CN105618501A - Remanufacturing method for scrap titanium chips through ball milling-equal channel angularpressing - Google Patents

Remanufacturing method for scrap titanium chips through ball milling-equal channel angularpressing Download PDF

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Publication number
CN105618501A
CN105618501A CN201510992894.1A CN201510992894A CN105618501A CN 105618501 A CN105618501 A CN 105618501A CN 201510992894 A CN201510992894 A CN 201510992894A CN 105618501 A CN105618501 A CN 105618501A
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titanium
chip
equal channel
channel angular
ball
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CN201510992894.1A
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CN105618501B (en
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罗蓬
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上海电机学院
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00Extruding metal; Impact extrusion
    • B21C23/02Making uncoated products
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/10Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/08Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/10Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity, by vibration
    • B08B3/12Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity, by vibration by sonic or ultrasonic vibrations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00Extruding metal; Impact extrusion
    • B21C23/001Extruding metal; Impact extrusion to improve the material properties, e.g. lateral extrusion
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00Extruding metal; Impact extrusion
    • B21C23/32Lubrication of metal being extruded or of dies, or the like, e.g. physical state of lubricant, location where lubricant is applied
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing 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
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon

Abstract

The invention provides a remanufacturing method for scrap titanium chips through ball milling-equal channel angular pressing. The remanufacturing method sequentially comprises the step of recovering and pretreating titanium chips, the step of performing ball milling treatment on the titanium chips, the step of loading the titanium chips into an equal channel angular pressing mold, the step of performing preprocessing at a room temperature through the equal channel angular pressing, the step of curing and processing at a high temperature, and the step of quenching. The ball milling-equal channel angular pressing composite technique provided by the invention is simple and practical to operate and high in controllability. Through remanufacturing, not only can nanometer block titanium materials (smaller than 200nanometers) with full densification be obtained, but also the metallurgical defect of the continuous distribution and gathering of large sliced oxides can be eliminated. In addition, the shapes of the titanium chips are refined and reformed, and anisotropy caused by deformation texture in hexagonal close packed titanium materials is restrained. The yield strength of the remanufactured nanometer titanium materials reaches to the level of 5-grade titanium, the distribution of nanometer particles of the oxides presents a dispersed uniform state, and through the isotropy of the properties of the materials, the remanufacturing of scrap titanium resources for value increase at low cost is realized.

Description

The ball milling of discarded titanium chip-equal channel angular extruding reproducing method

Technical field

The present invention relates to the solid cycle of discarded titanium chip and re-manufacturing technology, in particular to the method adopting the recovering and processing discarded titanium chip of ball milling-equal channel angular extrusion process.

Background technology

The circulation of discarded metals resources is one of key factor realizing Sustainable development with manufacturing again. Titanium (Ti) is extremely important, but the metals resources that smelting cost is higher, its biocompatibility is excellent, solidity to corrosion is good, mechanical property is suitable, is the important materials manufacturing medicine equipment, joint prosthesis, large-scale derived energy chemical container etc. But, in order to manufacture high precision titanium structure, bigger process redundancy need to be designed. The starting material of significant proportion will be converted into discarded chip. Traditional chip process technology is high temperature founding, and energy consumption is big, pollution is heavy, and efficiency is low, and cast structure's crystal grain is thick, poor-performing. At present, the research and development of solid cycle and re-manufacturing technology, because avoiding high temperature founding, are the effective ways realizing resource high-efficiency, clean cycle.

By severe plastic deformation, metallic substance is applied high level strain, with remarkable crystal grain thinning, thus develop high-strength material, at present existing series report. it is noted that as a kind of typical severe plastic deformation technology, equal channel angular extruding (Equalchannelangularpressing is called for short ECAP) has been applied to preparing blocks of large ultrafine grain metal material. by means of ECAP, can the discrete raw material such as curing powder so that it is be changed into the block materials of full densification. Xia and Wu delivers in " BackpressureequalchannelangularconsolidationofpureAlpart icles (the back pressure equal channel angular solidification of pure Al particle) " literary composition for 2005 at " ScriptaMaterialia " on 53 volume 11 phase 1225-1229 pages, propose from pure aluminium (Al) micron particle raw material, carry out curing powder by ECAP mould, prepare the block materials of full densification. simultaneously, Wu and Xia rolls up at " JournalofMaterialsProcessingTechnology " 192-193 in 2007 and delivers " Backpressureequalchannelangularconsolidation-Application inproducingaluminiummatrixcompositeswithfineflyashpartic les (application that back pressure equal channel angular is solidificated in the aluminium base fine powdered coal particulate composite of preparation) " literary composition on 355-359 page, taking Al powder and superfined flyash particle as starting material, prepare the Al based composites containing flyash two-phase by ECAP technology.

