CN115519116A - High-biocompatibility magnesium-based amorphous alloy powder and preparation method thereof - Google Patents
High-biocompatibility magnesium-based amorphous alloy powder and preparation method thereof Download PDFInfo
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- CN115519116A CN115519116A CN202211294815.6A CN202211294815A CN115519116A CN 115519116 A CN115519116 A CN 115519116A CN 202211294815 A CN202211294815 A CN 202211294815A CN 115519116 A CN115519116 A CN 115519116A
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- 239000000843 powder Substances 0.000 title claims abstract description 37
- 239000011777 magnesium Substances 0.000 title claims abstract description 36
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910000808 amorphous metal alloy Inorganic materials 0.000 title claims abstract description 27
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000000956 alloy Substances 0.000 claims abstract description 11
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- 229910045601 alloy Inorganic materials 0.000 claims description 9
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 8
- 229910052772 Samarium Inorganic materials 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000000889 atomisation Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 14
- 230000007797 corrosion Effects 0.000 abstract description 14
- 239000012890 simulated body fluid Substances 0.000 abstract description 8
- 238000010146 3D printing Methods 0.000 abstract description 5
- 210000000988 bone and bone Anatomy 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000005501 phase interface Effects 0.000 abstract description 2
- 238000005204 segregation Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 8
- 238000005303 weighing Methods 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 229910000861 Mg alloy Inorganic materials 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 230000004580 weight loss Effects 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000001727 in vivo Methods 0.000 description 2
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/005—Amorphous alloys with Mg as the major constituent
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/08—Metallic powder characterised by particles having an amorphous microstructure
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/002—Making metallic powder or suspensions thereof amorphous or microcrystalline
- B22F9/008—Rapid solidification processing
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
Abstract
The invention relates to the field of alloy materials, in particular to high-biocompatibility magnesium-based amorphous alloy powder and a preparation method thereof, wherein the magnesium-based amorphous alloy powder has a structural general formula as follows: mg (magnesium) 50‑ x Cu 37 Ti 4.5 Zr 3 Co 2.5 Hf 2 Ca 1 RE x (ii) a RE in the general structural formula is rare earth element; x is 0.1-0.4, the material can be used for manufacturing medical parts of human bodies by 3D printing, has the density close to that of human bones, has the advantages of excellent mechanical strength, wear resistance, corrosion resistance and the like, and does not have the factors which are easy to cause corrosion such as crystal boundary, dislocation, phase interface and the likeThe preparation method has the advantages that a compact, uniform and stable passive film can be rapidly formed, no chemical segregation exists in simulated body fluid at 37 ℃, excellent corrosion resistance is realized, the problems of fatigue failure and the like caused by corrosion do not exist, and therefore, the preparation method has a certain application prospect in the field of biological medical treatment.
Description
Technical Field
The invention relates to the field of alloy materials, in particular to high-biocompatibility magnesium-based amorphous alloy powder and a preparation method thereof.
Background
Biocompatibility of a material refers to the ability of the material to produce no deleterious effects on the host during service in vivo such as: stability during service, has similar properties to those of replaced tissues, and does not generate corrosion or abrasion products and the like harmful to human bodies. Magnesium is an indispensable macroelement for human bodies, the mechanical property of the alloy is similar to that of human bones and can be degraded and absorbed in human bodies, so that the magnesium alloy is always a focus of academic interest as a biomedical material, and the amorphous magnesium alloy and the crystalline magnesium alloy have better mechanical property because of different structures and no defects such as dislocation, grain boundary and the like, but still face the problems of corrosion fatigue failure and the like of implanted metal materials caused by the combined action of alternating stress generated by a bone system and a corrosive environment in vivo when the magnesium alloy is used as an implanted material.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the technical problems, the invention provides magnesium-based amorphous alloy powder with high biocompatibility and a preparation method thereof.
The adopted technical scheme is as follows:
a high biocompatibility magnesium-based amorphous alloy powder has a structural general formula as follows:
Mg 50-x Cu 37 Ti 4.5 Zr 3 Co 2.5 Hf 2 Ca 1 RE x ；
RE in the general structural formula is rare earth element;
x is 0.1-0.4.
Further, x is 0.3.
Furthermore, RE is any one or combination of La, sm, Y, gd, ce and Dy.
Further, RE is Sm and Gd.
Further, the mass ratio of Sm to Gd is 1-5:1-5.
