CN103820744A - Preparation method of ultrafine-grain titanium matrix composite material by using mushy-zone titanium alloy as matrix - Google Patents
Preparation method of ultrafine-grain titanium matrix composite material by using mushy-zone titanium alloy as matrix Download PDFInfo
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Abstract
The invention relates to a preparation method of an ultrafine-grain titanium matrix composite material by using a mushy-zone titanium alloy as a matrix. The preparation method comprises the following steps: carrying out hot working of a titanium matrix composite material; cutting to form a blank material, and polishing; simultaneously preheating a sample and a die, and uniformly smearing the surface of the sample and the inner wall of the die with a graphite lubricant; respectively carrying out heating and heat insulation of the die and the sample; putting the sample in a die channel to make the sample completely go through the channel corner of the equal-diameter corner extrusion die, and cooling the sample with water to complete a primary extruding technology; and machining the sample, carrying out 90DEG anticlockwise rotation, beveling the head, and carrying out 2-4 time equal-diameter bending channel extrusion deformation to obtain the ultrafine-grain titanium matrix composite material. The preparation method realizes the strength and plasticity deformation of the titanium matrix composite material, effectively refines the internal crystal grain size, has the advantages of short process flow, easy operation, high efficiency, low cost and strong adaptability, and can be used in the titanium matrix composite material processing field.
Description
Technical field
The invention belongs to the Technology of Plastic Processing field of material, be specifically related to a kind of preparation method of the ultra-fine grain titanium matrix composite take two-phase region titanium alloy as matrix.
Background technology
Titanium or titanium alloy, because of good mechanical property and physicals, has been 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 since the forties in last century just the industrialization of titanium sponge and the production in enormous quantities of titanium alloy material, the trial production that China also starts titanium sponge in 1958, has formed complete titanium industrial system now.But in the time that titanium alloy material develops into the ceiling that approaches certain performance, simple rely on the raising that changes solid solution element and be difficult to have matter in performance, now find by two kinds of approach can be acquired can better titanium alloy.A kind of approach is to prepare Ultra-fine Grained 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, thereby show much uncommon physics, chemistry and mechanical property, improve the intensity of titanium alloy by this refined crystalline strengthening mode.(application number is 200810017288.8 to Chinese patent application, publication number is CN101219444A, open day is on July 16th, 2008) the pure titanium bulk of a kind of high strength industrial room temperature equal-diameter bending passage deformation preparation method disclosed, this invention has at room temperature been carried out ECAP distortion to industrially pure titanium, room temperature strength and the comprehensive mechanical property thereof of industrially pure titanium are improved, grain-size has refine to 0.25～0.3 μ m by 28 original μ m, room temperature yield strength has been brought up to 680MPa by 390MPa, and unit elongation has dropped to 16.8% by 36.4%.(application number is 200910023545.3 to Chinese patent application, publication number is CN101624690A, open day on January 13rd, 2010) a kind of difficult-to-deformation metal block material room temperature equal-diameter bending passage deformation production method disclosed, this invention has at room temperature been carried out ECAP distortion to industrially pure titanium, and initial grain size is 23 μ m, yield strength 407MPa, unit elongation 33%, grain-size≤0.4 μ m after ECAP processes 2 passages, yield strength 738MPa, unit elongation 17%; μ m in grain-size≤0.25 after 8 passages, yield strength 801MPa, unit elongation 30%.
Another kind of approach is in alloy, to add reinforcement to prepare titanium matrix composite to obtaining higher performance.The research of titanium matrix composite starts from the seventies in last century, to titanium matrix composite, development provides good opportunity and huge fund to guarantee in the enforcement of u.s. space shuttle (NASP) and overall HPTE Technologies (IHPTET) and Europe, Japanese similar evolutionary operation(EVOP), thereby has promoted the development of titanium matrix composite to make it the focus into above-mentioned age material science.Titanium matrix composite has not only kept the advantageous property of titanium but also have 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 these two kinds of approach are combined, the titanium matrix composite of Ultra-fine Grained is prepared in research and exploration, and the General Promotion of the performance to titanium matrix composite is had to vital role.At home and abroad there is no at present the relevant report about the Study on Structure Property of ultra-fine grain titanium matrix composite.
