CN116987921A - TiAl-based composite material with full-lamellar network structure and preparation method thereof - Google Patents
TiAl-based composite material with full-lamellar network structure and preparation method thereof Download PDFInfo
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- 229910010038 TiAl Inorganic materials 0.000 title claims abstract description 165
- 239000002131 composite material Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 213
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 70
- 239000000956 alloy Substances 0.000 claims abstract description 70
- 238000000498 ball milling Methods 0.000 claims abstract description 49
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 49
- 238000005245 sintering Methods 0.000 claims abstract description 43
- 230000002787 reinforcement Effects 0.000 claims abstract description 38
- 230000007704 transition Effects 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 72
- 239000011812 mixed powder Substances 0.000 claims description 49
- 229910052786 argon Inorganic materials 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 31
- 238000010438 heat treatment Methods 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 18
- 238000012216 screening Methods 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 16
- 230000009466 transformation Effects 0.000 claims description 15
- 230000003014 reinforcing effect Effects 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 238000002490 spark plasma sintering Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 238000009849 vacuum degassing Methods 0.000 claims description 9
- 229910021389 graphene Inorganic materials 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 6
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 230000002776 aggregation Effects 0.000 abstract description 10
- 238000005054 agglomeration Methods 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 9
- 238000007873 sieving Methods 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 238000011068 loading method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000011065 in-situ storage Methods 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 238000004663 powder metallurgy Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a full-lamellar network structure TiAl-based composite material and a preparation method thereof, wherein the method comprises the following steps: 1. selecting spherical TiAl prealloyed powder, metal powder and reinforcement powder; 2. performing primary high-energy ball milling on the spherical TiAl prealloyed powder and the metal powder to obtain TiAl alloy powder with a transition layer on the surface; 3. performing secondary high-energy ball milling on the TiAl alloy powder with the transition layer on the surface and the reinforcement powder to obtain TiAl alloy powder with the surface uniformly coated with the reinforcement; 4. sieving to obtain powder to be sintered; 5. and sintering at three stages of temperatures. According to the invention, the transition layer is introduced through high-energy ball milling, so that the combination property of the reinforcement and the matrix powder is improved, the reinforcement powder is uniformly coated on the surface of the transition layer, the ball milling agglomeration phenomenon of the reinforcement is eliminated, the TiAl-based composite material with a full-lamellar network structure is obtained, and the high-temperature strength and the microstructure stability of the TiAl-based composite material are greatly improved.
Description
Technical Field
The invention belongs to the technical field of TiAl alloy and composite materials thereof, and particularly relates to a full-lamellar mesh-structure TiAl-based composite material and a preparation method thereof.
Background
With the rapid development of aviation industry, the improvement of thrust and weight reduction of an aeroengine have become core driving forces for the progress of engine materials, which require lower density of the engine materials to achieve the purpose of weight reduction, and meanwhile, the engine materials have good high temperature resistance, high temperature oxidation resistance and corrosion resistance.
As a novel light high-temperature structural material, the TiAl alloy has excellent specific strength and specific modulus, good high-temperature creep resistance and oxidation resistance, the service temperature can reach 850 ℃, and the TiAl alloy becomes a potential material which is only expected to replace nickel-based superalloy in the temperature range of 700-900 ℃. Meanwhile, the TiAl alloy is used as a novel advanced engineering material and has lower density (3.9 g/cm 3 ~4.2g/cm 3 ) Is widely applied in the aerospace and automobile industries.
The current preparation methods of TiAl alloy include casting, directional solidification, smelting and powder metallurgy. However, the cast TiAl alloy products have low yield and have the same problems of coarse structure and segregation of components as the smelting method. The directional solidification technology is difficult to apply in a short term in the process exploration stage. The powder metallurgy can overcome the defect that TiAl alloy is difficult to process and form, can obtain fine and uniform tissues, and has wide application prospect. The existing single TiAl alloy has a series of problems of poor room temperature plasticity, insufficient high temperature strength, poor high temperature stability and the like, and the problems can be improved by introducing a reinforcing phase into a transition layer to prepare the TiAl-based composite material with a special structure.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a full-lamellar network structure TiAl-based composite material aiming at the defects in the prior art. The method adopts a powder metallurgy method, introduces a transition layer through high-energy ball milling, obviously improves the combination property of the reinforcement and matrix powder, ensures that the reinforcement powder is uniformly coated on the surface of the transition layer, eliminates the agglomeration phenomenon of the reinforcement in the ball milling process, obtains the full-lamellar network structure TiAl-based composite material, solves the agglomeration problem of the reinforcement in the ball milling process, and improves the high-temperature strength of the TiAl-based composite material.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the TiAl-based composite material with the full-lamellar network structure is characterized by comprising the following steps of:
step one, raw material preparation: selecting spherical TiAl prealloy powder with the particle size of 50-150 mu m, selecting metal powder with the particle size of 50-1000 nm, and selecting reinforcement powder with the particle size of 50-100 nm;
step two, primary high-energy ball milling treatment: uniformly mixing the spherical TiAl prealloy powder and the metal powder in the first step to obtain primary mixed powder, vacuumizing a ball milling tank, introducing argon, filling the primary mixed powder into the ball milling tank into which the argon is introduced, and placing the ball milling tank into a planetary ball mill for primary high-energy ball milling treatment to obtain TiAl alloy powder with a transition layer on the surface;
thirdly, performing secondary high-energy ball milling treatment: uniformly mixing the TiAl alloy powder with the transition layer on the surface obtained in the second step with the reinforcement powder in the first step to obtain secondary mixed powder, vacuumizing a ball milling tank, introducing argon, filling the secondary mixed powder into the ball milling tank into which the argon is introduced, and placing the secondary mixed powder into a planetary ball mill for secondary high-energy ball milling treatment to obtain TiAl alloy powder with the surface uniformly coated with the reinforcement;
step four, screening treatment: screening the TiAl alloy powder with the surface uniformly coated with the reinforcement body obtained in the step three by adopting a 100-mesh screen to obtain undersize to be sintered powder;
step five, powder sintering: and (3) placing the powder to be sintered obtained in the step (IV) into a die, then carrying out vacuum degassing, and then carrying out three-stage temperature sintering to obtain the full-lamellar network structure TiAl-based composite material.
