CN112899514A - Preparation method of biological foam magnesium alloy - Google Patents
Preparation method of biological foam magnesium alloy Download PDFInfo
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- CN112899514A CN112899514A CN202110100837.3A CN202110100837A CN112899514A CN 112899514 A CN112899514 A CN 112899514A CN 202110100837 A CN202110100837 A CN 202110100837A CN 112899514 A CN112899514 A CN 112899514A
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- magnesium alloy
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 63
- 239000006260 foam Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 94
- 239000000843 powder Substances 0.000 claims abstract description 90
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 47
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims abstract description 44
- 239000011667 zinc carbonate Substances 0.000 claims abstract description 44
- 235000004416 zinc carbonate Nutrition 0.000 claims abstract description 44
- 229910000010 zinc carbonate Inorganic materials 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 9
- 239000011777 magnesium Substances 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 31
- 239000002245 particle Substances 0.000 claims description 20
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000008188 pellet Substances 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 238000004898 kneading Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 14
- 239000011148 porous material Substances 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000004088 foaming agent Substances 0.000 abstract description 5
- 239000012620 biological material Substances 0.000 abstract description 4
- 238000003723 Smelting Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 abstract description 2
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 abstract description 2
- 239000011258 core-shell material Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 229910052725 zinc Inorganic materials 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 10
- 238000001125 extrusion Methods 0.000 description 6
- 238000002791 soaking Methods 0.000 description 6
- 230000035882 stress Effects 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- 238000005187 foaming Methods 0.000 description 4
- 239000010425 asbestos Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052895 riebeckite Inorganic materials 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 229940099259 vaseline Drugs 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011833 salt mixture Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/08—Alloys with open or closed pores
-
- 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
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
-
- 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
- B22F3/16—Both compacting and sintering in successive or repeated steps
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Materials For Medical Uses (AREA)
Abstract
The invention discloses a preparation method of a biological foam magnesium alloy, belonging to the technical field of foam alloy manufacture and comprising the following steps: drying magnesium alloy powder, zinc carbonate and calcium carbonate spherulites, mixing, cold pressing and sintering to obtain the foam magnesium alloy; the foaming agent adopts the spherulites with the core-shell structure formed by zinc carbonate, calcium carbonate coarse powder and fine powder, which not only solves the problem of uneven hole distribution, but also solves the problem of corrosivity caused by excessive use of calcium carbonate; the preparation method can obtain the foam magnesium alloy with uniform pores, has proper porosity and uniform pore size distribution; sintering by using a powder metallurgy method avoids the difficulty of smelting and is suitable for large-scale industrial production; the foam magnesium alloy prepared by the invention contains Mg, Zn and Ca which are beneficial to human bodies, and the obtained material has excellent performance, meets the application requirements of biological materials, and is a biological foam magnesium alloy with good application prospect.
Description
Technical Field
The invention belongs to the technical field of foam alloy manufacturing, and particularly relates to a preparation method of a biological foam magnesium alloy.
Background
The porous foam magnesium alloy is a novel structural functional material developed in recent years, has a series of unique mechanical, thermal, electrical and acoustic properties due to small density and large specific strength, can be widely applied to the building, ship, aviation and automobile manufacturing industries and packaging industries, and has attracted great interest in academic and industrial fields, such as functional structural materials for buildings, filling materials for automobile shock-proof boxes and doors, valuable instrument packaging materials, safety protection materials for lifting mechanisms, aircraft sandwich materials, sound-insulation and noise-reduction materials, electromagnetic shielding materials and the like. Particularly, with the improvement of the living standard of people and the aggravation of the aging of population at present, the requirement on the degradable biological material is higher and higher. Since the foam magnesium alloy gold has similar density and elastic modulus with human bone, good biocompatibility, and the advantages of biodegradation and drug portability, the research on the biological foam magnesium alloy is urgent.
