CN103820744B - The preparation method of the ultra-fine grain titanium matrix composite being matrix with two-phase region titanium alloy - Google Patents
The preparation method of the ultra-fine grain titanium matrix composite being matrix with two-phase region titanium alloy Download PDFInfo
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Abstract
The present invention relates to a kind of with the preparation method of the two-phase region titanium alloy ultra-fine grain titanium matrix composite that is matrix, comprise the steps: titanium matrix composite to carry out hot-work; Then cut into blank and carry out grinding process; By sample and mould preheating simultaneously, at specimen surface and mould inner wall uniform application oildag; Mould and sample are carried out heating and thermal insulation respectively; Then sample is put into die channel, make sample completely by the channel corner place of equal channel angular extrusion mould, then immediately water-cooled is carried out to sample, complete the first passage extrusion process; Be rotated counterclockwise 90 ° after again sample being carried out mechanical workout, head chamfering, after 2 ~ 4 equal-diameter bending passage crimp, obtain ultra-fine grain titanium matrix composite.Present invention achieves the forced plasticity deforming of titanium matrix composite, its internal grain size of effective refinement, this technical process is short, simple to operate; Efficiency is high, and cost is low; Strong adaptability, can be used for the manufacture field of titanium matrix composite.
Description
Technical field
The invention belongs to the Technology of Plastic Processing field of material, be specifically related to a kind of with the preparation method of the two-phase region titanium alloy ultra-fine grain titanium matrix composite that is matrix.
Background technology
Titanium or titanium alloy, because of excellent mechanical property and physicals, is widely used in Aeronautics and Astronautics, each economic fields such as the energy, electric power, oil, chemical industry, biology, medicine.The U.S., Russia, Japan and European Countries just start the industrialization of titanium sponge and the production in enormous quantities of titanium alloy material from the forties in last century, and China also started the trial production of titanium sponge in 1958, defined now complete Ti industry system.But when titanium alloy material develops into the ceiling close to certain performance, simple dependence changes solid solution element and has been difficult to the raising having matter in performance, now find by two kinds of approach can acquired can better titanium alloy.A kind of approach prepares ultra-fine grain titanium alloy by forced plasticity deforming, a large amount of inner boundaries and Non-equilibrium Grain Boundary structure are contained in ultrafine-grained (UFG) microstructure, thus show much uncommon physics, chemistry and mechanical property, improved the intensity of titanium alloy by this refined crystalline strengthening mode.(application number is 200810017288.8 to Chinese patent application, publication number is CN101219444A, publication date is on July 16th, 2008) disclose a kind of high strength industrial pure titanium bulk room temperature equal-diameter bending passage deformation preparation method, this invention has at room temperature carried out ECAP distortion to industrially pure titanium, improve room temperature strength and the comprehensive mechanical property thereof of industrially pure titanium, grain-size has refine to 0.25 ~ 0.3 μm by original 28 μm, room-temperature yield strength has brought up to 680MPa by 390MPa, and unit elongation have decreased to 16.8% by 36.4%.(application number is 200910023545.3 to Chinese patent application, publication number is CN101624690A, publication date on January 13rd, 2010) disclose a kind of difficult-to-deformation metal block material room temperature equal-diameter bending passage deformation production method, this invention has at room temperature carried out ECAP distortion to industrially pure titanium, and initial grain size is 23 μm, yield strength 407MPa, unit elongation 33%, grain-size≤0.4 μm after 2 passages is processed, yield strength 738MPa, unit elongation 17% through ECAP; Grain-size≤0.25 μm after 8 passages, yield strength 801MPa, unit elongation 30%.
Another kind of approach in alloy, adds reinforcement prepare titanium matrix composite to obtaining higher performance.The research of titanium matrix composite starts from the seventies in last century, the enforcement of u.s. space shuttle (NASP) and overall HPTE Technologies (IHPTET) and Europe, Japanese similar evolutionary operation(EVOP) provides good opportunity to titanium matrix composite development and huge fund ensures, thus the development facilitating titanium matrix composite has made it the focus into above-mentioned age material science.Titanium matrix composite not only maintains the advantageous property of titanium but also has the specific tenacity higher than titanium and specific modulus.Above two kinds of approach all make the performance of titanium alloy obtain raising in various degree, if combined by these two kinds of approach, research and explore the titanium matrix composite preparing Ultra-fine Grained, has vital role by the General Promotion of the performance to titanium matrix composite.At home and abroad there is no the relevant report of the Study on Structure Property about ultra-fine grain titanium matrix composite at present.