The invention also provides a preparation method of the high-biocompatibility magnesium-based amorphous alloy powder, which comprises the following steps:
weighing raw materials according to the proportion in the structural general formula, repeatedly smelting for 3-5 times under a vacuum condition to obtain an alloy ingot, and atomizing to obtain powder.
Furthermore, the smelting temperature is 1500-1600 ℃.
Further, atomizing by using close coupling atomization equipment, wherein the atomization gas is argon, the atomization gas pressure is 8-12MPa, the superheat degree is 150-200 ℃, and the diameter of the flow guide pipe is 3-6mm.
Further, the particle size of the obtained powder is 10 to 100. Mu.m.
The invention has the beneficial effects that:
the invention provides high-biocompatibility magnesium-based amorphous alloy powder which can be used for manufacturing human medical parts through 3D printing, has the advantages of high mechanical strength, wear resistance, corrosion resistance and the like, has the density close to that of human bones, can quickly form a compact, uniform and stable passive film due to the absence of factors which are easy to cause corrosion such as crystal boundaries, dislocations, phase interfaces and the like, has no chemical segregation in simulated body fluid at 37 ℃, has high corrosion resistance, does not have the problems of fatigue failure and the like caused by corrosion, and has a certain application prospect in the field of biological medical treatment.
Drawings
Fig. 1 is an XRD diffraction pattern of the mg-based amorphous alloy powder prepared in example 1 of the present invention, which shows a broad diffuse scattering peak, generally called "amorphous pocket", only in the vicinity of 2 θ =44 ° within the effective resolution of the diffraction, and does not show a sharp diffraction peak characterizing the crystalline phase, thus indicating a substantially single amorphous structure inside.
Detailed Description
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
Example 1:
a high biocompatibility magnesium-based amorphous alloy powder has a structural general formula as follows:
Mg 49.7 Cu 37 Ti 4.5 Zr 3 Co 2.5 Hf 2 Ca 1 RE 0.3
RE is 1:1 Sm and Gd;
the preparation method comprises the following steps:
weighing raw materials according to the proportion in the structural general formula, putting the raw materials into a vacuum arc melting furnace, vacuumizing to 0.1Pa, introducing argon of 0.5Pa, striking an arc for melting, repeatedly melting for 5 times at 1600 ℃ to obtain an alloy ingot, atomizing by using tightly-coupled atomizing equipment, wherein the atomizing gas is argon, the atomizing pressure is 12MPa, the superheat degree is 180 ℃, the diameter of a flow guide pipe is 6mm, and powder with the particle size of 10-100 mu m is obtained.
Example 2:
a high biocompatibility magnesium-based amorphous alloy powder has a structural general formula as follows:
Mg 49.7 Cu 37 Ti 4.5 Zr 3 Co 2.5 Hf 2 Ca 1 RE 0.3
RE is 2:1 Sm and Gd;
the preparation method comprises the following steps:
weighing raw materials according to the proportion in the structural general formula, putting the raw materials into a vacuum arc melting furnace, vacuumizing to 0.1Pa, introducing argon of 0.5Pa, striking an arc for melting, repeatedly melting for 5 times at 1600 ℃ to obtain an alloy ingot, atomizing by using tightly-coupled atomizing equipment, wherein the atomizing gas is argon, the atomizing pressure is 12MPa, the superheat degree is 200 ℃, and the diameter of a flow guide pipe is 6mm, so that powder with the particle size of 10-100 mu m is obtained.
Example 3:
a high biocompatibility magnesium-based amorphous alloy powder has a structural general formula as follows:
Mg 49.7 Cu 37 Ti 4.5 Zr 3 Co 2.5 Hf 2 Ca 1 RE 0.3
RE is 3:1 Sm and Gd;
the preparation method comprises the following steps:
weighing raw materials according to the proportion in the general formula, putting the raw materials into a vacuum arc melting furnace, vacuumizing to 0.1Pa, introducing argon of 0.5Pa, striking an arc for melting, repeatedly melting for 4 times at 1550 ℃ to obtain an alloy ingot, atomizing by using tightly-coupled atomizing equipment, wherein the atomizing gas is argon, the atomizing pressure is 10MPa, the superheat degree is 160 ℃, and the diameter of a flow guide pipe is 6mm, so that powder with the particle size of 10-100 mu m is obtained.
