CN117359232A - Pearl layer-imitated bricking composite material and preparation method thereof - Google Patents
Pearl layer-imitated bricking composite material and preparation method thereof Download PDFInfo
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- CN117359232A CN117359232A CN202311494636.1A CN202311494636A CN117359232A CN 117359232 A CN117359232 A CN 117359232A CN 202311494636 A CN202311494636 A CN 202311494636A CN 117359232 A CN117359232 A CN 117359232A
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- 239000002131 composite material Substances 0.000 title claims abstract description 136
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000005096 rolling process Methods 0.000 claims abstract description 121
- 238000004321 preservation Methods 0.000 claims abstract description 50
- 230000009467 reduction Effects 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 29
- 238000005496 tempering Methods 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 238000007731 hot pressing Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 238000003466 welding Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 230000002035 prolonged effect Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000011449 brick Substances 0.000 abstract description 62
- 230000001105 regulatory effect Effects 0.000 abstract description 5
- 229910010380 TiNi Inorganic materials 0.000 description 31
- 238000010586 diagram Methods 0.000 description 9
- 238000005520 cutting process Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000003014 reinforcing effect Effects 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 5
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000011664 nicotinic acid Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- IHCCLXNEEPMSIO-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 IHCCLXNEEPMSIO-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 238000010146 3D printing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 239000002648 laminated material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21D22/00—Shaping without cutting, by stamping, spinning, or deep-drawing
- B21D22/02—Stamping using rigid devices or tools
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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Abstract
The invention provides a pearl layer-imitated brickwork composite material and a preparation method thereof, wherein the laminated composite material is placed in a heat treatment furnace which is heated to a selected temperature for heat preservation; rolling in a rolling mill for multiple times, and performing heat preservation tempering among each pass, and stopping after rolling to a certain rolling reduction; placing the composite material into a heat treatment furnace which is heated to a higher temperature for heat preservation; and then placing the materials into a rolling mill for multi-pass rolling, carrying out heat preservation tempering among each pass, and stopping rolling until the rolling quantity is selected, thus obtaining the pearl layer-like composite material. According to the invention, the brick structure is regulated and controlled by changing the rolling temperature and rolling quantity in the low-temperature stage and the high-temperature stage, so that the performance of the brick structure is regulated and controlled, and the brick structure is very flexible; the preparation method is simple to operate and high in practicability.
Description
Technical Field
The invention relates to a pearl layer-imitated brickwork composite material and a preparation method thereof, and the preparation method adopts a variable-temperature rolling process. Belongs to the technical field of bionic composite material preparation.
Background
The composite material combines two or more materials with different properties, takes advantage of the shortages, and generates a synergistic effect, so that the composite material has better comprehensive performance than the original composition material and meets various different requirements.
The bionic composite material is designed by inspiring the structure and the function of a natural organism, and can obtain the artificial composite material with the performance similar to the natural organism. Unlike common composite material, the bionic composite material has important comprehensive performance including impact resistance, damage resistance, etc. through fine combination of simple composition and complex structure.
The brick and mortar structure of the shell pearl layer ensures that the shell pearl layer has excellent mechanical properties. In recent years, more and more researchers have begun to design pearl layer-like composite materials, and many novel preparation methods such as an assembly method, a pouring method, a freezing casting method, 3D printing and the like are presented. However, due to the limitations of equipment and process, complex and large-sized bulk materials cannot be manufactured. The existing preparation method of the pearl-like brick composite material capable of being produced on a large scale solves the problem that the brick composite material cannot be produced on a large scale by applying a hot-pressing hot-rolling technology with higher industrialization maturity through the invention of the college of materials of Beijing university (patent number 202011441944.4). The method has the advantages of simple process, various raw material obtaining methods, no need of special equipment, good practicability, and the like, but still has the defects that the method only rolls at a fixed temperature, and the mechanical properties of the composite material can be regulated and controlled by changing the reduction at a temperature and further changing related parameters of bricks, so that the method is single and inflexible.
