CN117399637A - High-performance in-situ autogenous Ti 5 Si 3 Near-net forming method of phase reinforced titanium-aluminum-based composite material - Google Patents
High-performance in-situ autogenous Ti 5 Si 3 Near-net forming method of phase reinforced titanium-aluminum-based composite material Download PDFInfo
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- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000002131 composite material Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 63
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 52
- 239000010936 titanium Substances 0.000 claims abstract description 110
- 239000000463 material Substances 0.000 claims abstract description 32
- 239000000758 substrate Substances 0.000 claims abstract description 29
- 238000001816 cooling Methods 0.000 claims abstract description 28
- 239000011159 matrix material Substances 0.000 claims abstract description 28
- 230000008021 deposition Effects 0.000 claims abstract description 24
- 230000005496 eutectics Effects 0.000 claims abstract description 22
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 21
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 16
- 238000007711 solidification Methods 0.000 claims abstract description 15
- 230000008023 solidification Effects 0.000 claims abstract description 15
- 229910010038 TiAl Inorganic materials 0.000 claims abstract description 14
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 230000001105 regulatory effect Effects 0.000 claims abstract description 7
- 230000002708 enhancing effect Effects 0.000 claims abstract description 4
- 229910004349 Ti-Al Inorganic materials 0.000 claims abstract 3
- 229910004692 Ti—Al Inorganic materials 0.000 claims abstract 3
- 238000010894 electron beam technology Methods 0.000 claims description 35
- 239000000654 additive Substances 0.000 claims description 28
- 230000000996 additive effect Effects 0.000 claims description 28
- 238000000151 deposition Methods 0.000 claims description 27
- 239000010410 layer Substances 0.000 claims description 20
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 8
- 230000001133 acceleration Effects 0.000 claims description 8
- 238000013461 design Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910000765 intermetallic Inorganic materials 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001073 sample cooling Methods 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 244000137852 Petrea volubilis Species 0.000 claims description 4
- 230000007246 mechanism Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000002356 single layer Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 238000004781 supercooling Methods 0.000 claims description 3
- -1 titanium-aluminum-silicon Chemical compound 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 229910021330 Ti3Al Inorganic materials 0.000 claims 1
- 229910009871 Ti5Si3 Inorganic materials 0.000 claims 1
- 230000001276 controlling effect Effects 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 21
- 238000002360 preparation method Methods 0.000 description 9
- 238000009826 distribution Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000002787 reinforcement Effects 0.000 description 4
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 229910000601 superalloy Inorganic materials 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000000713 high-energy ball milling Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 101100172628 Caenorhabditis elegans eri-1 gene Proteins 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001887 electron backscatter diffraction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention relates to high-performance in-situ autogenous Ti 5 Si 3 The near-net forming process of phase reinforced Ti-Al base composite material includes in-situ reaction of Ti, al and Si elements in molten bath to form Ti 5 Si 3 Reinforcing phase, ti 3 Al and TiAl substrates; the solidification path is regulated and controlled by the cooling condition in the solidification process, the components of a molten pool and the like, so as to realize the primary Ti 5 Si 3 Phase and eutectic Ti 5 Si 3 Phase ratio change and based on eutectic reaction, ti is formed 5 Si 3 Enhancing phase and matrix brand new phase relation characteristics; layer-by-layer deposition is realized through multi-axis movement of a working platform, and in-situ autogenous Ti with high performance is realized 5 Si 3 Near net shape formation of the phase reinforced titanium aluminum matrix composite. The invention can realize near net forming of the large-scale titanium-aluminum-based composite material component, has higher forming efficiency, and is not easy to generate defects such as cracks, deformation and the like in the material adding process; compared with the titanium-aluminum-based composite material reported in the prior art, the strength of the titanium-aluminum-based composite material prepared by the method has equivalent plasticity, but the yield strength at the temperature of 750 ℃ is obviously improved.
Description
Technical Field
The invention relates to the technical field of preparation of titanium-aluminum-based composite materials, in particular to high-performance in-situ self-generated Ti 5 Si 3 A near net shape forming method of phase reinforced titanium-aluminum based composite material.
