CN107937782B - A kind of preparation method of gradient Mg-Zn alloy bar - Google Patents

A kind of preparation method of gradient Mg-Zn alloy bar Download PDF

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Publication number
CN107937782B
CN107937782B CN201711185027.2A CN201711185027A CN107937782B CN 107937782 B CN107937782 B CN 107937782B CN 201711185027 A CN201711185027 A CN 201711185027A CN 107937782 B CN107937782 B CN 107937782B
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powder
tube
materials
outer diameter
gradient
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CN107937782A (en
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周小平
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Hubei University of Technology
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Hubei University of Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/04Alloys based on magnesium with zinc or cadmium as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0408Light metal alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/047Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a kind of preparation methods of gradient Mg-Zn alloy bar, and the Mg-Zn mixed-powder that mass ratio is Mg:Zn=95:5 is pressed intoBar;The Mg-Zn mixed-powder that mass ratio is Mg:Zn=90:10, which is pressed into outer diameter, isInternal diameter isMaterials in the tube;The Mg-Zn mixed-powder that mass ratio is Mg:Zn=80:20, which is pressed into outer diameter, isInternal diameter isMaterials in the tube;Bar and materials in the tube are assembled, internal layer isBar, middle layer is that outer diameter isInternal diameter isMaterials in the tube, outer layer is that outer diameter isInternal diameter isMaterials in the tube, after assembling be packed into internal diameter beSteel barrel in be sintered together, then apply vertical pressure to barrel one end, the other end is with outer diameterRotary press head carry out rotary squeezing, the rubbing action of rotary press head and storeroom makes the material of contact area in molten condition, and under the action of pressure at right angle, the material of melting is overflowed and solidified from the through-hole among rotary press head to get to gradient Mg-Zn alloy bar.

