CN106756689B - A kind of cured ball milling of pure titanium chip cycle-accumulation rolls folding method - Google Patents
A kind of cured ball milling of pure titanium chip cycle-accumulation rolls folding method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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Abstract
The present invention proposes that a kind of pure titanium chip recycles cured ball milling accumulation rolling folding method, includes the following steps：(1) Ti chip recyclings pre-process：Titanium chip is cleaned, degreasing and impurity are removed；(2) the BM processing of Ti chips：The pretreated titanium chip of step (1) is subjected to ball milling processing；(3) the jacket encapsulation of BM Ti chips：BM Ti chips are filled in titanium cylinder cavity, then with hand press by chip preliminary consolidation；(4) cold rolling at room temperature of jacket encapsulation BM Ti chips：Step (3) is subjected to cold rolling through jacket encapsulation BM Ti chips, produces Cold-rolled Pure Ti planks；(5) annealing of cold rolling Ti planks：Cold-reduced sheet is heated to 750 DEG C~850 DEG C, keeps the temperature 30~40 minutes, it is then air-cooled；(6) ARB hot settings process Ti chips：Ti planks after step (5) is annealed are overlapped by the rolling of 2 passages, prepare block Ti materials；(7) it quenches：The block Ti materials obtained in step (6) are quickly quenching into room temperature by water-cooling pattern.
Description
Technical field
The present invention is to belong to metal material processing field, is related to the solid phase Recycling and reuse of discarded metal resource, especially
It is the titanium resource for high smelting cost, researches and develops a kind of titanium chip of high-efficiency cleaning and remanufacture new technology.More particularly to it is a kind of
Pure titanium chip recycles cured ball milling-accumulation and rolls folding method.
Background technology
Titanium is the metals resources of high smelting cost, and biocompatibility is excellent, corrosion resistance is good, mechanical property is suitable, is system
Make the important materials of medical instrument, joint prosthesis, large-scale derived energy chemical container etc..But it in order to manufacture high-precision Ti structures, needs
Larger allowance is designed, a large amount of raw material translate into discarded chip.Traditional high temperature founding processing energy consumption is big, pollutes
Weight, efficiency is low, and cast sturcture's coarse grains, performance are poor.Solid phase is recycled and is remanufactured because avoiding high temperature founding, is to realize gold
One effective way of category resource high-efficiency, cleaning circulation.By the literature search discovery to the prior art, equal channel angular is squeezed
(Equal channel angular pressing, the abbreviation ECAP) technology of pressure is applied to processing borings, can refine crystalline substance
Grain improves the microstructure form for remanufacturing material, improves mechanical performance.Lapovok etc. exists《Journal of Materials
Science》" Multicomponent materials from machining are delivered on 1193-1204 pages of volume 49 within 2014
Chips compacted by equal-channel angular pressing are (by Equal-channel Angular Pressing chip formation system
Standby multi-component material) " text, it was recently reported that by being mutually mixed for aluminium chip and magnesium chip, by the multigroup division of ECAP circular regenerations
Golden material；Luo etc. exists《Journal of Materials Science》It delivers on 4606-4612 pages of volume 45 within 2010
“Recycling of titanium machining chips by severe plastic deformation
Consolidation (the severe plastic deformation solid cycle of titanium chip) " texts, propose through 2 grades of discarded titanium (ASTM of recycling
Grade 2) chip, and by ECAP technologies block materials are remanufactured to recycle.In addition, Zhao etc. exists《Scripta
Materialia》" Microstructure and properties of pure are delivered on 542-545 pages of volume 59 within 2008
(the rooms titanium processed by equal-channel angular pressing at room temperature "
Warm Equal-channel Angular Pressing prepares the micro-structure and property of pure titanium) text, single pass ECAP deformation process titaniums are used at room temperature
Material.In order to reduce resistance of deformation, ECAP molds angle increases to 120 degree by 90 degree, and extruding rate is relatively low (0.5mm/s),
It reduce the Rate of strain accumulation of ECAP and processing efficiencies.
