CN103305725B - Al base composite material and method for rapidly preparing TiAl base composite material plate by utilizing same - Google Patents

Al base composite material and method for rapidly preparing TiAl base composite material plate by utilizing same Download PDF

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Publication number
CN103305725B
CN103305725B CN201310169061.6A CN201310169061A CN103305725B CN 103305725 B CN103305725 B CN 103305725B CN 201310169061 A CN201310169061 A CN 201310169061A CN 103305725 B CN103305725 B CN 103305725B
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composite material
based composites
tial
paper tinsel
pure
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CN103305725A (en
Inventor
耿林
吴昊
范国华
崔喜平
黄猛
郑镇洙
逄锦程
杜岩
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention relates to an Al base composite material and a method for rapidly preparing a TiAl base composite material plate by utilizing the same. The invention relates to a composite material and a method for preparing a plate by utilizing the same, which aim at solving the problem that the production cycle is too long due to the low reaction rate in the preparation of TiAl base alloy in the prior art. The Al base composite material is prepared from Al and a reinforcing body, or prepared from Al and an alloying element. The method comprises the steps of: 1. polishing; 2. cleaning; 3. hot pressing; and 4. annealing and densification treatment. According to the Al base composite material and the method, the reaction rate is high, the production cycle is short, the production process is easy and feasible, the cost is low, and the textile is small and controllable. The Al base composite material and the method are used for preparing the TiAl base composite material plate.

Description

A kind of Al based composites and utilize this Al based composites to prepare the method for TiAl-matrix composite material board fast
Technical field
The present invention relates to matrix material and utilize matrix material to prepare the method for sheet material.
Background technology
TiAl-base alloy is a kind of novel light heat resistant structure material, proportion is less than 50% of nickel-base alloy, there is lightweight, the advantage such as high-strength, anti-corrosion, wear-resisting, high temperature resistant, and there is excellent normal temperature and high-temperature behavior, become the emphasis material of Aeronautics and Astronautics and military field investigation and application in worldwide.Through the effort of decades, current TiAl-base alloy has entered practical developmental stage.Wherein, the most urgent to the demand of TiAl base alloy plate and foil.Utilize Ti and Al element plate to react annealing preparation TiAl sheet material can avoid, to the direct distortion of TiAl brittlement phase, showing greatly superiority, but speed of reaction causes its production cycle long excessively slowly.In addition, single-phase TiAl metal carbonyl compound there is hot strength and creep property is not enough, and the matrix material prepared after adding reinforcement can address this problem effectively, but too increases the preparation difficulty of TiAl-matrix composite material board.
In sum, there is the problem that speed of reaction causes its production cycle long excessively slowly in current preparation TiAl-base alloy.
Summary of the invention
The present invention will solve at present preparation TiAl-base alloy and there is the problem that speed of reaction causes its production cycle long excessively slowly, and provides a kind of Al based composites and utilize this Al based composites to prepare the method for TiAl-matrix composite material board fast.
A kind of Al based composites, is made up of the Al of 88% ~ 99.9% and the reinforcement of 0.1% ~ 12% according to volume fraction; Or a kind of Al based composites is made up of the Al of 85% ~ 99.9% and the alloying element of 0.1% ~ 15% according to massfraction; Wherein reinforcement is SiC, B 4c, TiB 2, TiC and Ti 5si 3in the combination of one or more, alloying element is the combination of one or more in Ti, Si, B and Fe.
