CN106825585A - Electric discharge quick consolidation method and device that a kind of titanium chip circulation is remanufactured - Google Patents
Electric discharge quick consolidation method and device that a kind of titanium chip circulation is remanufactured Download PDFInfo
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- CN106825585A CN106825585A CN201611030103.8A CN201611030103A CN106825585A CN 106825585 A CN106825585 A CN 106825585A CN 201611030103 A CN201611030103 A CN 201611030103A CN 106825585 A CN106825585 A CN 106825585A
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- chips
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- graphite
- rapidly solidified
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F8/00—Manufacture of articles from scrap or waste metal particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
Abstract
The present invention proposes the quick consolidation method and device that a kind of titanium chip circulation is remanufactured, and comprises the following steps：Pretreatment is reclaimed in step (1) Ti cuttings；Degassing is dried in step (2) Ti chips；The pretreatment of colding pressing of step (3) Ti chips；Step (4) Ti chips cold pressing base high-density current it is rapidly solidified.The rapidly solidified reproducing method of Ti chips high-density current proposed by the present invention, avoid high temperature founding, it is the metals resources recycling technology of a kind of low cost and high-efficiency cleaning, it is applied to the Recycling and reuse for carrying out the smelting cost metals resources high with Ti as representative.
Description
Technical field
The present invention relates to metal material processing field, it is related to the solid phase Recycling and reuse of discarded metal resource, particularly
For the titanium resource of smelting cost high, research and develop a kind of titanium chip of high-efficiency cleaning and remanufacture new technology.
Background technology
At present, the PM technique researched and developed for solidification powder body material mainly includes hot pressed sintering (Hot-pressing
Sintering, abbreviation HPS), discharge plasma sintering (Spark plasma sintering, abbreviation SPS), and high pressure is high
Temperature sintering (High-pressure and high-temperature sintering, abbreviation HPHTS) etc..HPS technologies are extensive
The preparation of metal-base composites is applied to, for example, Lim etc. exists《Wear》Delivered on the 4th 629-637 pages of the phases of volume 255 in 2003
" (magnesium-based SiC particulate increases Wear behaviour of SiCp-reinforced magnesium matrix composites
The abrasional behavior of strong composite) ", with Mg, Al and SiC powder are raw material, after mixed powder homogenization, apply 100bar pressure pair
Mixed powder is colded pressing；The base that will cold pressing is preheated 30 minutes at 350 DEG C, is then inserted vacuum environment and is sintered 4h at 450 DEG C,
And carry out extruding to improve performance at 350 DEG C by sintered specimen.
Meanwhile, SPS technologies can be used for the solidification of ceramic powders, for example, Bernard-Granger and Guizard exist
《Journal of Materials Research》" Densification is delivered on the 1st 179-186 pages of the phases of volume 24 in 2009
mechanism involved during spark plasma sintering of a co-dopedα-alumina
material:(discharge plasma sintering is blended the densification of α-Al2O3 materials to Part I.Formal sintering analysis
Change mechanism：The analysis of part i sintering) " in a text, from α-Al2O3, CaO, and TiO2 blended powders, system sets out, by applying
DC pulse, the curing powder under 1200 DEG C and 50MPa pressure prepares the sub-micron crystal block materials of full densification.
Additionally, used as novel PM technique, HPHTS has been used for the preparation of intermetallic compound.Examined by document
Suo Faxian, Wang etc. exist《Journal of Materials Research》Sent out on the 6th 2089-2096 pages of the phases of volume 24 in 2009
Table " High-pressure and high-temperature sintering of nanostructured bulk NiAl
Materials (the high pressure-temperature sintering of nano block NiAl materials) ", proposes with NiAl nanometer powders as raw material, through at 500 DEG C
Vacuum degassing pretreatment (1h), then 0.5-1h is sintered at 1-5GPa pressure and 600-1500 DEG C, and sintered specimen is quenched
To room temperature.The bulk nanostructured material of full densification can be prepared by HPHTS techniques.