Background
As a key base material of an aeroengine, a further development of a light high-strength superalloy material is needed in the prior art to meet the requirement of light weight of aeronautical equipment. The light high-strength titanium-aluminum alloy is the best candidate material for replacing nickel-based superalloy in the temperature range of 650-850 ℃, and the strength of the titanium-aluminum alloy is obviously improved by adding alloy elements with high melting point and excellent oxidation resistance. The specific strength of the titanium-aluminum alloy is higher than that of the nickel-based superalloy in the range of 650-850 ℃, but the strength of the titanium-aluminum alloy is drastically reduced in the temperature range of more than 850 ℃, so that the use temperature of the titanium-aluminum alloy is limited. The composite technology is used as an important means for improving the performance of the titanium-aluminum alloy, and TiB is utilized 2 、TiC、Al 2 O 3 、B 4 C and Ti 2 AlC and the like are used as reinforcements in the titanium-aluminum alloy correspondingly, and the comprehensive performance is improved through layer penetration fracture, interface debonding, crack deflection, fiber extraction and the like.
In general, the reinforcing phase is introduced into the titanium-aluminum alloy matrix by adopting a direct addition mode, for example: the invention patent with publication number of CN202010925825.X discloses a novel titanium-aluminum-based composite material and a preparation method thereof, and is beneficial toBy Ti, al, nb, Y, caF 2 、TiC、TiB 2 The powder was sintered by hot pressing to form a matrix of Ti45Al8Nb0.5Y, 7.5wt% TiC and 3wt% TiB 2 The maximum bending strength of the titanium-aluminum-based composite material serving as the reinforcing phase is 502MPa. However, the reinforcing phase is directly added into the titanium-aluminum alloy matrix, and is formed by hot-pressing sintering, the positional relationship between the reinforcing phase and the matrix is random, the interface strength is insufficient, and the reinforcing effect is difficult to fully develop.
The interface bonding strength between the titanium aluminum alloy and the matrix can be enhanced by adopting an enhanced phase in-situ autogenous method, and the performance of the titanium aluminum alloy matrix is obviously improved. The invention patent with publication number CN201911298379.8 discloses a preparation method of a high-strength plastic-accumulation TiAl-based composite material, which comprises the steps of introducing high-melting-point Nb element into a titanium-aluminum alloy matrix, and obtaining fibrous tough Nb-rich phase and granular Ti through the processes of powder mixing, extrusion treatment such as vacuum heat, high-temperature sheath extrusion and the like 2 An AlNb phase composite reinforced high-strength plastic product TiAl intermetallic compound-based composite material. The invention patent with publication number CN109694971B discloses a powder metallurgy titanium aluminum-based composite material and a preparation method thereof, wherein the material combines high-energy ball milling and spark plasma sintering, and comprises 30-40% by weight of Ti powder and 2-8% by weight of TiO 2 Powder, 1% -5% of Nb 2 O 5 The powder and the balance of aluminum powder are mixed to prepare the titanium-aluminum-based composite material, and the method can realize the Al of a second phase in the high-energy ball milling stage 2 O 3 In situ synthesis of particles. Although the reinforcement phase in the above method is formed in situ by self-generation, the preparation process is complex, and near-net-shape formation of the sample is difficult to achieve.
The in-situ autogenous of the reinforcing phase in the titanium-aluminum alloy matrix can be realized through reasonable element addition and simple process design. The invention patent with publication number of CN20201101013311. X discloses a tough titanium-aluminum-based composite material and a preparation method thereof, wherein TiC is added into a titanium-aluminum alloy, and the titanium-aluminum-based composite material is prepared by adopting a vacuum melting method. In-situ autogenous precipitation of Ti using high content of C element 3 AlC reinforcement, which resists crack formation and propagation by second phase strengthening and dislocation strengthening of the reinforcementThe fragile interface in the tissue under the condition of high temperature is scattered and pinned, so that the high-temperature ultimate tensile strength of the titanium-aluminum-based composite material is remarkably improved. However, the titanium-aluminum-based composite material obtained by the method has poor plasticity and is difficult to process subsequently. Therefore, the preparation of the titanium-aluminum-based composite material faces the difficulties of in-situ autogenous reinforcement phase design and sample processing preparation.
The additive manufacturing provides a new method for preparing the titanium-aluminum-based composite material, but at the present stage, electron beam selective melting is mainly adopted, so that the processing efficiency is low, and the large-scale industrial production is difficult to meet; the titanium-aluminum alloy prepared by the arc additive is extremely easy to oxidize, and the exploring stage of the titanium-aluminum binary alloy is also stopped at the present stage. The electron beam fuse additive manufacturing is used as a high-vacuum and high-efficiency forming method, and has important application potential in the preparation of titanium-aluminum alloy and titanium-aluminum-based composite materials. While additive manufacturing of titanium-aluminum based composites has the following problems: the in-situ autogenous component design problem of the enhancement phase, the structure characteristics and the position relation regulation and control of the enhancement phase and the like.