Accumulation rolling overlapping (Accumulative roll-bonding, abbreviation ARB) be it is a kind of prepare block body ultrafine grain gold
Belong to the severe plastic deformation technology of material.Tsuji etc. exists《Advanced Engineering Materials》2003 volume 5
" ARB (Accumulative roll-bonding) and other new techniques to are delivered on 338-344 pages
(ARB for preparing bulk ultrafine-grained materials (it is folded to accumulate rolling to produce bulk ultrafine grained materials "
Close) and other new technologies) text, it describes and uses processing Al and alloy and steel plate under ARB technologies at different temperatures
Material.Saito etc. exists《Scripta Materialia》" Ultra-fine is delivered on 1221-1227 pages of volume 39 within 1998
Grained bulk aluminum produced by accumulative roll-bonding (ARB) process " (accumulations
Rolling overlapping (ARB) technique prepares block body ultrafine grain aluminium) text, the pure Al planks of business are handled to obtain block body ultrafine with ARB
Brilliant Al materials.In ARB techniques, the plank of rolling is cut, stacking, then is rolled.During rolling again, between plank interface
Solid-State Welding occurs under violent squeezing action to close.Have Ultra-fine Grained microstructure special by the block materials that multi-pass ARB is prepared
Sign.
Ball milling (Ball milling, abbreviation BM) is another violent plasticity change for being widely used in and preparing superfine powdery material
Shape technology.Mahboubi Soufiani etc., which exist, to be found to the retrieval of existing technical literature《Materials and Design》
" Formation mechanism and characterization of are delivered on 152-160 pages of volume 37 within 2012
(prepared by mechanical alloying by nanostructured Ti6Al4V alloy prepared by mechanical alloying
The Forming Mechanism and characterization of Ti6Al4V alloy nanostructures) " text, it reports using titanium, aluminium, vanadium powder and micron as raw material, passes through BM skills
Art prepares the Ti-6Al-4V alloys of nanoscale (being less than 100nm).In addition, Zadra exists《Materials Science and
Engineering A》Deliver within 2013 that " Mechanical alloying of titanium be (titanium on 105-113 pages of volume 583
Mechanical alloying) " literary, a Ti powder of the initial feed less than 150 μm, pass through BM processing, pure titanium of the acquisition less than 25 μm first
Superfines, and block titanium is obtained by discharge plasma sintering.
The traditional technology of discarded metal chip circular treatment is remelting+casting.However, high temperature founding energy consumption is big, pollution weight,
Efficiency is low, and cast sturcture's coarse grains, mechanical performance are poor.To avoid high temperature founding, solid phase processing mode can be used.But
It is that, when solid phase handles Ti chips, existing ECAP and BM technologies respectively have its limitation.Ti is easy to aoxidize, chip surface oxidation
Object exists in the form of TiO2, strong but pliable in texture, and the Strain Accumulation efficiency of ECAP technology single pass processing is low.Even if being handled through multi-pass
Afterwards, oxide to a certain extent be crushed, disperse, still, larger oxide it is continuously distributed will be formed microstructure in smelting
Golden defect weakens the mechanical performance of material.Meanwhile there is the refinement limit in ECAP processing, i.e., when dynamic recrystallization and strain refine
When effect reaches balance, then ECAP will be difficult to that microstructure is made further to refine.On the other hand, although BM technologies can be prepared effectively
Superfine powder.But after BM processing, must carry out hot pressed sintering or powder squeeze/the subsequent processings process such as forging and stamping to be to obtain block
Because heating (sintering) time is long and the influence of the factors such as dynamic recrystallization crystal grain will occur for material, and in these processes
Roughening weakens the strength of materials.These technical problems not yet well solve at present.
Therefore, we are it is necessary to improve such a structure, to overcome drawbacks described above.