Except above-mentioned using powder body as raw material and prepare block body ultrafine grain metal material by ECAP, the circulation that application ECAP technology also can realize discarded borings with manufacture again. Luo etc. deliver " AmodifiedHall-Petchrelationshipinultrafine-grainedtitani umrecycledfromchipsbyequalchannelangularpressing (by chip by the correction Hall-Petch relation in the ultra-fine brilliant titanium of equal channel angular extrusion cycle) " literary composition for 2012 at " ScriptaMaterialia " on 66 volume 785-788 pages, report, by reclaiming discarded 2 grade Ti (ASTMGrade2) chip, manufactures block materials again by ECAP technology. Thereafter related work comprises: Lapovok etc. deliver " Multicomponentmaterialsfrommachiningchipscompactedbyequa l-channelangularpressing (extrudes chip formation by equal channel angular and prepares multi-component material) " literary composition for 2014 at " JournalofMaterialsScience " on 49 volume 1193-1204 pages, report the mutual mixing by Al chip and Mg chip, prepare multi-component alloys material by ECAP.

Meanwhile, ball milling (Ballmilling is called for short BM) is another technology for the preparation of superfine powdery material. MahboubiSoufiani etc. deliver " FormationmechanismandcharacterizationofnanostructuredTi6 Al4Valloypreparedbymechanicalalloying Forming Mechanism and the sign of Ti6Al4V alloy nano structure (mechanical alloying prepare) " literary composition for 2012 at " MaterialsandDesign " on 37 volume 152-160 pages, report taking micron (��m) powder of Ti, Al, V as raw material, synthesized superfine Ti-6Al-4V powdered alloy by BM technology. In addition, Zadra delivers " Mechanicalalloyingoftitanium (mechanical alloying of titanium) " for 2013 at " MaterialsScienceandEngineeringA " on 583 volume 105-113 pages civilian, the Ti powder that initial feed employing median size is less than 150 ��m, first by BM process, obtain the pure ti powder being less than 25 ��m, and at 900 DEG C, obtain block materials by discharge plasma sintering.

ECAP technology is used for the Ti chip (3-10mm) that solidification treatment milli is meter-sized, it is possible to the crystal grain of refinement circulation Ti material, thus improves mechanical property. But, ECAP processes in Ti material containing the oxide compound (TiO being derived from original chip surface2), it is strong but pliable in texture, can partly rupture although processing rear oxidation thing through multi-pass ECAP, but, the continuity distribution of bigger (mm level) sheet oxide compound in microtexture and gathering are serious metallurgical imperfections. Meanwhile, there is the refinement limit in ECAP, and namely when dynamic recrystallization reaches balance with strain thinning effect, then ECAP will be difficult to make microtexture to be refined to nano level (< 200nm). In addition, (solid matter six side) Ti material of ECAP process is easy to form deformation texture, and namely because of the material anisotropy that preferable grain orientation causes, this will weaken (desired) Ti wood property energy isotropy.

Although adopting BM technology can prepare superfine powdery material, but after BM process, the operations such as sintering must be carried out to obtain blocks of large material. And in follow-up sintering operation, due to the impact of the factors such as long-time (diffusion) heating and recrystallize, super fine organization very easily occurs grain coarsening, it is difficult to ensure in final block materials, still obtain (maintenance) ultrafine-grained (UFG) microstructure, thus cause loss of strength.

Summary of the invention

It is an object of the invention to provide the ball milling of a kind of discarded titanium chip-equal channel angular extruding reproducing method, to overcome the above-mentioned defect that prior art exists.

The ball milling of the discarded titanium chip of the present invention-equal channel angular extruding reproducing method, in turn includes the following steps: the BM procedure of processing of Ti chip recycling pre-treatment step, Ti chip, be packed into ECAP molding process, ECAP room temperature preliminary step, ECAP hot setting procedure of processing and quenching step.