Disclosure of Invention
The invention aims to provide a high-performance in-situ self-generated Ti 5 Si 3 The near-net forming method of the phase reinforced titanium-aluminum base composite material utilizes the solidification condition design to obtain a reinforced phase with a special phase relation, improves the interface bonding strength of the reinforced phase and a matrix, avoids the brittleness increase caused by the introduction of the reinforced phase, further improves the high-temperature strength of the titanium-aluminum base matrix, and realizes the service of the titanium-aluminum base matrix at a higher temperature.
The invention adopts the technical proposal for solving the technical problems that:
high-performance in-situ autogenous Ti 5 Si 3 Near-net forming method of phase reinforced titanium-aluminum-based composite material, ti is formed by utilizing in-situ reaction of Ti, al and Si elements in a molten pool in the electron beam double-wire additive manufacturing process 5 Si 3 Reinforcing phase, ti 3 Al and TiAl substrates; the solidification path is regulated and controlled by the cooling condition in the solidification process, the components of a molten pool and the like, so as to realize the primary Ti 5 Si 3 Phase and eutectic Ti 5 Si 3 Phase ratio change and based on eutectic reaction, ti is formed 5 Si 3 Enhancing phase and matrix brand new phase relation characteristics; layer-by-layer deposition is realized through multi-axis movement of a working platform, and in-situ autogenous Ti with high performance is realized 5 Si 3 Near net shape formation of the phase reinforced titanium aluminum matrix composite.
Further, the method comprises three processes of pre-heating, layer-by-layer deposition and sample cooling, and comprises the following specific steps:
(1) Pre-heating in the early stage: fixing a titanium alloy substrate polished by sand paper and cleaned by ethanol on a working platform of an electron beam fuse additive manufacturing system, and placing the working platform in a vacuum chamber of the electron beam fuse additive manufacturing system; when the vacuum degree reaches 7 multiplied by 10 -2 In Pa, preheating the substrate by adopting an electron beam rapid scanning mode until the titanium alloy substrate is red hot;
(2) Layer by layer deposition: respectively placing aluminum wires and titanium wires in independent wire feeding mechanisms of an electron beam fuse wire material adding system, adjusting the angle and the height of a wire feeding gun, setting wire feeding speeds of the aluminum wires and the titanium wires, feeding the wires into a common molten pool, depositing according to a set path, cooling for 60-80 seconds after single-pass deposition, and lowering a workbench for a certain distance to continue deposition to ensure that an electron beam focus is on the surface of the material adding component until the deposition is completed;
(3) Sample cooling: placing the titanium aluminum intermetallic compound component subjected to in-situ material addition in a vacuum environment for cooling until the titanium aluminum intermetallic compound component is cooled to room temperature;
wherein, the basic parameters of the substrate preheating are as follows: acceleration voltage is 60kV, focusing current is 1000-1200mA, scanning frequency is 300-600Hz, scanning range is 300-600%, scanning mode is circular, and scanning speed is 20mm/s; the preheating mode adopts step preheating, namely the preheating beam current is gradually increased from 5mm to 25mm until the substrate is red hot, namely the preheating is finished; the angle adjustment range of the wire feeding gun is 45-55 degrees; the distance between the front section wire material of the wire feeding gun and the substrate is within 1mm, so that molten drops can be continuously transited to realize forming; the cooling process of the material-added sample needs to be carried out under vacuum environment by adopting sectional cooling, namely cooling for 2-3 hours under high vacuum degree, preserving heat for 10-15 hours under low vacuum degree, and the high vacuum range is lower than 7 multiplied by 10 -2 Pa, the low vacuum range is 0-10Pa.
Further, in-situ autogenous Ti 5 Si 3 The near-net forming process of the phase reinforced titanium-aluminum-based composite material adopts ERti-1 wire and ER4047 wire as raw materials, and the diameter is 1.0-2.0 mm; ERTI-1 wire consists of C not greater than 0.03wt%, O0.03-0.10 wt%, N not greater than 0.012wt%, H not greater than 0.005wt%, fe not greater than 0.08wt% and Ti for the rest; the ER4047 wire comprises 12wt% of Si, less than 0.15wt% of Mn, less than 0.05wt% of Cu, less than 0.15wt% of Ti, less than 0.20wt% of Zn, less than 0.6wt% of Fe and the balance of Al.
