CN114703433A - Preparation method of biodegradable medical metal magnesium and magnesium alloy plate - Google Patents

Preparation method of biodegradable medical metal magnesium and magnesium alloy plate Download PDF

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CN114703433A
CN114703433A CN202210387663.8A CN202210387663A CN114703433A CN 114703433 A CN114703433 A CN 114703433A CN 202210387663 A CN202210387663 A CN 202210387663A CN 114703433 A CN114703433 A CN 114703433A
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magnesium
heat treatment
plate
treatment furnace
chain
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帅歌国
殷怡婷
崔宏
沈鸣昱
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Changshu Microtube Technology Co ltd
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    • 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
    • C22F1/06Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
    • 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
    • B21C37/00Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/02Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of sheets
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/0081Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
    • 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
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F3/00Brightening metals by chemical means
    • C23F3/02Light metals
    • C23F3/03Light metals with acidic solutions

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Metal Rolling (AREA)

Abstract

The invention discloses a preparation method of a biodegradable medical magnesium metal and magnesium alloy plate, which comprises the following steps: s1: selecting magnesium section bars, wherein the magnesium section bars are pure magnesium and magnesium-zinc alloy, and the zinc content is wt 2-wt 6%; s2: preparing a magnesium plate with a certain thickness, wherein the thickness of the magnesium plate can be less than 40 mm; s3: then, the oxide skin of the magnesium plate is fully removed for standby; s4: setting the running beats of the heat treatment furnace, wherein each beat corresponds to the heat preservation time of the heat treatment furnace; s5: opening a feeding port to place the magnesium plate into a heat treatment conveying device; when the plate is placed on the chain roller of the heat treatment furnace, the chain roller can rotate to convey the magnesium plate to the central part of the chain roller; the device can stabilize the temperature rolling of the magnesium plate without being influenced by external temperature, and simultaneously uses protective gas for quenching treatment at the discharge port of the rolling mill to obtain a fine, uniform and stable structure of crystal grains; automatic production is realized, and the yield is higher.