Step (1)-Ti chip recycling pre-treatment: adopt ethanol to be cleaned by Ti chip starting material, with the greasy dirt that removes in starting material and impurity. Ti chip starting material can adopt the chip that generates of 2 grades of Ti (ASTMGrade2) obtained by end mill processing, cleans the method preferably adopting ultrasonic cleaning, such as, clean in ultrasonic activation groove, ethanol used preferably 99.9% ethanol.

The BM process of step (2)-Ti chip: pretreated Ti chip is inserted in the BM container including steel ball, simultaneously adition process control agent, ball milling 10-20 hour under the protection of inert gas atmosphere, rotating speed 280-350rpm.

Preferably, between described Ti chip and steel ball, mass ratio is 12-20:1, and the diameter of described steel ball is 7-12mm, described process control agent can be selected from stearic acid, straight iron powder etc., preferred stearic acid, the add-on (mass percent, wt%) of described process control agent is between 0.5-2wt%. Rare gas element can be nitrogen, argon gas, helium etc., it is preferable that argon gas. Inert atmosphere is kept to be to prevent chip over oxidation in BM process. In addition, passing to liquid nitrogen circulation preferably by external container, to reduce the friction temperature of chip-steel ball, and machine often runs for some time (such as 1-2 hour) and suspends several minutes (such as 10-15 minute).

Step (3)-through BM process Ti chip be packed into ECAP mould:

Cylindrical steel billet is wrapped up with steel foil, described steel billet diameter is slightly less than die channel diameter, one layer of solid lubrication oxidant layer is wrapped up in again outside steel foil, steel billet-steel foil-solid lubrication oxidant layer is inserted die channel, take out steel billet, form solid lubrication oxidant layer-steel foil cavity, the Ti chip processed through BM is filled in above-mentioned cavity.

Preferably, the stainless steel foil of described steel foil preferably annealed process, described solid lubricant can select graphite paper, masking foil etc., it is preferable that graphite paper. After the Ti chip processed through BM is filled in described solid lubricant-steel foil cavity, preferably again with hand press by preliminary for chip compacting.

Step (4)-ECAP room temperature preprocessing:

Being installed on a hydraulic press by the mould having loaded Ti chip, back pressure drift provides the constant backpressure of 150��200MPa, and continues to improve the pressure of feeding drift, when the pressure that feeding drift provides reaches 680��720MPa, stops ECAP process. This step can further improve the degree of packing of chip pressed compact, effectively prevents Ti chip over oxidation in ECAP hot setting is processed that BM processes.

Step (5)-ECAP hot setting is processed:

Heating mould is to 570-590 DEG C, and under the effect of hydraulicdirectional control valve, two drifts that passage imported and exported by control mould alternately provide solidifying pressure 1.0��1.2GPa and back pressure 150-200MPa, carry out 4-8 passage continuously.

Step (6)-quenching:

The block Ti material die sinking in hot state that will obtain in ECAP hot setting procedure of processing, adopts water-cooling pattern quench cooled to room temperature, obtains and manufactures nanometer Ti material again.

The present invention is as a kind of novelty, based on solid cycle and the reproducing method of severe plastic deformation theory, avoid high temperature founding, it it is a kind of low cost, and the metals resources circular treatment technology of high-efficiency cleaning, it is applicable to carry out the recovery of the high smelting cost metals resources taking Ti as representative and manufactures.

The present invention proposes BM-ECAP compound re-manufacturing technology, successfully prepare large size, block nanometer (< 200nm) high strength Ti material. Utilizing this technology, it is possible to from the chip of 2 grades of Ti (ASTMGrade2), manufacture by implementing BM-ECAP again, obtain the block nanometer Ti material of oxygen level��0.31wt%, its yield strength is about 800-1000MPa. This technical indicator is extremely excellent, because it confirms: in the level of approximate 2 grades of Ti (ASTMGrade2) oxygen level, BM-ECAP manufactures a nanometer Ti material again and not only obtains the yield strength far above 2 grades of business Ti materials (300-350MPa), can also obtain may than 5 grades of Ti (ASTMGrade5, i.e. Ti-6Al-4V alloy) yield strength (900-1050MPa), therefore the present invention technology meaning is, adopt discarded inferior grade Ti starting material, manufactured again by BM-ECAP, the yield strength of high-grade Ti can be obtained. Therefore, BM-ECAP technology is the waste resource increment reproducing method of a kind of low cost.