Description

A kind of preparation method of gradient Mg-Zn alloy bar
Technical field
The present invention relates to a kind of preparation methods of gradient Mg-Zn alloy bar, belong to field of material engineering technology.
Background technique
Mg-Zn alloy can be used as bio-medical material use, and the speed of initial phase degradation is wished in human body fluid environment Slowly, final stage can properly increase its degradation speed, and the material of ingredient of the same race is unable to satisfy this requirement.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of gradient Mg-Zn alloy bar.Using method of the invention, system Standby Mg-Zn alloy bar is gradually decreased from surface to the content of center portion Zn, and degradation speed can step up.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of gradient Mg-Zn alloy bar, comprising the following steps:
(1) Mg powder that mass ratio is respectively Mg:Zn=95:5, Mg:Zn=90:10 and Mg:Zn=80:20, Zn powder are mixed It closes uniformly, obtains the Mg-Zn mixed-powder of three kinds of different quality ratios;
(2) the Mg-Zn mixed-powder that mass ratio in step (1) is Mg:Zn=95:5 is packed into mold, is pressed on press machine It is madeBar;The Mg-Zn mixed-powder that mass ratio is Mg:Zn=90:10 is packed into mold, is pressed on press machine Outer diameter isInternal diameter isMaterials in the tube;The Mg-Zn mixed-powder that mass ratio is Mg:Zn=80:20 is packed into mold, is being pressed Being pressed into outer diameter on power machine isInternal diameter isMaterials in the tube;
(3) bar through step (2) compression moulding and materials in the tube are assembled, internal layer is that outer diameter isBar, middle layer is Outer diameter isInternal diameter isMaterials in the tube, outer layer is that outer diameter isInternal diameter isMaterials in the tube, after assembling be packed into internal diameter be Steel barrel in;
(4) it will be put into togerther in sintering furnace and be sintered through step (3) barrel and materials in the tube, bar, sintering temperature 660-750 ℃;
(5) after step (4) sintering, apply vertical pressure to barrel one end, the other end is with outer diameterRotation pressure Head carries out rotary squeezing, and the rotary press head is equipped with through-hole along central axis direction, and the rubbing action of rotary press head and storeroom makes The material of contact area is in molten condition, and under the action of pressure at right angle, the material of melting is from the through-hole among rotary press head It overflows and solidifies to get gradient Mg-Zn alloy bar is arrived.
In the step (1), Mg powder, Zn powder granularity be 20 μm~50 μm.
The quality of three kinds of pressed powders in the step (2) is equal, A be 10~50mm, B be 14~71mm, C be 17~ 87mm;Press machine press power is 100MPa-600MPa.
The material of barrel is 1Cr18Ni9Ti in the step (3), and the wall thickness of barrel is 20mm.
Sintering furnace is vacuum sintering furnace or gas-protecting sintering furnace in the step (4).
In the step (5), through-hole diameter is 5~30mm, and the revolving speed of rotary press head is 500~1000r/min, squeezes speed Degree is 10~20mm/min.
Technical principle of the invention is specific as follows:
(1) during the sintering process, Zn fusing and Mg react to form MgZn intermetallic after sintering temperature reaches 420 DEG C Object, sintering temperature remaining Mg fusing after reaching 650 DEG C, part Zn, which dissolves in Mg, forms solid solution Mg (Zn).The content of Zn is got over The MgZn intermetallic compound of height, generation is more.
(2) in process, the rubbing action of rotary press head and storeroom makes the material of contact area be in molten condition, Center portion Zn content is low, and MgZn intermetallic compound is few, melts first;Middle layer is taken second place;Between outermost layer Zn content height, MgZn metal Compound finally reaches molten condition.Under the action of pressure at right angle, the material of melting overflows from the through-hole among rotary press head It out and solidifies, the Mg-Zn alloy bar finally obtained is gradually decreased from surface to the content of center portion Zn.
(3) content of superficial layer Zn is higher, and MgZn intermetallic compound is more, and the degradation speed in human body fluid reduces. As the reduction of Zn content, MgZn intermetallic compound are reduced from surface to center portion, the degradation speed in human body fluid increases, and reaches The effect fast after first slow to degradation speed.