Invention content
Recycling and remanufacturing for discarded metal resource is the key that realize one of sustainable development.At traditional high temperature founding
Reason energy consumption is big, pollution is heavy, and efficiency is low, and cast sturcture's coarse grains, performance are poor.Solid phase is recycled and is remanufactured because avoiding high temperature
Founding, be realize metals resources efficiently, an effective way of cleaning circulation.The purpose of the present invention is remanufactured based on solid phase
Theory, research and develop a kind of Ti resources for high smelting cost environmentally friendly ball milling-accumulation rolling overlaps (BM-ARB) again
Manufacturing technology improves Strain Accumulation and processing efficiency to overcome disadvantages mentioned above of the existing technology, prepares and is densified entirely
Blocks of large Ti materials realize efficient, the cleaning recycling for discarding Ti chips.
The present invention is technical solution used by solving its technical problem：
A kind of cured ball milling of pure titanium chip cycle-accumulation rolls folding method, includes the following steps：
(1) Ti chip recyclings pre-process：Titanium chip is cleaned, degreasing and impurity are removed；
(2) the BM processing of Ti chips：The pretreated titanium chip of step (1) is subjected to ball milling processing；
(3) the jacket encapsulation of BM-Ti chips：BM-Ti chips are filled in titanium cylinder cavity, then will be cut with hand press
Consider preliminary consolidation to be worth doing；
(4) cold rolling at room temperature of jacket encapsulation BM-Ti chips：The BM-Ti chips that step (3) is encapsulated through jacket carry out cold
It rolls, produces Cold-rolled Pure Ti planks；
(5) annealing of cold rolling Ti planks：Cold-reduced sheet is heated to 750 DEG C~850 DEG C, keeps the temperature 30~40 minutes, so
It is air-cooled afterwards；
(6) ARB hot settings process Ti chips：Ti planks after step (5) is annealed are overlapped by the rolling of 2 passages,
Prepare block Ti materials；
(7) it quenches：The block Ti materials obtained in step (6) are quickly quenching into room temperature by water-cooling pattern；
Further, in step (1), the titanium chip generated using 2 grades of titaniums of end mill is filled as raw material using ultrasonic cleaning
It sets and is cleaned, to remove the greasy dirt and impurity in raw material, ultrasonic cleaning equipment is using 99.9% ethyl alcohol as washing
Liquid；
Further, in step (2), the pretreated titanium chip of step (1) is placed in the BM containers containing steel ball, simultaneously
Adition process controlling agent, ball milling 10~20 hours under the protection of inert gas atmosphere, drum's speed of rotation are 280~350rpm；
Further, mass ratio is 12~20 between Ti chips and steel ball:1, a diameter of 7~12mm of the steel ball；Institute
It states process control agent and can be selected from stearic acid and straight iron powder, the addition of the process control agent is between 0.5~2wt%；It is described
Inert gas can be nitrogen, argon gas or helium；The external container also passes to liquid nitrogen cycle, and machine is often run 1~2 hour
Then suspend 10~15 minutes；
Further, titanium cylinder described in step (3) is wrapped with one layer of kollag, and drum diameter is smaller logical with mold
Titanium cylinder-kollag is placed in cold stamping die, BM-Ti chips is filled in titanium cylinder cavity by road diameter；The titanium cylinder material
It is 2 grades of Ti by annealing, graphite paper or masking foil can be selected in the kollag；
Further, cold rolling ratio is 50~70% in step (4)；
Further, in step (6), the annealing Ti planks obtained by step (5) are blocked at 1/2 position, to table of joint
Face uses ethyl alcohol to be cleaned to degrease and impurity, plank is piled up, and be heated to 600 DEG C, using 60% rolling than will
Plate rolling overlaps the first passage；The plank that the first passage overlaps is blocked at 1/2 position again, ethyl alcohol is used in combination to carry out cleaning surface
To degrease and impurity, plank is piled up, and be heated to 600 DEG C, using 60% rolling than plate rolling is overlapped second
It is secondary；This step is overlapped by the rolling of 2 passages, prepares block Ti materials.