Disclosure of Invention
The invention aims to solve the problems that the existing bricking composite material is single in preparation method, and the width, thickness and spacing of bricks cannot be flexibly adjusted so as to regulate and control the mechanical properties of the bricks, and provides a preparation method of a more various imitation pearl layer composite material, namely variable-temperature rolling.
The composite material is formed by alternately mixing a hard reinforcing phase and a ductile phase with plasticity in a brick mud mode, and when the composite material is broken, phenomena such as deflection, bridging and passivation occur to cracks, so that the tolerance of the composite material to the cracks is improved, the fracture toughness and the ductility are improved, and the strength loss is reduced. The raw material of the method is laminated composite material, and the pearl layer-like composite material is obtained by adopting a variable-temperature rolling method. The process is to roll at low temperature to make the laminated material produce certain amount of prefabricated cracks and roll at higher temperature to make the mortar filled fully.
Compared with the original preparation method, the variable-temperature rolling has more adjustable variables, and can better adjust and control the width, thickness and spacing of bricks so as to adjust and control the mechanical properties of the brick composite material, thereby obtaining the pearl layer-like brick composite material with required strength or plasticity.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
the preparation method of the pearl layer-imitated bricking composite material comprises the following steps:
step one, placing the laminated composite material in a heat treatment furnace which is heated to a selected temperature for heat preservation;
step two, placing the heated laminated composite material into a rolling mill for multi-pass rolling, carrying out heat preservation tempering between each pass, and stopping rolling until a certain rolling reduction is achieved;
step three, placing the composite material rolled to a certain rolling reduction in a heat treatment furnace which is heated to a higher temperature for heat preservation;
step four, putting the heated composite material into a rolling mill again for multi-pass rolling, carrying out heat preservation tempering among each pass, and stopping rolling until the rolling reduction is selected;
before the first step, the laminated composite material is placed in a metal sheath, the metal sheath is welded to be airtight, and the thickness of the sheath is 2-10mm; the metal sheath is selected based on the hardness of the laminate composite.
The heat preservation temperature in the first step is 50-500 ℃;
the total rolling quantity in the second step is 5% -20% of the thickness of the material, the tempering time of each pass is 2-20min, the heat preservation time is prolonged by 1min every 1mm of the thickness of the sample, and the tempering temperature is the same as the heat preservation temperature in the first step.
The temperature in the third step is 400-1000 ℃.
The total rolling reduction in the step four is 10% -90% of the thickness of the material, the tempering time of each pass is 2-20min, the heat preservation time is prolonged by 1min every 1mm of the thickness of the sample, and the tempering temperature is the same as the heat preservation temperature in the step three.
And fifthly, placing the graphite mold filled with the composite material in a hot pressing furnace, vacuumizing the hot pressing furnace, then heating the hearth to a selected temperature, preserving heat for 0.1-6 hours, applying a selected pressure, preserving heat and pressure for 1-8 hours, unloading the pressure, cooling to room temperature along with the furnace, and taking out to obtain the pearl layer-like composite material.
The temperature rising rate of the temperature rising in the step five is 10 ℃/min, and the vacuum degree of vacuumizing is less than 5 multiplied by 10 -3 Pa, the heat preservation temperature is selected according to the raw materials, and the pressure maintaining pressure is 5-20MPa.
The invention has the beneficial effects that:
compared with the original laminated composite material, the pearl layer-imitated composite material prepared by the invention has the advantages that the compression strength and the elongation are improved;
according to the invention, the parameters of the brick are regulated and controlled by changing the rolling temperature and rolling quantity in the low-temperature stage and the high-temperature stage, so that the performance of the brick is regulated and controlled, and the brick is very flexible;
the side surface of the pearl layer-imitated composite material prepared by variable-temperature rolling is more bricked than that of the pearl layer-imitated composite material prepared by single-temperature rolling, so that the structural non-uniformity is reduced, and the anisotropy of the material is reduced.
The preparation method of the imitation pearl layer composite material has the advantages of simplicity in operation, strong practicability, wide application range and good industrial application prospect.