In the BM-ECAP technology that the present invention proposes, first implement the first link, namely in BM process, chip surface oxide compound (TiO2) be able to broken completely under grinding in collision, the stranding of steel ball. Meanwhile, nanometer crystal microstructure can also be formed in Ti chip inside. Thus, the continuity distribution of bigger (mm level) sheet oxide compound can be prevented with assembling, eliminate the serious metallurgical imperfection manufacturing Ti material again; Raw-material nanometer can be realized again. On this basis, implement the 2nd link, namely by ECAP solidification processing, the Ti chip that BM processes is solidified into blocks of large nanometer Ti material. Due to the enforcement temperature of ECAP control Ti recrystallization temperature (��600 DEG C) below, therefore compared to other technology such as high temperature founding (��1200 DEG C) or discharge plasma sinterings (��900 DEG C), ECAP can suppress grain coarsening effectively, retains nanometer microtexture after BM process to the full extent. Meanwhile, ECAP is effectively closed microscopic void, thus realizes the full densification manufacturing nanometer Ti material again. In addition, BM-ECAP technology can the stranding of comprehensive BM grind, broken effect, and the multi-pass storage effect of violent plastix strain in ECAP comes refinement effectively and reformation Ti chip form. Thus, compared to (solid matter six side) the 2 grades of business Ti materials easily producing deformation texture, BM-ECAP technology can effectively overcome the material property anisotropy because preferable grain orientation causes, manufacturing the isotropy realizing material property in 2 grades of nanometers of high strength Ti materials again, this has important actual value for the solid matter six side Ti easily forming deformation texture (preferable grain orientation). The above another technology meaning being the present invention.

In sum, compared with prior art, BM-ECAP technology provided by the invention is by inferior grade Ti (ASTMGrade2) raw material discarded, by implementing to manufacture again, the intensity index of high-grade Ti (ASTMGrade5) can be obtained, its technological operation is simple and practical, and controllability is strong. By this technology, the yield strength (��800-1000MPa) obtaining nano-structure (< 200nm) and excellence in Ti material can manufactured again, the continuity distribution in the material of bigger sheet oxide compound can be prevented again to the full extent with assembling, thus eliminate this serious metallurgical imperfection manufacturing Ti material again. Meanwhile, in BM-ECAP Combined Processing, the form of Ti chip is able to effective refinement and reformation, is easy to cause the property anisotropy caused by texture (preferable grain orientation) after overcoming ECAP processing in solid matter six side's Ti material. Its result: (1) produces a nanometer Ti material again by the success of BM-ECAP technology, and the distribution disperse of its oxide nano particles is even; (2) yield strength manufacturing nanometer Ti material again is significantly higher than 2 grades of business Ti materials (ASTMGrade2) of similar oxygen content level, may than the strength level of 5 grades of titanium materials (ASTMGrade5, i.e. Ti-6A-4V alloy); (3) its performance isotropy of nanometer Ti material is manufactured again.

Accompanying drawing explanation

Fig. 1 is the TEM photo manufacturing nano titanium material again adopting the inventive method to obtain.

Embodiment

The better embodiment of the present invention is provided, so that the technical scheme of the present invention to be described in detail below in conjunction with accompanying drawing.

Step (1)-Ti chip recycling pre-treatment:

2 grades of Ti (ASTMGrade2) chip generated in end mill mode is as starting material, after collecting chip, adopt inductively coupled plasma atomic emission spectrum (Inductivelycoupledplasmaatomicemissionspectroscopy, it is called for short ICP-AES) analyze its chemical composition (mass percent, wt%), analytical results is as shown in table 1. As shown in Table 1,2 grades of its chemical composition of the Ti chips (such as oxygen level) processed through end mill meet ASTM standard scope. Meanwhile, the ethanol of 99.9% is adopted to clean Ti chip in ultrasonic activation groove, with the greasy dirt removed in starting material and impurity etc.