Not yet find to realize that discarded metal chip is circulated and the related work for remanufacturing by the step of PM technique one at present
Make reports.
The conventional art of discarded metal chip circular treatment is remelting+casting.However, high temperature founding to there is energy consumption big, dirty
The low defect of dye weight, efficiency, and cast sturcture's coarse grains, mechanical performance are poor.To avoid high temperature founding, can be burnt using solid phase
Knot mode.But, existing PM technique, process is more, and technique (sintering) cycle is long.In prolonged high-temperature concretion
During, Ti chips will aggravate to aoxidize, and cause to form more serious metallurgical imperfection in microstructure, weaken material property.At present
The technical problem is not yet solved well.Therefore, anxious one kind rapidly solidified forming technique of a step easy to operate yet-to-be developed, with height
The Ti chips of effect circulation smelting cost high.
Therefore, we are necessary to improve such a structure, to overcome drawbacks described above.
The content of the invention
The circulation of discarded metal resource is with to remanufacture be one of the key of realizing sustainable development.Titanium (Ti) is that height is smelted into
This metals resources, its biocompatibility is excellent, corrosion resistance is good, mechanical property is suitable, be manufacture medicine equipment, joint prosthesis,
The important materials of large-scale derived energy chemical container etc..But, in order to manufacture high precision titanium structure, larger allowance need to be designed,
Substantial amounts of raw material translate into discarded chip.Traditional high temperature founding treatment energy consumption is big, pollution weight, and efficiency is low, and casting group
Knit coarse grains, poor-performing.Solid phase is circulated and remanufactured because avoiding high temperature founding, is to realize that metals resources are efficient, clean and follow
One effective way of ring.The purpose of the present invention, is that research and development are a kind of to be directed to Gao Ye based on the rapidly solidified principle of high-density current
The quick re-manufacturing technology of this Ti resources is smelt, full densification, large-sized block Ti materials is prepared, discarded Ti chips are realized
Efficiently, recycling is cleaned.
The present invention is for the solution technical scheme that is used of its technical problem：
The electric discharge quick consolidation method that a kind of titanium chip circulation is remanufactured, comprises the following steps：
Pretreatment is reclaimed in step (1)-Ti cuttings：The chip generated with 2 grades of Ti of end mill (ASTM Grade 2) is as 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
Analysis result is as follows：Initial Ti cuttings (mass percent, wt.%) O=0.15, N ＜ 0.01, C ＜ 0.01, Fe=0.10；By dividing
Analysis result understands that its chemical composition (oxygen content) meets ASTM standard scope through 2 grades of Ti chips of Milling Process；Meanwhile, use
99.9% ethanol cleans Ti chips in ultrasonic activation groove, to remove the greasy dirt in raw material and impurity；
Degassing is dried in step (2)-Ti chips：The Ti chips obtained by step (1) are put into baking oven, are done at a temperature of 60 DEG C
Dry 40min；
The pretreatment of colding pressing of step (3)-Ti chips：The drying Ti chips that will be obtained by step (2) insert what graphite was made
Cylindrical shape cold stamping die (external diameterInternal diameterHeight 50mm), the chip put into mould is colded pressing
(50MPa) is producing pressed compact；
Step (4)-Ti chips cold pressing base high-density current it is rapidly solidified：The Ti chips of colding pressing that will be obtained by step (3)
Pressed compact is put into rapidly solidified process unit together with mould；Mould containing pressed compact is put between the left and right electrode of consolidation device,
Agglomerating chamber is vacuumized into (residual pressure~4Pa), applies the single shaft pressure of 200MPa by the left and right drift of mould by hydraulic system
Power, and apply high density alternating current (350kA/cm2) chip is consolidated, the rate of heat addition is 150 DEG C/s, first by pressed compact
500 DEG C are warming up to, 2min is incubated；Further it is heated to~1000 DEG C, soaking time 6min；It is naturally cold that consolidation finishes rear sample
But.