Drawings
FIG. 1 is TiNi/Ti in example 1 2 Stereo spelling of cross section back scattering scanning electron microscope (BSEM) picture of Ni imitation pearl layer composite materialDrawing;
FIG. 2a is TiNi/Ti of example 1 2 One of the X-ray energy spectrum (EDS) diagrams of the Ni-imitation pearl layer composite material;
FIG. 2b is TiNi/Ti of example 1 2 A second X-ray energy spectrum (EDS) diagram of the Ni imitation pearl layer composite material;
FIG. 3 is a single temperature roll prepared TiNi/Ti in example 1 2 A three-dimensional splice diagram of a cross-section back scattering scanning electron microscope (BSEM) diagram of the Ni-simulated nacreous layer composite material;
FIG. 4 is TiNi/Ti in example 2 2 A three-dimensional splice diagram of a cross-section back scattering scanning electron microscope (BSEM) diagram of the Ni-simulated nacreous layer composite material;
FIG. 5 is TiNi/Ti in example 3 2 A three-dimensional splice of a cross-sectional back-scattered scanning electron microscope (BSEM) image of the Ni-imitation pearl layer composite material.
FIG. 6 is TiNi/Ni in example 4 3 A three-dimensional splice diagram of a cross-section back scattering scanning electron microscope (BSEM) diagram of the Ti imitation pearl layer composite material.
FIG. 7 is a perspective view of a cross-sectional back-scattered scanning electron microscope (BSEM) of the Ti/TiC nacreous layer-like composite of example 6.
Detailed Description
The invention is further described below with reference to the drawings and examples.
Example 1
TiNi/Ti obtained by variable-temperature rolling 2 Ni brick composite material, the composite material is made of Ti 2 Ni and TiNi are alternately mixed in the form of "brick mud" in which the plane Ti parallel to the rolling direction 2 The Ni brick width was about 45 μm, the brick thickness was about 18 μm, and the average brick spacing was about 49 μm. In a plane perpendicular to the rolling direction Ti 2 The Ni brick width was about 62 μm, the brick thickness was about 19 μm, and the average brick spacing was about 54 μm.
TiNi/Ti 2 The preparation method of the Ni-imitation pearl layer composite material comprises the following steps,
step one: tiNi/Ti with the length of 200mm, the width of 80mm and the thickness of 20mm 2 Ni laminated composite materialPutting the material into a stainless steel sheath, welding the sheath to enable the sheath to be airtight, wherein the thickness of the sheath is 4mm;
step two: tiNi/Ti coated by the sheath 2 Placing the Ni laminated composite material in a heat treatment furnace which is heated to 500 ℃ for heat preservation;
step three: tiNi/Ti coated by a heated sheath 2 The Ni laminated composite material is put into a rolling mill for multi-pass rolling, the rolling reduction of each pass is 0.5mm, heat preservation tempering is carried out at 500 ℃ between each pass, and the rolling is stopped after the rolling reduction is 10%;
step four: placing the composite material rolled to 10% in a heat treatment furnace heated to 700 ℃ for heat preservation;
step five: the TiNi/Ti after heat preservation 2 The Ni composite material is put into a rolling mill for multi-pass rolling, the rolling reduction of each pass is 5 percent of the residual thickness of the material, heat preservation tempering is carried out at 700 ℃ between each pass, and the rolling is stopped after the total rolling reduction is 60 percent of the thickness of the material;
step six, cutting and dismantling the metal sheath to take out the composite material, and taking out TiNi/Ti 2 Placing the Ni composite material into a graphite mold;
step seven, tiNi/Ti is filled 2 Placing a graphite mold of the Ni composite material in a vacuum hot-pressing furnace, vacuumizing the vacuum hot-pressing furnace, wherein the vacuum degree is 4 multiplied by 10 -3 Pa, then raising the temperature of the hearth to 900 ℃, preserving heat for 1h, applying 8MPa pressure, preserving heat and pressure for 2h, unloading pressure, cooling to room temperature along with the furnace, and taking out to obtain a sample.