Further, the high-performance titanium-aluminum-based composite material comprises the components of Ti- (34-38) at% Al- (5.5-9.5) at% Si; the relation between the wire feeding speed and the components is as follows:
wherein E is x And A x The design mass fraction and the atomic fraction of the main elements are respectively; e (E) xi (i=1, 2 … …, n) is the mass fraction of elements in the wire; s is S i The unit is mm/min, which is the wire feeding speed; d (D) i The diameter of the wire is in mm; ρ i Is the density of the wire material, and the unit is g/cm 3 ；M x Is the relative atomic mass of the element; the electron beam fuse material-adding process can cause burning loss of different elements, so that the actual atomic fraction of the different elementsIs that
λ x The evaporation coefficient of the element is 1, 1.15 and 0.71, wherein only volatilization of Ti, al and Si elements is considered; the wire feeding speed ranges from 300mm/min to 800mm/min.
Further, high performance titanium aluminum based compositeThe material is mainly prepared from micron-scale primary polygon Ti 5 Si 3 Eutectic acicular Ti of phase and nano scale 5 Si 3 Phases and Ti 3 Eutectoid lamellar structure of Al+TiAl, wherein, eutectic acicular Ti 5 Si 3 Phase of Ti 3 The eutectoid sheet of Al+TiAl has the following special phase relation
Furthermore, titanium element can react with silicon, aluminum element and the like, and the content ratio of the aluminum element to the silicon element is changed near the titanium aluminum silicon eutectic composition point, so that the primary polygon Ti is realized 5 Si 3 Phase-co-crystal needle-like Ti 5 Si 3 The phase ratio is regulated and controlled to regulate the mechanical performance of the Ti-Al-base composite material.
Further, the electron beam double-wire additive obtains Ti with special phase relation 5 Si 3 The phase reinforced titanium-aluminum-based composite material needs to provide high superheat solidification condition of more than 1000K in the process of material addition, so as to obtain supercooling degree of more than 200K, and produce L- & gtalpha+Ti in the solidification process 5 Si 3 Is a eutectic reaction of (a).
Further, the realized additive process parameters are as follows: acceleration voltage is 60kV, focusing current is 1000-1200mA, scanning frequency is 600-900Hz, scanning range is 700-900%, scanning mode is circular, deposition speed is 1-5 mm/s, monolayer height is 0.75-2mm, and electron beam current is 25mA-45mA; and the cooling speed is controlled to be 300-500K/s through the waiting time between layers of 50-70 s.
Compared with the prior art, the invention has the remarkable advantages that: the invention can realize near net forming of the large-scale titanium-aluminum-based composite material component, has higher forming efficiency, and is not easy to generate defects such as cracks, deformation and the like in the material adding process; compared with the titanium-aluminum-based composite material reported in the prior art, the strength of the titanium-aluminum-based composite material prepared by the method has equivalent plasticity, but the yield strength at the temperature of 750 ℃ is obviously improved.
Drawings
FIG. 1 is a high performance in situ autogenous Ti 5 Si 3 Physical pictures of the phase-reinforced titanium-aluminum-based composite material.
FIG. 2 is a high performance in situ autogenous Ti 5 Si 3 Phase-reinforced titanium-aluminum-based composite microstructure photograph, a microstructure photograph in additive component layer, b lamellar structure and acicular eutectic Ti 5 Si 3 Phase, c eutectic Ti 5 Si 3 Phase and primary Ti 5 Si 3 Phase morphology, d microstructure photographs between additive component layers.
FIG. 3 is an in situ autogenous Ti 5 Si 3 Phase relation between reinforcing phase and titanium-aluminum alloy matrix in phase reinforced titanium-aluminum matrix composite material, alpha EBSD test gray level diagram, b titanium-aluminum matrix composite material component phase diagram, and c Ti in additive component 3 Al phase pole diagram, d Ti in additive component 5 Si 3 Phase pole diagram, tiAl phase pole diagram in e additive component.
FIG. 4 is an in situ autogenous Ti 5 Si 3 Phase boundary distribution with phase and matrix having special phase relation aTi 5 Si 3 Phase of Ti 3 Special grain boundary distribution of Al phase, b TiAl phase and Ti phase 5 Si 3 Phase and Ti 3 Al phase special grain boundary distribution, c special grain boundary distribution frequency statistics, d grain boundary statistics of different phases.
FIG. 5 is an in situ self-generated Ti 5 Si 3 Phase-enhanced titanium-aluminum-based composite material performance test result and performance comparison with existing materials, namely a nano indentation test result of different phases, and b in-situ autogenous Ti 5 Si 3 Compression test result of phase reinforced titanium-aluminum-based composite material at room temperature and 750 ℃, and c in-situ autogenous Ti 5 Si 3 And comparing the performance of the phase-reinforced titanium-aluminum-based composite material with that of the existing titanium-aluminum alloy and composite material.
