CN113827781B - Magnetic resonance imaging compatible conductive thin film alloy material and preparation method thereof - Google Patents
Magnetic resonance imaging compatible conductive thin film alloy material and preparation method thereof Download PDFInfo
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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Abstract
The invention discloses a conductive thin film alloy material compatible with magnetic resonance imaging and a preparation method thereof. The conductive film alloy material is applied to implantable medical equipment, a neural interface or a brain-computer interface, and is prepared by taking a paramagnetic substance and a diamagnetic substance as co-sputtering materials and adopting a micro-nano processing technology of magnetron co-sputtering coating. The invention utilizes a magnetron co-sputtering coating method to respectively optimize and set parameters such as the sputtering current intensity, the power and the like of a paramagnetic substance-a diamagnetic substance and specific film-forming air pressure to prepare the alloy material. Therefore, the magnetron sputtering preparation conditions of the conductive thin film alloy material applicable to the implantation instrument are determined, so that the conductive thin film alloy material has better conductivity and electrochemical properties, does not cause imaging artifacts influencing the observation of an implantation part in magnetic resonance imaging, and has good magnetic resonance imaging compatibility.
Description
Technical Field
The invention relates to the technical field of biomedical engineering, medical instruments and micro-nano processing, in particular to a magnetic resonance imaging compatible conductive thin film alloy material and a preparation method thereof.
Background
Magnetic resonance imaging has become a common clinical diagnostic tool, and studies on implantable medical devices, neural interfaces, and brain-computer interfaces have been intensively conducted. However, due to the huge difference in magnetization properties between the conventional implantable medical device and the biological tissue, the magnetic field distortion of the implant in the magnetic resonance imaging environment can be caused, and imaging artifacts are generated, thereby affecting the clinical application of the magnetic resonance imaging diagnosis. Among other things, the conductive components in the implantable device are often the primary source of magnetic resonance imaging artifacts. Therefore, there is a need to invent a conductive material compatible with magnetic resonance imaging for reducing or even eliminating artifacts in medical images of an implanted medical device.
According to a search of the prior art, muller-Bierl B, graf H, steidle G et al, medical physics, 32 (1): 76-84, 2005, written "Compensation of magnetic field disorders from paramagnetic information by encoded digital information: measurements and numerical simulations", compensated for the magnetic field distortions caused by paramagnetic devices by diamagnetic materials, investigated the ability of combining diamagnetic and paramagnetic materials in a coating manner to effectively reduce the size of electrode tip artifacts in a 1.5T magnetic resonance scan. However, magnetic field distortions cannot be completely avoided by means of coatings, and therefore artifact problems still remain in imaging at higher spatial resolutions. Kodama T, nakai R, goto K et al in Magnetic Resonance Imaging, 44: 38-45,2017, preparation of an Au-Pt alloy free from artifacts in Magnetic Resonance Imaging, showed that the artifacts produced by the homogeneous Au-35Pt alloy in Magnetic Resonance Imaging were less than 0.5 mm. However, the research mainly aims at a larger implant instead of a micro-implantable medical device, and a high-temperature annealing process is used in the preparation process, so that the high-temperature annealing process is not suitable for a high-precision micro-nano processing process and is limited in practical application.
In summary, although research on magnetic resonance compatible materials has been advanced to some extent, no conductive thin film material which is applicable to micro-nano processing technology and is compatible with magnetic resonance imaging is reported in the literature.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a conductive thin film alloy material which is applied to implantable instruments, neural interfaces and brain-computer interfaces and is compatible with magnetic resonance imaging and a preparation method thereof, is suitable for micro-nano processing technology, has better electrochemical properties and has no artifacts in magnetic resonance imaging. The magnetic resonance imaging compatibility means that after the electronic device prepared by processing the material is implanted into biological tissues, image artifacts and defects in the magnetic resonance imaging cannot be caused, even if the implanted material is in a magnetic resonance imaging area.
The invention provides a magnetic resonance imaging compatible conductive thin film alloy material, which is applied to implantable medical equipment, a neural interface or a brain-computer interface, a paramagnetic substance and a diamagnetic substance are used as co-sputtering materials, and the thin film alloy material is prepared by a micro-nano processing technology of magnetron co-sputtering coating, wherein the magnetic susceptibility of the material is close to the magnetic susceptibility (-11 to-7 ppm) of human tissues, so that the magnetic resonance imaging is free from artifacts. The co-sputtered materials are one paramagnetic species and one diamagnetic species. The invention is illustrated by using gold and platinum as examples, but not limited to these two materials.
In the invention, the film alloy material is a gold-platinum film alloy material, gold is a diamagnetic substance, and platinum is a paramagnetic substance.
In the gold-platinum thin film alloy material, the mass ratio of gold to platinum in the alloy is 3:7-9:4.
In the invention, the thickness of the gold-platinum thin film alloy material is 15-500nm.
In the invention, the volume magnetic susceptibility of the gold-platinum film alloy material is-29 to 11 ppm.
The invention also provides a preparation method of the conductive film alloy material, which comprises the following specific steps:
(1) Fixing target materials of paramagnetic substances and diamagnetic substances on a magnetron sputtering direct current or radio frequency target position; exposing the surfaces of the implantable device, the neural interface and the brain-computer interface which need to be subjected to the conductive film coating, putting the devices into a sputtering chamber, and vacuumizing the sputtering chamber;
(2) Introducing argon, and controlling the pressure of the argon to be stable;
(3) Respectively adjusting parameters of the sputtering current intensity, voltage, incident power and reflected power of paramagnetic substances and diamagnetic substances to ionize and glow argon, opening a baffle after sputtering parameters are stable, and starting a magnetron sputtering process;
(4) And (5) closing the sputtering power supply and ending the magnetron sputtering process.