Characterization of experimental results: the simulated nacreous layer composite material was found to have similar "brick mud" alternate mix structural characteristics as the nacreous layer through the BSEM diagram shown in fig. 1. In combination with the EDS patterns shown in fig. 2a and 2b, dark "bricks" were found to be reinforcing phases Ti 2 The light-colored mud matrix is TiNi. The interface between the two phases is clear, the compression strength measured by the uniaxial static compression test can reach 2023MPa, the elongation after fracture can reach 20%, and the strength and the elongation are both higher. The uniaxial static compressive strength of the laminated composite material is 1774Mpa, and the elongation after break is 15%. Compared with the laminated composite material, the pearl layer-like composite material prepared by variable-temperature rollingThe compressive strength of the material is improved by 14%, the elongation after fracture is improved by 33%, and the strength and the plasticity of the material are improved. And (3) comparing the microstructure graphs of the simulated nacreous layer composite material subjected to variable-temperature rolling and single-temperature rolling (namely comparing the graphs of fig. 1 and 3), wherein the side surface of the microstructure of the simulated nacreous layer composite material prepared by variable-temperature rolling is more bricked than that of the simulated nacreous layer composite material prepared by single-temperature rolling, and the structural non-uniformity is reduced.
Example 2
TiNi/Ti 2 Ni imitation pearl layer composite material, which is made of Ti 2 Ni and TiNi are alternately mixed in the form of "brick mud" in which the plane Ti parallel to the rolling direction 2 The Ni brick width was about 30 μm, the brick thickness was about 18 μm, and the average brick spacing was about 31 μm. In a plane perpendicular to the rolling direction Ti 2 The Ni brick width was about 34 μm, the brick thickness was about 17 μm, and the average brick spacing was about 24 μm.
TiNi/Ti 2 The preparation method of the Ni-imitation pearl layer composite material comprises the following steps,
step one: tiNi/Ti with the length of 200mm, the width of 80mm and the thickness of 20mm 2 Putting the Ni laminated composite material into a stainless steel sheath, welding the sheath to enable the sheath to be airtight, wherein the thickness of the sheath is 4mm;
step two: tiNi/Ti coated by the sheath 2 Placing the Ni laminated composite material in a heat treatment furnace which is heated to 350 ℃ for heat preservation;
step three: tiNi/Ti coated by a heated sheath 2 The Ni laminated composite material is put into a rolling mill for multi-pass rolling, the rolling reduction of each pass is 0.3mm, heat preservation tempering is carried out at 350 ℃ between each pass, and the rolling is stopped after the rolling reduction is 15% of the thickness of the material;
step four: placing the composite material rolled to 15% in a heat treatment furnace heated to 800 ℃ for heat preservation;
step five: the TiNi/Ti after heat preservation 2 The Ni composite material is put into a rolling mill for multi-pass rolling, the rolling reduction of each pass is 4 percent of the residual thickness of the material, the heat preservation tempering is carried out at 800 ℃ between each pass, and the rolling is stopped after the total rolling reduction is 70 percent of the thickness of the material;
step six, cutting and dismantling the metal sheath to take out the composite material, and taking out TiNi/Ti 2 Placing the Ni composite material into a graphite mold;
step seven, tiNi/Ti is filled 2 Placing a graphite mold of the Ni composite material in a vacuum hot-pressing furnace, vacuumizing the vacuum hot-pressing furnace, wherein the vacuum degree is 4 multiplied by 10 -3 Pa, then raising the temperature of the hearth to 800 ℃, preserving heat for 1h, applying 10MPa pressure, preserving heat and pressure for 4h, unloading pressure, cooling to room temperature along with the furnace, and taking out to obtain a sample.
Characterization of experimental results: the simulated nacreous layer composite material was found to have similar "brick mud" alternate mix structural characteristics as the nacreous layer, as seen in the perspective view of the BSEM splice shown in FIG. 4 (the direction of the arrow in FIG. 4 is the rolling direction). In combination with EDS spectrum, dark "brick" is the reinforcing phase Ti 2 The light-colored mud matrix is TiNi. The interface between the two phases is clear, and the strength and the elongation are high.
