CN115747571B - Magnetic compatible near alpha-Zr type biomedical alloy and preparation method and application thereof - Google Patents
Magnetic compatible near alpha-Zr type biomedical alloy and preparation method and application thereof Download PDFInfo
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- 239000002763 biomedical alloy Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims description 9
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 56
- 239000000956 alloy Substances 0.000 claims abstract description 56
- 239000010955 niobium Substances 0.000 claims abstract description 19
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 18
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 14
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 14
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 6
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011733 molybdenum Substances 0.000 claims abstract description 6
- 239000010703 silicon Substances 0.000 claims abstract description 6
- 238000003723 Smelting Methods 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 10
- 239000007943 implant Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 8
- 239000003870 refractory metal Substances 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 241001062472 Stokellia anisodon Species 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000002595 magnetic resonance imaging Methods 0.000 abstract description 14
- 229910052715 tantalum Inorganic materials 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001093 Zr alloy Inorganic materials 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 210000001519 tissue Anatomy 0.000 description 4
- 210000000988 bone and bone Anatomy 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005275 alloying Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910001257 Nb alloy Inorganic materials 0.000 description 1
- 229910000791 Oxinium Inorganic materials 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000002059 diagnostic imaging Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 210000003709 heart valve Anatomy 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 210000004394 hip joint Anatomy 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 210000000629 knee joint Anatomy 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005404 magnetometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100000065 noncytotoxic Toxicity 0.000 description 1
- 230000002020 noncytotoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 210000000323 shoulder joint Anatomy 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 230000002792 vascular Effects 0.000 description 1
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Abstract
The invention discloses a magnetic compatible near alpha-Zr biomedical alloy, which comprises the following chemical components in percentage by weight: 2.3 to 2.7 percent of niobium, 0.8 to 1.2 percent of alloy element X, wherein X is one of alloy elements of silicon, tantalum, molybdenum and ruthenium, and the balance is zirconium and unavoidable impurities, and the weight percentage of the zirconium is more than 95 percent. The near alpha-Zr biomedical alloy has lower magnetic susceptibility than the current common biomedical alloy and no biotoxic element, and can better serve the magnetic resonance imaging technology under a higher magnetic field.
Description
Technical Field
The invention belongs to the technical field of metal materials, relates to a zirconium alloy, and in particular relates to a magnetic compatible near alpha-Zr biomedical alloy, and a preparation method and application thereof.
Background
Magnetic resonance imaging MRI (Magneticresonance imaging) is a novel medical imaging technique. Protons (1H) of hydrogen atoms in the substance generate resonance phenomenon with radio frequency with a certain frequency under the action of an external magnetic field, after the radio frequency is canceled, the protons generate weak radio signals in the process of returning to an initial state, 1H of different tissues generate different radio signals, and a technology for acquiring and applying the radio signals to perform three-dimensional imaging is called magnetic resonance imaging. The higher the magnetic field strength, the higher the resolution of MRI, and in recent years, the research of "the electrician theory and key technology of the advanced magnetic resonance imaging system" is one of the important projects of engineering and materials, and the research aims to solve the problems of the magnetic performance degradation of the MRI system under the ultra-high magnetic field and ensure the autonomous controllability of the advanced MRI technology.
Under the ultra-high magnetic field, the magnetic susceptibility of biomedical implants is particularly critical, and the strong magnetic field can cause three adverse effects of the metal implants, namely (1) displacement dislocation; (2) heating affects surrounding tissue; (3) artifacts are created upon imaging. Artifact area and implant and human tissue (-10 to-7 x 10) -6 ) Volume magnetism betweenThe difference in the chemical susceptibility is related to the fact that the larger the difference in the magnetic susceptibility is, the larger the artifact area is. Zr (109X 10) -6 ) Possessing a higher purity than currently used Ti (170X 10) -6 )、Ti-6Al-4V(179×10 -6 ) Stainless steel (3520-6700X 10) -6 ) And Co-Cr (960X 10) -6 ) The alloy has lower volume magnetic susceptibility. In addition, for Zr, its phase composition is closely related to magnetic susceptibility (χ), generally χ ω ＜χ α ＜χ β . There are studies reporting lower susceptibility to beta-Zr, but higher susceptibility to beta-Zr than alpha-Zr and omega-Zr, making it more artifact prone to MRI. Oxinium based on thermally oxidized Zr-2.5Nb alloys has been currently subjected to Smith&Nephew is used for orthopedic implantation, and there is no report of using near alpha-Zr alloy in MRI to reduce magnetic susceptibility in China.