At present, the method for preparing the porous foam magnesium alloy mainly comprises the following steps: one is a melt foaming method, namely, a foaming agent is added into a magnesium alloy melt, and the foaming agent is decomposed at a certain temperature to form holes, so that a closed-cell material is mainly prepared; the method for preparing magnesium alloy by directly foaming melt as disclosed in CN1966748 and the method for preparing foamed magnesium by foaming melt as disclosed in CN101135015 belong to the melt foaming method. However, the method has the defects of difficult control of foam pores, complex process of the casting process of the smelting liquid and higher cost. Another type is open-celled materials obtained by infiltration casting, i.e. infiltration of a metal melt into a preform. For example, a method for preparing foam magnesium alloy disclosed in CN101220424 and a preparation process of foam magnesium disclosed in CN 1544671. The method has the advantages of easy occurrence of explosion danger in the manufacturing process, higher cost, large operation difficulty, more product defects such as insufficient seepage, seepage flow passing and the like. Finally, a powder sintering method is a new process for preparing foam magnesium, and the method is characterized in that a pore-forming agent is added into magnesium alloy powder, and the magnesium alloy powder is mixed, then cold-pressed and sintered, and finally the pore-forming agent is heated, decomposed or dissolved subsequently. For example, CN103862051A discloses a method for preparing foamed magnesium for use in a cushioning energy-absorbing material. However, in the sintering process, the prepared porous foam magnesium alloy cannot be used for biological materials due to the complex thermal decomposition product of urea and difficult temperature control.
Therefore, various problems exist in the preparation of the biological foam magnesium alloy, and the development of a novel pore-forming agent and a corresponding preparation method are urgently needed, so that the defects existing in the preparation process of the existing foam magnesium alloy are overcome, and the biological foam magnesium alloy with uniform pore distribution, controllable pore size and good comprehensive performance is obtained.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a biological foam magnesium alloy.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a biological foam magnesium alloy comprises the following steps:
and drying the zinc carbonate, the calcium carbonate spherulites and the magnesium alloy powder, mixing, cold pressing and sintering to obtain the foam magnesium alloy.
Further, the magnesium content of the magnesium alloy powder is more than or equal to 75 wt%.
Further, the particle size of the magnesium alloy powder is more than or equal to 80 meshes.
Further, the zinc carbonate and calcium carbonate spherulites take zinc carbonate coarse powder and calcium carbonate coarse powder as cores and zinc carbonate fine powder and calcium carbonate fine powder as shells;
the particle sizes of the zinc carbonate coarse powder and the calcium carbonate coarse powder are both larger than 100 meshes and smaller than 140 meshes; the granularity of the zinc carbonate fine powder and the calcium carbonate fine powder is more than or equal to 140 meshes.
Further, the preparation method of the zinc carbonate and calcium carbonate spherulites comprises the following steps: mixing zinc carbonate coarse powder and calcium carbonate coarse powder to obtain a mixture A; mixing the zinc carbonate fine powder and the calcium carbonate fine powder to obtain a mixture B; kneading 62-80 wt% of the mixture A and 20-38 wt% of a polyvinyl alcohol aqueous solution, and extruding by using an extruder to obtain particles; the granules were then placed in mixture B and rolled to give pellets.
Further, the concentration of the polyvinyl alcohol aqueous solution was 5 wt%.
Furthermore, the particle sizes of the zinc carbonate pellets and the calcium carbonate pellets are both 1-3 mm.
Furthermore, the mass ratio of the zinc carbonate and calcium carbonate spherulites to the magnesium alloy powder is 1: 8-10, and the mass ratio of the zinc carbonate and the calcium carbonate in the zinc carbonate and calcium carbonate spherulites is 3-5: 1.
By adopting a series of magnesium salt mixtures with different particle sizes and volume ratios, the spatial distribution of holes and porosity can be regulated and controlled, and the biological foam material with uniformly distributed holes and uniform density is manufactured; the porosity can be precisely controlled by adjusting the volume ratio of the magnesium alloy powder to the foaming agent.
Further, the cold pressing is carried out at room temperature, the pressure is 40MPa, and the pressure maintaining time is 3-4 min.
Further, the sintering is carried out in a closed environment, the sintering temperature is 450-530 ℃, and the sintering time is 25-35 min.
Compared with the prior art, the invention has the following beneficial effects:
(1) the magnesium alloy powder, the zinc carbonate and the calcium carbonate spherulites are dried before cold pressing, so that the oxidation in the processing process is reduced; the sintering by using the powder metallurgy method avoids the difficulty of smelting, simplifies the production process, reduces the production cost and is suitable for large-scale industrial production.
(2) The foaming agent adopts spherulite zinc carbonate and calcium carbonate with a core-shell structure formed by coarse powder and fine powder, so that the problem of uneven hole distribution is solved, and the problem of corrosivity caused by excessive use of calcium carbonate is also solved.
(3) The preparation method can obtain the foam magnesium alloy with uniform holes, has proper porosity, uniform pore size distribution, consistent hole wall thickness, excellent performance and good application prospect.
