CN101928899A - Nanocrystalline reinforcement method of Ti-15-3 alloy plate - Google Patents
Nanocrystalline reinforcement method of Ti-15-3 alloy plate Download PDFInfo
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- CN101928899A CN101928899A CN 201010179120 CN201010179120A CN101928899A CN 101928899 A CN101928899 A CN 101928899A CN 201010179120 CN201010179120 CN 201010179120 CN 201010179120 A CN201010179120 A CN 201010179120A CN 101928899 A CN101928899 A CN 101928899A
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Abstract
The invention discloses a nanocrystalline reinforcement method of a Ti-15-3 alloy plate, relating to a nanocrystalline reinforcement method of a titanium alloy plate and solving the problems that when the Ti-15-3 alloy plate with a nanometer structure is processed with the prior process, the crystallites prepared with an equal channel extrusion method have large dimension, and large size plates cannot be processed with a high-pressure torsion method. The method comprises the following steps of: 1, making a Ti-15-3 alloy plate in a solid-solution state subjected to cold rolling without carrying out intermediate annealing, and 2, placing the Ti-15-3 into a vacuum thermal treatment furnace, for ageing, and air cooling to complete the nanocrystalline reinforcement treatment of the Ti-15-3 alloy plate. The method greatly improves the strength and the hardness of the Ti-15-3 alloy plate which has the matrix beta-phase crystallite dimension of smaller than 100nm and the precipitated phase of about 30nm and can be used at 450 DEG C. The cold rolling is adopted for manufacturing large size plates and large size bulky nanometer alloy materials meeting industrial application requirements.
Description
Technical field
The present invention relates to the nanocrystalline enhancement method of a kind of titanium alloy plate.
Background technology
Nanostructured metal since have very little grain-size (20～500nm) and unique defect structure (as high-angle boundary), thus show the physicals and the mechanical property of a series of excellences.Traditional pressure processing technology (as rolling, extruding, drawing etc.) can crystal grain thinning, yet wants to adopt traditional plastic processing method to prepare nanostructured metal, just must obtain very big viscous deformation.Because large plastometric set has the great potential that the grain refining of coarse grained metal is arrived nanoscale, and acutely the plastic deformation method compares with other preparation methods (for example vapor phase process, ball milled etc.), has the advantage of many uniquenesses, is widely used.For example: it can avoid existing in the sample of other method preparation problem such as hole, compactness difference and purity that ball milling caused low, be difficult to the practical application of production large size base substrate and block nanometer material than problems such as difficulties.But adopt violent viscous deformation to prepare nanostructured metal and must consider following factors: at first, the nanostructure that acquisition has high-angle boundary is the prerequisite that guaranteed performance is improved; Next, the nanostructure that sample has homogeneous on the whole is that the stable institute of guaranteed performance is requisite; The 3rd, behind the large plastometric set, sample should not have breakage or cracking; The particularly important is, to obtain big plastix strain under relatively low temperature and high pressure, true strain need surpass 6～8 in principle.
At present commonly used among the violent plastic deformation method of the preparation block nanometer material of report passage extrusion process and high pressure torsion method such as have.Advantage Deng the passage extrusion process is to prepare the bar-shaped sample of large size, there is its diameter of report can reach 60mm, but the shortcoming of this method is to prepare the grain-size of material usually greater than 200nm, belongs to submicron material, has limited the further raising of material property.The shortcoming of high pressure torsion method is to prepare undersized film sample (thickness is at 0.2-0.5mm, and diameter is at the roundel of 10-20mm), only for the related basic research that carries out nano metal material in laboratory scale.
In addition, these two kinds of methods are very high to the cold deformation Capability Requirement of metal, for example, can't at room temperature wait passage crimp for temperature-room type plasticity up to 30% pure titanium, and common distortion initial temperature need be up to 450 ℃.
Summary of the invention
Purpose of the present invention is big for the grain-size of passage extrusion processs such as the Ti-15-3 sheet alloy existence preparation that solves existing processes nanostructure, the problem that the high pressure torsion method can't machining large-sized sheet material.
The nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step among the present invention: one, cold rolling with the no process annealing that the draft of 10%/passage ~ 40%/passage carries out 3 ~ 11 passages to the Ti-15-3 sheet alloy of solid solution attitude, wherein the Ti-15-3 sheet alloy is the Ti-15V-3Sn-3Al-3Cr sheet alloy; Two, will put into vacuum heat treatment furnace through the Ti-15-3 sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
The inventive method is separated out nano level α phase on the nanocrystalline matrix of single-phase β, formation biphase tissue, stronger interaction takes place in this biphase tissue and dislocation, hinder its motion effectively, thereby the intensity of Ti-15-3 sheet alloy and hardness are increased substantially, yield strength reaches more than the 1450MPa, and tensile strength reaches more than the 1540MPa; Matrix β phase grain-size is less than 100nm, and the precipitated phase size is about 30nm.Adopt cold rollingly can prepare large size plate, satisfy the blocks of large Nanoalloy material of requirement on industrial application.Can be through the Ti-15-3 sheet alloy that the inventive method is handled 450 ℃ of uses.
Description of drawings
Fig. 1 is the photomacrograph of cold rolling back of 1 passage Ti-15-3 sheet alloy in the embodiment 11; Fig. 2 is the photomacrograph of cold rolling back of 2 passages Ti-15-3 sheet alloy in the embodiment 11; Fig. 3 is the photomacrograph of cold rolling back of 3 passages Ti-15-3 sheet alloy in the embodiment 11; Fig. 4 is the vertical section metallographic microstructure photo of cold rolling back of 1 passage Ti-15-3 sheet alloy in the embodiment 11; Fig. 5 is the vertical section metallographic microstructure photo of cold rolling back of 2 passages Ti-15-3 sheet alloy in the embodiment 11; Fig. 6 is the vertical section metallographic microstructure photo of cold rolling back of 3 passages Ti-15-3 sheet alloy in the embodiment 11; Fig. 7 be in the embodiment 11 the cold rolling time back of 1 passage Ti-15-3 sheet alloy transmission electron microscope tissue (dark field image) photo; Fig. 8 be in the embodiment 11 the cold rolling time back of 2 passages Ti-15-3 sheet alloy transmission electron microscope tissue (dark field image) photo; Fig. 9 is transmission electron microscope tissue (dark field image) photo of cold rolling back of 3 passages Ti-15-3 sheet alloy in the embodiment 11; Figure 10 be in the embodiment 11 behind the ageing treatment 4h transmission electron microscope of Ti-15-3 sheet alloy organize photo (bright field image); Figure 11 is the diffraction pattern of Figure 10 correspondence; Figure 12 is the details in a play not acted out on stage, but told through dialogues image pattern of encircled spot correspondence among Figure 11; Figure 13 is the transmission electron microscope organization chart (bright field image) of Ti-15-3 sheet alloy behind the ageing treatment 20h in the embodiment 11; Figure 14 is the transmission electron microscope organization chart (diffraction pattern) of Ti-15-3 sheet alloy behind the ageing treatment 20h in the embodiment 11; Figure 15 is the XRD spectrum under each treated state, and a represents the solid solution attitude among the figure, and b represents 1 passage, and c represents 2 passages, and d represents 3 passages, e represents cold rolling+aging state.
Embodiment
Embodiment one: the nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step in the present embodiment: one, cold rolling with the no process annealing that the draft of 10%/passage ~ 40%/passage carries out 3 ~ 11 passages to the Ti-15-3 sheet alloy of solid solution attitude, wherein the Ti-15-3 sheet alloy is the Ti-15V-3Sn-3Al-3Cr sheet alloy; Two, will put into vacuum heat treatment furnace through the Ti-15-3 sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
Present embodiment obtains sheet alloy matrix β phase grain-size less than 100nm, and the precipitated phase size is about 30nm, and its yield strength reaches more than the 1450MPa, and tensile strength reaches more than the 1550MPa.
Embodiment two: what present embodiment and embodiment one were different is: the thickness of the described Ti-15V-3Sn-3Al-3Cr sheet alloy of step 1 is 3mm.Other step is identical with embodiment one with parameter.
Embodiment three: what present embodiment was different with embodiment one or two is: step 1 adopts the unidirectional cold rolling mode of not having the cold rolling of process annealing or commutation and do not have process annealing to carry out cold rolling.Other step is identical with embodiment one or two with parameter.