Forced plasticity deforming technique (Severe Plastic Deformation is called for short SPD) is a kind of technology that realizes the nanometer of material grains under the large stress condition of low temperature.It is the most promising method of preparing block nanometer and super fine crystal material that this technology is known as by international material educational circles.At present, the method that realizes SPD mainly contains two kinds: large stress rotational method (High Pressure Torsion, HPT), the folded hypodesmus of accumulation (being called for short ARB) and equal channel angular extrusion method (Equal Channel Angular Pressing, 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 of developing.Compared with additive method, the advantage of equal channel angular pressing platen press is that distortion front and back do not change the shape of 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 that obtain large size submicron or nano level block materials.Therefore, it is a tera incognita that is worth researcher research and explores that ECAP forced plasticity deforming is applied to the titanium matrix composite field that polynary many sizes reinforcement mixes strengthening, and the Microstructural evolution in forced plasticity deforming process has good theoretical investigation and is worth to titanium matrix especially to disclose polynary many sizes reinforcement.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the ultra-fine grain titanium matrix composite take two-phase region titanium alloy as matrix, the method is that under hot conditions, to adopt interior angle Φ be that 90 °～135 ° moulds carry out equal-diameter bending passage deformation to titanium matrix composite, thereby obtains the titanium matrix composite of Ultra-fine Grained.Repeatedly extrusion technique of Equal-channel Angular Pressing technology that method provided by the invention is integrated and accumulation, 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 preparation method of the ultra-fine grain titanium matrix composite take two-phase region titanium alloy as 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%;
The titanium matrix composite after hot-work is cut into rectangular body blank by step (2), 120 ° of head chamferings, and effects on surface and seamed edge carry out grinding process, surface working roughness Ra≤3.2 μ m;
Step (3) sample and mould are preheated to 150～200 ℃ simultaneously, evenly smear oildag at specimen surface and mould inner wall, and thickness is 0.05～0.1mm;
A process furnace is warming up to 500～550 ℃ by step (4), puts into mould insulation 65～70 minutes, and No. two process furnace are warming up to after extrusion temperature, and sample is put into and is wherein incubated 15～20 minutes;
Die channel put into by sample by step (5), put into depression bar, apply squeeze, make sample completely by the channel corner place of equal channel angular extrusion mould, then sample is carried out to water-cooled immediately, sample produces strong shearing strain and compression set in this process, and so far, sample completes the first passage extrusion process;
By completing, sample after the first passage crimp digs step (6), milling mechanical workout, remove surface scale, surface working roughness Ra≤3.2 μ m, sample is rotated counterclockwise 90 °, 120 ° of head chamferings, 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: it is 1200 ℃ that temperature is forged in cogging, 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, sample enters direction in die channel and goes up a time and be rotated counterclockwise 90 °.
Compared with prior art, the present invention has following beneficial effect:
1, the present invention has carried out the strong plasticity crimp of isometrical corner to titanium matrix composite, and material is size constancy before and after extruding, can realize the processing of relatively large material, its smooth surface after extruding, zero defect, has realized the grain refining of titanium matrix composite, and its intensity is improved greatly.
2, mould device of the present invention can carry out strong shearing strain and not cause material production limit split and rupture material at a lower temperature, effectively avoid the containment of grain growth to forced plasticity deforming crystal grain thinning ability under excessive temperature, thus more effective crystal grain thinning.
3, mould device of the present invention is simple in structure, reasonable in design, low cost of manufacture, and the adaptability of mould device that the design departing from press improves, technical process of the present invention is short, and efficiency is high, simple to operate.
4, the present invention, using titanium matrix composite as point of penetration, takes the lead in metal-base composites to carry out the strong plasticity crimp of isometrical corner, for the thin brilliant metal-base composites of preparation nanometer has been made guide and Beneficial.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art further to understand the present invention, but not limit in any form the present invention.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
embodiment 1
The present embodiment relates to a kind of preparation method of the ultra-fine grain titanium matrix composite take two-phase region titanium alloy as 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 is after vacuum consumable smelting, and 1200 ℃ are swaged into Φ 76mm bar on higher than transformation temperature; Original structure coarse grains, grain-size is 20 μ m; Titanium matrix composite line cuts into 10 × 10 × 140mm sample, 120 ° of head chamferings, surface working roughness Ra≤3.2 μ m; Die channel angle is 120 °; Above-mentioned extruded sample is preheated to 200 ℃ together with mould, and at specimen surface, die channel inwall is evenly smeared oildag, and thickness is 0.05～0.1mm; Mould is installed according to assembling position, and by bolted; Then, mould is put in the process furnace that temperature reaches 500～550 ℃ and is incubated 65 minutes, sample is put into No. two process furnace that are heated to extrusion temperature, be incubated 15 minutes, then sample is put into die channel, put into depression bar, mould is put to the position of design in advance on hydraulic machine together with put into sample, applied squeeze on depression bar, extruding rate is 8mm/s, sample completely by mould corner, completes the first passage extrusion process under the effect of squeeze; By completing, sample after the first passage crimp digs along its length, milling processing, remove surface scale, be rotated counterclockwise 120 ° of 90 ° of chamferings, surface working roughness Ra≤3.2 μ m, and make its sectional dimension meet sectional dimension 300～500 μ m that are less than 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 extruding, the 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, completes after the distortion of ECAP4 passage, obtains ganoid ultra-fine grain titanium matrix composite, grain-size has refine to 600nm by 20 original μ m, and yield strength has been brought up to 1235MPa by initial 980MPa.