Description

Preparation method of biodegradable medical metal magnesium and magnesium alloy plate
Technical Field
The invention relates to the technical field of medical consumables, in particular to a preparation method of a biodegradable medical metal magnesium and magnesium alloy plate.
Background
The density of magnesium is 1.74g/cm3, the density of magnesium is only 2/3 of the density of aluminum, and the density of steel is 1/4, so that pure magnesium is widely applied to the fields of automobiles, aerospace, electronic communication, production and living, medical appliances and the like, and is a metal structure magnesium plate with the greatest application prospect in the 21 st century, however, magnesium is in a close-packed hexagonal structure, can only slide along a basal plane at room temperature, and is poor in plasticity at room temperature and not easy to deform. Therefore, the improvement of the mechanical property of pure magnesium is a core problem to be solved urgently at present. Research shows that the grain size has a significant influence on the strength and plasticity of the magnesium metal plate, because the smaller the grains are, the more the grain boundaries are, the stronger the binding force between the metals is, thereby restricting the movement of dislocation, and therefore, the mechanical property of pure magnesium can be improved by means of fine grain strengthening.
At present, the fine grain strengthening of the metal magnesium plate is mainly realized by large plastic deformation, which is a process for preparing block ultra-fine grain magnesium plate by a mechanical method, and the rolling is a process for pulling a rolled piece into rollers with different rotating directions by the friction force between the rolled piece and the rollers to generate plastic deformation, and has the advantages of low requirement on equipment and simple operation, but also has obvious defects: when the magnesium plate is rolled, the magnesium material is taken out from the heat treatment equipment to be sent into a roller, the temperature of the magnesium material is lower than the optimal rolling temperature in the cooling process when rolling occurs, and then the phenomena of cracks, brittle fracture and the like are easy to occur, especially when the external temperature is lower, so that the rolling is unstable according to the change of the external environment and the temperature, and the performance of the magnesium plate is seriously influenced.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide a method for preparing a biodegradable medical magnesium metal and magnesium alloy plate, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of biodegradable medical magnesium metal and magnesium alloy plates comprises the following steps:
s1: selecting magnesium section bars, wherein the magnesium section bars are pure magnesium and magnesium-zinc alloy, and the zinc content is wt 2-wt 6%;
s2: preparing a magnesium plate with a certain thickness, wherein the thickness of the magnesium plate can be less than 40 mm;
s3: then, the oxide skin of the magnesium plate is fully removed for standby;
s4: setting the running beats of the heat treatment furnace, wherein each beat corresponds to the heat preservation time of the heat treatment furnace;
s5: opening a feeding port to place the magnesium plate into a heat treatment conveying device; when the plate is placed on the chain type roller at the feeding port of the heat treatment furnace, the chain type roller at the feeding port is transmitted like a conveyor belt, and the magnesium plate is conveyed to the central part of the chain type roller in the heat treatment furnace from the chain type roller at the feeding port;
s6: the plate placed on the chain roller can be automatically subjected to heat treatment in the heat treatment furnace and is conveyed to a discharge hole of the heat treatment furnace close to the tail part of the chain roller through a feeding hole;
s7: when the plate is conveyed to the discharge port of the heat treatment furnace, the rollers on the chain rollers start rolling, the plate is conveyed out to enter rolling equipment through the chain rollers close to the discharge port of the heat treatment furnace, the rollers need preheating treatment, and the temperature is 250 ℃;
s8: further quenching the plate according to the requirement whether the plate after rolling is sprayed with protective gas or not;
s9: further leveling the rolled magnesium plate, wherein the lower pressure is 5-30MPa, the temperature of a leveling machine is kept at 300 ℃ for 1-10 Min;
s10: further polishing the magnesium plate, wherein the polishing solution is phosphoric acid: ethylene glycol 2: 3, proportioning, and polishing for 1-10 minutes; and after polishing, fully washing in an alcohol solution, and airing for later use.