The BM process of step (2)-Ti chip:

Steel BM container is inserted in the Ti chip obtained by step (1), and between chip and steel ball (diameter 10mm), mass ratio is 15:1. Meanwhile, the stearic acid adding 1wt.% is as process control agent, and BM container is filled with argon gas as protection atmosphere, to prevent chip over oxidation in BM process. The rotating speed of planetary BM machine is 300rpm; When BM runs total, length is 15 hours. In BM process, Ti chip issues raw food weldering, hardening and fragmentation at shock and the stranding stone roller of steel ball. Being processed by BM, Ti chip profile size and oxide on surface are able to remarkable refinement. Meanwhile, by the external container liquid nitrogen friction temperature of circulation to reduce chip-steel ball, and machine often runs 1 hour and will suspend 12 minutes. After BM terminates, adopting ICP-AES to analyze chip chemical composition, result is as shown in table 1. As shown in Table 1; through BM process Ti chip under argon gas shielded; its oxygen level only slightly rises (rising to 0.17wt% by 0.15wt%); and iron level rises to 0.64wt% by 0.10wt%, this is worn due to steel ball in BM process (and Steel Vessel wall face) and is mixed into caused by chip.

Step (3)-through BM process Ti chip be packed into ECAP mould:

First wrap up cylindrical steel billet (its diameter is slightly less than ECAP channel diameter) with annealed stainless steel foil, outside steel foil, wrap up in one layer of graphite paper (solid lubricant) again. Steel billet-steel foil-graphite paper is inserted ECAP passage, takes out steel billet, then form graphite paper-steel foil cavity. Insert the Ti chip that obtains by step (2) in cavity, then with hand press by preliminary for chip compacting.

Step (4)-BM processes the ECAP room temperature preprocessing of Ti chip:

The ECAP mould having loaded Ti chip through step (3) is installed on hydropress, at room temperature carries out ECAP preprocessing, to improve the degree of packing of chip pressed compact further, prevent BM from processing Ti chip over oxidation in ECAP hot setting is processed. In this step, the back pressure drift offer��200MPa constant backpressure of ECAP mould; When the pressure of feeding drift reach��700MPa time, stop ECAP process, complete room temperature preprocessing. Measure through Archimedes's method (Archimedes), its relative density of Ti chip of ECAP room temperature preprocessing 99.0%.

Step (5)-ECAP hot setting is processed:

Mould is wrapped up, the recrystallization temperature (��600 DEG C) being heated to Ti certain level (such as, 590 DEG C) below with armouring electric blanket, and by the scope of temperature regulator equilibrium temperature at �� 1 DEG C. For the Ti chip pressed compact that step (4) obtains, carry out the processing of ECAP hot setting. ECAP processes speed��10mm/min. Under the effect of programmable logic controller and hydraulicdirectional control valve, ECAP mould import and export passage two drifts (feeding drift, it can provide solidifying pressure; Back pressure drift, can provide back pressure) solidifying pressure (up to��1.2GPa) and back pressure (150-200MPa) can be alternately provided. So, ECAP processing can accumulate multiple passage (avoiding taking out sample between passage) continuously. By the accumulation of 4-8 passage, the block obtaining full densification (measure, relative density > 99.9%) by Archimedes's method manufactures Ti material again. Multiple spot is observed under a scanning electron microscope, does not find that microscopic void exists. Adopting ICP-AES to analyze Ti material chemical composition, its result is as shown in table 1. As shown in Table 1, the oxygen level manufacturing Ti material through BM-ECAP again rises to 0.31wt% by the 0.15wt% of original chip, is still similar to the oxygen level of 2 grades of Ti (ASTMGrade2).

Step (6)-BM-ECAP manufactures a nanometer quenching for Ti material again:

The block Ti material die sinking in hot state step (5) obtained, adopts water-cooling pattern quench cooled to room temperature, keeps nano-structure to the full extent. According to BM-ECAP re-manufacturing technology, from the chip of 2 grades of Ti (ASTMGrade2), obtain the Ti material of manufacture nanometer again of oxygen level��0.31wt%, by transmission electron microscope (Transmissionelectronmicroscopy, it is called for short TEM) observe (as shown in Figure 1), its microtexture refine to nanoscale (< 200nm), and the distribution of oxide nano particles is the uniform state of disperse. Meanwhile, by Linear cut��4.00 �� 4.00 �� 6.00mm sample, and on universal testing machine, Mechanics Performance Testing is carried out, it has been found that BM-ECAP manufactures the yield strength��800-1000MPa of nanometer Ti material again.