In the present invention, by implementing BM processing, chip surface oxide (TiO2) is able in the case where collision, the stranding of steel ball are ground
It is complete broken.It effectively prevent the continuity of larger defect oxide to be distributed and assemble.On this basis, implement cold rolling and ARB
Hot setting is processed, and BM-Ti chips are solidified into blocks of large Ti materials.In ARB techniques, the plank of rolling is cut, heap
Pile, then roll.Solid-State Welding occurs under violent squeezing action during rolling again, between plank interface to close.By multi-pass
The block materials that ARB is prepared have Ultra-fine Grained Microstructure characteristics.Due to squeeze temperature control Ti recrystallization temperature (~
600 DEG C) hereinafter, therefore compared to other technologies such as high temperature founding (~1200 DEG C) or discharge plasma sintering (~900 DEG C), ARB
Technique can effectively inhibit grain coarsening, retain BM treated ultra-fine microstructures to the full extent.Utilize the technology
2 grades of Ti (ASTM Grade 2) chips are handled, the block nanometer Ti materials of oxygen content~0.24wt% are obtained, yield strength is about
650-750MPa.In the level of approximate 2 grades of Ti (ASTM Grade 2) oxygen content, remanufactures Ti materials and obtain higher than 2 grades of Ti quotient
The yield strength (300-350MPa) of industry bar.
The advantage of the invention is that：
The traditional technology of discarded metal chip circular treatment is remelting+casting.However, high temperature founding energy consumption is big, pollution weight,
Efficiency is low, and cast sturcture's coarse grains, mechanical performance are poor.To avoid high temperature founding, solid phase processing mode can be used.But
It is that, when solid phase handles Ti chips, existing ECAP and BM technologies respectively have its limitation.Ti is easy to aoxidize, chip surface oxidation
Object exists in the form of TiO2, strong but pliable in texture, and the Strain Accumulation efficiency of ECAP technology single pass processing is low.Even if being handled through multi-pass
Afterwards, oxide to a certain extent be crushed, disperse, still, larger oxide it is continuously distributed will be formed microstructure in smelting
Golden defect weakens the mechanical performance of material.Meanwhile there is the refinement limit in ECAP processing, i.e., when dynamic recrystallization and strain refine
When effect reaches balance, then ECAP will be difficult to that microstructure is made further to refine.On the other hand, although BM technologies can be prepared effectively
Superfine powder.But after BM processing, must carry out hot pressed sintering or powder squeeze/the subsequent processings process such as forging and stamping to be to obtain block
Because heating (sintering) time is long and the influence of the factors such as dynamic recrystallization crystal grain will occur for material, and in these processes
Roughening weakens the strength of materials.These technical problems not yet well solve at present.
BM-ARB technical solutions proposed by the present invention overcome above-mentioned existing limitation, can realize the invention skill
Art effect.First, pass through BM technical finesse Ti chips.The oxide (TiO2) of chip surface is filled in the case where collision, the stranding of steel ball are ground
Divide broken.Then, cure BM-Ti chips at 570-600 DEG C by ARB techniques.In ARB techniques, the plank of rolling is cut,
Stacking, then roll.Solid-State Welding occurs under violent squeezing action during rolling again, between plank interface to close.By multiple tracks
The block materials that secondary ARB is prepared have Ultra-fine Grained Microstructure characteristics.Since the control of extruding temperature is in the recrystallization temperature of Ti
(~600 DEG C) hereinafter, therefore compared to other technologies such as high temperature founding (~1200 DEG C) or discharge plasma sintering (~900 DEG C),
ARB techniques can effectively inhibit grain coarsening, retain BM treated ultra-fine microstructures to the full extent.And thoroughly disappear
Except porosity defects.It is remanufactured, is obtained complete fine and close by implementing from 2 grades of Ti (ASTM Grade 2) chip according to this method
Change block Ti materials, yield strength is about 650-750MPa, hence it is evident that be higher than the yield strength (300- of 2 grades of Ti business bars
350MPa).Regeneration Ti materials are significantly improved in terms of strength character.