The preparation method of the full-lamellar network structure TiAl-based composite material is characterized in that the spherical Ti in the step oneThe Al prealloy powder is Ti-48Al-2Cr-2Nb, ti-45Al-2Nb-2Mn-0.8TiB 2 ，Ti-47Al-2W-0.5Si，Ti-47Al-2Nb-2Mn-0.8TiB 2 Ti-47Al-1.5Nb-1Mn-1Cr-0.7 (Si, B), ti-45.5Al-4 (Nb, cr, ta, B), ti-46Al-3 (Nb, cr, mo) -x (B, C), wherein x<1, ti-46Al-6.5Nb-0.6Cr-0.2Ni or Ti-45Al-5Nb-yB-zC, wherein y<1，z<1；
The metal powder is Ti powder or/and Al powder;
the reinforcing body powder is B 4 C. Graphene, carbon black, carbon nanotubes or graphene oxide.
The Ti powder and the Al powder in the metal powder selected by the invention are all main constituent elements of the TiAl alloy, and can be well combined with the spherical TiAl prealloy powder; the reinforcement powder selected by the invention can react with the TiAl alloy matrix to generate carbide or boride reinforcement reinforcing phase.
The preparation method of the TiAl-based composite material with the full-lamellar network structure is characterized in that the rotating speed of the primary high-energy ball milling treatment in the second step is 150-300 r/min, the time is 2-5 h, the rotating speed of the secondary high-energy ball milling treatment in the third step is 150-300 r/min, the time is 2-5 h, and the total time of the secondary high-energy ball milling treatment is less than 8h. The invention avoids the danger of serious powder breakage and overhigh temperature of a ball milling tank body caused by overhigh ball milling rotating speed by controlling the rotating speed of twice high-energy ball milling, and avoids the phenomenon that metal powder and reinforcement powder are difficult to be coated on the surface of prealloyed powder in turn due to overhigh ball milling rotating speed; meanwhile, the metal powder and the reinforcement powder are fully dispersed by ball milling twice, so that the phenomenon that the TiAl-based composite material with the full-lamellar network structure cannot be obtained due to aggregation of the metal powder and the reinforcement powder is avoided.
The preparation method of the full-lamellar network structure TiAl-based composite material is characterized in that the three-stage temperature sintering method in the fifth step is spark plasma sintering or hot-pressing sintering. The plasma generated by pulse current in the SPS spark plasma sintering process is favorable for densification of powder, the compactness of the TiAl-based composite material is improved, and the vacuum hot-pressed sintering can be used for preparing large-size materials, so that the method has the characteristic of high efficiency.
The preparation method of the full-lamellar network structure TiAl-based composite material is characterized in that the three-stage temperature sintering process in the step five is as follows: firstly, heating from room temperature to 100-300 ℃ below Te temperature within 8-15 min, preserving heat for 1-5 min, then heating to 200-250 ℃ below Taα temperature within 6-10 min, preserving heat for 4-10 min, heating to 0-50 ℃ below Taα temperature within 3-5 min, preserving heat for 4-10 min, finally cooling to 100-300 ℃ below Te temperature within 3-5 min, and cooling to room temperature along with a furnace, wherein Te is the eutectoid transformation temperature of TiAl alloy, taα is the alpha phase transformation initial temperature of TiAl alloy. According to the invention, three-stage temperature sintering is adopted, the transition layer formed by the metal powder is combined with the matrix powder and the reinforcement powder through the first-stage temperature sintering, and simultaneously degassing is carried out at a lower temperature, so that the oxygen content of the composite material is controlled at a lower level; then the reinforcement body and the matrix are fully reacted to generate carbide and boride reinforcement phases and are distributed in a net shape through the second-stage temperature sintering; and then sintering is carried out near the single-phase region by controlling the temperature of the third section, so as to obtain the full-lamellar structure.