Disclosure of Invention
Aiming at the technical problems, the invention aims to provide a magnetic compatible near alpha-Zr biomedical alloy, which comprises the following chemical components in percentage by weight: 2.3 to 2.7 percent of niobium, 0.8 to 1.2 percent of alloy element X, wherein X is one of alloy elements silicon (Si), tantalum (Ta), molybdenum (Mo) and ruthenium (Ru), and the balance is zirconium and unavoidable impurities, and the weight percentage of the zirconium is more than 95 percent;
preferably, niobium is 2.4 to 2.6%, the alloying element X is 0.9 to 1.1%, more preferably, niobium is 2.5%, and the alloying element X is 1.0%.
Preferably, the chemical composition of the biomedical alloy is calculated as Zr-2.5Nb-1Si in weight percent.
Preferably, the chemical composition of the biomedical alloy is calculated as Zr-2.5Nb-1Ta in weight percent.
Preferably, the chemical composition of the biomedical alloy is calculated as Zr-2.5Nb-1Mo in weight percent.
Preferably, the chemical composition of the biomedical alloy is calculated as Zr-2.5Nb-1Ru in weight percent.
Another object of the present invention is to provide a method for preparing an alloy as defined in any one of the above, comprising the steps of:
(1) Weighing the raw materials: weighing zirconium, niobium and alloy element X according to weight percentage;
(2) Alloy smelting: the smelting temperature is 2700-3000 ℃, and inert gas is filled into smelting equipment to smelt the cast ingot under protective atmosphere.
Smelting by adopting refractory metal suspension smelting equipment, and regulating the vacuum degree of the smelting equipment to be 4 multiplied by 10 -3 MPa, in order to ensure the components to be uniform, the cast ingot is repeatedly turned over and remelted at least three times.
The raw materials are zirconium sponge, niobium blocks and X powder, and the purity of the raw materials is above 99.0 wt%.
A final object of the present invention is to provide the use of an alloy according to any of the above in the preparation of biomedical implants.
Preferably, the biomedical implant is a human implant, such as a bone fixation clamp, a cranium, a hip joint, a shoulder joint, a knee joint, a vascular dilator, a heart valve, or the like.
According to the invention, the beta stable element or neutral element (silicon, tantalum, molybdenum or ruthenium) with low magnetic susceptibility is added into the Zr-Nb alloy, the element with lower magnetic susceptibility is dissolved into the alpha-Zr to replace part of Zr atoms, more volume fraction omega-Zr and alpha-Zr with low magnetic susceptibility alloy element are obtained by designing the alloy, and the magnetic susceptibility of the alloy is effectively reduced.
The invention has the following beneficial effects:
(1) compared with the prior reported beta-Zr alloy, the near alpha-type zirconium alloy has lower magnetic susceptibility (92-102 multiplied by 10) -6 ) To match human tissue; (2) the near alpha-type zirconium alloy has lower Young's modulus (62.4-78.4 GPa) to match human bones, so that the damage to the human bones due to stress shielding effect is avoided; (3) the alloy elements selected by the near alpha-type zirconium alloy are non-cytotoxic elements, so that the damage to human bodies is avoided; (4) experiments show that when X=Ru, the design alloy has lower magnetic susceptibility and lower Young modulus than other three design alloys, and has better prospect in MRI application; (5) the alloy prepared by the invention can be applied to MRI with higher magnetic field, and makes up the performance deficiency of the traditional biomedical alloy in the biomedical field.