Forced plasticity deforming technique (SeverePlasticDeformation is called for short SPD) is a kind of technology realizing the nanometer of material grains under the large stress condition of low temperature.It is the most promising method preparing block nanometer and super fine crystal material that this technology is known as by international material educational circles.At present, the method realizing SPD mainly contains two kinds: large stress rotational method (HighPressureTorsion, HPT), the folded hypodesmus of accumulation (being called for short ARB) and equal channel angular extrusion method (EqualChannelAngularPressing, ECAP).Wherein equal channel angular pressing platen press be the eighties in 20th century the former Russian scholar Segal obtain pure shear to be out of shape the method for a kind of large plastometric set developed.Compared with additive method, the advantage of equal channel angular pressing platen press is to be out of shape the shape that front and back do not change material, and preparation is simple, and cost is low, and grain refining effect is obvious, the block grained material that applicable preparation is larger.Equal-diameter bending passage deformation (ECAP) technology is one of effective ways obtaining large size submicron or nano level block materials.Therefore, ECAP forced plasticity deforming is applied to the tera incognita that titanium matrix composite field that polynary many sizes reinforcement mixes strengthening is the research of worth researcher and explores, especially discloses polynary many sizes reinforcement and to the Microstructural evolution of titanium matrix in forced plasticity deforming process, there is good theoretical investigation and be worth.
Summary of the invention
The object of the present invention is to provide a kind of with the preparation method of the two-phase region titanium alloy ultra-fine grain titanium matrix composite that is matrix, the method adopts interior angle Φ to be that 90 ° ~ 135 ° moulds carry out equal-diameter bending passage deformation to titanium matrix composite under the high temperature conditions, thus obtain the titanium matrix composite of Ultra-fine Grained.Method integration provided by the invention Equal-channel Angular Pressing technology and accumulation repeatedly extrusion technique, not only simple to operation, and also cost is low.
Object of the present invention is achieved through the following technical solutions, and the present invention relates to a kind of with the preparation method of the two-phase region titanium alloy ultra-fine grain titanium matrix composite that is matrix, comprises the following steps:
Titanium matrix composite is carried out hot-work by step (1), described titanium matrix composite is made up of matrix alloy and reinforcement, described matrix alloy is alpha+beta two-phase region titanium alloy, described reinforcement is fibrous by TiC, rare earth oxide particles and TiB, and described TiC, rare earth oxide particles and the volume percent content of TiB fiber in titanium matrix composite are respectively 0 ~ 3%, 0 ~ 3% and 0 ~ 10%;
Titanium matrix composite after hot-work is cut into rectangular parallelepiped blank by step (2), head chamfering 120 °, and effects on surface and seamed edge carry out grinding process, surface working roughness Ra≤3.2 μm;
Step (3) sample and mould are preheated to 150 ~ 200 DEG C simultaneously, and at specimen surface and mould inner wall uniform application oildag, thickness is 0.05 ~ 0.1mm;
A process furnace is warming up to 500 ~ 550 DEG C by step (4), puts into mould insulation 65 ~ 70 minutes, after No. two process furnace are warming up to extrusion temperature, are put into by sample and be wherein incubated 15 ~ 20 minutes;
Sample is put into die channel by step (5), put into depression bar, apply squeeze, make sample completely by the channel corner place of equal channel angular extrusion mould, then immediately water-cooled is carried out to sample, sample produces Strong shear distortion and compression set in the process, and so far, sample completes the first passage extrusion process;
Sample after completing the first passage crimp carries out digging by step (6), milling mechanical workout, remove surface scale, surface working roughness Ra≤3.2 μm, sample is rotated counterclockwise 90 °, head chamfering 120 °, repeating step (3) ~ (5), after 2 ~ 4 equal-diameter bending passage crimp, obtain ganoid ultra-fine grain titanium matrix composite.
Preferably, in step (1), described hot-work comprises following detailed process: cogging forging temperature is 1200 DEG C, is swaged into Φ 76mm bar.
Preferably, in step (2), the titanium matrix composite after hot-work is cut into the rectangular parallelepiped blank of 10 × 10 × 140mm.
Preferably, in step (3), mould interior angle Φ is 90 ° ~ 135 °, and exterior angle ψ is 0 ° ~ 45 °.
Preferably, in step (4), described extrusion temperature is less than or equal to the recrystallization temperature of titanium matrix composite.
Preferably, in step (6), extruding path adopts Bc route, and after described 2 ~ 4 equal-diameter bending passage crimps, the sample direction entered in die channel is comparatively gone up a time and is rotated counterclockwise 90 °.
Compared with prior art, the present invention has following beneficial effect:
1, the present invention has carried out the strong plastic extrusion distortion of isometrical corner to titanium matrix composite, and material is rear size constancy before extrusion, can realize the processing of relatively large material, its smooth surface after extruding, zero defect, achieves the grain refining of titanium matrix composite, and its intensity is improved greatly.