embodiment 2
The present embodiment relates to a kind of preparation method of the ultra-fine grain titanium matrix composite take two-phase region titanium alloy as matrix, comprises following concrete steps: selecting titanium matrix composite is (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, completes after the distortion of ECAP4 passage, obtains ganoid ultra-fine grain titanium matrix composite, and grain-size has refine to 500nm by 22 original μ m, and yield strength has been brought up to 1250MPa by initial 990MPa.
embodiment 3
The present embodiment relates to a kind of preparation method of the ultra-fine grain titanium matrix composite take two-phase region titanium alloy as matrix, comprise following concrete steps: selecting titanium matrix composite is (TiB+TiC)/TC11 matrix, TiB (Vol2.5%), TiC (Vol2.5%); Die channel angle is 120 °; The other the same as in Example 1, completes after the distortion of ECAP4 passage, obtains ganoid ultra-fine grain titanium matrix composite, and grain-size has refine to 550nm by 17 original μ m, and yield strength has been brought up to 1240MPa by initial 970.
Above specific embodiments of the invention are described.It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and those skilled in the art can make various distortion or modification within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (6)
1. a preparation method for the ultra-fine grain titanium matrix composite take two-phase region titanium alloy as matrix, 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%;
The titanium matrix composite after hot-work is cut into rectangular body blank by step (2), 120 ° of head chamferings, and effects on surface and seamed edge carry out grinding process, surface working roughness Ra≤3.2 μ m;
Step (3) sample and mould are preheated to 150～200 ℃ simultaneously, evenly smear oildag at specimen surface and mould inner wall, and thickness is 0.05～0.1mm;
A process furnace is warming up to 500～550 ℃ by step (4), puts into mould insulation 65～70 minutes, and No. two process furnace are warming up to after extrusion temperature, and sample is put into and is wherein incubated 15～20 minutes;
Die channel put into by sample by step (5), put into depression bar, apply squeeze, make sample completely by the channel corner place of equal channel angular extrusion mould, then sample is carried out to water-cooled immediately, sample produces strong shearing strain and compression set in this process, and so far, sample completes the first passage extrusion process;
By completing, sample after the first passage crimp digs step (6), milling mechanical workout, remove surface scale, surface working roughness Ra≤3.2 μ m, sample is rotated counterclockwise 90 °, 120 ° of head chamferings, repeating step (3)～(5), after 2～4 equal-diameter bending passage crimp, obtain ganoid ultra-fine grain titanium matrix composite.
2. preparation method as claimed in claim 1, is characterized in that, in step (1), described hot-work comprises following detailed process: it is 1200 ℃ that temperature is forged in cogging, is swaged into Φ 76mm bar.
3. preparation method as claimed in claim 1, is characterized in that, in step (2), the titanium matrix composite after hot-work is cut into the rectangular parallelepiped blank of 10 × 10 × 140mm.
4. preparation method as claimed in claim 1, is characterized in that, in step (3), mould interior angle Φ is 90 °～135 °, and exterior angle ψ is 0 °～45 °.
5. preparation method as claimed in claim 1, is characterized in that, in step (4), described extrusion temperature is less than or equal to the recrystallization temperature of titanium matrix composite.
6. 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, sample enters direction in die channel and goes up a time and be rotated counterclockwise 90 °.
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| CN105154800A (en) * | 2015-08-25 | 2015-12-16 | 山东建筑大学 | Method for preparing titanium alloy nano materials through warm extrusion of herringbone channel mold |
| CN106011514A (en) * | 2016-06-21 | 2016-10-12 | 山东建筑大学 | Ultra-high-strength Ti-based composite material preparation method by repeated equal-channel 45-degree equal-channel angular pressing |
| 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 |
| CN111783234A (en) * | 2019-03-18 | 2020-10-16 | 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 |
| CN116689531A (en) * | 2023-08-09 | 2023-09-05 | 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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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105154800A (en) * | 2015-08-25 | 2015-12-16 | 山东建筑大学 | Method for preparing titanium alloy nano materials through warm extrusion of herringbone channel mold |
| CN106011514A (en) * | 2016-06-21 | 2016-10-12 | 山东建筑大学 | Ultra-high-strength Ti-based composite material preparation method by repeated equal-channel 45-degree equal-channel angular pressing |
| 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 |
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| 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 |
| CN116689531A (en) * | 2023-08-09 | 2023-09-05 | 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 |
| 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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