Detailed description of the invention
Fig. 1 is gradient Mg-Zn alloy bar machining sketch chart;Wherein, 1- barrel, 2- outer diameter areInternal diameter isPipe Material, 3- outer diameter areBar, 4- outer diameter isInternal diameter isMaterials in the tube, 5- diameter isRotary press head.
Specific embodiment
Technical solution of the present invention is further described below by way of specific embodiment, but protection of the invention Range is not limited to these examples.It is all that guarantor of the invention is included in without departing substantially from the change of present inventive concept or equivalent substitute Within the scope of shield.
Embodiment 1: the preparation of gradient Mg-Zn alloy bar
(1) Mg powder, Zn powder that mass ratio is Mg:Zn=95:5, Mg:Zn=90:10 and Mg:Zn=80:20 are mixed respectively It closes uniformly, obtains the Mg-Zn mixed-powder of three kinds of different proportions;Wherein, Mg powder, Zn powder granularity be 20 μm~50 μm.
It (2) is the mixed of Mg:Zn=95:5 by mass ratio in step (1) under conditions of press machine press power is 100MPa Powder is closed to be pressed intoBar, the mixed-powder that mass ratio is Mg:Zn=90:10 is pressed into outer diameter and is Internal diameter isMaterials in the tube, the mixed-powder that mass ratio is Mg:Zn=80:20 is pressed into outer diameter and isInternal diameter is Materials in the tube.
(3) bar through step (2) compression moulding and materials in the tube are assembled, internal layer isBar, middle layer is outer Diameter isInternal diameter isMaterials in the tube, outer layer is that outer diameter isInternal diameter isMaterials in the tube, assembling Being packed into internal diameter afterwards isBarrel in, the material of barrel is 1Cr18Ni9Ti, and the wall thickness of barrel is 20mm.
(4) it will be put into togerther in vacuum sintering furnace and be sintered through step (3) barrel and material, sintering temperature is 660 DEG C.
(5) after step (4) sintering, apply vertical pressure to barrel one end, the other end is with outer diameter's Rotary press head carries out rotary squeezing, and under the action of pressure at right angle, the material of melting is overflowed from the through-hole among rotary press head And it solidifies to get gradient Mg-Zn alloy bar is arrived;The intermediate bore dia of rotary press head is 5mm, and the revolving speed of rotary press head is 500r/ Min, extrusion speed 10mm/min.
Embodiment 2: the preparation method of gradient Mg-Zn alloy bar
Unlike the first embodiment:
(1) mixed-powder that mass ratio is Mg:Zn=95:5 is pressed intoBar;Mass ratio is Mg:Zn= The mixed-powder of 90:10 is pressed into outer diameterInternal diameter isMaterials in the tube;Mass ratio is Mg:Zn=80:20 Mixed-powder be pressed into outer diameter and beInternal diameter isMaterials in the tube.
(2) press machine press power is 300MPa.
(3) bar of compression moulding and materials in the tube assembling, internal layer areBar, middle layer is that outer diameter isInternal diameter isMaterials in the tube, outer layer is that outer diameter isInternal diameter isMaterials in the tube, filled after assembling Entering internal diameter isBarrel in.
(4) it is sintered in gas-protecting sintering furnace, sintering temperature is 700 DEG C.
(5) outer diameter of rotary press head isThe intermediate bore dia of rotary press head is 20mm, the revolving speed of rotary press head For 700r/min, extrusion speed 15mm/min.
The synthetic method of embodiment 3:Mg (Zn)-MgSb intermetallic compound structure material
Unlike the first embodiment:
(1) mixed-powder that mass ratio is Mg:Zn=95:5 is pressed intoBar;Mass ratio is Mg:Zn= The Mg-Zn mixed-powder of 90:10 is pressed into outer diameter and isInternal diameter isMaterials in the tube;Mass ratio is Mg:Zn= The mixed-powder of 80:20 is pressed into outer diameterInternal diameter isMaterials in the tube.
(2) press machine press power is 600MPa.
(3) bar of compression moulding and materials in the tube assembling, internal layer areBar, middle layer is that outer diameter isInternal diameter isMaterials in the tube, outer layer is that outer diameter isInternal diameter isMaterials in the tube, be packed into after assembling Internal diameter isBarrel in.
(4) it is sintered in gas-protecting sintering furnace, sintering temperature is 750 DEG C.
(5) outer diameter of rotary press head isThe intermediate bore dia of rotary press head is 30mm, the revolving speed of rotary press head For 1000r/min, extrusion speed 20mm/min.