(4) The foam magnesium alloy prepared by the invention contains Mg, Zn and Ca which are beneficial to human bodies, and the obtained material has excellent performance, meets the application requirements of biological materials, and is a biological foam magnesium alloy with good application prospect.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
In the following examples, the magnesium content of the magnesium alloy powder used was 85 wt%;
the granularity of the used zinc carbonate coarse powder and calcium carbonate coarse powder is larger than 100 meshes and smaller than 140 meshes; the granularity of the used zinc carbonate fine powder and calcium carbonate fine powder is more than or equal to 140 meshes;
the coarse powder with the granularity of more than 100 meshes and less than 140 meshes is salt powder which can pass through a 100-mesh Taylor standard sieve and can not pass through a 140-mesh Taylor standard sieve and is remained in the 140-mesh Taylor standard sieve; the fine powder with the granularity of more than or equal to 140 meshes is salt powder passing through a Taylor standard sieve with 140 meshes;
the description will not be repeated below.
Example 1
The preparation of the biological foam magnesium alloy comprises the following steps:
(1) uniformly mixing zinc carbonate coarse powder and calcium carbonate coarse powder in a mass ratio of 3: 1 to obtain a mixture A; uniformly mixing zinc carbonate fine powder and calcium carbonate fine powder in a mass ratio of 3: 1 to obtain a mixture B; putting a 62 wt% mixture A and a 38 wt% polyvinyl alcohol aqueous solution into a kneader for kneading, wherein the concentration of the polyvinyl alcohol aqueous solution is 5 wt%, putting the kneaded mixture C into a plastic container for standing for 24 hours, putting the mixture C into an extruder for extruding at room temperature, the extruding speed is 0.3m/min, obtaining particles with the particle size of about 1mm, directly putting the particles obtained by extruding into a mixture B, rolling the particles into round balls with the diameter of 1-3 mm, and drying the round balls for 20min at 100 ℃;
(2) respectively placing 100 meshes of magnesium alloy powder and the balls obtained in the step (1) in a drying oven at 120 ℃, drying for 10min, weighing the magnesium alloy powder and the balls according to the mass ratio of the balls to the magnesium alloy powder of 1: 9, and uniformly mixing;
fully and uniformly mixing the magnesium alloy powder and the round balls in the powder mixing stage;
(3) placing the mixture obtained in the step (2) on a 50-ton press, cold pressing at room temperature, using vaseline as a lubricant during extrusion, wherein the extrusion speed is 1mm/s, the pressure is 40MPa, and keeping the pressure for 3 min;
(4) and (4) placing the precast block obtained by cold pressing in the step (3) in a closed stainless steel container, filling and compacting with an asbestos mesh, sintering at the temperature of 450 ℃ for 30min, and then cooling along with a furnace to obtain the biological foam magnesium alloy.
Example 2
Preparing a biological foam magnesium alloy:
(1) uniformly mixing zinc carbonate coarse powder and calcium carbonate coarse powder in a mass ratio of 4: 1 to obtain a mixture A; uniformly mixing zinc carbonate fine powder and calcium carbonate fine powder in a mass ratio of 4: 1 to obtain a mixture B; putting 80 wt% of mixture A and 20 wt% of polyvinyl alcohol aqueous solution into a kneader for kneading, wherein the concentration of the polyvinyl alcohol aqueous solution is 5 wt%, putting the kneaded mixture C into a plastic container for standing for 20 hours, putting the mixture C into an extruder for extruding at room temperature, the extruding speed is 0.5m/min, obtaining particles with the particle size of about 1mm, directly putting the particles obtained by extruding into the mixture B, rolling the particles into round balls with the diameter of 1-3 mm, and drying the round balls for 20min at 100 ℃;
(2) respectively placing 80-mesh magnesium alloy powder and the balls obtained in the step (1) in a drying oven at 120 ℃, drying for 5min, weighing the magnesium alloy powder and the balls according to the mass ratio of the balls to the magnesium alloy powder of 1: 8, and uniformly mixing;
(3) placing the mixture obtained in the step (2) on a 50-ton press, cold pressing at room temperature, using vaseline as a lubricant during extrusion, wherein the extrusion speed is 2mm/s, the pressure is 40MPa, and keeping the pressure for 4 min;
(4) and (4) placing the precast block obtained by cold pressing in the step (3) in a closed stainless steel container, filling and compacting with an asbestos mesh, sintering at 500 ℃ for 30min, and cooling along with a furnace to obtain the biological foam magnesium alloy.