In addition, the invention also discloses a full-lamellar network structure TiAl-based composite material which is characterized by being prepared by the method.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the transition layer is formed on the surface of TiAl alloy powder through primary high-energy ball milling, then the reinforcing body is coated on the surface of the TiAl alloy powder through secondary high-energy ball milling, the bonding performance of the reinforcing body and matrix powder is obviously improved by utilizing the transition layer, so that the reinforcing body powder is uniformly coated on the surface of the transition layer to form excellent interface bonding, the agglomeration phenomenon of the reinforcing body during ball milling is eliminated, and the reinforcing phase generated by the reinforcing body is separated out at the grain boundary and distributed in a net shape through sintering, so that the TiAl-based composite material with a full-sheet net-shaped structure is obtained, the grain boundary is pinned through net-shaped distribution of the reinforcing phase, crystal grains are obviously thinned, and the matrix load is borne, thereby greatly improving the high-temperature strength and the microstructure stability of the TiAl-based composite material.
2. According to the invention, three-stage temperature sintering is adopted to enable the surface to be uniformly coated with the TiAl alloy powder of the reinforcement body to be molded, and the oxygen content in the composite material is effectively controlled at a lower level by controlling the technological parameters of the three-stage temperature sintering, so that the reinforcement phase is ensured to be in net-shaped distribution, and the full-lamellar tissue is obtained.
3. The powder metallurgy forming process does not need to add any additive or adhesive, does not need to be pressed and formed in advance, has high heat efficiency, high heating rate and short sintering time, is easy to prepare the sintered body composite material with uniform quality, compactness, high quality and tiny and uniform structure, and is suitable for industrial production.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
Fig. 1 is an SEM image of the powder to be sintered prepared in example 1 of the present invention.
FIG. 2 is a schematic diagram of a three-stage temperature sintering process in example 1 of the present invention.
FIG. 3 is a low-magnification microstructure of the full-lamellar network TiAl-based composite material prepared in example 1 of the present invention.
FIG. 4 is a high-magnification microstructure of the full-lamellar network TiAl-based composite material prepared in example 1 of the present invention.
Fig. 5 is an SEM image of the powder to be sintered prepared in example 2 of the present invention.
FIG. 6 is a low-magnification microstructure of the full-lamellar network TiAl-based composite material prepared in example 2 of the present invention.
FIG. 7 is a high magnification microstructure of the full lamellar network TiAl-based composite material prepared in example 2 of the present invention.
Fig. 8 is an SEM image of the powder to be sintered prepared in example 3 of the present invention.
FIG. 9 is a low-magnification microstructure of the full-lamellar network TiAl-based composite material prepared in example 3 of the present invention.
FIG. 10 is a high magnification microstructure of the full lamellar network TiAl-based composite material prepared in example 3 of the present invention.
Fig. 11 is an SEM image of the powder to be sintered prepared in example 4 of the present invention.
FIG. 12 is a low-magnification microstructure of the full-lamellar network TiAl-based composite material prepared in example 4 of the present invention.
FIG. 13 is a high magnification microstructure of the full lamellar network TiAl matrix composite material prepared in example 4 of the present invention.
Fig. 14 is an SEM image of the powder to be sintered prepared in example 5 of the present invention.
FIG. 15 is a low-magnification microstructure of the full-lamellar network TiAl-based composite material prepared in example 5 of the present invention.