Detailed Description
The invention is further described in connection with the following embodiments in order to make the technical means, the creation features, the achievement of the purpose and the effect of the invention easy to understand.
High-performance in-situ autogenous Ti 5 Si 3 Near-net forming method of phase reinforced titanium-aluminum-based composite material, ti is formed by utilizing in-situ reaction of Ti, al and Si elements in a molten pool in the electron beam double-wire additive manufacturing process 5 Si 3 Reinforcing phase, ti 3 Al and TiAl substrates; the solidification path is regulated and controlled by the cooling condition in the solidification process, the components of a molten pool and the like, so as to realize the primary Ti 5 Si 3 Phase and eutectic Ti 5 Si 3 Phase ratio change and based on eutectic reaction, ti is formed 5 Si 3 Enhancing phase and matrix brand new phase relation characteristics; layer-by-layer deposition is realized through multi-axis movement of a working platform, and in-situ autogenous Ti with high performance is realized 5 Si 3 Near net shape formation of the phase reinforced titanium aluminum matrix composite.
Further, the method comprises three processes of pre-heating, layer-by-layer deposition and sample cooling, and comprises the following specific steps:
(1) Pre-heating in the early stage: fixing a titanium alloy substrate polished by sand paper and cleaned by ethanol on a working platform of an electron beam fuse additive manufacturing system, and placing the working platform in a vacuum chamber of the electron beam fuse additive manufacturing system; when the vacuum degree reaches 7 multiplied by 10 -2 In Pa, preheating the substrate by adopting an electron beam rapid scanning mode until the titanium alloy substrate is red hot;
(2) Layer by layer deposition: respectively placing aluminum wires and titanium wires in independent wire feeding mechanisms of an electron beam fuse wire material adding system, adjusting the angle and the height of a wire feeding gun, setting wire feeding speeds of the aluminum wires and the titanium wires, feeding the wires into a common molten pool, depositing according to a set path, cooling for 60-80 seconds after single-pass deposition, and lowering a workbench for a certain distance to continue deposition to ensure that an electron beam focus is on the surface of the material adding component until the deposition is completed;
(3) Sample cooling: placing the titanium aluminum intermetallic compound component subjected to in-situ material addition in a vacuum environment for cooling until the titanium aluminum intermetallic compound component is cooled to room temperature;
wherein, the basic parameters of the substrate preheating are as follows: acceleration voltage is 60kV, focusing current is 1000-1200mA, scanning frequency is 300-600Hz, scanning range is 300-600%, and scanning mode is roundThe scanning speed is 20mm/s; the preheating mode adopts step preheating, namely the preheating beam current is gradually increased from 5mm to 25mm until the substrate is red hot, namely the preheating is finished; the angle adjustment range of the wire feeding gun is 45-55 degrees; the distance between the front section wire material of the wire feeding gun and the substrate is within 1mm, so that molten drops can be continuously transited to realize forming; the cooling process of the material-added sample needs to be carried out under vacuum environment by adopting sectional cooling, namely cooling for 2-3 hours under high vacuum degree, preserving heat for 10-15 hours under low vacuum degree, and the high vacuum range is lower than 7 multiplied by 10 -2 Pa, the low vacuum range is 0-10Pa.
Further, in-situ autogenous Ti 5 Si 3 The near-net forming process of the phase reinforced titanium-aluminum-based composite material adopts ERti-1 wire and ER4047 wire as raw materials, and the diameter is 1.0-2.0 mm; ERTI-1 wire consists of C not greater than 0.03wt%, O0.03-0.10 wt%, N not greater than 0.012wt%, H not greater than 0.005wt%, fe not greater than 0.08wt% and Ti for the rest; the ER4047 wire comprises 12wt% of Si, less than 0.15wt% of Mn, less than 0.05wt% of Cu, less than 0.15wt% of Ti, less than 0.20wt% of Zn, less than 0.6wt% of Fe and the balance of Al.
Further, the high-performance titanium-aluminum-based composite material comprises the components of Ti- (34-38) at% Al- (5.5-9.5) at% Si; the relation between the wire feeding speed and the components is as follows:
wherein E is x And A x The design mass fraction and the atomic fraction of the main elements are respectively; e (E) xi (i=1, 2 … …, n) is the mass fraction of elements in the wire; s is S i The unit is mm/min, which is the wire feeding speed; d (D) i The diameter of the wire is in mm; ρ i Is the density of the wire material, and the unit is g/cm 3 ；M x Is the relative atomic mass of the element; the electron beam fuse material-adding process can cause burning loss of different elements, so that the actual atomic fraction of the different elementsIs that
λ x In the method, only volatilization of Ti, al and Si elements is considered, wherein the volatilization coefficients are 1, 1.15 and 0.71; the wire feeding speed ranges from 300mm/min to 800mm/min.