BM-ARB complex technique controllabilitys in the present invention are strong, high in machining efficiency, not only obtain nano-structure, but also eliminate metallurgical
Defect segregation in the material.By implementing BM processing, chip surface oxide (TiO2) be able in the case where collision, the stranding of steel ball are ground
Complete is broken.It effectively prevent the continuity of larger defect oxide to be distributed and assemble.On this basis, implement cold rolling and ARB high
Temperature solidification processing, blocks of large Ti materials are solidified by BM-Ti chips.In ARB techniques, the plank of rolling is cut, stacking,
It rolls again.Solid-State Welding occurs under violent squeezing action during rolling again, between plank interface to close.By multi-pass ARB
The block materials prepared have Ultra-fine Grained Microstructure characteristics.ARB technologies based entirely on rolling accumulative effect of strain, compared to
The technologies such as ECAP, improve processing efficiency.The recrystallization temperature (~600 DEG C) in Ti is controlled hereinafter, ARB works due to squeezing temperature
Artistic skill enough effectively inhibits grain coarsening, retains BM treated ultra-fine microstructures to the full extent.And thoroughly eliminate hole
Gap defect.Using the technical finesse 2 grades of Ti (ASTM Grade 2) chip, by remanufacturing, the intensity of regeneration Ti materials is higher than 2 grades
Ti business bars.The present invention is a kind of metals resources solid phase circular treatment technology of high-efficiency cleaning, and which obviate high temperature foundings, fit
For carry out using Ti as the recycling of the high smelting cost metals resources of representative with remanufacture.
Description of the drawings
Fig. 1 is to accumulate to roll in a kind of cured ball milling of pure titanium chip cycle proposed by the present invention-accumulation rolling folding method
System overlapping remanufactures (i.e. BM-ARB is remanufactured) process schematic representation.
Specific implementation mode
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Diagram and specific embodiment are closed, the present invention is further explained.
As shown in Figure 1, a kind of pure titanium chip proposed by the present invention, which recycles cured ball milling-accumulation, rolls folding method, packet
Include following steps：
Step (1)-Ti chip recyclings pre-process：The chip generated using 2 grades of Ti of end mill (ASTM Grade 2) is former material
Material, after collecting chip, using inductively coupled plasma atomic emission spectrum (Inductively coupled plasma
Atomic emission spectroscopy, abbreviation ICP-AES) its chemical composition (mass percent, wt.%) is analyzed, point
The results are shown in Table 1 for analysis.As shown in Table 1, its chemical composition (oxygen content) of 2 grades of Ti chips through Milling Process meets ASTM standard
Range.Meanwhile Ti chips are cleaned in ultrasonic activation slot using 99.9% ethyl alcohol, to remove greasy dirt in raw material and miscellaneous
Matter etc.；
The BM processing of step (2)-Ti chips：The Ti chips that will be obtained by step (1) are placed in steel BM containers, chip and steel
Mass ratio is 15 between ball (diameter 10mm):1.Meanwhile the stearic acid of 1wt.% is added as process control agent, and by BM containers
Argon gas is filled with as protection atmosphere, to prevent chip excessive oxidation during BM.The rotating speed of planetary BM machines is 300rpm；
It is 15 hours that BM, which runs total duration,.During BM, Ti chips issue raw food weldering, hardening with stranding stone roller in the shock of steel ball and break
It is broken.It is processed by BM, Ti chip profiles size and oxide on surface are significantly refined.Meanwhile by external container liquid nitrogen
Cycle is to reduce the friction temperature of chip-steel ball, and machine often runs 1 hour and will suspend 12 minutes.After BM, use
ICP-AES analyzes chip chemical composition, and the results are shown in Table 1.As shown in Table 1, through BM handle Ti chips under protection of argon gas,
Its oxygen content only slightly rises (rising to 0.17wt% by 0.15wt%), and iron content rises to 0.64wt% by 0.10wt%, this
It is caused by steel ball (and steel vessel wall surface) is worn and is mixed into chip during BM.