Example 3
TiNi/Ti 2 Ni imitation pearl layer composite material, which is made of Ti 2 Ni and TiNi are alternately mixed in the form of "brick mud" in which the plane Ti parallel to the rolling direction 2 The Ni brick width was about 28 μm, the brick thickness was about 21 μm, and the average brick spacing was about 25 μm. In a plane perpendicular to the rolling direction Ti 2 The Ni brick width was about 37 μm, the brick thickness was about 20 μm, and the average brick spacing was about 29 μm.
TiNi/Ti 2 The preparation method of the Ni-imitation pearl layer composite material comprises the following steps,
step one: tiNi/Ti with the length of 300mm, the width of 100mm and the thickness of 10mm 2 Putting the Ni laminated composite material into a stainless steel sheath, welding the sheath to enable the sheath to be airtight, wherein the thickness of the sheath is 2mm;
step two: tiNi/Ti coated by the sheath 2 Placing the Ni laminated composite material in a heat treatment furnace which is heated to 200 ℃ for heat preservation;
step three: tiNi/Ti coated by a heated sheath 2 The Ni laminated composite material is put into a rolling mill for multi-pass rolling, and the rolling reduction of each pass isHeat preservation tempering is carried out at 200 ℃ between each pass of 0.1mm, and rolling is stopped after the rolling reduction is 8% of the thickness of the material;
step four: placing the composite material rolled to 8% in a heat treatment furnace heated to 600 ℃ for heat preservation;
step five: the TiNi/Ti after heat preservation 2 The Ni composite material is put into a rolling mill for multi-pass rolling, the rolling reduction of each pass is 2 percent of the residual thickness of the material, heat preservation tempering is carried out at 500 ℃ between each pass, and the rolling is stopped after the total rolling reduction is 50 percent of the thickness of the material;
step six, cutting and dismantling the metal sheath to take out the composite material, and taking out TiNi/Ti 2 Placing the Ni composite material into a graphite mold;
step seven, tiNi/Ti is filled 2 Placing a graphite mold of the Ni composite material in a vacuum hot-pressing furnace, vacuumizing the vacuum hot-pressing furnace, wherein the vacuum degree is 4 multiplied by 10 -3 Pa, then raising the temperature of the hearth to 950 ℃, preserving heat for 1h, applying 20MPa pressure, preserving heat and pressure for 7h, unloading pressure, cooling to room temperature along with the furnace, and taking out to obtain a sample.
Characterization of experimental results: the simulated nacreous layer composite material was found to have similar "brick mud" alternate mix structural characteristics as the nacreous layer, as seen in the perspective view of the BSEM splice shown in FIG. 5 (FIG. 5: arrow direction is rolling direction). In combination with EDS spectrum, dark "brick" is the reinforcing phase Ti 2 The light-colored mud matrix is TiNi. The interface between the two phases is clear, and the strength and the elongation are high.
Example 4
TiNi/Ni 3 Ti imitation pearl layer composite material, the composite material is made of Ni 3 Ti and TiNi are alternately mixed in the form of "brick mud" in which Ni in a plane parallel to the rolling direction 3 The Ti brick width was about 49 μm, the brick thickness was about 9 μm, and the average brick spacing was about 31 μm. In a plane Ni perpendicular to the rolling direction 3 The Ti blocks were about 25 μm wide, the thickness of the blocks was about 7 μm, and the average spacing of the blocks was about 25 μm.
TiNi/Ni 3 The preparation method of the Ti imitation pearl layer composite material comprises the following steps,
step one: tiNi/Ni with the length of 50mm, the width of 40mm and the thickness of 15mm 3 Putting the Ti laminated composite material into a stainless steel sheath, welding the sheath to enable the sheath to be airtight, wherein the thickness of the sheath is 3mm;
step two: tiNi/Ni coated by sheath 3 Placing the Ti laminated composite material in a heat treatment furnace which is heated to 300 ℃ for heat preservation;
step three: tiNi/Ni coated by a heated sheath 3 The Ti laminated composite material is put into a rolling mill for multi-pass rolling, the rolling reduction of each pass is 0.2mm, the heat preservation tempering is carried out at 300 ℃ between each pass, and the rolling is stopped after the rolling reduction is 10% of the thickness of the material;
step four: placing the composite material rolled to 10% in a heat treatment furnace heated to 900 ℃ for heat preservation;
step five: the TiNi/Ni after heat preservation 3 The Ti composite material is put into a rolling mill for multi-pass rolling, the rolling reduction of each pass is 7 percent of the residual thickness of the material, heat preservation tempering is carried out at 900 ℃ between each pass, and the rolling is stopped after the total rolling reduction is 62 percent of the thickness of the material;
step six, cutting and dismantling the metal sheath to take out TiNi/Ni 3 Ti composite material to obtain a sample;
characterization of experimental results: the simulated nacreous layer composite material was found to have similar "brick mud" alternate mix structural characteristics as the nacreous layer, as seen in the perspective view of the BSEM splice shown in FIG. 6 (FIG. 6: arrow direction is rolling direction). Light-colored "brick" in the picture is reinforcing phase Ni 3 Ti, the dark color mud matrix is TiNi, and the interface between the two phases is clear.