Further, the rapidly solidified device of electric discharge that the titanium cutting circulation is remanufactured includes tubular graphite jig, described
A cavity is provided with inside graphite jig, thermocouple passes through graphite jig to cavity top, described graphite jig or so two ends to be all provided with
There is moveable graphite drift, electrode is respectively connected with outside the graphite drift at left and right two ends, between the electrode and graphite drift
Billet is folded with, titanium cutting is placed in and pressed compact is formed in cavity.
Further, graphite jig inwall can be lined with graphite paper.
Ti cuttings are cleaned in ultrasonic activation groove using the ethanol of 99.9% concentration, oil removing can be largely gone
Dirty and impurity, simultaneously as the ethanol of 99.9% concentration for using can directly volatilize, it is to avoid greasy dirt magazine remains in Ti tables
The situation in face.
The billet being provided between electrode and graphite drift can improve operating efficiency.
The advantage of the invention is that：
The rapidly solidified reproducing method of Ti chips high-density current proposed by the present invention, it is to avoid high temperature founding, is a kind of
The metals resources recycling technology of low cost and high-efficiency cleaning, it is applied to the smelting cost metal high carried out with Ti as representative
The Recycling and reuse of resource.
The Joule heat that the present invention is produced using high density (350kA/cm2) electric current, and apply uniaxial tension (~200MPa),
The middle integration for realizing consolidation and densification under the coupling in electric field, thermal field and the field of force.With heating rate it is big (~150 DEG C/
S), consolidation pressure is big, and the technical characterstic such as consolidation cycle short (8min).Therefore, the present invention is high with production efficiency, and product is micro-
The advantages of seeing uniform small grains.Using the present invention, the block Ti materials remanufactured by 2 grades of Ti (ASTM Grade 2) chip its bend
Intensity (~420MPa) is taken higher than 2 grades of yield strengths (300-350MPa) of Ti business bars, for high-compactness secondary metal
Efficient, the inexpensive preparation of material has larger value.
Brief description of the drawings
Fig. 1 is the structural representation of the rapidly solidified device of electric discharge that a kind of titanium chip circulation proposed by the present invention is remanufactured.
Fig. 2 is that the present invention uses the initial Ti chips of ICP-AES technical Analysis, and high-density current is rapidly solidified remanufactures
The chemical component table of Ti materials.
Numeral and the corresponding component title represented by letter in figure：
1st, graphite jig 2, cavity 3, thermocouple 4, graphite drift 5, electrode 6, billet
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Diagram and specific embodiment are closed, the present invention is expanded on further.
As shown in figure 1, the electric discharge quick consolidation method that a kind of titanium chip circulation proposed by the present invention is remanufactured, including it is as follows
Step：
Pretreatment is reclaimed in step (1)-Ti cuttings：The chip generated with 2 grades of Ti of end mill (ASTM Grade 2) is as 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
Analysis result is as follows：Initial Ti cuttings (mass percent, wt.%) O=0.15, N ＜ 0.01, C ＜ 0.01, Fe=0.10；By dividing
Analysis result understands that its chemical composition (oxygen content) meets ASTM standard scope through 2 grades of Ti chips of Milling Process；Meanwhile, use
99.9% ethanol cleans Ti chips in ultrasonic activation groove, to remove the greasy dirt in raw material and impurity；
Degassing is dried in step (2)-Ti chips：The Ti chips obtained by step (1) are put into baking oven, are done at a temperature of 60 DEG C
Dry 40min；
The pretreatment of colding pressing of step (3)-Ti chips：The drying Ti chips that will be obtained by step (2) insert what graphite was made
Cylindrical shape cold stamping die (external diameterInternal diameterHeight 50mm), the chip put into mould is colded pressing
(50MPa) is producing pressed compact；
Step (4)-Ti chips cold pressing base high-density current it is rapidly solidified：The Ti chips of colding pressing that will be obtained by step (3)
Pressed compact is put into rapidly solidified process unit together with mould；Mould containing pressed compact is put between the left and right electrode of consolidation device,
Agglomerating chamber is vacuumized into (residual pressure~4Pa), applies the single shaft pressure of 200MPa by the left and right drift of mould by hydraulic system
Power, and apply high density alternating current (350kA/cm2) chip is consolidated, the rate of heat addition is 150 DEG C/s, first by pressed compact
500 DEG C are warming up to, 2min is incubated；Further it is heated to~1000 DEG C, soaking time 6min；It is naturally cold that consolidation finishes rear sample
But.