FIG. 16 is a high magnification microstructure of the full lamellar network TiAl matrix composite material prepared in example 5 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, raw material preparation: selecting spherical TiAl prealloy powder with particle size of 50-150 μm, selecting Ti powder with particle size of 100nm, and selecting B with particle size of 50nm 4 C, powder; the spherical TiAl prealloyed powder is Ti-48Al-2Cr-2Nb;
step two, primary high-energy ball milling treatment: uniformly mixing 96.1g of spherical TiAl prealloy powder in the first step and 3g of Ti powder to obtain primary mixed powder, vacuumizing a ball milling tank, introducing argon, loading the primary mixed powder into the ball milling tank which is filled with the argon, placing the ball milling tank into a planetary ball mill, and performing primary high-energy ball milling treatment for 3 hours at a rotating speed of 200r/min to obtain TiAl alloy powder with a Ti transition layer on the surface;
thirdly, performing secondary high-energy ball milling treatment: mixing TiAl alloy powder with Ti transition layer on the surface and 0.9g B in the first step 4 Uniformly mixing the powder C to obtain secondary mixed powder, vacuumizing a ball milling tank, introducing argon, loading the secondary mixed powder into the ball milling tank which is filled with the argon, placing the secondary mixed powder into a planetary ball mill, and performing secondary high-energy ball milling treatment for 3 hours at a rotating speed of 200r/min to obtain the surface uniform coating B 4 The TiAl alloy powder of C;
step four, screening treatment: by 100 meshesUniformly coating the surface obtained in the step three with the screen cloth B 4 C, screening the TiAl alloy powder to obtain undersize powder to be sintered, wherein the Ti powder and the reinforcing body B in the undersize powder are as shown in figure 1, and can be seen from figure 1 4 The C powder is relatively uniformly distributed on the surface of the spherical TiAl prealloyed powder, and the reinforcement B does not occur 4 Agglomeration of powder C;
step five, powder sintering: placing the powder to be sintered obtained in the step four into a die with the diameter phi of 50mm, then carrying out vacuum degassing, and carrying out three-stage temperature sintering by using spark plasma sintering to obtain a full-sheet-layer network-structured TiAl-based composite material; as shown in fig. 2, the three-stage temperature sintering process is as follows: heating from room temperature to 800 ℃ in 8min and preserving heat for 1min, heating to 1150 ℃ in 6min and preserving heat for 5min, heating to 1300 ℃ in 3min and preserving heat for 7min, cooling to 800 ℃ in 3min, and cooling to room temperature along with a furnace, wherein Te is the eutectoid transformation temperature of TiAl alloy Ti-48Al-2Cr-2Nb, and Tα is the alpha phase transformation initial temperature of TiAl alloy Ti-48Al-2Cr-2 Nb.
Fig. 3 is a low-magnification microstructure of the full-lamellar network-structured TiAl-based composite material prepared in this example, and fig. 4 is a high-magnification microstructure of the full-lamellar network-structured TiAl-based composite material prepared in this example, and it can be seen from fig. 3 and fig. 4 that the lamellar clusters of the full-lamellar network-structured TiAl-based composite material prepared in this example are fine and uniform, and precipitation-enhanced phases are generated in situ at grain boundaries and distributed in a network shape.
The reinforcement powder selected in this embodiment may also be graphene, carbon black, carbon nanotubes or graphene oxide; the spherical TiAl prealloyed powder can also be Ti-45Al-2Nb-2Mn-0.8TiB 2 ，Ti-47Al-2W-0.5Si，Ti-47Al-2Nb-2Mn-0.8TiB 2 Ti-45.5Al-4 (Nb, cr, ta, B), ti-47Al-1.5Nb-1Mn-1Cr-0.7 (Si, B), or Ti-46Al-6.5Nb-0.6Cr-0.2Ni.
Example 2
The embodiment comprises the following steps:
step one, raw material preparation: selecting spherical TiAl prealloy powder with particle size of 50-150 μm, selecting Ti powder with particle size of 100nm and Al powder with particle size of 50nm, and selecting Ti powder with particle size of 50nmB 4 C, powder; the spherical TiAl prealloyed powder is Ti-48Al-2Cr-2Nb;
step two, primary high-energy ball milling treatment: uniformly mixing 96.7g of spherical TiAl prealloy powder in the first step, 1.9g of Ti powder and 1.1g of Al powder to obtain primary mixed powder, vacuumizing a ball milling tank, introducing argon, then placing the primary mixed powder into the ball milling tank which is filled with the argon, placing the primary mixed powder into a planetary ball mill, and performing primary high-energy ball milling treatment for 3 hours at a rotating speed of 200r/min to obtain TiAl alloy powder with a Ti/Al transition layer on the surface;
thirdly, performing secondary high-energy ball milling treatment: mixing TiAl alloy powder with Ti/Al transition layer on the surface and 0.3g B in the first step 4 Uniformly mixing the powder C to obtain secondary mixed powder, vacuumizing a ball milling tank, introducing argon, loading the secondary mixed powder into the ball milling tank which is filled with the argon, placing the secondary mixed powder into a planetary ball mill, and performing secondary high-energy ball milling treatment for 3 hours at a rotating speed of 200r/min to obtain the surface uniform coating B 4 The TiAl alloy powder of C;
step four, screening treatment: uniformly coating the surface obtained in the step three with a 100-mesh screen 4 The TiAl alloy powder of C is subjected to screening treatment to obtain undersize as powder to be sintered, as shown in FIG. 5, as can be seen from FIG. 5, ti powder, al powder and reinforcement B in the powder to be sintered 4 The C powder is relatively uniformly distributed on the surface of the spherical TiAl prealloyed powder, and the reinforcement B does not occur 4 Agglomeration of powder C;
step five, powder sintering: placing the powder to be sintered obtained in the step four into a die with the diameter phi of 50mm, then carrying out vacuum degassing, and carrying out three-stage temperature sintering by using spark plasma sintering to obtain a full-sheet-layer network-structured TiAl-based composite material; the three-stage temperature sintering process comprises the following steps: heating from room temperature to 800 ℃ in 8min and preserving heat for 1min, heating to 1150 ℃ in 6min and preserving heat for 5min, heating to 1300 ℃ in 3min and preserving heat for 7min, cooling to 800 ℃ in 3min, and cooling to room temperature along with a furnace, wherein Te is the eutectoid transformation temperature of TiAl alloy Ti-48Al-2Cr-2Nb, and Tα is the alpha phase transformation initial temperature of TiAl alloy Ti-48Al-2Cr-2 Nb.