Preferably, a plurality of chain type rollers are uniformly arranged inside the heat treatment furnace, a feeding port is formed in one side wall of each chain type roller, rolling equipment is installed on the other side wall of the heat treatment furnace, a discharge port of the heat treatment furnace is formed between the rolling equipment and the heat treatment furnace, an air outlet pipe and a discharge port of a rolling mill are respectively formed in the upper side and the lower side of the side wall of the rolling equipment, and a magnesium plate is arranged at the top end of each chain type roller.
The invention has the technical effects and advantages that:
the device can stabilize the temperature rolling of the magnesium plate without being influenced by external temperature, and simultaneously uses protective gas for quenching treatment at the discharge port of the rolling mill to obtain a fine, uniform and stable structure of crystal grains; automatic production is realized, and the yield is high.
Drawings
FIG. 1 is a schematic view of the working structure of the magnesium plate process of the present invention;
FIG. 2 is a schematic view of the structure of the chain roller of the present invention.
In the figure: 1. a heat treatment furnace; 2. a chain drum; 3. a feeding port of the heat treatment furnace; 4. a rolling mill; 5, discharging a material outlet of the heat treatment furnace; 6. an air outlet pipe; 7. a magnesium plate; 8. and (4) discharging a material outlet of the rolling mill.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of biodegradable medical magnesium metal and magnesium alloy plates comprises the following steps:
s1: selecting magnesium section bars, wherein the magnesium section bars are pure magnesium and magnesium-zinc alloy, and the zinc content is wt 2-wt 6%;
s2: preparing a magnesium plate 7 with a certain thickness, wherein the thickness of the magnesium plate 7 can be less than 40 mm;
s3: then the magnesium plate 7 is fully removed of oxide skin for standby;
s4: setting running beats of the heat treatment furnace 1, wherein each beat corresponds to the heat preservation time of the heat treatment furnace 1;
s5: opening the feeding port 3 and placing the magnesium plate 7 into a heat treatment conveying device; when the plate is placed on the chain roller 2 at the feeding port 3 of the heat treatment furnace 1, the chain roller 2 at the feeding port 3 is driven like a conveyor belt, and the magnesium plate 7 is conveyed from the chain roller 2 at the feeding port 3 to the central part of the chain roller 2 in the heat treatment furnace 1;
s6: the plate placed on the chain roller 2 is automatically subjected to heat treatment in the heat treatment furnace 1 and is conveyed to a position close to a discharge port 5 of the heat treatment furnace at the tail part of the chain roller 2 through a feeding port 3;
s7: when the plate is conveyed to the discharge port 5 of the heat treatment furnace, the rollers on the chain rollers 2 start rolling, the plate is conveyed out to enter rolling equipment 4 through the chain rollers 2 close to the discharge port 5 of the heat treatment furnace, the rollers need preheating treatment, and the temperature is 100-250 ℃;
s8: further quenching the plate by spraying protective gas or not after rolling according to the requirement;
s9: further leveling the rolled magnesium plate 7, wherein the lower pressure is 5-30MPa, the temperature of a leveling machine is kept at 300 ℃ for 100 ℃ and the setting time is 1Min-10 Min;
s10: further polishing the magnesium plate 7, wherein the polishing solution is phosphoric acid: ethylene glycol 2: 3, proportioning, and polishing for 1-10 minutes; and after polishing, fully washing in an alcohol solution, and airing for later use.
Further, a plurality of chain type rollers 2 are uniformly arranged inside the heat treatment furnace 1, a feeding port 3 is formed in one side wall of each chain type roller 2, a rolling device 4 is installed on the other side wall of the heat treatment furnace 1, a heat treatment furnace discharge port 5 is formed between the rolling device 4 and the heat treatment furnace 1, an air outlet pipe 6 and a rolling mill discharge port 8 are respectively formed in the upper side and the lower side of the side wall of the rolling device 4, and a magnesium plate 7 is arranged on the top end of each chain type roller 2.
3. The above method gives the following results:
the first embodiment is as follows:
preparing a magnesium metal plate 7 with the magnesium content of 99.98 percent by weight of a pure magnesium metal ingot, the length, the width and the thickness of 120 x 80 x 1mm respectively, setting the takt time according to the plate thickness according to the following table, setting the heat treatment time from a feeding port 3 to a discharge port 5 of a heat treatment furnace to be 60 minutes, setting the temperature of the heat treatment furnace 1 to be 350 ℃, and setting the temperature of a preheating rolling chain type roller to be 200 ℃; the thickness of the rolled magnesium plate is 0.85mm, 0.7mm, 0.58mm, 0.47mm, 0.39mm, 0.36mm, 0.29mm and 0.20mm, when the thickness of the rolled magnesium plate reaches 0.2mm, a protective gas injection device is started at a discharge port 5 of a heat treatment furnace, the plate is subjected to quenching treatment, the rolled magnesium plate 7 is further subjected to leveling treatment, the magnesium plate 7 is further subjected to polishing treatment, and the alcohol solution is cleaned.
In this example, 12 sets of chain drums were used, and the heat treatment time and takt time for each different plate thickness are shown in the following table:
Figure BDA0003594304320000051
example two:
preparing a magnesium metal plate 7 with the magnesium content of 99.98 percent by weight of a pure magnesium metal ingot, the length, the width and the thickness of 150 x 100 x 1mm respectively, setting the takt time according to the following table of the plate thickness, setting the heat treatment time from a feeding port 3 to a discharge port 5 of a heat treatment furnace to be 120 minutes, setting the temperature of the heat treatment furnace 1 to be 320 ℃, and setting the temperature of a preheating rolling chain type roller to be 150 ℃; the thickness of the rolled magnesium plate is 0.85mm, 0.7mm, 0.58mm, 0.47mm, 0.39mm, 0.36mm, 0.29mm, 0.20mm, 0.15mm and 0.1mm, when the thickness of the rolled magnesium plate reaches 0.1mm, a protective gas injection device is started at a discharge port 5 of the heat treatment furnace, the plate is subjected to quenching treatment, the rolled magnesium plate 7 is further subjected to leveling treatment, the magnesium plate 7 is further subjected to polishing treatment, and the magnesium plate is cleaned by alcohol solution.
In this example, 12 sets of chain drums were used, and the heat treatment time and takt time for each different plate thickness are shown in the following table:
Figure BDA0003594304320000061
example three:
preparing a magnesium-zinc alloy ingot with the zinc content of 2 wt%, preparing a magnesium metal plate 7 with the length, width and thickness of 150 x 100 x 1mm respectively, setting the takt time according to the following table according to the plate thickness, setting the heat treatment time from a feeding port 3 to a discharge port 5 of a heat treatment furnace to be 90 minutes, setting the temperature of the heat treatment furnace 1 to be 380 ℃, and setting the temperature of a preheating rolling chain type roller to be 180 ℃; the thickness of the rolled magnesium plate is 0.85mm, 0.7mm, 0.58mm, 0.47mm, 0.39mm, 0.36mm, 0.29mm, 0.20mm, 0.15mm and 0.1mm, when the thickness of the rolled magnesium plate reaches 0.1mm, a protective gas injection device is started at a discharge port 5 of the heat treatment furnace, the plate is subjected to quenching treatment, the rolled magnesium plate 7 is further subjected to leveling treatment, the magnesium plate 7 is further subjected to polishing treatment, and the magnesium plate is cleaned by alcohol solution.
In this example, 12 sets of chain drums were used, and the heat treatment time and takt time for each different plate thickness are shown in the following table:
Figure BDA0003594304320000071
example four:
preparing a magnesium plate 7 with the length, width and thickness of 150 x 100 x 1mm, setting the takt time according to the plate thickness, setting the heat treatment time from a feeding port 3 to a discharge port 5 of a heat treatment furnace to be 120 minutes, setting the temperature of the heat treatment furnace 1 to be 400 ℃, and setting the temperature of a preheating rolling chain type roller to be 200 ℃; further, the thicknesses of the rolled steel sheets are respectively set to be 0.85mm, 0.7mm, 0.58mm, 0.47mm, 0.39mm, 0.36mm, 0.29mm, 0.20mm, 0.15mm, 0.1mm, 0.08mm and 0.06 mm; when the thickness of the sheet reaches 0.06mm, a protective gas injection device is started at a discharge port 5 of the heat treatment furnace to perform a rapid cooling treatment on the sheet, further perform a leveling treatment on the rolled magnesium plate 7, further perform a polishing treatment on the magnesium plate 7, and clean the magnesium plate with an alcohol solution.
In this example, 12 sets of chain drums were used, and the heat treatment time and takt time for each different plate thickness are shown in the following table:
Figure BDA0003594304320000081
and finally: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (2)