Example 3
The preparation of the biological foam magnesium alloy comprises the following steps:
(1) uniformly mixing zinc carbonate coarse powder and calcium carbonate coarse powder in a mass ratio of 5: 1 to obtain a mixture A; uniformly mixing zinc carbonate fine powder and calcium carbonate fine powder in a mass ratio of 5: 1 to obtain a mixture B; putting 70 wt% of the mixture A and 30 wt% of polyvinyl alcohol aqueous solution into a kneader for kneading, wherein the concentration of the polyvinyl alcohol aqueous solution is 5 wt%, putting the kneaded mixture C into a plastic container for standing for 12 hours, putting the mixture C into an extruder for extruding at room temperature, the extruding speed is 0.4m/min, obtaining particles with the particle size of about 1mm, directly putting the particles obtained by extruding into the mixture B, rolling into round balls with the diameter of 1-3 mm, and drying the round balls for 20min at 100 ℃;
(2) respectively placing 120-mesh magnesium alloy powder and the balls obtained in the step (1) in a drying oven at 120 ℃, drying for 10min, weighing the magnesium alloy powder and the balls according to the mass ratio of the balls to the magnesium alloy powder of 1: 10, and uniformly mixing;
(3) placing the mixture obtained in the step (2) on a 50-ton press, cold pressing at room temperature, using vaseline as a lubricant during extrusion, wherein the extrusion speed is 1.5mm/s, the pressure is 40MPa, and keeping the pressure for 3.5 min;
(4) and (4) placing the precast block obtained by cold pressing in the step (3) in a closed stainless steel container, filling and compacting with an asbestos mesh, sintering at 530 ℃ for 30min, and cooling along with a furnace to obtain the biological foam magnesium alloy.
Comparative example 1
The difference from example 1 is that step (2) is: weighing 100 meshes of magnesium alloy powder and the balls obtained in the step (1) according to the mass ratio of the balls to the magnesium alloy powder of 1: 9, and uniformly mixing.
Comparative example 2
The same as example 1 except that in the step (1), only calcium carbonate coarse powder and fine powder were used, and zinc carbonate coarse powder and zinc carbonate fine powder were not added; and the dosage of the calcium carbonate coarse powder is the sum of the dosages of the calcium carbonate coarse powder and the zinc carbonate coarse powder in the step (1), and the dosage of the calcium carbonate fine powder is the sum of the dosages of the calcium carbonate fine powder and the zinc carbonate fine powder in the step (1).
Comparative example 3
The difference from example 1 is that, in step (1), mixture B was obtained by uniformly mixing zinc carbonate coarse powder and calcium carbonate coarse powder at a mass ratio of 3: 1.
Comparative example 4
The difference from example 1 is that, in step (1), mixture A was obtained by uniformly mixing zinc carbonate fine powder and calcium carbonate fine powder at a mass ratio of 3: 1.
Effect verification
1. The pore size range and porosity of the bio-foam magnesium alloys prepared in examples 1 to 3 and comparative examples 1 to 4 were measured, and the results are shown in table 1.
2. Detecting the compressive stress, the corrosion resistance and the thermal diffusion coefficient of the biological foam magnesium alloy prepared in the embodiments 1-3 and the comparative examples 1-4, wherein the compressive stress detection is carried out at normal temperature, the compression rate is 1mm/min, and the compressive stress when the strain reaches 50% is recorded; the corrosion resistance test adopts a soaking experiment method: soaking the biological foam magnesium alloy in 3 wt% NaCl solution, cleaning and drying with dilute nitric acid before soaking, taking out after soaking for 6h, 12h and 24h respectively, cleaning with dilute nitric acid, removing corrosive substances on the surface, weighing after drying, and calculating the weight loss ratio by adopting the following formula:
wherein M is0The initial mass before soaking of the foamed magnesium alloy, MXIs the mass after soaking for x hours.
The results of the compressive stress and thermal diffusion coefficient measurements are shown in table 1; the weight loss ratio is shown in table 2.
TABLE 1
| Group of | Pore size range/. mu.m | Porosity/% | Compressive stress/MPa | Thermal diffusivity per meter2/s |
| Example 1 | 290～410 | 75 | 51 | 21.2 |
| Example 2 | 315～380 | 72 | 53 | 22.3 |
| Example 3 | 305～415 | 76.3 | 51 | 19.5 |
| Comparative example 1 | 245～435 | 70 | 50 | 26.8 |
| Comparative example 2 | 285～423 | 78 | 42 | 19.2 |
| Comparative example 3 | 275～432 | 62 | 52 | 36.6 |
| Comparative example 4 | 270～484 | 68 | 50 | 30.5 |
TABLE 2
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (10)
1. The preparation method of the biological foam magnesium alloy is characterized by comprising the following steps of:
and drying the zinc carbonate, the calcium carbonate spherulites and the magnesium alloy powder, mixing, cold pressing and sintering to obtain the foam magnesium alloy.