Further, the rapidly solidified device of electric discharge that the titanium cutting circulation is remanufactured includes tubular graphite jig, described
A cavity is provided with inside graphite jig, thermocouple passes through graphite jig to cavity top, described graphite jig or so two ends to be all provided with
There is moveable graphite drift, electrode is respectively connected with outside the graphite drift at left and right two ends, between the electrode and graphite drift
Billet is folded with, titanium cutting is placed in and pressed compact is formed in cavity.
Further, graphite jig inwall can be lined with graphite paper.
Degassing is dried in step (2) chip：The Ti chips obtained by step (1) are put into baking oven, are dried at a temperature of 60 DEG C
40min.Its object is to：Due to ethanol high volatility, disappeared before drying, so step main purpose is by drying
The vapor of removal chip surface absorption
The chemical composition of sintered specimen is analyzed using ICP-AES, analysis result is as follows：The rapidly solidified Ti materials (quality of electric current
Percentage, wt.%) O=0.16, N ＜ 0.01, C ＜ 0.01, Fe=0 learns the rapidly solidified Ti materials of remanufacturing of high-density current
Oxygen content only rises 0.01wt.% compared with original chip, and nitrogen content is constant.Chemical composition meets 2 grades of Ti (ASTM
Grade 2) ingredient level.By wire cutting~4.00 × 4.00 × 6.00mm samples, and opened on universal testing machine
Exhibition compression experiment, obtains yield strength~420MPa, i.e., Ti materials its intensity for being remanufactured by 2 grades of Ti (ASTM Grade 2) chip
Higher than 2 grades of yield strengths (300-350MPa) of Ti business bars.
The present invention proposes a kind of rapidly solidified technology of high-density current, and treatment is circulated to discarded Ti chips, prepares
Large scale, block body ultrafine grain high intensity Ti materials.In the present invention, by applying high-density current (300kA/cm2) to chip pressure
Base is heated up.Meanwhile, apply uniaxial tension (200MPa) to promote chip to solidify.Rapidly solidified technology proposed by the present invention
One of technical characteristic is the rate of heat addition high, and in the presence of high-density current, its rate of heat addition is up to 150 DEG C/s, far above SPS
The rate of heat addition (4-5 DEG C/s) of technology, another feature is that consolidation is rapid, and (1000 DEG C) total insulation residence time is only at high temperature
It is 8 minutes.By rapidly solidified, suppress the grain coarsening tendency in solidification process, and microscopic void closed under impressed pressure,
Realization remanufactures the full densification of Ti materials.
The rapidly solidified technical scheme of high-density current proposed by the present invention, overcomes above-mentioned limitation, and can realize invention mesh
In the technique effect pointed out.In the present invention, chip pressed compact is risen by applying high-density current (350kA/cm2)
Temperature.Meanwhile, apply uniaxial tension (~200MPa) to promote chip to solidify.The one of rapidly solidified technology proposed by the present invention is to add
Hot speed is high, and in the presence of high-density current, its rate of heat addition is up to 150 DEG C/s, far above the rate of heat addition of SPS technologies
(4-5 DEG C/s), two is rapid consolidation, and (1000 DEG C) total insulation residence time is only 8 minutes at high temperature.By quick solid
Knot, suppresses the grain coarsening tendency in solidification process, and microscopic void is closed under impressed pressure, and realization remanufactures the complete of Ti materials
Densification.Fine grain Ti materials can efficiently be remanufactured out.