2, mould device of the present invention can carry out Strong shear distortion to material at a lower temperature and not cause material generation limit split and rupture, under efficiently avoid excessive temperature, grain growth is to the containment of forced plasticity deforming crystal grain thinning ability, thus more effective crystal grain thinning.
3, mould device structure of the present invention is simple, and reasonable in design, low cost of manufacture, the adaptability of the mould device that the design departed from press improves, present invention process flow process is short, and efficiency is high, simple to operate.
4, the present invention is using titanium matrix composite as point of penetration, takes the lead in having carried out the strong plastic extrusion distortion of isometrical corner, for the thin brilliant metal-base composites of preparation nanometer has made guide and Beneficial to metal-base composites.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
The present embodiment relates to a kind of with the preparation method of the two-phase region titanium alloy ultra-fine grain titanium matrix composite that is matrix, comprise following concrete steps: that the matrix alloy of titanium matrix composite is selected is TC4, TiC (vol0%), rare earth oxide particles (vol1.16%), TiB (vol3.64%) fiber hybrid reinforced composite; Material after vacuum consumable smelting, higher than on transformation temperature 1200 DEG C be swaged into Φ 76mm bar; Original structure coarse grains, grain-size is 20 μm; Titanium matrix composite Linear cut becomes 10 × 10 × 140mm sample, head chamfering 120 °, surface working roughness Ra≤3.2 μm; Die channel angle is 120 °; Above-mentioned extruded sample is preheated to 200 DEG C together with mould, at specimen surface, die channel inwall uniform application oildag, thickness is 0.05 ~ 0.1mm; Mould is installed according to assembling position, and by bolted; Then, mould is put into temperature reach in a process furnace of 500 ~ 550 DEG C be incubated 65 minutes, sample is put into No. two process furnace being heated to extrusion temperature, be incubated 15 minutes, then sample is put into die channel, put into depression bar, mould is put the position designed in advance to hydraulic machine together with put into sample, depression bar applies squeeze, extruding rate is 8mm/s, sample completely by mould corner, completes the first passage extrusion process under the effect of squeeze; Sample after completing the first passage crimp is carried out along its length dig, Milling Machining, remove surface scale, be rotated counterclockwise 90 ° of chamferings 120 °, surface working roughness Ra≤3.2 μm, and its sectional dimension is met be less than the sectional dimension 300 ~ 500 μm of passage in counterdie, sample can be slided and be positioned in passage; Repeat the first passage preparation work, sample and the first passage are rotated counterclockwise 90 ° and put into die channel, then extrude, 3rd passage is counterclockwise half-twist on the basis of the second passage, four-pass is another mistake hour hands half-twist on the basis of the 3rd passage, after the distortion completing ECAP4 passage, obtains ganoid ultra-fine grain titanium matrix composite, grain-size has refine to 600nm by original 20 μm, and yield strength has brought up to 1235MPa by initial 980MPa.
embodiment 2
The present embodiment relates to a kind of with the preparation method of the two-phase region titanium alloy ultra-fine grain titanium matrix composite that is matrix, comprises following concrete steps: select titanium matrix composite to be (TiB+TiC+La
2o
3)/TC18, TiB (Vol8.16%), TiC (Vol1.26%), La
2o
3(Vol0.58%), die channel angle is 90 °; The other the same as in Example 1, after the distortion completing ECAP4 passage, obtains ganoid ultra-fine grain titanium matrix composite, and grain-size has refine to 500nm by original 22 μm, and yield strength has brought up to 1250MPa by initial 990MPa.