2. The method according to claim 1, wherein the magnesium content of the magnesium alloy powder is not less than 75 wt%.
3. The method according to claim 1, wherein the particle size of the magnesium alloy powder is 80 mesh or larger.
4. The method of manufacturing according to claim 1, wherein the zinc carbonate and calcium carbonate pellets have a core of zinc carbonate coarse powder and calcium carbonate coarse powder, and a shell of zinc carbonate fine powder and calcium carbonate fine powder;
the particle sizes of the zinc carbonate coarse powder and the calcium carbonate coarse powder are both larger than 100 meshes and smaller than 140 meshes; the granularity of the zinc carbonate fine powder and the calcium carbonate fine powder is more than or equal to 140 meshes.
5. The method of claim 4, wherein the zinc carbonate and calcium carbonate pellets are prepared by: mixing zinc carbonate coarse powder and calcium carbonate coarse powder to obtain a mixture A; mixing the zinc carbonate fine powder and the calcium carbonate fine powder to obtain a mixture B; kneading 62-80 wt% of the mixture A and 20-38 wt% of a polyvinyl alcohol aqueous solution, and extruding by using an extruder to obtain particles; the granules were then placed in mixture B and rolled to give pellets.
6. The method according to claim 5, wherein the concentration of the aqueous polyvinyl alcohol solution is 5 wt%.
7. The method of claim 4, wherein the zinc carbonate and calcium carbonate pellets have a particle size of 1 to 3 mm.
8. The preparation method according to claim 1, wherein the mass ratio of the zinc carbonate and calcium carbonate pellets to the magnesium alloy powder is 1: 8-10, and the mass ratio of the zinc carbonate and the calcium carbonate in the zinc carbonate and calcium carbonate pellets is 3-5: 1.
9. The production method according to claim 1, wherein the cold pressing is performed at room temperature, at a pressure of 40MPa, and at a dwell time of 3 to 4 min.
10. The preparation method according to claim 1, wherein the sintering is performed in a closed environment, the sintering temperature is 450-530 ℃, and the sintering time is 25-35 min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110100837.3A CN112899514B (en) | 2021-01-26 | 2021-01-26 | Preparation method of biological foam magnesium alloy |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110100837.3A CN112899514B (en) | 2021-01-26 | 2021-01-26 | Preparation method of biological foam magnesium alloy |
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| Publication Number | Publication Date |
|---|---|
| CN112899514A true CN112899514A (en) | 2021-06-04 |
| CN112899514B CN112899514B (en) | 2022-03-15 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003239027A (en) * | 2002-02-15 | 2003-08-27 | Honda Motor Co Ltd | Foamed/porous metal and manufacturing method |
| CN1974808A (en) * | 2006-12-15 | 2007-06-06 | 中国科学院长春应用化学研究所 | Prepn process of pore forming agent for porous magnesium alloy and porous aluminium and its pore forming method |
| CN102698667A (en) * | 2012-06-19 | 2012-10-03 | 重庆大学 | Spherical pore foaming agent with nuclear shell structure and three-dimensional cytoskeleton prepared by same |
| CN104046826A (en) * | 2014-05-29 | 2014-09-17 | 河海大学 | Foamed magnesium-based material and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003239027A (en) * | 2002-02-15 | 2003-08-27 | Honda Motor Co Ltd | Foamed/porous metal and manufacturing method |
| DE60300068D1 (en) * | 2002-02-15 | 2004-11-11 | Honda Motor Co Ltd | Metal foam and process for its production |
| CN1974808A (en) * | 2006-12-15 | 2007-06-06 | 中国科学院长春应用化学研究所 | Prepn process of pore forming agent for porous magnesium alloy and porous aluminium and its pore forming method |
| CN102698667A (en) * | 2012-06-19 | 2012-10-03 | 重庆大学 | Spherical pore foaming agent with nuclear shell structure and three-dimensional cytoskeleton prepared by same |
| CN104046826A (en) * | 2014-05-29 | 2014-09-17 | 河海大学 | Foamed magnesium-based material and preparation method thereof |
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