Embodiment four: what present embodiment was different with one of concrete mode one to three is: the draft by 20%/passage in the step 1 does not have the cold rolling of process annealing.Other step is identical with one of embodiment one to three with parameter.
Embodiment five: what present embodiment was different with one of embodiment one to three is: the draft by 30%/passage in the step 1 does not have the cold rolling of process annealing.Other step is identical with one of embodiment one to three with parameter.
Embodiment six: what present embodiment was different with one of embodiment one to five is: the cold rolling pass that does not have process annealing in the step 1 is 5 passages.Other step is identical with one of embodiment one to five with parameter.
Embodiment seven: what present embodiment was different with one of embodiment one to five is: the cold rolling pass that does not have process annealing in the step 1 is 8 passages.Other step is identical with one of embodiment one to five with parameter.
Embodiment eight: the nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step in the present embodiment: one, adopt Ф 200 * 400mm type two-roll cold rolling mill to the Ti-15V-3Sn-3Al-3Cr sheet alloy of solid solution attitude with 30%/passage (be each draught be rolling before thickness 30%) draft carry out 5 passages and do not have process annealing unidirectional cold rolling (thickness of sheet material is about 0.5mm); Two, will put into vacuum heat treatment furnace through the Ti-15V-3Sn-3Al-3Cr sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
Present embodiment obtains sheet alloy matrix β phase grain-size less than 100nm, and the precipitated phase size is about 30nm, and its yield strength is 1485 MPa, and tensile strength is 1540MPa.
Embodiment nine: the nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step in the present embodiment: the cold-rolling mill that, adopts Ф 200 * 400mm type two rollers not have process annealing carries out the no process annealing unidirectional cold rolling (thickness of sheet material is about 0.5mm) of 8 passages with the draft of 20%/passage to the Ti-15V-3Sn-3Al-3Cr sheet alloy of solid solution attitude; Two, will put into vacuum heat treatment furnace through the Ti-15V-3Sn-3Al-3Cr sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
Present embodiment obtains sheet alloy matrix β phase grain-size less than 100nm, and the precipitated phase size is about 30nm, and its yield strength is 1483MPa, and tensile strength is 1564 MPa.
Embodiment ten: the nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step in the present embodiment: one, adopt Ф 200 * 400mm type two-roll cold rolling mill the Ti-15V-3Sn-3Al-3Cr sheet alloy of solid solution attitude to be carried out the no process annealing unidirectional cold rolling (thickness of sheet material is about 0.5mm) of 11 passages with the draft of 10%/passage; Two, will put into vacuum heat treatment furnace through the Ti-15V-3Sn-3Al-3Cr sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
Present embodiment obtains sheet alloy matrix β phase grain-size less than 100nm, and the precipitated phase size is about 30nm, and its yield strength is 1490 MPa, and tensile strength is 1568MPa.
Embodiment 11: the nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step in the present embodiment: one, adopt Ф 200 * 400mm type two-roll cold rolling mill the Ti-15V-3Sn-3Al-3Cr sheet alloy of solid solution attitude to be carried out the no process annealing unidirectional cold rolling (thickness of sheet material is about 0.5mm) of 3 passages with the draft of 40%/passage; Two, will put into vacuum heat treatment furnace through the Ti-15V-3Sn-3Al-3Cr sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
Be to be about the cold rolling attitude of 0.5mm and photomacrograph, microtexture and the X-ray diffraction spectral line of aging state Ti-15-3 sheet alloy below with the thickness that the present embodiment method obtains.