Drawings
FIG. 1 is an XRD spectrum of the alloy of examples 1-4 of the invention.
FIG. 2 is a microscopic electron microscope scan of the alloy of example 1 of the present invention.
FIG. 3 is a microscopic electron microscope scan of the alloy of example 2 of the present invention.
FIG. 4 is a microscopic image of the alloy of example 3 of the present invention.
FIG. 5 is a chart showing the structure of the electron back-scattering diffraction pattern of the alloy of example 3 of the present invention.
FIG. 6 is a microscopic image of the alloy of comparative example 4 of the present invention.
FIG. 7 is a chart showing the structure of the electron back-scattering diffraction pattern of the alloy of example 4 of the present invention.
FIG. 8 is the bulk susceptibility results for the alloys of examples 1-4 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following embodiments for a full understanding of the objects, features, and effects of the present invention. The technical method or the device related to the invention is a conventional method or device in the field unless specifically stated. The following terms have the meanings commonly understood by those skilled in the art unless otherwise indicated.
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention.
The magnetic compatible near alpha-Zr biomedical alloy comprises, by weight, 2.3-2.7wt% of niobium (Nb), 0.8-1.2wt% of X, one of alloy elements Si, ta, mo and Ru, and the balance of Zr and unavoidable impurities.
The magnetically compatible near alpha-Zr biomedical alloy disclosed by the invention is prepared by adopting a conventional method in the technical field of alloys, for example, the following method can be adopted, and the following steps are adopted for operation: and (1) weighing raw materials: according to the types of alloy element components, selecting sponge zirconium, niobium blocks and X powder with the purity of more than 99.0wt% as raw materials, wherein X is selected from alloy elements of silicon (Si), tantalum (Ta), molybdenum (Mo) and ruthenium (Ru)Weighing and proportioning according to the weight percentage. (2) alloy smelting: smelting by adopting refractory metal suspension smelting equipment, wherein the smelting temperature is 2700-3000 ℃, and the vacuum degree of the smelting equipment is regulated to be 4 multiplied by 10 -3 And (3) filling inert gas argon into the furnace under the pressure of MPa to smelt the cast ingot in a protective atmosphere, and repeatedly overturning and remelting the cast ingot for at least three times to ensure uniform components.
The magnetic susceptibility measurement method in the following examples is described with reference to GB/Z26082-2010 "method for measuring DC magnetic susceptibility (magnetic moment) of nanomaterial" and literature (Suyalatu, N. Nomura, K. Oya, et al acta Biomaterialia 6 (2010) 1033-1038.Doi:10.1016/j. Actbio.2009.09.013), in particular steps as follows:
and cutting a square sample of 4 x 2mm on the cast ingot by linear cutting, adopting metallographic sand paper to clean surface oxide skin, and then placing the polished surface oxide skin in a vibrating magnetometer (VSM), wherein the magnetic field strength is 1T, and the magnetic field direction is perpendicular to a plane of 4 x 4 mm. The obtained data are subjected to linear fitting by adopting origin software, and the slope of the straight line is the mass magnetic susceptibility (χ) m ) Then converts the magnetic field into volume magnetic susceptibility (χ) v ) The formula is χ v ＝χ m X ρ×4pi, (ρ is alloy density and pi is circumference ratio).
The elastic modulus test method in the following examples is referred to GB/T228.1-2021 section 1 Metal Material tensile test method: room temperature test method, and comprises the following specific steps:
and cutting a stretching sample on an ingot by linear cutting, polishing the surface oxide skin clean by adopting metallographic abrasive paper, carrying out uniaxial stretching by using a universal stretcher with an optical extensometer to obtain a strain-stress curve of the uniaxial stretching sample, and carrying out linear fitting on a straight line segment of the strain-stress curve, wherein the slope of the straight line is the Young modulus.