Claims (6)

1. a kind of preparation method of gradient Mg-Zn alloy bar, which comprises the following steps:
(1) Mg powder, Zn powder that mass ratio is respectively Mg:Zn=95:5, Mg:Zn=90:10 and Mg:Zn=80:20 are mixed equal It is even, obtain the Mg-Zn mixed-powder of three kinds of different quality ratios;
(2) the Mg-Zn mixed-powder that mass ratio in step (1) is Mg:Zn=95:5 is packed into mold, is pressed on press machineBar;The Mg-Zn mixed-powder that mass ratio is Mg:Zn=90:10 is packed into mold, outer diameter is pressed on press machine ForInternal diameter isMaterials in the tube;The Mg-Zn mixed-powder that mass ratio is Mg:Zn=80:20 is packed into mold, in press machine On be pressed into outer diameter and beInternal diameter isMaterials in the tube;
(3) bar through step (2) compression moulding and materials in the tube are assembled, internal layer is that outer diameter isBar, middle layer is outer diameter ForInternal diameter isMaterials in the tube, outer layer is that outer diameter isInternal diameter isMaterials in the tube, after assembling be packed into internal diameter beSteel In barrel processed;
(4) it will be put into togerther in sintering furnace and be sintered through step (3) barrel and materials in the tube, bar, sintering temperature is 660-750 DEG C;
(5) after step (4) sintering, apply vertical pressure to barrel one end, the other end is with outer diameterRotary press head into Row rotary squeezing, the rotary press head are equipped with through-hole along central axis direction, and the rubbing action of rotary press head and storeroom makes to contact The material in region is in molten condition, and under the action of pressure at right angle, the material of melting is overflowed from the through-hole among rotary press head And it solidifies to get gradient Mg-Zn alloy bar is arrived.
2. the preparation method of gradient Mg-Zn alloy bar according to claim 1, it is characterised in that: in the step (1), Mg powder, Zn powder granularity be 20 μm~50 μm.
3. the preparation method of gradient Mg-Zn alloy bar according to claim 1, it is characterised in that: in the step (2) The quality of three kinds of pressed powders is equal, and A is 10~50mm, and B is 14~71mm, and C is 17~87mm;Press machine press power is 100MPa-600MPa。
4. the preparation method of gradient Mg-Zn alloy bar according to claim 1, it is characterised in that: material in the step (3) The material of cylinder is 1Cr18Ni9Ti, and the wall thickness of barrel is 20mm.
5. the preparation method of gradient Mg-Zn alloy bar according to claim 1, it is characterised in that: burnt in the step (4) Freezing of a furnace is vacuum sintering furnace or gas-protecting sintering furnace.
6. the preparation method of gradient Mg-Zn alloy bar according to claim 1, it is characterised in that: in the step (5), Through-hole diameter is 5~30mm, and the revolving speed of rotary press head is 500~1000r/min, and extrusion speed is 10~20mm/min.
CN201711185027.2A 2017-11-23 2017-11-23 A kind of preparation method of gradient Mg-Zn alloy bar Expired - Fee Related CN107937782B (en)

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CN109998660B (en) * 2019-04-09 2023-12-19 南通罗伯特医疗科技有限公司 Degradable magnesium-zinc alloy bone fracture plate and additive manufacturing device and method thereof

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CN102093148A (en) * 2010-12-06 2011-06-15 西北有色金属研究院 Palladium-ruthenium/aluminum-magnesium composite metal wire and preparation method thereof
CN103085395A (en) * 2012-12-25 2013-05-08 湖北工业大学 Cu-Ti2 AlC functionally gradient material and preparation method thereof
CN104308353A (en) * 2014-08-21 2015-01-28 中国科学技术大学 Surface roughened bar explosive pressing fit method
CN105385986A (en) * 2015-11-10 2016-03-09 中南大学 Tungsten-based heavy alloy bar with gradient-changing hardness and producing method thereof
CN106885054A (en) * 2017-03-03 2017-06-23 苏州创浩新材料科技有限公司 A kind of titanium copper steel three-layer metal composite fin tubing and its preparation technology
CN107385251A (en) * 2017-08-03 2017-11-24 太原理工大学 A kind of preparation method of zinc-magnesium functionally gradient Biocomposite material

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WO2006110667A2 (en) * 2005-04-11 2006-10-19 Intematix Corporation Biased target ion beam deposition (btibd) for the production of combinatorial materials libraries

Patent Citations (7)

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Publication number Priority date Publication date Assignee Title
CN1360980A (en) * 2000-12-28 2002-07-31 北京有色金属研究总院 Extrusion process of bimetallic composite material
CN102093148A (en) * 2010-12-06 2011-06-15 西北有色金属研究院 Palladium-ruthenium/aluminum-magnesium composite metal wire and preparation method thereof
CN103085395A (en) * 2012-12-25 2013-05-08 湖北工业大学 Cu-Ti2 AlC functionally gradient material and preparation method thereof
CN104308353A (en) * 2014-08-21 2015-01-28 中国科学技术大学 Surface roughened bar explosive pressing fit method
CN105385986A (en) * 2015-11-10 2016-03-09 中南大学 Tungsten-based heavy alloy bar with gradient-changing hardness and producing method thereof
CN106885054A (en) * 2017-03-03 2017-06-23 苏州创浩新材料科技有限公司 A kind of titanium copper steel three-layer metal composite fin tubing and its preparation technology
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