Table 1 adopts ICP-AES methods analyst Ti chip in virgin state, BM processing and BM-ECAP manufacture again after chemical composition.

Table 1

Element O N C Fe Original Ti chip chemical composition (wt%) 0.15 <0.01 <0.01 0.10 Ti chip chemical composition (wt%) after BM process 0.17 <0.01 0.22 0.64 BM-ECAP manufactures nanometer Ti material chemical composition (wt%) again 0.31 0.11 0.34 -

Claims (10)

1. the ball milling of a discarded titanium chip-equal channel angular extruding reproducing method, it is characterized in that, in turn include the following steps: the ball-milling processing step of titanium chip recycling pre-treatment step, titanium chip, be packed into equal channel angular extrusion die step, equal channel angular extruding room temperature preliminary step, equal channel angular extruding hot setting procedure of processing and quenching step.
2. the method for claim 1, it is characterised in that, described titanium chip recycling pre-treatment step adopts ethanol to be cleaned by titanium chip starting material.
3. the method for claim 1, it is characterised in that, the ball-milling processing step of described titanium chip; it is that pretreated titanium chip is inserted in the ball mill container including steel ball; adition process control agent simultaneously, ball milling 10-20 hour under the protection of inert gas atmosphere, rotating speed 280-350rpm.
4. method as claimed in claim 3, it is characterised in that, between described titanium chip and steel ball, mass ratio is 12-20:1, and the diameter of described steel ball is 7-12mm, and described process control agent is stearic acid or straight iron powder, and its add-on is between 0.5-2.0wt%.
5. the method for claim 1, it is characterized in that, described it is packed into equal channel angular extrusion die step, being wrap up cylindrical steel billet with steel foil, described steel billet diameter is slightly less than die channel diameter, wraps up in one layer of solid lubrication oxidant layer outside steel foil again, steel billet-steel foil-solid lubrication oxidant layer is inserted die channel, take out steel billet, form solid lubrication oxidant layer-steel foil cavity, then the titanium chip through ball-milling processing is filled in above-mentioned cavity.
6. method as claimed in claim 5, it is characterised in that, described steel foil is through the stainless steel foil of anneal, and described solid lubricant is graphite paper or masking foil.
7. method as claimed in claim 5, it is characterised in that, after being filled in described solid lubricant-steel foil cavity through the titanium chip of ball-milling processing, then with hand press by preliminary for chip compacting.
8. the method for claim 1, it is characterized in that, described equal channel angular extruding room temperature preliminary step, comprise and the mould having loaded titanium chip is installed on a hydraulic press, back pressure drift provides the constant backpressure of 150��200MPa, and continue to improve the pressure of feeding drift, when the pressure that feeding drift provides reaches 680��720MPa, stop equal channel angular extrusion process.
9. the method for claim 1, it is characterized in that, described equal channel angular extruding hot setting procedure of processing, comprise heating mould to 570-590 DEG C, under the effect of hydraulicdirectional control valve, two drifts that passage imported and exported by control mould alternately provide solidifying pressure 1.0��1.2GPa and back pressure 150-200MPa, carry out 4-8 passage continuously.
10. the method for claim 1, it is characterized in that, described quenching step, it is that equal channel angular is extruded in hot setting procedure of processing the block titanium material die sinking in hot state obtained, adopt water-cooling pattern quench cooled to room temperature, obtain and manufacture nano titanium material again.
CN201510992894.1A 2015-12-25 2015-12-25 Ball milling-Equal-channel Angular Pressing reproducing method of discarded titanium chip CN105618501B (en)