Fig. 6 is a low-magnification microstructure of the full-lamellar network-structured TiAl-based composite material prepared in this example, and fig. 7 is a high-magnification microstructure of the full-lamellar network-structured TiAl-based composite material prepared in this example, and it can be seen from fig. 6 and fig. 7 that the lamellar clusters of the full-lamellar network-structured TiAl-based composite material prepared in this example are fine and uniform, and precipitation-enhanced phases are generated in situ at grain boundaries and distributed in a network shape.
Example 3
The embodiment comprises the following steps:
step one, raw material preparation: selecting spherical TiAl prealloy powder with particle size of 50-150 μm, selecting Ti powder with particle size of 100nm and Al powder with particle size of 50nm, and selecting B with particle size of 50nm 4 C, powder; the spherical TiAl prealloyed powder is Ti-48Al-2Cr-2Nb;
step two, primary high-energy ball milling treatment: uniformly mixing 96.4g of spherical TiAl prealloy powder in the first step, 1.9g of Ti powder and 1.1g of Al powder to obtain primary mixed powder, vacuumizing a ball milling tank, introducing argon, then placing the primary mixed powder into the ball milling tank which is filled with the argon, placing the primary mixed powder into a planetary ball mill, and performing primary high-energy ball milling treatment for 3 hours at a rotating speed of 200r/min to obtain TiAl alloy powder with a Ti/Al transition layer on the surface;
thirdly, performing secondary high-energy ball milling treatment: mixing TiAl alloy powder with Ti/Al transition layer on the surface and 0.6g B in the first step 4 Uniformly mixing the powder C to obtain secondary mixed powder, vacuumizing a ball milling tank, introducing argon, loading the secondary mixed powder into the ball milling tank which is filled with the argon, placing the secondary mixed powder into a planetary ball mill, and performing secondary high-energy ball milling treatment for 3 hours at a rotating speed of 200r/min to obtain the surface uniform coating B 4 The TiAl alloy powder of C;
step four, screening treatment: uniformly coating the surface obtained in the step three with a 100-mesh screen 4 The TiAl alloy powder of C is subjected to screening treatment to obtain undersize as powder to be sintered, as shown in figure 8, ti powder, al powder and reinforcement B in the powder to be sintered 4 The C powder is relatively uniformly distributed on the surface of the spherical TiAl prealloy powder,no reinforcement B occurs 4 Agglomeration of powder C;
step five, powder sintering: placing the powder to be sintered obtained in the step four into a die with the diameter phi of 50mm, then carrying out vacuum degassing, and carrying out three-stage temperature sintering by using spark plasma sintering to obtain a full-sheet-layer network-structured TiAl-based composite material; the three-stage temperature sintering process comprises the following steps: heating from room temperature to 800 ℃ in 8min and preserving heat for 1min, heating to 1150 ℃ in 6min and preserving heat for 5min, heating to 1300 ℃ in 3min and preserving heat for 7min, cooling to 800 ℃ in 3min, and cooling to room temperature along with a furnace, wherein Te is the eutectoid transformation temperature of TiAl alloy Ti-48Al-2Cr-2Nb, and Tα is the alpha phase transformation initial temperature of TiAl alloy Ti-48Al-2Cr-2 Nb.
Fig. 9 is a low-magnification microstructure of the full-lamellar network-structured TiAl-based composite material prepared in this example, and fig. 10 is a high-magnification microstructure of the full-lamellar network-structured TiAl-based composite material prepared in this example, and it can be seen from fig. 9 and 10 that the lamellar clusters of the full-lamellar network-structured TiAl-based composite material prepared in this example are fine and uniform, and precipitation-enhanced phases are generated in situ at grain boundaries and distributed in a network shape.
