CN115747571A - Magnetic-compatible near-alpha-Zr biomedical alloy and preparation method and application thereof - Google Patents
Magnetic-compatible near-alpha-Zr biomedical alloy and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims description 9
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- 239000000956 alloy Substances 0.000 claims abstract description 52
- 239000010955 niobium Substances 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 17
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 14
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 14
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052707 ruthenium Inorganic materials 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 5
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 5
- 239000011733 molybdenum Substances 0.000 claims abstract description 5
- 239000010703 silicon Substances 0.000 claims abstract description 5
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 5
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003723 Smelting Methods 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 11
- 239000007943 implant Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
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- 238000005275 alloying Methods 0.000 claims description 4
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- 239000000725 suspension Substances 0.000 claims description 4
- 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 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000002595 magnetic resonance imaging Methods 0.000 abstract description 14
- 238000005516 engineering process Methods 0.000 abstract description 5
- 229910001093 Zr alloy Inorganic materials 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
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- 229910000791 Oxinium Inorganic materials 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 1
- 102400001284 Vessel dilator Human genes 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 108010090012 atrial natriuretic factor prohormone (31-67) Proteins 0.000 description 1
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- 238000009864 tensile test Methods 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 of zirconium and inevitable impurities, and the weight percent of zirconium is more than 95 percent. The near alpha-Zr biomedical alloy has lower magnetic susceptibility than the current common biomedical alloy and no biotoxicity 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 particularly relates to a magnetic-compatible near alpha-Zr biomedical alloy, and a preparation method and application thereof.
Background
Magnetic resonance imaging MRI (magnetic resonance imaging) is a new medical imaging technique. The proton (1H) of hydrogen atom in the substance generates resonance with radio frequency with certain frequency under the action of an external magnetic field, after the radio frequency is cancelled, the proton generates weak radio signals in the process of returning to the initial state, the 1H of different tissues can generate different radio signals, and the technology of collecting and using the radio signals to carry out three-dimensional imaging is called magnetic resonance imaging. The higher the magnetic field strength is, the higher the resolution of MRI is, and in recent years, research on "electrical theory and key technology of advanced magnetic resonance imaging system" is one of the major projects of the department of engineering and materials, which aims to solve the problems of magnet performance degradation and the like of the MRI system under ultrahigh magnetic field and ensure the autonomous controllability of the advanced MRI technology.
Under the condition of an ultrahigh magnetic field, the magnetic susceptibility of the biomedical implant is particularly critical, and the strong magnetic field can cause the metal implant to generate three adverse effects of (1) displacement dislocation; (2) fever affects surrounding tissues; (3) artifacts are generated during imaging. Artifact area and implant and human tissue (-10 to-7X 10) -6 ) There is a relationship between the volume magnetic susceptibility differences, and the larger the magnetic susceptibility difference, the larger the artifact area. Zr (109X 10) -6 ) Has pure Ti (170 multiplied by 10) which is commonly used at present -6 )、Ti-6Al-4V(179×10 -6 ) Stainless steel (3520-6700 multiplied by 10) -6 ) And Co-Cr (960X 10) -6 ) The lower volume magnetic susceptibility of the alloy. In addition, for Zr, its phase composition is closely related to magnetic susceptibility (χ), generally speaking, χ ω ＜χ α ＜χ β . Studies have reported that β -Zr has a lower magnetic susceptibility, but the magnetic susceptibility of β -Zr is higher than α -Zr and ω -Zr, making it more artifact under MRI. OXINIUM based on thermally oxidized Zr-2.5Nb alloys has been previously Smith&Nephew is applied to orthopedic implantation, and reports that near alpha-Zr alloy is applied to MRI to reduce magnetic susceptibility are lacked in China.