Example 5
Ti/Al 3 Ti imitation pearl layer composite material, which is made of Al 3 Ti and Ti are alternately mixed in the form of "brick mud" in which Al is present in a plane parallel to the rolling direction 3 The Ti brick width was about 372 μm, the brick thickness was about 65 μm, and the average brick spacing was about 340 μm. In a plane perpendicular to the rolling direction Al 3 The Ti brick width was about 401 μm, the brick thickness was about 68 μm, and the average brick spacing was about 378 μm.
The method comprises the following steps ofTi/Al 3 The preparation method of the Ti imitation pearl layer composite material comprises the following steps:
step one: ti/Al with a length of 50mm, a width of 40mm and a thickness of 17mm 3 Putting the Ti laminated composite material into a stainless steel sheath, welding the sheath to enable the sheath to be airtight, wherein the thickness of the sheath is 5mm;
step two: coating the Ti/Al of the sheath 3 Placing the Ti laminated composite material in a heat treatment furnace which is heated to 200 ℃ for heat preservation;
step three: coating the heated jacket with Ti/Al 3 The Ti laminated composite material is put into a rolling mill for multi-pass rolling, the rolling reduction of each pass is 0.4mm, heat preservation tempering is carried out at 200 ℃ between each pass, and the rolling is stopped after the rolling reduction is 15% of the thickness of the material;
step four: placing the composite material rolled to 15% in a heat treatment furnace heated to 950 ℃ for heat preservation;
step five: heat-insulating Ti/Al 3 The Ti composite material is put into a rolling mill for multi-pass rolling, the rolling reduction of each pass is 10 percent of the residual thickness of the material, heat preservation tempering is carried out at 950 ℃ between each pass, and the rolling is stopped after the total rolling reduction is 70 percent of the thickness of the material;
step six, cutting and dismantling the metal sheath to take out Ti/Al 3 Ti composite material, obtain the imitation pearl layer brick composite material;
example 6
A Ti/TiC pearl-like layer composite material is prepared from Al 3 Ti and Ti were alternately mixed in the form of "brick mud" in which TiC bricks had a width of about 194 μm, a thickness of about 81 μm and a spacing average of about 70 μm in a plane parallel to the rolling direction. The width of the TiC blocks in the plane perpendicular to the rolling direction was about 207 μm, the thickness of the blocks was about 90 μm, and the average spacing of the blocks was about 87 μm.