Example 4:
a high biocompatibility magnesium-based amorphous alloy powder has a structural general formula as follows:
Mg 49.7 Cu 37 Ti 4.5 Zr 3 Co 2.5 Hf 2 Ca 1 RE 0.3
RE is 4:1 Sm and Gd;
the preparation method comprises the following steps:
weighing raw materials according to the proportion in the general formula, putting the raw materials into a vacuum arc melting furnace, vacuumizing to 0.1Pa, introducing argon gas of 0.5Pa, striking an arc for melting, repeatedly melting for 3 times at 1500 ℃ to obtain an alloy ingot, atomizing by using close-coupled atomizing equipment, wherein the atomizing gas is argon gas, the atomizing pressure is 8MPa, the superheat degree is 150 ℃, the diameter of a guide pipe is 3mm, and powder with the particle size of 10-100 mu m is obtained.
Example 5:
a high biocompatibility magnesium-based amorphous alloy powder has a structural general formula as follows:
Mg 49.7 Cu 37 Ti 4.5 Zr 3 Co 2.5 Hf 2 Ca 1 RE 0.3
RE is 5:1 Sm and Gd;
the preparation method comprises the following steps:
weighing raw materials according to the proportion in the general formula, putting the raw materials into a vacuum arc melting furnace, vacuumizing to 0.1Pa, introducing argon gas of 0.5Pa, striking an arc for melting, repeatedly melting for 3 times at 1600 ℃ to obtain an alloy ingot, atomizing by using tightly-coupled atomizing equipment, wherein the atomizing gas is argon, the atomizing pressure is 12MPa, the superheat degree is 150 ℃, and the diameter of a flow guide pipe is 6mm, so that powder with the particle size of 10-100 mu m is obtained.
Example 6:
a high biocompatibility magnesium-based amorphous alloy powder has a structural general formula as follows:
Mg 49.7 Cu 37 Ti 4.5 Zr 3 Co 2.5 Hf 2 Ca 1 RE 0.3
RE is 1:5 Sm and Gd;
the preparation method comprises the following steps:
weighing raw materials according to the proportion in the structural general formula, putting the raw materials into a vacuum arc melting furnace, vacuumizing to 0.1Pa, introducing argon of 0.5Pa, striking an arc for melting, repeatedly melting for 5 times at 1500 ℃ to obtain an alloy ingot, atomizing by using close-coupled atomizing equipment, wherein the atomizing gas is argon, the atomizing pressure is 8MPa, the superheat degree is 200 ℃, the diameter of a guide pipe is 3mm, and powder with the particle size of 10-100 mu m is obtained.
Example 7:
essentially the same as example 1, except that RE is Sm.
Example 8:
essentially the same as example 1, except that RE is Gd.
Example 9:
essentially the same as example 1 except that RE is La.
Example 10:
basically the same as example 1 except that RE is Dy.
And (3) performance testing:
the magnesium-based amorphous alloy powder prepared in the embodiments 1-10 of the invention is respectively subjected to 3D printing to obtain a sample, the 3D printing equipment is an EOSINT-M280-3D printer, and the printing parameters are as follows:
construction rate: 40cm 3 H, laser scanning speed: 10m/s, layer thickness: 30 μm.
(1) The density, hardness and abrasion resistance of the samples are shown in Table 1.
The density is measured by a drainage method, the hardness is measured by an HV-1000A micro Vickers hardness tester, five points of hardness are taken for a sample, the average Vickers hardness of the sample is finally obtained, the wear resistance is subjected to a wear test by an MLS-225 type wet rubber wheel abrasive wear tester, and the test parameters are as follows: rotating speed of the rubber wheel: 240 rpm, rubber wheel diameter: 178mm, rubber wheel hardness: 60 (shore hardness), load: 10kg, abrasion time: 250s, rubber wheel revolution: about 1000 revolutions, abrasive: the wear resistance of a sample of 40-70-mesh quartz sand is measured by the weight loss of wear, Q235 steel is used as a comparison part during experiments, and the ratio of the weight loss of the comparison part to the weight loss of the sample is used as the relative wear resistance: relative wear resistance = contrast wear amount/specimen wear amount.
Table 1:
(2) the corrosion resistance test of the sample is carried out in a simulated body fluid at 37 ℃ in the selected environment, and the ion concentration table of the simulated body fluid is shown in the following table 2:
table 2:
the corrosion resistance test of the test sample is mainly divided into a soaking experiment and a hydrogen evolution experiment.