Disclosure of Invention
In view of the above technical problems, the present invention aims to provide a magnetic-compatible near α -Zr biomedical alloy, which comprises the following chemical components 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 (Si), tantalum (Ta), molybdenum (Mo) and ruthenium (Ru), the balance is zirconium and inevitable impurities, and the weight percent of zirconium is more than 95 percent;
preferably 2.4 to 2.6% niobium, 0.9 to 1.1% alloying element X, more preferably 2.5% niobium, and 1.0% alloying element X.
Preferably, the chemical composition of the biomedical alloy is Zr-2.5Nb-1Si in percentage by weight.
Preferably, the chemical composition of the biomedical alloy is Zr-2.5Nb-1Ta in weight percent.
Preferably, the chemical composition of the biomedical alloy is Zr-2.5Nb-1Mo in percentage by weight.
Preferably, the chemical composition of the biomedical alloy is Zr-2.5Nb-1Ru in percentage by weight.
It is another object of the present invention to provide a method for preparing the alloy described in any of the above, comprising the steps of:
(1) Weighing raw materials: weighing zirconium, niobium and an alloy element X according to the weight percentage;
(2) Alloy smelting: the smelting temperature is 2700-3000 ℃, inert gas is filled into the smelting equipment, and the ingot is smelted under the protective atmosphere.
Smelting by refractory metal suspension smelting equipment, and regulating the vacuum degree of the smelting equipment to be 4 multiplied by 10 -3 And MPa, repeatedly turning and remelting the ingot for at least three times to ensure uniform components.
The raw materials are sponge zirconium, niobium blocks and X powder, and the purity of the raw materials is more than 99.0 wt%.
The final object of the invention is to provide the use of an alloy according to any of the above for the preparation of a biomedical implant.
Preferably, the biomedical implant is a human implant, such as a bone fixation clip, a skull, a hip, a shoulder, a knee, a vessel dilator, or a heart valve, among others.
The invention adds beta stable elements or neutral elements (silicon, tantalum, molybdenum or ruthenium) with low magnetic susceptibility into Zr-Nb alloy, and dissolves elements with lower magnetic susceptibility into alpha-Zr to replace partial Zr atoms, so more volume fractions of omega-Zr and alpha-Zr dissolved with low magnetic susceptibility alloy elements 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 reported beta-Zr alloy, the near alpha-Zr alloy of the invention has lower magnetic susceptibility (9)2～102×10 -6 ) To match human tissue; (2) the near-alpha type zirconium alloy has lower Young modulus (62.4-78.4 GPa) to match human skeleton, so that the stress shielding effect is prevented from damaging the near-alpha type zirconium alloy; (3) the selected alloy elements of the near-alpha type zirconium alloy are non-cytotoxic elements, so that the harm to a human body is avoided; (4) experiments show that when X = Ru, the designed alloy has lower magnetic susceptibility and lower Young modulus compared with other three designed alloys, and has better prospect in MRI; (5) the alloy prepared by the invention can be applied to MRI with higher magnetic field, and makes up for the performance deficiency of the traditional biomedical alloy in the biomedical field.
Drawings
FIG. 1 is an XRD spectrum of the alloys of examples 1-4 of the present invention.
FIG. 2 is a microscopic structural electron micrograph of the alloy of example 1 of the present invention.
FIG. 3 is a microstructure electron micrograph of the alloy of example 2 of the present invention.
FIG. 4 is a microstructure electron micrograph of the alloy of example 3 of the present invention.
FIG. 5 is a phase structure representation of the electron back-scattering diffraction pattern of the alloy of example 3 of the present invention.
FIG. 6 is a microstructure electron microscope scan of the alloy of comparative example 4 of the present invention.
FIG. 7 is a phase structure representation of the electron back-scattering diffraction pattern of the alloy of example 4 of the present invention.
FIG. 8 is the volume magnetic 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 in order to fully understand the objects, features and effects of the invention. The process or apparatus of the present invention is conventional in the art and, unless otherwise specified, is not limited to the particular apparatus or process described herein. The following noun terms have meanings commonly understood by those skilled in the art unless otherwise specified.