A preparation method of a Ti/TiC pearl-like layer composite material comprises the following steps:
step one: putting the Ti/TiC laminated composite material with the length of 50mm, the width of 40mm and the thickness of 12mm into a stainless steel sheath, welding the sheath to enable the sheath to be airtight, wherein the thickness of the sheath is 4mm;
step two: placing the Ti/TiC laminated composite material coated by the sheath in a heat treatment furnace which is heated to 200 ℃ for heat preservation;
step three: the Ti/TiC laminated composite material coated by the heated sheath is put into a rolling mill for multi-pass rolling, the rolling reduction of each pass is 0.4mm, heat preservation tempering is carried out at 200 ℃ between each pass, and the rolling is stopped after the rolling reduction is 5% of the thickness of the material;
step four: placing the composite material rolled to 5% in a heat treatment furnace heated to 700 ℃ for heat preservation;
step five: placing the heat-preserving Ti/TiC composite material into a rolling mill for multi-pass rolling, wherein the rolling reduction of each pass is 10% of the residual thickness of the material, heat-preserving tempering is carried out at 700 ℃ between each pass, and rolling is stopped after the total rolling reduction is 60% of the thickness of the material;
cutting and dismantling the metal sheath, and taking out the Ti/TiC composite material to obtain the pearl layer-like composite material;
characterization of experimental results: the simulated nacreous layer composite material was found to have similar "brick mud" alternate mix structural characteristics as the nacreous layer, as seen in the perspective view of the BSEM splice shown in FIG. 7 (FIG. 7: arrow direction is rolling direction). In the picture, dark brick is reinforcing phase TiC, light mud is Ti, and the interface between the two phases is clear.
The foregoing description of the preferred embodiment of the invention has been presented. It should be noted that the present invention is not limited to the above embodiments, and any modifications, equivalent substitutions, improvements, and the like, which are possible to meet the requirements of the scope of the claims, the summary of the invention, the drawings, and the like, are intended to be included in the scope of the present invention.
Claims (9)
1. The preparation method of the pearl layer-imitated bricking composite material is characterized by comprising the following steps:
step one, placing the laminated composite material in a heat treatment furnace which is heated to a selected temperature for heat preservation;
step two, placing the heated laminated composite material into a rolling mill for multi-pass rolling, carrying out heat preservation tempering between each pass, and stopping rolling until a certain rolling reduction is achieved;
step three, placing the composite material rolled to a certain rolling reduction in a heat treatment furnace which is heated to a higher temperature for heat preservation;
and fourthly, putting the heated composite material into a rolling mill again for multi-pass rolling, carrying out heat preservation tempering between each pass, and stopping rolling until the rolling reduction is selected.
2. The method for preparing the pearl layer-imitated bricking composite material according to claim 1, wherein the method further comprises, before the first step, placing the laminated composite material in a metal sheath, welding the metal sheath to seal the metal sheath, wherein the thickness of the sheath is 2-10mm; the metal sheath is selected based on the hardness of the laminate composite.
3. The method for producing a nacreous layer-like bricking composite material according to claim 1, wherein the heat-insulating temperature in the step one is 50 ℃ to 500 ℃.
4. The method for preparing the imitation pearl layer bricking composite material according to claim 1, wherein the total rolling reduction in the second step is 5% -20% of the thickness of the material, the tempering time of each pass is 2-20min, the sample thickness is increased by 1mm, the heat preservation time is prolonged by 1min, and the tempering temperature is the same as the heat preservation temperature in the first step.
5. The method for producing a pearl layer-like bricked composite material according to claim 1, wherein the heat-insulating temperature in the step three is 400 ℃ to 1000 ℃.
6. The method for preparing the imitation pearl layer bricking composite material according to claim 1, wherein the total rolling reduction in the fourth step is 10% -90% of the thickness of the material, the tempering time of each pass is 2-20min, the sample thickness is increased by 1mm, the heat preservation time is prolonged by 1min, and the tempering temperature is the same as the heat preservation temperature in the third step.
7. The method for preparing the imitation pearl layer bricking composite material according to claim 1, which is characterized by further comprising the steps of placing a graphite mold filled with the composite material in a hot pressing furnace, vacuumizing the hot pressing furnace, then heating a hearth to a selected temperature, preserving heat for 0.1-6 h, applying a selected pressure, preserving heat and pressure for 1-8h, unloading the pressure, cooling to room temperature along with the furnace, and taking out to obtain the imitation pearl layer bricking composite material.
8. The method for preparing a composite material for simulating nacreous layer bricking according to claim 7, wherein the heating rate of the heating in the fifth step is 10 ℃/min, and the vacuum degree of the vacuuming is less than 5 x 10 -3 Pa, the heat preservation temperature is selected according to the raw materials, and the pressure maintaining pressure is 5-20MPa.
9. A nacreous layer-like bricked composite material, characterized in that it is obtainable by a process according to any one of claims 1 to 8.
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