Example 4
The embodiment comprises the following steps:
step one, raw material preparation: selecting spherical TiAl prealloy powder with particle size of 50-150 μm, selecting Ti powder with particle size of 100nm and Al powder with particle size of 50nm, and selecting B with particle size of 50nm 4 C, powder; the spherical TiAl prealloyed powder is Ti-48Al-2Cr-2Nb;
step two, primary high-energy ball milling treatment: uniformly mixing 96.1g of spherical TiAl prealloy powder in the first step, 1.9g of Ti powder and 1.1g of Al powder to obtain primary mixed powder, vacuumizing a ball milling tank, introducing argon, then placing the primary mixed powder into the ball milling tank which is filled with the argon, placing the primary mixed powder into a planetary ball mill, and performing primary high-energy ball milling treatment for 3 hours at a rotating speed of 200r/min to obtain TiAl alloy powder with a Ti/Al transition layer on the surface;
thirdly, performing secondary high-energy ball milling treatment: mixing the TiAl alloy powder with Ti transition layer on the surface and 0.9g stepB in step one 4 Uniformly mixing the powder C to obtain secondary mixed powder, vacuumizing a ball milling tank, introducing argon, loading the secondary mixed powder into the ball milling tank which is filled with the argon, placing the secondary mixed powder into a planetary ball mill, and performing secondary high-energy ball milling treatment for 3 hours at a rotating speed of 200r/min to obtain the surface uniform coating B 4 The TiAl alloy powder of C;
step four, screening treatment: uniformly coating the surface obtained in the step three with a 100-mesh screen 4 The TiAl alloy powder of C is subjected to screening treatment to obtain undersize as powder to be sintered, as shown in FIG. 11, ti powder, al powder and reinforcement B in the powder to be sintered 4 The C powder is relatively uniformly distributed on the surface of the spherical TiAl prealloyed powder, and the reinforcement B does not occur 4 Agglomeration of powder C;
step five, powder sintering: placing the powder to be sintered obtained in the step four into a die with the diameter phi of 50mm, then carrying out vacuum degassing, and carrying out three-stage temperature sintering by using spark plasma sintering to obtain a full-sheet-layer network-structured TiAl-based composite material; the three-stage temperature sintering process comprises the following steps: heating from room temperature to 800 ℃ in 8min and preserving heat for 1min, heating to 1150 ℃ in 6min and preserving heat for 5min, heating to 1300 ℃ in 3min and preserving heat for 7min, cooling to 800 ℃ in 3min, and cooling to room temperature along with a furnace, wherein Te is the eutectoid transformation temperature of TiAl alloy Ti-48Al-2Cr-2Nb, and Tα is the alpha phase transformation initial temperature of TiAl alloy Ti-48Al-2Cr-2 Nb.
Fig. 12 is a low-magnification microstructure of the full-lamellar network-structured TiAl-based composite material prepared in this example, and fig. 13 is a high-magnification microstructure of the full-lamellar network-structured TiAl-based composite material prepared in this example, and it can be seen from fig. 12 and fig. 13 that the lamellar clusters of the full-lamellar network-structured TiAl-based composite material prepared in this example are fine and uniform, and precipitation-enhanced phases are generated in situ at grain boundaries and distributed in a network shape.
Example 5
The embodiment comprises the following steps:
step one, raw material preparation: selecting spherical TiAl prealloy powder with particle size of 50-150 μm, selecting Ti powder with particle size of 100nm and Al powder with particle size of 50nmSelecting B with particle size of 50nm 4 C, powder; the spherical TiAl prealloyed powder is Ti-48Al-2Cr-2Nb;
step two, primary high-energy ball milling treatment: uniformly mixing 95.5g of spherical TiAl prealloy powder in the first step, 1.9g of Ti powder and 1.1g of Al powder to obtain primary mixed powder, vacuumizing a ball milling tank, introducing argon, then placing the primary mixed powder into the ball milling tank which is filled with the argon, placing the primary mixed powder into a planetary ball mill, and performing primary high-energy ball milling treatment for 3 hours at a rotating speed of 200r/min to obtain TiAl alloy powder with a Ti/Al transition layer on the surface;
thirdly, performing secondary high-energy ball milling treatment: mixing TiAl alloy powder with Ti transition layer on the surface and 1.5g B in the first step 4 Uniformly mixing the powder C to obtain secondary mixed powder, vacuumizing a ball milling tank, introducing argon, loading the secondary mixed powder into the ball milling tank which is filled with the argon, placing the secondary mixed powder into a planetary ball mill, and performing secondary high-energy ball milling treatment for 3 hours at a rotating speed of 200r/min to obtain the surface uniform coating B 4 The TiAl alloy powder of C;
step four, screening treatment: uniformly coating the surface obtained in the step three with a 100-mesh screen 4 The TiAl alloy powder of C is subjected to screening treatment to obtain undersize as powder to be sintered, as shown in FIG. 14, ti powder, al powder and reinforcement B in the powder to be sintered 4 The C powder is relatively uniformly distributed on the surface of the spherical TiAl prealloyed powder, and the reinforcement B does not occur 4 Agglomeration of powder C;
step five, powder sintering: placing the powder to be sintered obtained in the step four into a die with the diameter phi of 50mm, then carrying out vacuum degassing, and carrying out three-stage temperature sintering by using spark plasma sintering to obtain a full-sheet-layer network-structured TiAl-based composite material; the three-stage temperature sintering process comprises the following steps: heating from room temperature to 800 ℃ in 8min and preserving heat for 1min, heating to 1150 ℃ in 6min and preserving heat for 5min, heating to 1300 ℃ in 3min and preserving heat for 7min, cooling to 800 ℃ in 3min, and cooling to room temperature along with a furnace, wherein Te is the eutectoid transformation temperature of TiAl alloy Ti-48Al-2Cr-2Nb, and Tα is the alpha phase transformation initial temperature of TiAl alloy Ti-48Al-2Cr-2 Nb.