The mechanical property of solid solution attitude, rolling attitude and cold rolling+aging state alloy is as shown in table 1.The yield strength and the tensile strength of solid solution attitude sheet material are respectively 723MPa and 753MPa, through 40%/passage-3 passage cold rolling after, the yield strength of Nanoalloy sheet material and tensile strength are brought up to 1025MPa and 1086MPa respectively, and increase rate is respectively 42% and 44%.Cold rolling attitude alloy is behind 450 ℃ of timeliness 4h, and yield strength and tensile strength can improve 45% and 44% again than cold rolling attitude up to 1483MPa and 1562MPa respectively, and Vickers' hardness is 532.8, has improved 41% than cold rolling attitude.In the Ti-15-3 alloy sheets through 3 passages cold roller and deformed 80%, formed fibrous tissue (see figure 6) in a big way, its inside has formed the nanometer-size die (see figure 9) about 30nm.Research thinks that the forming process of nano-structure is divided into three phases, at first, and owing to plastic instability forms partial cut band (see figure 4); Next, the shear zone that elongation banded structure inside is arranged in parallel intersects and fragmentation gradually mutually; Three phases forms fibrous tissue in a big way, its inside fully fragmentation be the nanocrystal (see figure 6).Along with the increase of cold rolling pass, the diffraction spot of nano-area is gradually by the circular-arc polycrystalline ring (seeing Fig. 7-9) that becomes continuous whole.Cold rolling alloy is separated out nano level α phase on the nanocrystalline matrix of single-phase β (grain-size is about 100nm) after 450 ℃ of insulation 4h timeliness, form biphase tissue (seeing Figure 10-12).Stronger interaction takes place in biphase tissue and dislocation, hinder its motion effectively, thereby the intensity of making and hardness increases substantially.With solid solution attitude alloy phase ratio, the intensity of biphase alloy has improved about 107%.In existing report, for the Ti-15-3 alloy, tensile strength does not all reach the 1562MPa in this patent.Cold rolling attitude alloy nanocrystalline grain size behind 450 ℃ of timeliness 20h still remains on about 100nm (sees Figure 13-14), illustrate the cold rolling attitude alloy with nano-structure can be behind 450 ℃ of timeliness 4h nano-structure basicly stable, prolongation along with aging time, grain-size remains at about 100nm (sees Figure 10-14), therefore cold rolling attitude alloy can be 450 ℃ of uses, thereby help practical application.
In the alloy cold-rolled process and the XRD figure spectrum after the timeliness see Figure 15.The β phase diffraction peak shape of solid solution aspect product is narrow and high.Through behind the various roll process, its peak shape all has obvious broadening, and microstrain and grain refining have caused the broadening of diffraction peak shape jointly.Confirmed the existence of nanocrystal to a certain extent.The XRD of alloy spectrum as can be seen after the timeliness, the diffraction peak shape broadening phenomenon of β phase still exists in the matrix, microstrain also not elimination after this heat-treated has been described on the one hand, on the other hand, illustrate that nanocrystal is imitated at this moment and unstability do not taken place after the art breading and grow up.In addition, separated out the α phase on matrix, each diffraction peak shape of α phase is broad also, has illustrated that also the size of α precipitated phase is less.
The mechanical property table of table 1 Ti-15-3 alloy different treatment state
| Treated state | Yield strength (MPa) | Tensile strength (MPa) | Unit elongation (%) | Vickers' hardness (HV) |
| The solid solution attitude | 723 | 753 | 33.0 | 356.5 |
| The cold rolling attitude of not having process annealing | 1025 | 1086 | 5.5 | 378.1 |
| Cold rolling+the aging state that does not have process annealing | 1483 | 1562 | 2.0 | 532.8 |
Embodiment 12: the nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step in the present embodiment: one, adopt Ф 200 * 400mm type two-roll cold rolling mill the Ti-15V-3Sn-3Al-3Cr sheet alloy of solid solution attitude to be carried out the no process annealing intersection commutation cold rolling (thickness of sheet material is about 0.5mm) of 3 passages with the draft of 40%/passage; Two, will put into vacuum heat treatment furnace through the Ti-15V-3Sn-3Al-3Cr sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
Present embodiment obtains sheet alloy matrix β phase grain-size less than 100nm, and the precipitated phase size is about 30nm, and its yield strength is 1580 MPa, and tensile strength is 1655 MPa.
Embodiment 13: the nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step in the present embodiment: one, adopt Ф 200 * 400mm type two-roll cold rolling mill the Ti-15V-3Sn-3Al-3Cr sheet alloy of solid solution attitude to be carried out the no process annealing intersection commutation cold rolling (thickness of sheet material is about 0.5mm) of 5 passages with the draft of 30%/passage; Two, will put into vacuum heat treatment furnace through the Ti-15V-3Sn-3Al-3Cr sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
Present embodiment obtains sheet alloy matrix β phase grain-size less than 100nm, and the precipitated phase size is about 30nm, and its yield strength is 1584MPa, and tensile strength is 1646MPa.