General principle of the invention, principal character and advantages of the present invention has been shown and described above.The technology of the industry
Personnel it should be appreciated that the present invention is not limited to the above embodiments, simply explanation described in above-described embodiment and specification this
The principle of invention, various changes and modifications of the present invention are possible 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 appending claims and its
Equivalent is defined.
Claims (3)
1. the electric discharge quick consolidation method that a kind of titanium chip circulation is remanufactured, it is characterised in that comprise the following steps：
Pretreatment is reclaimed in step (1)-Ti cuttings：The chip generated with 2 grades of Ti of end mill (ASTM Grade 2) is searched as raw material
After collection 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, analysis result is such as
Under：Initial Ti cuttings (mass percent, wt.%) O=0.15, N ＜ 0.01, C ＜ 0.01, Fe=0.10；Can by analysis result
Know, through 2 grades of Ti chips of Milling Process, its chemical composition (oxygen content) meets ASTM standard scope；Meanwhile, using 99.9%
Ethanol cleans Ti chips in ultrasonic activation groove, to remove the greasy dirt in raw material and impurity；
Degassing is dried in step (2)-Ti chips：The Ti chips obtained by step (1) are put into baking oven, are dried at a temperature of 60 DEG C
40min；
The pretreatment of colding pressing of step (3)-Ti chips：The cylinder that graphite is made is inserted in the drying Ti chips that will be obtained by step (2)
Shape cold stamping die (external diameterInternal diameterHeight 50mm), the chip put into mould is colded pressing
(50MPa) is producing pressed compact；
Step (4)-Ti chips cold pressing base high-density current it is rapidly solidified：The Ti chip pressed compacts of colding pressing that will be obtained by step (3)
Rapidly solidified process unit is put into together with mould；Mould containing pressed compact is put between the left and right electrode of consolidation device, will be burnt
Knot room vacuumizes (residual pressure~4Pa), applies the uniaxial tension of 200MPa by the left and right drift of mould by hydraulic system, and
Apply high density alternating current (350kA/cm2) to consolidate chip, the rate of heat addition is 150 DEG C/s, and pressed compact heats up first
To 500 DEG C, 2min is incubated；Further it is heated to~1000 DEG C, soaking time 6min；Consolidation finishes rear sample natural cooling.
2. the rapidly solidified device of electric discharge that a kind of titanium chip circulation according to claim 1 is remanufactured, it is characterised in that：Institute
Stating the titanium cutting rapidly solidified device of electric discharge that remanufactures of circulation includes tubular graphite jig, and a chamber is provided with inside the graphite jig
Body, thermocouple passes through graphite jig to cavity top, described graphite jig or so two ends to be equipped with moveable graphite drift, left
Electrode is respectively connected with outside the graphite drift at right two ends, billet is folded between the electrode and graphite drift, titanium cutting is put
In forming pressed compact in cavity.
3. the rapidly solidified device of electric discharge that a kind of titanium chip circulation according to claim 2 is remanufactured, it is characterised in that：Stone
Black mould inner wall can be lined with graphite paper.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611030103.8A CN106825585A (en) | 2016-11-15 | 2016-11-15 | Electric discharge quick consolidation method and device that a kind of titanium chip circulation is remanufactured |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611030103.8A CN106825585A (en) | 2016-11-15 | 2016-11-15 | Electric discharge quick consolidation method and device that a kind of titanium chip circulation is remanufactured |
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Family
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| CN201611030103.8A Pending CN106825585A (en) | 2016-11-15 | 2016-11-15 | Electric discharge quick consolidation method and device that a kind of titanium chip circulation is remanufactured |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110280770A (en) * | 2019-08-12 | 2019-09-27 | 哈尔滨工业大学 | A kind of method of discharge plasma sintering recycling light-alloy processing bit |
| CN112846175A (en) * | 2021-01-08 | 2021-05-28 | 中南大学 | Device and method for realizing high-speed compaction and sintering of powder by utilizing electro-magnetic energy |
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| US5937265A (en) * | 1997-04-24 | 1999-08-10 | Motorola, Inc. | Tooling die insert and rapid method for fabricating same |
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Application publication date: 20170613 |