Utilize above-mentioned a kind of Al based composites to prepare the method for TiAl-matrix composite material board fast, specifically prepare according to following steps:
One, be 1.01 ~ 1.09:1 according to the Thickness Ratio of pure Ti plate and a kind of Al based composites according to claim 1, pure Ti plate and Al based composites are polished into pure Ti paper tinsel and Al based composites paper tinsel, wherein the thickness of pure Ti paper tinsel is 50 μm ~ 250 μm;
Two, adopt volumetric concentration be 5% ~ 20% the pure Ti paper tinsel that obtains of HF solution cleaning step one, adopt mass concentration be 5% ~ 20% the Al based composites paper tinsel that obtains of NaOH solution cleaning step one, then by the ultrasonic cleaning drying in acetone of pure Ti paper tinsel and Al based composites paper tinsel;
Three, the pure Ti paper tinsel after step 2 process and Al based composites paper tinsel alternative stacked are placed, then carry out hot-pressing processing, controlling hot pressing temperature is 350 DEG C ~ 550 DEG C, and pressure is 20MPa ~ 50MPa, and soaking time is 1h ~ 2h, obtains Ti-Al based composite material sheet material;
Four, Ti-Al based composite material sheet material step 3 obtained is put into vacuum hotpressing stove and is carried out reaction annealing, control temperature is 650 DEG C ~ 800 DEG C, insulation 4h ~ 10h, be warming up to 1000 DEG C ~ 1300 DEG C again and carry out densification, controlling densification pressure is 20MPa ~ 100MPa, soaking time is 0.5h ~ 10h, then under temperature is 1300 DEG C ~ 1400 DEG C conditions, is incubated 10min ~ 60min, obtains TiAl-matrix composite material board.
The invention has the beneficial effects as follows: TiAl-matrix composite material board prepared by the present invention, by adjusting kind and the content of reinforcement and alloying element in the relative thickness of pure Ti paper tinsel and Al based composites paper tinsel, Al based composites paper tinsel, realizes the raising of TiAl-matrix composite material board mechanical behavior under high temperature.
The present invention by introducing alloying element or reinforcement in Al element plate, utilize hot pressing and reaction annealing preparation TiAl-matrix composite material board, effectively can improve at present preparation TiAl-base alloy and there is the problem that speed of reaction causes its production cycle long excessively slowly, make the scale production of TiAl-matrix composite material board become possibility.
The inventive method has the following advantages:
(1) speed of reaction is very fast, with short production cycle;
(2) the disposable preparation completing TiAl-matrix composite material board, production technique is simple, and cost is low;
(3) preparation process is pollution-free, and material is fine and close;
(4) fine microstructures and controlled.
The present invention is for the preparation of TiAl-matrix composite material board.
Accompanying drawing explanation
Fig. 1 be in embodiment one step 5 660 DEG C reaction annealing 1h after transmission electron microscope picture, Fig. 2 be the diffraction spot point diagram of Al as shown, Fig. 3 is TiAl 3diffraction spot point diagram, Fig. 4 is the scanning electron microscope (SEM) photographs at 660 DEG C of reaction annealing 1h rear interface places, the composition analysis figure of Fig. 5 to be the composition analysis figure of interfacial layer, Fig. 6 be interface Si element;
Fig. 7 is the scanning electron microscope (SEM) photograph of TiAl-matrix composite material board prepared by embodiment one;
Fig. 8 is the scanning electron microscope (SEM) photograph of TiAl-matrix composite material board prepared by embodiment two.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of Al based composites of present embodiment, is made up of the Al of 88% ~ 99.9% and the reinforcement of 0.1% ~ 12% according to volume fraction; Or a kind of Al based composites is made up of the Al of 85% ~ 99.9% and the alloying element of 0.1% ~ 15% according to massfraction; Wherein reinforcement is SiC, B 4c, TiB 2, TiC and Ti 5si 3in the combination of one or more, alloying element is the combination of one or more in Ti, Si, B and Fe.
Present embodiment by introducing alloying element or reinforcement in Al element plate, utilize hot pressing and reaction annealing preparation TiAl-matrix composite material board, effectively can improve at present preparation TiAl-base alloy and there is the problem that speed of reaction causes its production cycle long excessively slowly, make the scale production of TiAl-matrix composite material board become possibility.
Embodiment two: present embodiment and embodiment one unlike: the particle diameter of Al is 10 μm ~ 200 μm, and the particle diameter of reinforcement is 40nm ~ 10 μm.Other is identical with embodiment one.