Example 1
The magnetic compatible near alpha-Zr biomedical alloy comprises the following chemical components in percentage by weight, namely 2.5 weight percent of Nb, 1 weight percent of Si, and the balance of Zr and unavoidable impurities.
The preparation method of the magnetic compatible near alpha-Zr biomedical alloy comprises the following steps:
(1) Weighing the raw materials: according to the types of alloy element components, selecting sponge zirconium, niobium blocks and silicon powder with the industrial purity of more than 99.0 weight percent as raw materials, and weighing and proportioning according to the weight percentage. (2) alloy smelting: smelting by adopting refractory metal suspension smelting equipment, adjusting the vacuum degree of the smelting equipment, smelting under the protection of argon, and repeatedly overturning and remelting the cast ingot for at least three times in order to ensure uniform components.
The XRD spectra of the obtained alloy samples are shown in FIG. 1, and the scanning photographs and magnetic susceptibility are shown in FIG. 2 and FIG. 8, respectively. The volume magnetic susceptibility of the Zr-2.5Nb-1Si alloy is 98 multiplied by 10 -6 Young's modulus of 78.4GPa.
Example 2
The magnetic compatible near alpha-Zr biomedical alloy comprises the following chemical components in percentage by weight, namely 2.5 weight percent of Nb, 1 weight percent of Ta and the balance of Zr and unavoidable impurities.
The preparation method of the magnetic compatible near alpha-Zr biomedical alloy of the embodiment is the same as that of the embodiment 1.
The XRD spectra of the obtained alloy samples are shown in FIG. 1, and the scanning photographs and magnetic susceptibility are shown in FIG. 3 and FIG. 8, respectively. The volume magnetic susceptibility of the Zr-2.5Nb-1Ta alloy is 102 multiplied by 10 -6 Young's modulus of 67.4GPa.
Example 3
The magnetic compatible near alpha-Zr biomedical alloy comprises the following chemical components in percentage by weight, namely 2.5 weight percent of Nb, 1 weight percent of Mo and the balance of Zr and unavoidable impurities.
The preparation method of the magnetic compatible near alpha-Zr biomedical alloy of the embodiment is the same as that of the embodiment 1.
The XRD patterns, scanning photographs, electron back-scattering diffraction patterns and magnetic susceptibility of the obtained alloy samples are shown in FIG. 1, and FIGS. 4, 5 and 8, respectively. As can be seen from the electron back-scattering diffraction pattern, the bulk omega-Zr phase with lower magnetic susceptibility exists in the alloy, and the volume magnetic susceptibility of the Zr-2.5Nb-1Mo alloy of the example is 92 multiplied by 10 -6 Young's modulus of 69.7GPa.
Example 4
The magnetic compatible near alpha-Zr biomedical alloy comprises the following chemical components in percentage by weight, namely 2.5 weight percent of Nb, 1 weight percent of Ru and the balance of Zr and unavoidable impurities.
The preparation method of the magnetic compatible near alpha-Zr biomedical alloy of the embodiment is the same as that of the embodiment 1.
The XRD patterns, scanning photographs, electron back-scattering diffraction patterns and magnetic susceptibility of the obtained alloy samples are shown in FIG. 1, and FIGS. 6, 7 and 8, respectively. As can be seen from the electron back-scattering diffraction pattern, the bulk omega-Zr phase having a lower magnetic susceptibility exists in the alloy, and the bulk magnetic susceptibility of the Zr-2.5Nb-1Ru alloy of this example was 92X 10 -6 Young's modulus of 62.4GPa.
From the above experiments, it is seen that when x=ru, the design alloy has lower magnetic susceptibility and lower young's modulus than the other three design alloys, and has better prospects for application in MRI.
