, and mixing the Al powder and Ti 3 AlC 2 The powder is put into a ball milling tank for ball milling, the ball milling time is 8-15h, argon is introduced for protection during the ball milling process, and ethanol with the concentration of 1% is added as a process control agent, so that composite powder (2) is formed;
2) Acid-base cleaning Ti plate (1) and Al plate (3): treating a Ti plate (1) with the thickness of 0.5mm with a hydrofluoric acid solution with the concentration of 5%, taking out and cleaning with clear water, putting the Ti plate (1) cleaned with clear water into an ultrasonic cleaner for ultrasonic cleaning, and finally drying the Ti plate (1) cleaned with ultrasonic waves by using a blower; treating an Al plate (3) with the thickness of 0.5mm by using a sodium hydroxide solution with the concentration of 5%, taking out and cleaning by using clear water, putting the Al plate (3) cleaned by using the clear water into an ultrasonic cleaner for ultrasonic cleaning, and finally drying the Al plate (3) cleaned by using a blower;
3) And (3) laminating and packaging: alternately laminating the Ti plates (1) and the Al plates (3) subjected to acid-base cleaning, laminating composite powder (2) with the powder thickness of 0.1-0.15 and mm between the Ti plates (1) and the Al plates (3), and ensuring that the outermost layers are all the Ti plates (1) so as to form laminated plates, wherein the laminated plates are packaged by adopting Ti foil with the thickness of 20 mu m so as to form a packaging body;
4) Vacuum hot pressing sintering: placing the packaging body in a vacuum hot-pressing sintering furnace, and then performing vacuum hot-pressing sintering on the packaging body according to the following steps:
applying 20-30 MPa pressure to the obtained packaging body, increasing sintering temperature to 600 ℃ at a speed of 5-15 ℃/min, and preserving heat for 120 min, wherein the pressure is 3-5 MPa during the heat preservation period; />
Raising the sintering temperature to 660 ℃ at a speed of 5 ℃/min, and preserving heat for 90 min, wherein the pressure is 0.5-1MPa during the heat preservation period; />
Raising the sintering temperature to 665 ℃ at a speed of 5 ℃/min, and preserving heat for 210min, wherein the pressure is 0.5 MPa; />
Reducing the temperature to 550 ℃ at a speed of 5 ℃/min, and preserving the heat for 180min, wherein the pressure is 0.5-1 MPa; />
Reducing the temperature to 200 ℃ at a rate of 5 ℃/min and keeping the pressure at 0.5-1 MPa; />
And (3) closing a heating device of the vacuum hot-pressing sintering furnace, and cooling the packaging body along with the furnace to room temperature to finish the preparation, wherein the pressure is 0.5-1MPa during the cooling period. />
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