Further, the high-performance titanium-aluminum-based composite material mainly comprises micron-sized primary polygon Ti 5 Si 3 Eutectic acicular Ti of phase and nano scale 5 Si 3 Phases and Ti 3 Eutectoid lamellar structure of Al+TiAl, wherein, eutectic acicular Ti 5 Si 3 Phase of Ti 3 The eutectoid sheet of Al+TiAl has the following special phase relation
Furthermore, titanium element can react with silicon, aluminum element and the like, and the content ratio of the aluminum element to the silicon element is changed near the titanium aluminum silicon eutectic composition point, so that the primary polygon Ti is realized 5 Si 3 Phase-co-crystal needle-like Ti 5 Si 3 The phase ratio is regulated and controlled to regulate the mechanical performance of the Ti-Al-base composite material.
Further, the electron beam double-wire additive obtains Ti with special phase relation 5 Si 3 The phase reinforced titanium-aluminum-based composite material needs to provide high superheat solidification condition of more than 1000K in the process of material addition, so as to obtain supercooling degree of more than 200K, and produce L- & gtalpha+Ti in the solidification process 5 Si 3 Is a eutectic reaction of (a).
Further, the realized additive process parameters are as follows: acceleration voltage is 60kV, focusing current is 1000-1200mA, scanning frequency is 600-900Hz, scanning range is 700-900%, scanning mode is circular, deposition speed is 1-5 mm/s, monolayer height is 0.75-2mm, and electron beam current is 25mA-45mA; and the cooling speed is controlled to be 300-500K/s through the waiting time between layers of 50-70 s.
Example 1
The embodiment is high-performance in-situ autogenous Ti 5 Si 3 Near net forming method of phase reinforced titanium-aluminum base composite material, wherein ERi-1 and ER4047 wires with diameter of 1.6mm are used as raw materials, and base plate with size of 120×60×10mm is used 3 The substrate and wire composition of the pure titanium sheet are shown below.
The near net-shape process of the titanium-aluminum based composite material is as follows:
(1) Pre-heating in the early stage: and fixing the titanium alloy substrate polished by sand paper and cleaned by ethanol on a working platform of the electron beam fuse additive manufacturing system, and placing the working platform in a vacuum chamber of the electron beam fuse additive manufacturing system. When the vacuum degree reaches the working vacuum degree, preheating the substrate by adopting an electron beam fast scanning mode until the titanium alloy substrate is red hot;
(2) Layer by layer deposition: respectively placing aluminum wires and titanium wires in independent wire feeding mechanisms of an electron beam fuse wire material adding system, adjusting the angle and the height of a wire feeding gun, setting wire feeding speeds of the aluminum wires and the titanium wires, feeding the wires into a common molten pool, depositing according to a set path, cooling for 60 seconds after a single path is deposited, lowering a workbench for 1mm, and continuing to deposit to ensure that an electron beam focus is on the surface of the material adding component until the deposition is completed;
(3) And (3) cooling the additive component: the in-situ additive titanium aluminum intermetallic component is placed in a vacuum environment for cooling until the component is cooled to room temperature.
Wherein, the basic parameters of the substrate preheating are as follows: acceleration voltage is 60kV, focusing current is 1032mA, scanning frequency is 500Hz, scanning range is 600%, scanning mode is circular, and scanning speed is 20mm/s. The preheating mode adopts step preheating, namely the preheating beam current is gradually increased from 5mm to 25mm until the substrate is red hot, namely the preheating is finished; the angle of the wire feeding gun is set to be 45 degrees, and the distance between the wire material at the front section of the wire feeding gun and the substrate is 1mm.
The titanium wire feeding speed in the material adding process is set to be 380mm/min, and the aluminum wire feeding speed is set to be 420mm/min. The additive process parameters are set as follows: acceleration voltage is 60kV, focusing current 1141mA, scanning frequency is 600Hz, scanning range is 800%, scanning mode is circular, single-layer height is 1mm, electron beam current is 25mA, and interlayer waiting time is 60s.
The cooling process of the material-added sample needs to be carried out under vacuum environment by adopting sectional cooling, namely cooling for 3 hours under high vacuum degree, preserving heat for 15 hours under low vacuum degree, and the vacuum degree under high vacuum condition is 3 multiplied by 10 -2 Pa, the vacuum degree under high vacuum condition is 7Pa.