Embodiment three: utilize a kind of Al based composites described in embodiment one to prepare the method for TiAl-matrix composite material board fast, specifically prepare according to following steps:
One, be 1.01 ~ 1.09:1 according to the Thickness Ratio of pure Ti plate and a kind of Al based composites according to claim 1, pure Ti plate and Al based composites are polished into pure Ti paper tinsel and Al based composites paper tinsel, wherein the thickness of pure Ti paper tinsel is 50 μm ~ 250 μm;
Two, adopt volumetric concentration be 5% ~ 20% the pure Ti paper tinsel that obtains of HF solution cleaning step one, adopt mass concentration be 5% ~ 20% the Al based composites paper tinsel that obtains of NaOH solution cleaning step one, then by the ultrasonic cleaning drying in acetone of pure Ti paper tinsel and Al based composites paper tinsel;
Three, the pure Ti paper tinsel after step 2 process and Al based composites paper tinsel alternative stacked are placed, then carry out hot-pressing processing, controlling hot pressing temperature is 350 DEG C ~ 550 DEG C, and pressure is 20MPa ~ 50MPa, and soaking time is 1h ~ 2h, obtains Ti-Al based composite material sheet material;
Four, Ti-Al based composite material sheet material step 3 obtained is put into vacuum hotpressing stove and is carried out reaction annealing, control temperature is 650 DEG C ~ 800 DEG C, insulation 4h ~ 10h, be warming up to 1000 DEG C ~ 1300 DEG C again and carry out densification, controlling densification pressure is 20MPa ~ 100MPa, soaking time is 0.5h ~ 10h, then under temperature is 1300 DEG C ~ 1400 DEG C conditions, is incubated 10min ~ 60min, obtains TiAl-matrix composite material board.
Embodiment four: present embodiment and embodiment three unlike: in step one, the Thickness Ratio of pure Ti plate and a kind of Al based composites according to claim 1 is 1.08:1.Other is identical with embodiment three.
Embodiment five: present embodiment and embodiment three unlike: in step 2, the volumetric concentration of HF solution is 10% ~ 15%.Other is identical with embodiment three.
Embodiment six: present embodiment and embodiment three unlike: in step 2, the mass concentration of NaOH solution is 10% ~ 15%.Other is identical with embodiment three.
Embodiment seven: present embodiment and embodiment three unlike: controlling hot pressing temperature in step 3 is 360 DEG C ~ 540 DEG C, and pressure is 22MPa ~ 45MPa.Other is identical with embodiment three.
Embodiment eight: present embodiment and embodiment three unlike: in step 3, the number of plies of pure Ti paper tinsel is n+1 layer, Al based composites paper tinsel the number of plies be n layer, wherein n is positive integer, and n >=1.Other is identical with embodiment three.
Embodiment nine: present embodiment and embodiment three unlike: controlling densification pressure in step 4 is 22MPa ~ 98MPa, and soaking time is 0.7h ~ 9.8h.Other is identical with embodiment three.
Embodiment ten: one of present embodiment and embodiment three to nine unlike: controlling densification pressure in step 4 is 30MPa ~ 90MPa, and soaking time is 1h ~ 9h.Other is identical with one of embodiment three to nine.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one:
The present embodiment utilizes a kind of Al based composites to prepare the method for TiAl-matrix composite material board fast, specifically prepares according to following steps:
One, after reinforcement SiC being mixed with Al powder temperature be 610 DEG C, pressure be the condition of 30MPa under hot pressed sintering, then be rolled under temperature is 500 DEG C of conditions, obtain the Al based composites that thickness is 200 μm, wherein the volume fraction of Al is 97%, the volume fraction of SiC is 3%;
Two, the Al based composites that pure Ti plate and step one obtain is polished into pure Ti paper tinsel and Al based composites paper tinsel, wherein the thickness of pure Ti paper tinsel is 100 μm, and the thickness of Al based composites paper tinsel is 92 μm;
Three, adopt volumetric concentration be 10% the pure Ti paper tinsel that obtains of HF solution cleaning step two, adopt mass concentration be 10% the Al based composites paper tinsel that obtains of NaOH solution cleaning step two, then by the ultrasonic cleaning drying in acetone of pure Ti paper tinsel and Al based composites paper tinsel;
Four, the pure Ti paper tinsel after step 3 process and Al based composites paper tinsel alternative stacked are placed, then carry out hot-pressing processing, controlling hot pressing temperature is 515 DEG C, pressure is 40MPa, soaking time is 1.5h, obtains Ti-Al based composite material sheet material, and wherein pure Ti paper tinsel is of a size of 30 × 50 × 0.1mm 3, the number of plies is 15 layers, Al based composites paper tinsel is of a size of 30 × 50 × 0.092mm 3, the number of plies is 14 layers;
Five, Ti-Al based composite material sheet material step 4 obtained is put into vacuum hotpressing stove and is carried out reaction annealing, control temperature is 660 DEG C, insulation 6h, be warming up to 1225 DEG C again and carry out densification, controlling densification pressure is 40MPa, soaking time is 6h, then under temperature is 1400 DEG C of conditions, is incubated 20min, obtains TiAl-matrix composite material board.