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
The magnetic compatible near alpha-Zr biomedical alloy comprises the following chemical components, by weight, 2.3-2.7 wt% of niobium (Nb), 0.8-1.2 wt% of X, one of alloy elements including Si, ta, mo and Ru, and the balance of Zr and unavoidable impurities.
The magnetically compatible near α -Zr biomedical of the present invention is prepared by conventional methods in the field of alloy technology, for example, by the following steps: (1) weighing raw materials: according to the types of alloy element components, sponge zirconium, niobium blocks and X powder with industrial purity of over 99.0wt% are selected as raw materials, X is one of alloy elements of silicon (Si), tantalum (Ta), molybdenum (Mo) and ruthenium (Ru), and weighing and proportioning are carried out according to weight percentage. (2) alloy smelting: smelting by refractory metal suspension smelting equipment at 2700-3000 deg.c and 4 x 10 vacuum degree -3 And introducing inert gas argon to melt the ingot under a protective atmosphere, wherein the ingot is repeatedly turned and remelted for at least three times to ensure that the components are uniform.
The magnetic susceptibility measurement method in the following examples is referred to GB/Z26082-2010 "nanomaterial direct current magnetic susceptibility (magnetic moment) measurement method" and literature (suyalautu, n.nomura, k.oya, et al.acta biomaterials 6 (2010) 1033-1038.doi) as follows:
a4-2mm square sample is cut from the ingot through wire cutting, surface scales are polished clean through metallographic abrasive paper, and then the ingot is placed in a vibrating magnetometer (VSM), the magnetic field intensity is 1T, and the magnetic field direction is perpendicular to a 4-4 mm plane. Performing linear fitting on the obtained data by using origin software, wherein the slope of a straight line is the mass magnetic susceptibility (chi) m ) Then, the magnetic susceptibility is converted into volume magnetic susceptibility (χ) v ) The formula is x v ＝χ m X ρ × 4 π, (ρ is the alloy density and π is the circumferential ratio).
The elastic modulus test method in the following examples refers to GB/T228.1-2021 part 1 of tensile test of metal materials, room temperature test method, and comprises the following steps:
cutting a tensile sample on the cast ingot by linear cutting, polishing surface oxide skin by adopting metallographic abrasive paper, performing uniaxial tension by using a universal stretcher with an optical extensometer to obtain a strain-stress curve of the uniaxial tensile sample, and performing linear fitting on a straight line segment of the uniaxial tensile sample, 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, by weight, 2.5% of Nb, 1% of Si, and the balance of Zr and inevitable impurities.
The preparation method of the magnetic compatible near alpha-Zr biomedical alloy comprises the following steps:
(1) Weighing raw materials: according to the types of the components of the alloy elements, sponge zirconium with the industrial purity of over 99.0wt%, niobium blocks and silicon powder are selected as raw materials, and the raw materials are weighed and proportioned 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 an ingot for at least three times in order to ensure uniform components.
The XRD spectrum of the obtained alloy sample is shown in fig. 1, and the scanning photograph and magnetic susceptibility are shown in fig. 2 and 8, respectively. The volume magnetic susceptibility of the Zr-2.5Nb-1Si alloy is 98 x 10 -6 The Young's modulus was 78.4GPa.
Example 2
The magnetic compatible near-alpha-Zr biomedical alloy comprises the following chemical components, by weight, 2.5% of Nb, 1% of Ta, and the balance of Zr and inevitable 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 spectrum of the obtained alloy sample is shown in fig. 1, and the scanning photograph and magnetic susceptibility are shown in fig. 3 and 8, respectively. The volume magnetic susceptibility of the Zr-2.5Nb-1Ta alloy is 102X 10 -6 The Young's modulus was 67.4GPa.