With the method of this example, well formed in situ self-produced Ti was obtained 5 Si 3 The phase reinforced titanium-aluminum-based composite material is shown in figure 1, and the obtained titanium-aluminum-based composite material component has the advantages of uniform components, good interlayer bonding, no defects such as cracks and air holes, and the calculated components are Ti-42.88at% of Al-5.7at% of Si, and the actual components are Ti-34.74at% of Al-7.25at% of Si. FIG. 2 is a high performance in situ autogenous Ti 5 Si 3 Microscopic structure photo of phase reinforced titanium-aluminum base composite material, in-situ self-generated Ti can be clearly seen in the picture 5 Si 3 Phase and titanium-aluminum alloy matrix, wherein Ti 5 Si 3 Phase-separated into primary polygonal Ti 5 Si 3 Phase and eutectic acicular Ti 5 Si 3 And (3) phase (C). FIG. 3 is an in situ autogenous Ti 5 Si 3 The phase relation between the reinforcing phase and the titanium aluminum alloy matrix in the phase-reinforced titanium aluminum matrix composite material can be clearly seen that the phase relation between the reinforcing phase and the matrix is obvious; in-situ autogenous Ti according to FIG. 4 5 Si 3 The phase boundary distribution of the phase and the matrix with a special phase relationship can be found that the phase relationship is ubiquitous. FIG. 5 is an in situ self-generated Ti 5 Si 3 The room temperature yield strength of the phase reinforced titanium-aluminum-based composite material is obviously higher than that of the existing commercial Ti-48Al-2Nb-2Cr alloy, and the high temperature yield strength is equivalent to that of most materials.
The invention introduces Ti through an in-situ autogenous mode through an innovative titanium-aluminum alloy component 5 Si 3 The phase, the high-performance titanium aluminum base composite material is obtained, and the yield strength of the titanium aluminum base at room temperature and high temperature is greatly improved while the plasticity of the titanium aluminum base is not reduced.
Claims (8)
1. High-performance in-situ autogenous Ti 5 Si 3 The near-net forming method of the phase reinforced titanium-aluminum-based composite material is characterized in that Ti is formed by utilizing in-situ reaction of Ti, al and Si elements in a molten pool in the electron beam double-wire additive manufacturing process 5 Si 3 Reinforcing phase, ti 3 Al and TiAl substrates; the solidification path is regulated and controlled by the cooling condition in the solidification process, the components of a molten pool and the like, so as to realize the primary Ti 5 Si 3 Phase and eutectic Ti 5 Si 3 Phase ratio change and based on eutectic reaction, ti is formed 5 Si 3 Enhancing phase and matrix brand new phase relation characteristics; layer-by-layer deposition is realized through multi-axis movement of a working platform, and in-situ autogenous Ti with high performance is realized 5 Si 3 Near net shape formation of the phase reinforced titanium aluminum matrix composite.
2. High performance in situ self-generated Ti according to claim 1 5 Si 3 The near-net forming method of the phase reinforced titanium-aluminum-based composite material is characterized by comprising three processes of pre-heating, layer-by-layer deposition and sample cooling, and comprises the following specific steps:
(1) Pre-heating in the early stage: fixing a titanium alloy substrate polished by sand paper and cleaned by ethanol on a working platform of an electron beam fuse additive manufacturing system, and placing the working platform in a vacuum chamber of the electron beam fuse additive manufacturing system; when the vacuum degree reaches 7 multiplied by 10 -2 In Pa, preheating the substrate by adopting an electron beam rapid scanning mode until the titanium alloy substrate is red hot;
(2) Layer by layer deposition: respectively placing aluminum wires and titanium wires in independent wire feeding mechanisms of an electron beam fuse wire material adding system, adjusting the angle and the height of a wire feeding gun, setting wire feeding speeds of the aluminum wires and the titanium wires, feeding the wires into a common molten pool, depositing according to a set path, cooling for 60-80 seconds after single-pass deposition, and lowering a workbench for a certain distance to continue deposition to ensure that an electron beam focus is on the surface of the material adding component until the deposition is completed;
(3) Sample cooling: placing the titanium aluminum intermetallic compound component subjected to in-situ material addition in a vacuum environment for cooling until the titanium aluminum intermetallic compound component is cooled to room temperature;
wherein, the basic parameters of the substrate preheating are as follows: acceleration voltage is 60kV, focusing current is 1000-1200mA, scanning frequency is 300-600Hz, scanning range is 300-600%, scanning mode is circular, and scanning speed is 20mm/s; the preheating mode adopts step preheating, namely the preheating beam current is gradually increased from 5mm to 25mm until the substrate is red hot, namely the preheating is finished; the angle adjustment range of the wire feeding gun is 45-55 degrees; the distance between the front section wire material of the wire feeding gun and the substrate is within 1mm, so that molten drops can be continuously transited to realize forming; the cooling process of the material-added sample needs to be carried out under vacuum environment by adopting sectional cooling, namely cooling for 2-3 hours under high vacuum degree, preserving heat for 10-15 hours under low vacuum degree, and the high vacuum range is lower than 7 multiplied by 10 -2 Pa, the low vacuum range is 0-10Pa.