Fig. 15 is a low-magnification microstructure of the full-lamellar network-structured TiAl-based composite material prepared in this example, and fig. 16 is a high-magnification microstructure of the full-lamellar network-structured TiAl-based composite material prepared in this example, and it can be seen from fig. 15 and 16 that the lamellar clusters of the full-lamellar network-structured TiAl-based composite material prepared in this example are fine and uniform, and precipitation-enhanced phases are generated in situ at grain boundaries and distributed in a network shape.
Example 6
The embodiment comprises the following steps:
step one, raw material preparation: selecting spherical TiAl prealloy powder with the particle size of 50-150 mu m, selecting Ti powder with the particle size of 100nm, and selecting graphene oxide powder with the particle size of 100 nm; the spherical TiAl prealloyed powder is Ti-46Al-3Nb-0.2B;
step two, primary high-energy ball milling treatment: uniformly mixing 96.1g of spherical TiAl prealloy powder in the first step and 3g of Ti powder to obtain primary mixed powder, vacuumizing a ball milling tank, introducing argon, loading the primary mixed powder into the ball milling tank which is filled with the argon, placing the ball milling tank into a planetary ball mill, and performing primary high-energy ball milling treatment for 2 hours at a rotating speed of 150r/min to obtain TiAl alloy powder with a Ti transition layer on the surface;
thirdly, performing secondary high-energy ball milling treatment: uniformly mixing TiAl alloy powder with a Ti transition layer on the surface obtained in the second step with 0.9g of graphene oxide powder obtained in the first step to obtain secondary mixed powder, vacuumizing a ball milling tank, introducing argon, then filling the secondary mixed powder into the ball milling tank which is filled with the argon, placing the secondary mixed powder into a planetary ball mill, and performing secondary high-energy ball milling treatment for 5 hours at the rotating speed of 300r/min to obtain TiAl alloy powder with the surface uniformly coated with graphene oxide;
step four, screening treatment: screening the TiAl alloy powder with the surface uniformly coated with the graphene oxide, which is obtained in the step three, by adopting a 100-mesh screen to obtain undersize as powder to be sintered;
step five, powder sintering: placing the powder to be sintered obtained in the step four into a die with the diameter phi of 50mm, then carrying out vacuum degassing, and carrying out three-stage temperature sintering by utilizing vacuum hot-pressing sintering to obtain a full-sheet-layer network-structure TiAl-based composite material; the three-stage temperature sintering process comprises the following steps: heating from room temperature to 700 ℃ in 15min and preserving heat for 5min, heating to 1100 ℃ in 10min and preserving heat for 10min, heating to 1320 ℃ in 5min and preserving heat for 10min, cooling to 700 ℃ in 5min, and cooling to room temperature along with a furnace, wherein Te is the eutectoid transformation temperature of TiAl alloy Ti-46Al-3Nb-0.2B, and Tα is the alpha phase transition initial temperature of TiAl alloy Ti-46Al-3 Nb-0.2B.
Example 7
The embodiment comprises the following steps:
step one, raw material preparation: selecting spherical TiAl prealloy powder with the particle size of 50-150 mu m, selecting Ti powder with the particle size of 100nm, and selecting carbon black powder with the particle size of 100 nm; the spherical TiAl prealloyed powder is Ti-45Al-5Nb-0.2B-0.5C;
step two, primary high-energy ball milling treatment: uniformly mixing 96.1g of spherical TiAl prealloy powder in the first step and 3g of Ti powder to obtain primary mixed powder, vacuumizing a ball milling tank, introducing argon, loading the primary mixed powder into the ball milling tank which is filled with the argon, placing the ball milling tank into a planetary ball mill, and performing primary high-energy ball milling treatment at a rotating speed of 300r/min for 5 hours to obtain TiAl alloy powder with a Ti transition layer on the surface;
thirdly, performing secondary high-energy ball milling treatment: uniformly mixing TiAl alloy powder with a Ti transition layer on the surface obtained in the second step with 0.9g of carbon black powder in the first step to obtain secondary mixed powder, vacuumizing a ball milling tank, introducing argon, filling the secondary mixed powder into the ball milling tank which is filled with the argon, placing the secondary mixed powder into a planetary ball mill, and performing secondary high-energy ball milling treatment for 2 hours at a rotating speed of 300r/min to obtain TiAl alloy powder with the surface uniformly coated with carbon black;
step four, screening treatment: screening the TiAl alloy powder with the surface uniformly coated with the carbon black obtained in the step three by adopting a 100-mesh screen to obtain undersize to be sintered powder;