Embodiment 14: the nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step in the present embodiment: one, adopt Ф 200 * 400mm type two-roll cold rolling mill the Ti-15V-3Sn-3Al-3Cr sheet alloy of solid solution attitude to be carried out the no process annealing intersection commutation cold rolling (thickness of sheet material is about 0.5mm) of 8 passages with the draft of 20%/passage; Two, will put into vacuum heat treatment furnace through the Ti-15V-3Sn-3Al-3Cr sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
Present embodiment obtains sheet alloy matrix β phase grain-size less than 100nm, and the precipitated phase size is about 30nm, and its yield strength is 1586 MPa, and tensile strength is 1658 MPa.
Embodiment 15: the nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step in the present embodiment: one, adopt Ф 200 * 400mm type two-roll cold rolling mill the Ti-15V-3Sn-3Al-3Cr sheet alloy of solid solution attitude to be carried out the no process annealing intersection commutation cold rolling (thickness of sheet material is about 0.5mm) of 11 passages with the draft of 10%/passage; Two, will put into vacuum heat treatment furnace through the Ti-15V-3Sn-3Al-3Cr sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
Present embodiment obtains sheet alloy matrix β phase grain-size less than 100nm, and the precipitated phase size is about 30nm, and its yield strength is 1582 MPa, and tensile strength is 1652 MPa.
Claims (7)
1.Ti-15-3 the nanocrystalline enhancement method of sheet alloy, it is characterized in that the nanocrystalline enhancement method of Ti-15-3 sheet alloy is undertaken by following step: one, cold rolling with the no process annealing that the draft of 10%/passage ~ 40%/passage carries out 3 ~ 11 passages to the Ti-15-3 sheet alloy of solid solution attitude, wherein the Ti-15-3 sheet alloy is the Ti-15V-3Sn-3Al-3Cr sheet alloy; Two, will put into vacuum heat treatment furnace through the Ti-15-3 sheet alloy after the step 1 cold-rolling treatment, under 450 ℃ of conditions, be incubated the ageing treatment of 4h, the air cooling cooling; Promptly finish the nanocrystalline intensive treatment of Ti-15-3 sheet alloy.
2. the nanocrystalline enhancement method of Ti-15-3 sheet alloy according to claim 1, the thickness that it is characterized in that the described Ti-15-3 sheet alloy of step 1 is 3mm.
3. the nanocrystalline enhancement method of Ti-15-3 sheet alloy according to claim 1 and 2 is characterized in that step 1 adopts the unidirectional cold rolling mode of not having the cold rolling of process annealing or commutation and do not have process annealing to carry out cold rolling.
4. the nanocrystalline enhancement method of Ti-15-3 sheet alloy according to claim 3 is characterized in that the draft by 20%/passage does not have the cold rolling of process annealing in the step 1.
5. the nanocrystalline enhancement method of Ti-15-3 sheet alloy according to claim 3 is characterized in that the draft by 30%/passage does not have the cold rolling of process annealing in the step 1.
6. according to claim 1,2, the nanocrystalline enhancement method of 4 or 5 described Ti-15-3 sheet alloys, the cold rolling pass that it is characterized in that not having in the step 1 process annealing is 5 passages.
7. according to claim 1,2, the nanocrystalline enhancement method of 4 or 5 described Ti-15-3 sheet alloys, the cold rolling pass that it is characterized in that not having in the step 1 process annealing is 8 passages.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105951018A (en) * | 2016-06-13 | 2016-09-21 | 山东建筑大学 | Method for preparing nano-Ti-alloy material by adopting three-angle equal channel angular pressing |
| CN110055481A (en) * | 2019-06-04 | 2019-07-26 | 武汉轻工大学 | A kind of preparation method of nanometer crystalline Ni Ti latten |
-
2010
- 2010-05-21 CN CN 201010179120 patent/CN101928899A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《机械工程材料》 20100430 郭强等 Ti-15-3合金经冷轧和时效后的显微组织及力学性能 14-17 1-7 第34卷, 第04期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105951018A (en) * | 2016-06-13 | 2016-09-21 | 山东建筑大学 | Method for preparing nano-Ti-alloy material by adopting three-angle equal channel angular pressing |
| CN110055481A (en) * | 2019-06-04 | 2019-07-26 | 武汉轻工大学 | A kind of preparation method of nanometer crystalline Ni Ti latten |
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Open date: 20101229 |