3. High performance in situ self-generated Ti according to claim 1 5 Si 3 Near-net forming method of phase reinforced titanium-aluminum based composite material, which is characterized in that in-situ authigenic Ti 5 Si 3 The near-net forming process of the phase reinforced titanium-aluminum-based composite material adopts ERti-1 wire and ER4047 wire as raw materials, and the diameter is 1.0-2.0 mm; ERTI-1 wire consists of C not greater than 0.03wt%, O0.03-0.10 wt%, N not greater than 0.012wt%, H not greater than 0.005wt%, fe not greater than 0.08wt% and Ti for the rest; the ER4047 wire comprises 12wt% of Si, less than 0.15wt% of Mn, less than 0.05wt% of Cu, less than 0.15wt% of Ti, less than 0.20wt% of Zn, less than 0.6wt% of Fe and the balance of Al.
4. A high performance in situ self-priming according to claim 1Raw Ti 5 Si 3 The near-net forming method of the phase reinforced titanium-aluminum-based composite material is characterized in that the high-performance titanium-aluminum-based composite material comprises the components of Ti- (34-38) at% Al- (5.5-9.5) at% Si; the relation between the wire feeding speed and the components is as follows:
wherein E is x And A x The design mass fraction and the atomic fraction of the main elements are respectively; e (E) xi (i=1, 2 … …, n) is the mass fraction of elements in the wire; s is S i The unit is mm/min, which is the wire feeding speed; d (D) i The diameter of the wire is in mm; ρ i Is the density of the wire material, and the unit is g/cm 3 ；M x Is the relative atomic mass of the element; the electron beam fuse material-adding process can cause burning loss of different elements, so that the actual atomic fraction of the different elementsIs that
λ x The evaporation coefficient of the element is 1, 1.15 and 0.71, wherein only volatilization of Ti, al and Si elements is considered; the wire feeding speed ranges from 300mm/min to 800mm/min.
5. High performance in situ self-generated Ti according to claim 1 5 Si 3 The near-net forming process of phase reinforced Ti-Al base composite material includes the steps of 5 Si 3 Co-phase, nanoscaleAcicular Ti 5 Si 3 Phases and Ti 3 Eutectoid lamellar structure of Al+TiAl, wherein, eutectic acicular Ti 5 Si 3 Phase of Ti 3 The eutectoid sheet of Al+TiAl has the following special phase relation
{0001} Ti3Al //{0001} Ti5Si3 //{111} TiAl 。
6. High performance in situ self-generated Ti according to claim 1 5 Si 3 A near-net forming method of a phase-reinforced titanium-aluminum-based composite material is characterized in that based on the fact that titanium element can react with silicon and aluminum element, the content ratio of aluminum element and silicon element is changed near the eutectic composition point of titanium-aluminum-silicon, so as to form a primary polygon Ti 5 Si 3 Phase-co-crystal needle-like Ti 5 Si 3 The phase ratio is used for regulating and controlling the mechanical properties of the titanium-aluminum-based composite material.
7. High performance in situ self-generated Ti according to claim 1 5 Si 3 The near-net forming process of phase reinforced Ti-Al base composite material features that electron beam double filament material adding process to obtain Ti with special phase relation 5 Si 3 The phase reinforced titanium-aluminum-based composite material needs to provide high superheat solidification condition of more than 1000K in the process of material addition, so as to obtain supercooling degree of more than 200K, and produce L- & gtalpha+Ti in the solidification process 5 Si 3 Is a eutectic reaction of (a).
8. The high performance in situ self-generated Ti of claim 7 5 Si 3 The near-net forming method of the phase-reinforced titanium-aluminum-based composite material is characterized in that the realized additive technological parameters are as follows: acceleration voltage is 60kV, focusing current is 1000-1200mA, scanning frequency is 600-900Hz, scanning range is 700-900%, scanning mode is circular, deposition speed is 1-5 mm/s, monolayer height is 0.75-2mm, and electron beam current is 25mA-45mA;and the cooling speed is controlled to be 300-500K/s through the waiting time between layers of 50-70 s.
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