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CN106694890A (en) * 2016-11-15 2017-05-24 上海电机学院 Ball-milling-high-pressure torsion method for circulatory solidification of waste titanium cuttings
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CN106734063A (en) * 2016-11-29 2017-05-31 上海电机学院 Double undergauge cycle extrusion curings that the discarded chip of titanium is remanufactured
CN106756686A (en) * 2016-11-15 2017-05-31 上海电机学院 The hot extrusion rolloff method for annealing of titanium alloy chip circular treatment
CN106735253A (en) * 2016-11-24 2017-05-31 上海电机学院 The chip of discarded titanium circulates the ball milling for solidifying pier extrusion method repeatedly
CN106734297A (en) * 2016-11-24 2017-05-31 上海电机学院 The T-shaped channel pressings curing that the discarded chip of titanium is remanufactured
CN106756689A (en) * 2016-11-24 2017-05-31 上海电机学院 A kind of ball milling accumulation rolling folding method of pure titanium chip circulation solidification
CN106825585A (en) * 2016-11-15 2017-06-13 上海电机学院 Electric discharge quick consolidation method and device that a kind of titanium chip circulation is remanufactured
CN108526235A (en) * 2018-04-30 2018-09-14 西北有色金属研究院 A kind of method of high tough titanium alloy twice time equal channel angular cold extrusion

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CN106825585A (en) * 2016-11-15 2017-06-13 上海电机学院 Electric discharge quick consolidation method and device that a kind of titanium chip circulation is remanufactured
CN106694890A (en) * 2016-11-15 2017-05-24 上海电机学院 Ball-milling-high-pressure torsion method for circulatory solidification of waste titanium cuttings
CN106694891A (en) * 2016-11-15 2017-05-24 上海电机学院 Ball milling electric field pressure-assisted sintering remanufacturing method and device of titanium chips
CN106756686B (en) * 2016-11-15 2018-10-12 上海电机学院 Hot extrusion-rolloff-method for annealing of titanium alloy chip circular treatment
CN106552944A (en) * 2016-11-15 2017-04-05 上海电机学院 Many corner extrusion curings of titanium chip circular treatment
CN106756686A (en) * 2016-11-15 2017-05-31 上海电机学院 The hot extrusion rolloff method for annealing of titanium alloy chip circular treatment
CN106513690A (en) * 2016-11-24 2017-03-22 上海电机学院 Ball milling-isometric angle extrusion-annealing method for pure titanium waste chip circular curing
CN106734297A (en) * 2016-11-24 2017-05-31 上海电机学院 The T-shaped channel pressings curing that the discarded chip of titanium is remanufactured
CN106493372A (en) * 2016-11-24 2017-03-15 上海电机学院 The ball milling bending channel extruding curing of the discarded chip circular treatment of pure titanium
CN106493184A (en) * 2016-11-24 2017-03-15 上海电机学院 A kind of parallel channels corner undergauge coextrusion method of titanium chip circulation solidification
CN106756689A (en) * 2016-11-24 2017-05-31 上海电机学院 A kind of ball milling accumulation rolling folding method of pure titanium chip circulation solidification
CN106735253A (en) * 2016-11-24 2017-05-31 上海电机学院 The chip of discarded titanium circulates the ball milling for solidifying pier extrusion method repeatedly
CN106392085A (en) * 2016-11-24 2017-02-15 上海电机学院 Ball grinding-diameter shrinkage reciprocating extruding method for circular curing of waste titanium chips
CN106734063A (en) * 2016-11-29 2017-05-31 上海电机学院 Double undergauge cycle extrusion curings that the discarded chip of titanium is remanufactured
CN106583411A (en) * 2016-11-29 2017-04-26 上海电机学院 Wedge bending-roller straightening deformation method for circularly solidifying waste titanium chips
CN106552815A (en) * 2016-11-29 2017-04-05 上海电机学院 The straightening of the crimping repeatedly deformation curing that discarded titanium chip is remanufactured
CN106552815B (en) * 2016-11-29 2019-01-29 上海电机学院 The crimping repeatedly that discarded titanium chip remanufactures-straightening deformation curing method
CN106583411B (en) * 2016-11-29 2019-04-12 上海电机学院 The discarded chip circulation of titanium is cured to carve the straight deformation method of curved-roller
CN108526235A (en) * 2018-04-30 2018-09-14 西北有色金属研究院 A kind of method of high tough titanium alloy twice time equal channel angular cold extrusion
CN108526235B (en) * 2018-04-30 2019-08-30 西北有色金属研究院 A kind of method of high tough titanium alloy twice time equal channel angular cold extrusion

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