Example 3
The magnetic-compatibility near alpha-Zr biomedical alloy comprises the following chemical components, by weight, 2.5% of Nb, 1% of Mo, and the balance of Zr and inevitable 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 pattern of the obtained alloy sample is shown in fig. 1, and the scanning photograph, the electron back-scattering diffraction pattern and the magnetic susceptibility are shown in fig. 4, 5 and 8, respectively. The bulk omega-Zr phase with lower magnetic susceptibility of the alloy was observed from the electron back-scattering diffraction pattern, and the volume magnetic susceptibility of the Zr-2.5Nb-1Mo alloy of this example was 92X 10 -6 The Young's modulus was 69.7GPa.
Example 4
The magnetic compatible near-alpha-Zr biomedical alloy comprises the following chemical components, by weight, 2.5% of Nb, 1% of Ru, and the balance of Zr and inevitable 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 of the obtained alloy samples are shown in fig. 1, and the scanning photographs, the electron back-scattering diffraction patterns and the magnetic susceptibility are shown in fig. 6, 7 and 8, respectively. The bulk omega-Zr phase with lower magnetic susceptibility of the alloy was observed from the electron back-scattering diffraction pattern, and the volume magnetic susceptibility of the Zr-2.5Nb-1Ru alloy of this example was 92X 10 -6 The Young's modulus was 62.4GPa.
From the above experiments, it is seen that when X = Ru, the design alloy has a lower magnetic susceptibility and a lower young's modulus than the other three design alloys, and has better prospects for application to MRI.
Claims (10)
1. A magnetically compatible near- α -Zr biomedical alloy, characterized by: the alloy 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 of zirconium and inevitable impurities, and the weight percent of zirconium is more than 95 percent;
preferably 2.4 to 2.6% niobium, 0.9 to 1.1% alloying element X, more preferably 2.5% niobium, and 1.0% alloying element X.
2. The magnetically compatible near α -Zr biomedical alloy according to claim 1, characterized in that said biomedical alloy has the chemical composition, in weight percent, zr-2.5Nb-1Si.
3. The magnetically compatible near α -Zr biomedical alloy according to claim 1, characterized in that said biomedical alloy has a chemical composition, in weight percent, zr-2.5Nb-1Ta.
4. The magnetically compatible near α -Zr biomedical alloy according to claim 1, characterized in that said biomedical alloy has a chemical composition, in weight percent, zr-2.5Nb-1Mo.
5. The magnetically compatible near α -Zr biomedical alloy according to claim 1, characterized in that said biomedical alloy has a chemical composition, in weight percent, zr-2.5Nb-1Ru.
6. A method for preparing an alloy as claimed in any one of claims 1 to 5, characterized by comprising the steps of:
(1) Weighing raw materials: weighing and proportioning zirconium, niobium and an alloy element X according to the weight percentage;
(2) Alloy smelting: the smelting temperature is 2700-3000 ℃, inert gas is filled into the smelting equipment, and the ingot is smelted under the protective atmosphere.
7. The method of manufacturing according to claim 6, characterized in that: smelting by refractory metal suspension smelting equipment, and regulating the vacuum degree of the smelting equipment to 4 x 10 -3 And MPa, repeatedly turning and remelting the ingot for at least three times to ensure uniform components.
8. The method of claim 6, wherein: the raw materials are sponge zirconium, niobium blocks and X powder, and the purity of the raw materials is more than 99.0 wt%.
9. Use of an alloy according to any of claims 1 to 5 for the preparation of a biomedical implant.
10. Use according to claim 9, 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 |
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| 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 |
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| LUCYNA JAWORSKA, ET AL.: "The Pressure Compaction of Zr-Nb Powder Mixtures and Selected Properties of Sintered and KOBO-Extruded Zr-xNb Materials", MATERIALS, vol. 14, no. 12, pages 1 - 18 * |
| XINU TAN, ET AL.: ""Nanoscale face-centered-cubic zirconium dispersed in omega zirconium"", PHILOSOPHICAL MAGAZINE LETTERS, vol. 102, no. 7, pages 220 - 228 * |
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