The jacket of step (3)-BM-Ti chips encapsulates：One layer of graphite paper solid lubrication of cylinder outer wrapping made of 2 grades of Ti foils
Agent, the drum diameter are slightly less than die channel diameter, and steel cylinder-kollag is placed in cold stamping die, will be taken by step (2)
BM-Ti chips be filled in titanium cylinder cavity, then with hand press by chip preliminary consolidation.
The cold rolling at room temperature of step (4)-jacket encapsulation BM-Ti chips：It will be by the BM-Ti for the jacket encapsulation that step (3) obtains
Chip carries out cold rolling between roll, rolls ratio 50%, produces Cold-rolled Pure Ti planks.This step can further improve the tight of chip
Solidity prevents BM-Ti chips excessive oxidation in high temperature ARB solidifications.It is measured through Archimedes method (Archimedes), room temperature is cold
Ti chips its relative density~99.0% rolled.
The annealing of step (5)-cold rolling Ti planks：The cold-reduced sheet obtained by step (4) is heated to 800 DEG C, heat preservation
It is 30 minutes, then air-cooled.This step can adjust the stress state of Ti plates after cold rolling, reduces case hardness, is conducive to follow-up plank
Surface treatment.
Step (6)-ARB hot settings process Ti chips：It will be cut at 1/2 position by the annealing Ti planks that step (5) obtains
It is disconnected, use ethyl alcohol to be cleaned engagement surface to degrease and impurity, plank is piled up, and be heated to 600 DEG C, use
Plate rolling is overlapped the first passage by 60% rolling ratio, then the plank that the first passage overlaps is blocked at 1/2 position, and ethyl alcohol is used in combination
Cleaning surface is carried out to degrease and impurity, plank is piled up, and be heated to 600 DEG C, using 60% rolling than rolling plank
System the second passage of overlapping.This step is overlapped by the rolling of 2 passages, is prepared for block Ti materials.
Step (7)-quenches：It will be quenched and be cooled down by water-cooling pattern by the ARB hot settings block Ti materials that step (6) obtains
To room temperature.
It is measured by Archimedes method, block remanufactures Ti materials and realizes full densification (nearly 99.99%) of relative density.It is sweeping
It retouches multiple spot under electron microscope to observe, does not find that microscopic void exists.Ti material chemical compositions, result are analyzed using ICP-AES
As shown in table 1.As shown in Table 1, the oxygen content for remanufacturing Ti materials rises to 0.24wt% by the 0.15wt% of original chip, still approximate
In the oxygen content of 2 grades of Ti (ASTM Grade 2).Meanwhile by wire cutting~4.00 × 4.00 × 6.00mm samples, and ten thousand
Performance test can be carried out in Material Testing Machine, find the yield strength 650-750MPa for remanufacturing Ti materials.
Table 1 is to analyze initial Ti chips using ICP-AES technologies, and BM processing (BM-Ti) and ARB remanufacture (BM-ARB
Ti) the chemical composition of Ti chips afterwards.
Table 1
| Element | O | N | C | Fe |
| Initial Ti chips (wt.%) | 0.15 | <0.01 | <0.01 | 0.10 |
| BM-Ti chips (wt.%) | 0.17 | <0.01 | 0.22 | 0.64 |
| BM-ARB Ti chips (wt.%) | 0.24 | 0.02 | 0.23 | - |
The novelty of the present invention：The present invention is to discard titanium chip by recycling, and exploitation accumulation rolling overlapping is solid to implement
State is recycled and is remanufactured, to obtain a kind of technical method of block high intensity titanium.