1. A preparation method of biodegradable medical magnesium metal and magnesium alloy plates is characterized by comprising the following steps: the preparation method comprises the following steps:
s1: selecting magnesium section bars, wherein the magnesium section bars are pure magnesium and magnesium-zinc alloy, and the zinc content is wt 2-wt 6%;
s2: preparing a magnesium plate (7) with a certain thickness, wherein the thickness of the magnesium plate (7) can be less than 40 mm;
s3: then, the magnesium plate (7) is fully removed of oxide skin for standby;
s4: setting the running beats of the heat treatment furnace (1), wherein each beat corresponds to the heat preservation time of the heat treatment furnace (1);
s5: opening the feeding port (3) and placing the magnesium plate (7) into a heat treatment conveying device; when the plate is placed on the chain type roller (2) at the feeding port (3) of the heat treatment furnace (1), the chain type roller (2) at the feeding port (3) is driven like a conveyor belt, and the magnesium plate (7) is conveyed to the central position of the chain type roller (2) in the heat treatment furnace (1) from the chain type roller (2) at the feeding port (3);
s6, the plate placed on the chain roller (2) is automatically subjected to heat treatment in the heat treatment furnace (1) and is conveyed to the position of a discharge hole (5) of the heat treatment furnace close to the tail part of the chain roller (2) through a feeding hole (3);
s7: when the plate is conveyed to the discharge port (5) of the heat treatment furnace, the rollers on the chain rollers (2) start rolling, the plate is conveyed out to enter rolling equipment (4) through the chain rollers (2) close to the discharge port (5) of the heat treatment furnace, the rollers need preheating treatment, and the temperature is 100-250 ℃;
s8: further quenching the plate by spraying protective gas or not after rolling according to the requirement;
s9: further leveling the rolled magnesium plate (7), wherein the lower pressure is 5-30MPa, the temperature of a leveling machine is kept at 300 ℃ and 100 ℃, and the setting time is 1-10 Min;
s10: further polishing the magnesium plate (7), wherein the polishing solution is phosphoric acid: ethylene glycol 2: 3, proportioning, and polishing for 1-10 minutes; and after polishing, fully washing in an alcohol solution, and airing for later use.
2. The method for preparing biodegradable medical metal magnesium and magnesium alloy sheet material according to claim, characterized in that: the inside of heat treatment furnace (1) is even is provided with a plurality of chain formula cylinders (2), a lateral wall of chain formula cylinder (2) is provided with pay-off mouth (3), rolling equipment (4) are installed to another lateral wall of heat treatment furnace (1), and are provided with heat treatment furnace discharge gate (5) between rolling equipment (4) and heat treatment furnace (1), both sides are provided with tuber pipe (6) and rolling mill discharge gate (8) respectively about the lateral wall of rolling equipment (4), the top of chain formula cylinder (2) is provided with magnesium board (7).
CN202210387663.8A 2022-04-13 2022-04-13 Preparation method of biodegradable medical metal magnesium and magnesium alloy plate Pending CN114703433A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0889139A1 (en) * 1997-06-06 1999-01-07 Peter Helmut Dipl.-Ing. Ebner Device for flushing cold drawn coiled pipes in a roller-hearth furnace
CN101591799A (en) * 2008-05-30 2009-12-02 比亚迪股份有限公司 A kind of electrolytic polishing liquid of magnesium alloy and surface finish treatment process thereof
JP2013129914A (en) * 2011-11-22 2013-07-04 National Institute Of Advanced Industrial Science & Technology Method for producing magnesium alloy sheet material, magnesium alloy sheet material, and press molding using the same
CN105149352A (en) * 2015-09-30 2015-12-16 中镁镁业有限公司 Online temperature supplementing, constant-temperature rolling and coiling method for wrought magnesium alloy sheet strips
CN108603076A (en) * 2016-02-16 2018-09-28 3M创新有限公司 Polishing system and preparation and the method for using polishing system

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0889139A1 (en) * 1997-06-06 1999-01-07 Peter Helmut Dipl.-Ing. Ebner Device for flushing cold drawn coiled pipes in a roller-hearth furnace
CN101591799A (en) * 2008-05-30 2009-12-02 比亚迪股份有限公司 A kind of electrolytic polishing liquid of magnesium alloy and surface finish treatment process thereof
JP2013129914A (en) * 2011-11-22 2013-07-04 National Institute Of Advanced Industrial Science & Technology Method for producing magnesium alloy sheet material, magnesium alloy sheet material, and press molding using the same
CN105149352A (en) * 2015-09-30 2015-12-16 中镁镁业有限公司 Online temperature supplementing, constant-temperature rolling and coiling method for wrought magnesium alloy sheet strips
CN108603076A (en) * 2016-02-16 2018-09-28 3M创新有限公司 Polishing system and preparation and the method for using polishing system

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