embodiment 3
The present embodiment relates to a kind of with the preparation method of the two-phase region titanium alloy ultra-fine grain titanium matrix composite that is matrix, comprise following concrete steps: select titanium matrix composite to be (TiB+TiC)/TC11 matrix, TiB (Vol2.5%), TiC (Vol2.5%); Die channel angle is 120 °; The other the same as in Example 1, after the distortion completing ECAP4 passage, obtains ganoid ultra-fine grain titanium matrix composite, and grain-size has refine to 550nm by original 17 μm, and yield strength has brought up to 1240MPa by initial 970.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (4)
1., with a preparation method for the two-phase region titanium alloy ultra-fine grain titanium matrix composite that is matrix, it is characterized in that: comprise the steps:
Titanium matrix composite is carried out hot-work by step (1), described titanium matrix composite is made up of matrix alloy and reinforcement, described matrix alloy is alpha+beta two-phase region titanium alloy, described reinforcement is fibrous by TiC, rare earth oxide particles and TiB, and described TiC, rare earth oxide particles and the volume percent content of TiB fiber in titanium matrix composite are respectively 0 ~ 3%, 0 ~ 3% and 0 ~ 10%;
Titanium matrix composite after hot-work is cut into rectangular parallelepiped blank by step (2), head chamfering 120 °, and effects on surface and seamed edge carry out grinding process, surface working roughness Ra≤3.2 μm;
Step (3) sample and mould are preheated to 150 ~ 200 DEG C simultaneously, and at specimen surface and mould inner wall uniform application oildag, thickness is 0.05 ~ 0.1mm;
A process furnace is warming up to 500 ~ 550 DEG C by step (4), puts into mould insulation 65 ~ 70 minutes, after No. two process furnace are warming up to extrusion temperature, are put into by sample and be wherein incubated 15 ~ 20 minutes;
Sample is put into die channel by step (5), put into depression bar, apply squeeze, make sample completely by the channel corner place of equal channel angular extrusion mould, then immediately water-cooled is carried out to sample, sample produces Strong shear distortion and compression set in the process, and so far, sample completes the first passage extrusion process;
Sample after completing the first passage crimp carries out digging by step (6), milling mechanical workout, remove surface scale, surface working roughness Ra≤3.2 μm, sample is rotated counterclockwise 90 °, head chamfering 120 °, repeating step (3) ~ (5), after 2 ~ 4 equal-diameter bending passage crimp, obtain ganoid ultra-fine grain titanium matrix composite;
In step (2), the titanium matrix composite after hot-work is cut into the rectangular parallelepiped blank of 10 × 10 × 140mm;
In step (3), mould interior angle Φ is 90 ° ~ 135 °, and exterior angle Ψ is 0 ° ~ 45 °.
2. preparation method as claimed in claim 1, it is characterized in that, in step (1), described hot-work comprises following detailed process: cogging forging temperature is 1200 DEG C, is swaged into Φ 76mm bar.
3. preparation method as claimed in claim 1, it is characterized in that, in step (4), described extrusion temperature is less than or equal to the recrystallization temperature of titanium matrix composite.
4. preparation method as claimed in claim 1, it is characterized in that, in step (6), extruding path adopts Bc route, after described 2 ~ 4 equal-diameter bending passage crimps, the sample direction entered in die channel is comparatively gone up a time and is rotated counterclockwise 90 °.
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| CN105154800B (en) * | 2015-08-25 | 2017-01-25 | 山东建筑大学 | Method for preparing titanium alloy nano materials through warm extrusion of herringbone channel mold |
| CN106011514B (en) * | 2016-06-21 | 2017-12-12 | 山东建筑大学 | The method that the isochannel repeated extruding in 45 ° of turnings prepares superhigh intensity titanium matrix composite |
| CN108004430A (en) * | 2017-11-29 | 2018-05-08 | 成都创客之家科技有限公司 | A kind of titanium alloy metallic fiber for preparing filter core |
| CN111783234B (en) * | 2019-03-18 | 2022-03-22 | 西北工业大学 | Method and system for establishing extrusion process window of as-cast titanium alloy |
| CN112275817A (en) * | 2020-09-18 | 2021-01-29 | 中国航发北京航空材料研究院 | Equal-channel angular extrusion cogging method for high-temperature alloy cast ingot |
| CN115094354A (en) * | 2022-06-22 | 2022-09-23 | 南昌航空大学 | Preparation method of metal matrix composite material and stirring friction corner extrusion device |
| CN116689531B (en) * | 2023-08-09 | 2023-10-27 | 成都先进金属材料产业技术研究院股份有限公司 | Preparation method of high-strength TC4 pipe |
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| CN1528940A (en) * | 2003-09-26 | 2004-09-15 | 上海交通大学 | Micron fine-grained titanium-nickel alloy block material isodiametric corner extrusion preparing method |
| CN101219444A (en) * | 2008-01-14 | 2008-07-16 | 西安建筑科技大学 | Isometric bending channel deformation production method for high-strength commercial titanium block at room temperature |
| CN103572186A (en) * | 2013-10-14 | 2014-02-12 | 上海交通大学 | Method for preparing ultra-fine grain titanium-based composite material by adopting equant bending channel deformation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1528940A (en) * | 2003-09-26 | 2004-09-15 | 上海交通大学 | Micron fine-grained titanium-nickel alloy block material isodiametric corner extrusion preparing method |
| CN101219444A (en) * | 2008-01-14 | 2008-07-16 | 西安建筑科技大学 | Isometric bending channel deformation production method for high-strength commercial titanium block at room temperature |
| CN103572186A (en) * | 2013-10-14 | 2014-02-12 | 上海交通大学 | Method for preparing ultra-fine grain titanium-based composite material by adopting equant bending channel deformation |
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