In the present embodiment, Al based composites is SiC/Al based composites, and TiAl-matrix composite material board is Ti-(SiC/Al) forming laminated sheet material.
As shown in Figure 1, wherein the diffraction spot point diagram of Al as shown in Figure 2, TiAl for transmission electron microscope picture in the present embodiment step 5 after 660 DEG C of reaction annealing 1h 3diffraction spot point diagram as shown in Figure 3, the scanning electron microscope (SEM) photograph at 660 DEG C of reaction annealing 1h rear interface places as shown in Figure 4, wherein the composition analysis figure of interfacial layer as shown in Figure 5, and as shown in Figure 6, as can be seen from the figure Si has been solidly soluted into TiAl to the composition analysis figure of interface Si element 3in crystal grain, and the larger grain-size of solid solution capacity is less, and what Si was described exists refinement TiAl 3crystal grain, mean sizes is reduced to 2 μm by 5 μm, the TiAl less in interface 3crystal grain is pushed through in SiC/Al based composites layer, reduces the thickness of interfacial layer and the evolving path of Ti, Al element, improves speed of reaction.
The scanning electron microscope (SEM) photograph of TiAl-matrix composite material board prepared by the present embodiment as shown in Figure 7.
Embodiment two:
The present embodiment utilizes a kind of Al based composites to prepare the method for TiAl-matrix composite material board fast, specifically prepares according to following steps:
One, be 1.08:1 according to the Thickness Ratio of pure Ti plate and Al based composites, pure Ti plate and Al based composites are polished into pure Ti paper tinsel and Al based composites paper tinsel, wherein the thickness of pure Ti paper tinsel is 100 μm, and in Al based composites, the massfraction of Si is 6%, the massfraction of Al is 94%;
Two, adopt volumetric concentration be 10% the pure Ti paper tinsel that obtains of HF solution cleaning step one, adopt mass concentration be 10% the Al based composites paper tinsel that obtains of NaOH solution cleaning step one, then by the ultrasonic cleaning drying in acetone of pure Ti paper tinsel and Al based composites paper tinsel;
Three, the pure Ti paper tinsel after step 2 process and Al based composites paper tinsel alternative stacked are placed, then carry out hot-pressing processing, controlling hot pressing temperature is 515 DEG C, pressure is 40MPa, soaking time is 1.5h, obtains Ti-Al based composite material sheet material, and wherein pure Ti paper tinsel is of a size of 30 × 50 × 0.1mm 3, the number of plies is 15 layers, Al based composites paper tinsel is of a size of 30 × 50 × 0.092mm 3, the number of plies is 14 layers;
Four, Ti-Al based composite material sheet material step 3 obtained is put into vacuum hotpressing stove and is carried out reaction annealing, control temperature is 660 DEG C, insulation 6h, be warming up to 1225 DEG C again and carry out densification, controlling densification pressure is 40MPa, soaking time is 6h, then under temperature is 1400 DEG C of conditions, is incubated 20min, obtains TiAl-matrix composite material board.
In the present embodiment, Al based composites is Al-6Si (wt.%) Al based composites, and TiAl-matrix composite material board is Ti 5si 3/ TiAl-matrix composite material board.
The scanning electron microscope (SEM) photograph of TiAl-matrix composite material board prepared by the present embodiment as shown in Figure 8.