Claims (8)
1. A magnetic compatible near alpha-Zr biomedical alloy is characterized in that: the alloy comprises the following chemical components in percentage by weight: 2.3-2.7% of niobium, 0.8-1.2% of alloy element X, wherein X is one of alloy elements silicon, molybdenum and ruthenium, and the balance is zirconium and unavoidable impurities, and the weight percentage of the zirconium is more than 95%.
2. The magnetically compatible near- α -Zr biomedical alloy according to claim 1, wherein: the alloy comprises the following chemical components in percentage by weight: 2.4-2.6% of niobium, 0.9-1.1% of alloy element X, wherein X is one of alloy elements silicon, molybdenum and ruthenium, the balance is zirconium and unavoidable impurities, and the weight percentage of the zirconium is more than 95%.
3. The magnetically compatible near- α -Zr biomedical alloy according to claim 2, wherein: wherein, niobium is 2.5 percent and alloy element X is 1.0 percent.
4. A method of producing an alloy as claimed in any one of claims 1 to 3, comprising the steps of:
(1) Weighing the raw materials: weighing zirconium, niobium and alloy element X according to weight percentage;
(2) Alloy smelting: and (3) charging inert gas into smelting equipment at the smelting temperature of 2700-3000 ℃ to smelt the cast ingot in a protective atmosphere.
5. The method of manufacturing according to claim 4, wherein: smelting by adopting refractory metal suspension smelting equipment, and regulating the vacuum degree of the smelting equipment to be 4 multiplied by 10 -3 MPa, in order to ensure the components to be uniform, the cast ingot is repeatedly turned over and remelted at least three times.
6. The method of manufacturing according to claim 5, wherein: the raw materials are zirconium sponge, niobium blocks and X powder, and the purity of the raw materials is above 99.0 wt%.
7. Use of an alloy according to any one of claims 1 to 3 for the preparation of biomedical implants.
8. The use according to claim 7, characterized in that: the biomedical implant is a human implant.
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| CN101654751A (en) * | 2009-09-18 | 2010-02-24 | 西北有色金属研究院 | Niobium-containing zirconium base alloy used by nuclear fuel jacketing |
| CN102443720A (en) * | 2011-12-13 | 2012-05-09 | 广西大学 | Novel hard-tissue biological medical zirconium-based alloy and preparation method thereof |
| CN110408815A (en) * | 2019-08-21 | 2019-11-05 | 湘潭大学 | A kind of low elastic modulus, high-intensitive spinodal decomposition type Zr-Nb-Ti alloy material and preparation method thereof |
| JP2020084300A (en) * | 2018-11-30 | 2020-06-04 | 日立金属株式会社 | Zr ALLOY, Zr ALLOY MANUFACTURED ARTICLE AND Zr ALLOY COMPONENT |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654751A (en) * | 2009-09-18 | 2010-02-24 | 西北有色金属研究院 | Niobium-containing zirconium base alloy used by nuclear fuel jacketing |
| CN102443720A (en) * | 2011-12-13 | 2012-05-09 | 广西大学 | Novel hard-tissue biological medical zirconium-based alloy and preparation method thereof |
| JP2020084300A (en) * | 2018-11-30 | 2020-06-04 | 日立金属株式会社 | Zr ALLOY, Zr ALLOY MANUFACTURED ARTICLE AND Zr ALLOY COMPONENT |
| CN110408815A (en) * | 2019-08-21 | 2019-11-05 | 湘潭大学 | A kind of low elastic modulus, high-intensitive spinodal decomposition type Zr-Nb-Ti alloy material and preparation method thereof |
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| Title |
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| "Nanoscale face-centered-cubic zirconium dispersed in omega zirconium";Xinu Tan, et al.;PHILOSOPHICAL MAGAZINE LETTERS;第102卷(第7期);第220-228页 * |
| The Pressure Compaction of Zr-Nb Powder Mixtures and Selected Properties of Sintered and KOBO-Extruded Zr-xNb Materials;Lucyna Jaworska, et al.;materials;第14卷(第12期);第1-18页 * |
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