The soaking experiment is carried out according to the international soaking experiment standard ASTM-G31-12a, the ratio of the sample surface area to the simulated body fluid volume is 1cm 2 :20ml, will processPlacing the good sample into simulated body fluid, standing for 240h, taking out, and observing whether a corrosion trace exists;
the hydrogen evolution experiment is carried out by mixing a sample according to the international immersion test standard ASTM-G31-12a, wherein the volume ratio of the sample surface area to the simulated body fluid is 1cm 2 :150ml, the treated sample was placed in simulated body fluid for 24h and the gas generated was collected using a gas collection device and the gas generation volume was recorded.
The test results are shown in table 3 below:
TABLE 3
As shown in the above tables 1-3, the magnesium-based amorphous alloy powder prepared by the invention can be used for 3D printing to manufacture human medical parts, and has the advantages of excellent mechanical strength, wear resistance, corrosion resistance and the like, so that the magnesium-based amorphous alloy powder has a certain application prospect in the field of biological medical treatment.
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. The magnesium-based amorphous alloy powder with high biocompatibility is characterized by comprising the following structural general formula:
Mg 50-x Cu 37 Ti 4.5 Zr 3 Co 2.5 Hf 2 Ca 1 RE x ；
RE in the general structural formula is rare earth element;
x is 0.1-0.4.
2. The highly biocompatible magnesium-based amorphous alloy powder according to claim 1, wherein x is 0.3.
3. The highly biocompatible magnesium-based amorphous alloy powder according to claim 1, wherein RE is any one or combination of La, sm, Y, gd, ce and Dy.
4. The highly biocompatible magnesium-based amorphous alloy powder according to claim 3, wherein RE is Sm and Gd.
5. The highly biocompatible magnesium-based amorphous alloy powder according to claim 4, wherein the mass ratio of Sm to Gd is 1 to 5:1-5.
6. A method for preparing the high-biocompatibility magnesium-based amorphous alloy powder as claimed in any one of claims 1 to 5, wherein the raw materials are weighed according to the proportion in the structural formula, repeatedly melted for 3 to 5 times under a vacuum condition to obtain an alloy ingot, and atomized to obtain the powder.
7. The method for preparing highly biocompatible Mg-based amorphous alloy powder according to claim 6, wherein the melting temperature is 1500-1600 ℃.
8. The method of claim 6, wherein the atomization is performed by using a close-coupled atomization device, the atomization gas is argon, the atomization pressure is 8-12MPa, the superheat degree is 150-200 ℃, and the diameter of the flow guide tube is 3-5mm.
9. The method for preparing highly biocompatible magnesium-based amorphous alloy powder according to claim 6, wherein the obtained powder has a particle size of 10-100 μm.
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|---|---|---|---|---|
| US5348591A (en) * | 1991-09-06 | 1994-09-20 | Tsuyoshi Masumoto | High-strength amorphous magnesium alloy |
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| CN113502441A (en) * | 2021-06-23 | 2021-10-15 | 华中科技大学 | In-situ authigenic phase-reinforced magnesium-based amorphous composite material and preparation method thereof |
| CN113913709A (en) * | 2021-10-09 | 2022-01-11 | 华中科技大学 | In-situ authigenic hybrid phase reinforced magnesium-based amorphous composite material based on selective phase dissolution and preparation method thereof |
| CN114214550A (en) * | 2021-12-17 | 2022-03-22 | 河北科技大学 | Medical magnesium alloy and preparation method thereof |
| CN114672744A (en) * | 2022-03-09 | 2022-06-28 | 华中科技大学 | Endogenetic porous titanium reinforced magnesium-based amorphous composite material and preparation method thereof |
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2022
- 2022-10-21 CN CN202211294815.6A patent/CN115519116A/en active Pending
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|---|---|---|---|---|
| US5348591A (en) * | 1991-09-06 | 1994-09-20 | Tsuyoshi Masumoto | High-strength amorphous magnesium alloy |
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| CN113913709A (en) * | 2021-10-09 | 2022-01-11 | 华中科技大学 | In-situ authigenic hybrid phase reinforced magnesium-based amorphous composite material based on selective phase dissolution and preparation method thereof |
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| CN114672744A (en) * | 2022-03-09 | 2022-06-28 | 华中科技大学 | Endogenetic porous titanium reinforced magnesium-based amorphous composite material and preparation method thereof |
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