The creativeness of the present invention：Accumulation rolling overlapping is creatively combined by the present invention with ball milling, is successfully applied to back
Receive, titanium chip is discarded in processing, be a kind of new titanium resource solid cycle and reproducing method, can efficiently, will discard cleanly
Titanium chip is changed into block high intensity titanium.
The practicability of the present invention：Practical of the present invention can efficiently remanufacture out block titanium, and obtain high-strength
Degree.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent defines.
Claims (1)
1. a kind of pure titanium chip recycles cured ball milling-accumulation and rolls folding method, which is characterized in that include the following steps：
(1) Ti chip recyclings pre-process：Titanium chip is cleaned, degreasing and impurity are removed；
(2) the BM processing of Ti chips：The pretreated titanium chip of step (1) is subjected to ball milling processing；
(3) the jacket encapsulation of BM-Ti chips：BM-Ti chips are filled in titanium cylinder cavity, then will be at the beginning of chip with hand press
Step compacting；
(4) cold rolling at room temperature of jacket encapsulation BM-Ti chips：The BM-Ti chips that step (3) is encapsulated through jacket carry out cold rolling, system
Take Cold-rolled Pure Ti planks；
(5) annealing of cold rolling Ti planks：Cold-reduced sheet is heated to 750 DEG C~850 DEG C, keeps the temperature 30~40 minutes, it is then empty
It is cold；
(6) ARB hot settings process Ti chips：Ti planks after step (5) is annealed are overlapped by the rolling of 2 passages, are prepared
Go out block Ti materials；
(7) it quenches：The block Ti materials obtained in step (6) are quickly quenching into room temperature by water-cooling pattern；
Wherein, in step (1), the titanium chip generated using 2 grades of titaniums of end mill is carried out clear as raw material using ultrasonic cleaning equipment
It washes, to remove the greasy dirt and impurity in raw material, ultrasonic cleaning equipment is using 99.9% ethyl alcohol as cleaning solution；
Wherein, in step (2), the pretreated titanium chip of step (1) is placed in the BM containers containing steel ball, while adition process
Controlling agent, ball milling 10~20 hours under the protection of inert gas atmosphere, drum's speed of rotation are 280~350rpm；
Wherein, mass ratio is 12~20 between Ti chips and steel ball:1, a diameter of 7~12mm of the steel ball；It is described excessively program-controlled
Preparation can be selected from stearic acid or straight iron powder, and the addition of the process control agent is between 0.5~2wt%；The inert gas
Can be nitrogen, argon gas or helium；The external container also passes to liquid nitrogen cycle, and machine often runs 1~2 hour and then suspends 10
~15 minutes；
Wherein, titanium cylinder described in step (3) is wrapped with one layer of kollag, and drum diameter is smaller with die channel diameter,
Titanium cylinder-kollag is placed in cold stamping die, BM-Ti chips are filled in titanium cylinder cavity；The titanium cylinder material be by
Graphite paper or masking foil can be selected in 2 grades of Ti of annealing, the kollag；
Wherein, cold rolling ratio is 50~70% in step (4)；
Wherein in step (6), the annealing Ti planks obtained by step (5) are blocked at 1/2 position, ethyl alcohol is used to engagement surface
It is cleaned to degrease and impurity, plank is piled up, and be heated to 600 DEG C, using 60% rolling than folding plate rolling
Close the first passage；The plank that the first passage overlaps is blocked at 1/2 position again, ethyl alcohol is used in combination to carry out cleaning surface to degrease
And impurity, plank is piled up, and be heated to 600 DEG C, using 60% rolling than plate rolling is overlapped the second passage；This step is logical
The rolling overlapping for crossing 2 passages, prepares block Ti materials.
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| CN106756689A (en) | 2017-05-31 |
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