Claims (9)

1. utilize Al based composites to prepare the method for TiAl-matrix composite material board fast, it is characterized in that the method, specifically prepare according to following steps:
One, be 1.01 ~ 1.09:1 according to the Thickness Ratio of pure Ti plate and Al based composites, pure Ti plate and Al based composites are polished into pure Ti paper tinsel and Al based composites paper tinsel, wherein the thickness of pure Ti paper tinsel is 50 μm ~ 250 μm; Described Al based composites is made up of the Al of 85% ~ 99.9% and the alloying element of 0.1% ~ 15% according to massfraction; Wherein alloying element is the combination of one or more in Ti, Si, B and Fe;
Two, adopt volumetric concentration be 5% ~ 20% the pure Ti paper tinsel that obtains of HF solution cleaning step one, adopt mass concentration be 5% ~ 20% the Al based composites paper tinsel that obtains of NaOH solution cleaning step one, then by the ultrasonic cleaning drying in acetone of pure Ti paper tinsel and Al based composites paper tinsel;
Three, the pure Ti paper tinsel after step 2 process and Al based composites paper tinsel alternative stacked are placed, then carry out hot-pressing processing, controlling hot pressing temperature is 350 DEG C ~ 550 DEG C, and pressure is 20MPa ~ 50MPa, and soaking time is 1h ~ 2h, obtains Ti-Al based composite material sheet material;
Four, Ti-Al based composite material sheet material step 3 obtained is put into vacuum hotpressing stove and is carried out reaction annealing, control temperature is 650 DEG C ~ 800 DEG C, insulation 4h ~ 10h, be warming up to 1000 DEG C ~ 1300 DEG C again and carry out densification, controlling densification pressure is 20MPa ~ 100MPa, soaking time is 0.5h ~ 10h, then under temperature is 1300 DEG C ~ 1400 DEG C conditions, is incubated 10min ~ 60min, obtains TiAl-matrix composite material board.
2. the Al of utilization based composites according to claim 1 prepares the method for TiAl-matrix composite material board fast, it is characterized in that the particle diameter of Al in Al based composites described in step one is 10 μm ~ 200 μm.
3. the Al of utilization based composites according to claim 1 prepares the method for TiAl-matrix composite material board fast, it is characterized in that the Thickness Ratio of pure Ti plate and Al based composites in step one is 1.08:1.
4. the Al of utilization based composites according to claim 1 prepares the method for TiAl-matrix composite material board fast, it is characterized in that the volumetric concentration of HF solution in step 2 is 10% ~ 15%.
5. the Al of utilization based composites according to claim 1 prepares the method for TiAl-matrix composite material board fast, it is characterized in that the mass concentration of NaOH solution in step 2 is 10% ~ 15%.
6. the Al of utilization based composites according to claim 1 prepares the method for TiAl-matrix composite material board fast, and it is characterized in that controlling hot pressing temperature in step 3 is 360 DEG C ~ 540 DEG C, pressure is 22MPa ~ 45MPa.
7. the Al of utilization based composites according to claim 1 prepares the method for TiAl-matrix composite material board fast, it is characterized in that the number of plies of pure Ti paper tinsel in step 3 is n+1 layer, Al based composites paper tinsel the number of plies be n layer, wherein n is positive integer, and n >=1.
8. the Al of utilization based composites according to claim 1 prepares the method for TiAl-matrix composite material board fast, and it is characterized in that controlling densification pressure in step 4 is 22MPa ~ 98MPa, soaking time is 0.7h ~ 9.8h.
9. the Al of utilization based composites according to claim 8 prepares the method for TiAl-matrix composite material board fast, and it is characterized in that controlling densification pressure in step 4 is 30MPa ~ 90MPa, soaking time is 1h ~ 9h.
CN201310169061.6A 2013-05-09 2013-05-09 Al base composite material and method for rapidly preparing TiAl base composite material plate by utilizing same Expired - Fee Related CN103305725B (en)

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CN104372208B (en) * 2014-10-28 2019-03-29 赵遵成 A kind of endogenetic particle hybrid reinforced aluminum-matrix composite material and preparation method thereof
CN108330314B (en) * 2018-03-23 2019-09-13 哈尔滨工业大学 A kind of preparation method of cluster type (SiCp/Al)/Al composite material
CN111376572B (en) * 2018-12-28 2022-04-08 南京理工大学 Preparation method of heterogeneous layered aluminum-based composite material
CN109913678B (en) * 2019-03-15 2020-10-30 武汉大学 TiAl3Particle reinforced aluminum-based composite material and preparation method and application thereof

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