step five, powder sintering: placing the powder to be sintered obtained in the step four into a die with the diameter phi of 50mm, then carrying out vacuum degassing, and carrying out three-stage temperature sintering by using spark plasma sintering to obtain a full-sheet-layer network-structured TiAl-based composite material; the three-stage temperature sintering process comprises the following steps: heating from room temperature to 900 ℃ in 15min and preserving heat for 5min, heating to 1100 ℃ in 6min and preserving heat for 4min, heating to 1280 ℃ in 3min and preserving heat for 4min, cooling to 900 ℃ in 5min, and cooling to room temperature along with a furnace, wherein Te is the eutectoid transition temperature of TiAl alloy Ti-45Al-5Nb-0.2B-0.5C, and Taα is the alpha phase transition initial temperature of TiAl alloy Ti-45Al-5 Nb-0.2B-0.5C.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (6)
1. The preparation method of the TiAl-based composite material with the full-lamellar network structure is characterized by comprising the following steps of:
step one, raw material preparation: selecting spherical TiAl prealloy powder with the particle size of 50-150 mu m, selecting metal powder with the particle size of 50-1000 nm, and selecting reinforcement powder with the particle size of 50-100 nm;
step two, primary high-energy ball milling treatment: uniformly mixing the spherical TiAl prealloy powder and the metal powder in the first step to obtain primary mixed powder, vacuumizing a ball milling tank, introducing argon, filling the primary mixed powder into the ball milling tank into which the argon is introduced, and placing the ball milling tank into a planetary ball mill for primary high-energy ball milling treatment to obtain TiAl alloy powder with a transition layer on the surface;
thirdly, performing secondary high-energy ball milling treatment: uniformly mixing the TiAl alloy powder with the transition layer on the surface obtained in the second step with the reinforcement powder in the first step to obtain secondary mixed powder, vacuumizing a ball milling tank, introducing argon, filling the secondary mixed powder into the ball milling tank into which the argon is introduced, and placing the secondary mixed powder into a planetary ball mill for secondary high-energy ball milling treatment to obtain TiAl alloy powder with the surface uniformly coated with the reinforcement;
step four, screening treatment: screening the TiAl alloy powder with the surface uniformly coated with the reinforcement body obtained in the step three by adopting a 100-mesh screen to obtain undersize to be sintered powder;
step five, powder sintering: and (3) placing the powder to be sintered obtained in the step (IV) into a die, then carrying out vacuum degassing, and then carrying out three-stage temperature sintering to obtain the full-lamellar network structure TiAl-based composite material.
2. The method for preparing a full-lamellar network TiAl-based composite material according to claim 1, wherein the spherical TiAl prealloyed powder in the first step is Ti-48Al-2Cr-2Nb, ti-45Al-2Nb-2Mn-0.8TiB 2 ，Ti-47Al-2W-0.5Si，Ti-47Al-2Nb-2Mn-0.8TiB 2 Ti-47Al-1.5Nb-1Mn-1Cr-0.7 (Si, B), ti-45.5Al-4 (Nb, cr, ta, B), ti-46Al-3 (Nb, cr, mo) -x (B, C), wherein x<1, ti-46Al-6.5Nb-0.6Cr-0.2Ni or Ti-45Al-5Nb-yB-zC, wherein y<1，z<1；
The metal powder is Ti powder or/and Al powder;
the reinforcing body powder is B 4 C. Graphene, carbon black, carbon nanotubes or graphene oxide.
3. The preparation method of the full-lamellar network TiAl-based composite material according to claim 1, wherein the rotating speed of the primary high-energy ball milling treatment in the second step is 150-300 r/min, the time is 2-5 h, the rotating speed of the secondary high-energy ball milling treatment in the third step is 150-300 r/min, the time is 2-5 h, and the total time length of the secondary high-energy ball milling treatment is less than 8h.
4. The method for preparing the full-lamellar network TiAl-based composite material according to claim 1, wherein the three-stage temperature sintering method in the fifth step is spark plasma sintering or hot press sintering.
5. The method for preparing the full-lamellar network TiAl-based composite material according to claim 1, wherein the three-stage temperature sintering process in the fifth step is as follows: firstly, heating from room temperature to 100-300 ℃ below Te temperature within 8-15 min, preserving heat for 1-5 min, then heating to 200-250 ℃ below Taα temperature within 6-10 min, preserving heat for 4-10 min, heating to 0-50 ℃ below Taα temperature within 3-5 min, preserving heat for 4-10 min, finally cooling to 100-300 ℃ below Te temperature within 3-5 min, and cooling to room temperature along with a furnace, wherein Te is the eutectoid transformation temperature of TiAl alloy, taα is the alpha phase transformation initial temperature of TiAl alloy.
6. A full-lamellar network TiAl-based composite material, characterized in that it is produced by the method according to any one of claims 1 to 5.
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