In the invention, the paramagnetic substance is platinum, and the diamagnetic substance is gold.
In the invention, in the step (1), the sputtering chamber is vacuumized to 5 x 10 -4 Pascal or less; in the step (2), the flow rate of the introduced argon is controlled to be 10-25cm 3 In the range of/min, the pressure of argon is controlled between 0.05 and 0.5 pascal.
In the step (3), in the magnetron sputtering process, the incident sputtering power ratio of the diamagnetic substance to the paramagnetic substance is 1:5-1, and the reflection power is less than the corresponding incident power by 10%; the rotating speed of the sample stage is 5-10 r/min, which is beneficial to ensuring the uniformity of the film; the temperature range of the sample stage is 10-60 ℃, which is beneficial to ensuring the polycrystallinity of the film.
In the invention, in the step (3), the film sputtering rate is 15-80nm/min, the film thickness can be controlled by adjusting the sputtering duration, and the thickness of the conductive film can reach 15-500nm, so that the method is suitable for high-precision biological implant processing and preparation.
The invention also provides an implanted medical instrument, a nerve interface or a brain-computer interface with the conductive thin film alloy material coating, and imaging artifacts which affect the observation of an implanted part cannot be caused in the magnetic resonance imaging process.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a conductive film material compatible with magnetic resonance imaging according to the principle that gold is a diamagnetic material and platinum is a paramagnetic material, the conductive film material compatible with magnetic resonance imaging prepared by using specific parameters to sputter gold, platinum and specific air pressure has better electrochemical properties and is compatible with micro-nano processing technology, and implanted medical equipment, a nerve interface and a brain-computer interface prepared by using the conductive film material do not generate artifacts in magnetic resonance imaging.
Drawings
FIG. 1 is a graph of magnetic field strength versus magnetization for a representative MRI compatible gold-platinum alloy thin film material.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the concept of the invention. All falling within the scope of the present invention.
Example 1
The embodiment provides a specific preparation process for sputtering a gold-platinum alloy thin film coating with the thickness of 160 nanometers on a Parylene-C substrate:
(1) Depositing Parylene-C on a silicon wafer as a substrate material, and exposing the surface of a gold-platinum alloy film coating to be carried out; parylene-C is a biocompatible material commonly used in implantable medical devices, neural interfaces, or brain-machine interfaces;
(2) Respectively fixing gold and platinum targets on a magnetron sputtering target; putting the substrate material into a sputtering chamber, and vacuumizing the sputtering chamber to 2 x 10 by a vacuum pump and a molecular pump -4 Pascal;
(3) Introducing argon at a flow rate of 15 cubic centimeters per minute; adjusting the valve of the molecular pump to control the pressure of the argon gas to be stable
0.3 pascal;
(4) Respectively opening the sputtering target position baffle, adjusting the sputtering current intensity of the gold target to be 0.2 ampere and the sputtering current of the platinum target
The intensity is 0.15 ampere, so that the argon is ionized and started;
(5) The incident power of the gold target is adjusted to 250 watts, the incident power of the platinum target is adjusted to 150 watts, and the reflected power is smaller than the incident power
10% of;
(6) Adjusting a system cooling system, and controlling the temperature of the sample to be 25 ℃;
(7) After the sputtering parameters are stable, setting the rotation speed of the sample stage to be 5 revolutions per minute, opening the sample baffle, and starting
Performing magnetron sputtering; the sputtering time is 5 minutes;
(8) And (5) closing the sputtering power supply, closing the baffle plate and ending the magnetron sputtering process.
The gold-platinum alloy conductive film prepared by the embodiment has the advantages that the mass ratio of gold is 64.2%, the thickness of the metal layer is 160.22 nanometers, and no obvious imaging artifact is caused in magnetic resonance imaging. Fig. 1 shows a representative magnetic field strength versus magnetization curve for mri compatible gold-platinum alloy thin film materials. The magnetic susceptibility was-20.96 ppm, calculated from the data in the figure. The sheet resistance of the gold-platinum alloy conductive film is 0.15-1.39 ohm. The gold-platinum alloy conductive film is used as a conductive material to manufacture an electrode, the diameter of the electrode is 100 micrometers, and the electrochemical impedance at 1kHz is 100 k-1M ohm.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (6)
1. A conductive thin film alloy material compatible with magnetic resonance imaging is characterized by being applied to an implanted medical instrument, a neural interface or a brain-computer interface, a paramagnetic substance and a diamagnetic substance are used as co-sputtering materials, and a gold-platinum thin film alloy material is prepared by a micro-nano processing technology of magnetron co-sputtering coating, wherein the paramagnetic substance is platinum, the diamagnetic substance is gold, and the volume magnetic susceptibility of the gold-platinum thin film alloy material is-29 to 11 ppm.
2. The conductive thin film alloy material of claim 1, wherein the mass ratio of gold to platinum in the gold-platinum thin film alloy material is 3:7-9:4.
3. The conductive thin film alloy material as claimed in claim 1, wherein the thickness of the gold-platinum thin film alloy material is 15 to 500nm.
4. A method for preparing the conductive thin film alloy material according to any one of claims 1 to 3, which comprises the following steps:
(1) Fixing target materials of paramagnetic substances and diamagnetic substances on a magnetron sputtering direct current or radio frequency target position; exposing the surfaces of the implantable device, the neural interface and the brain-computer interface which need to be subjected to the conductive film coating, putting the devices into a sputtering chamber, and vacuumizing the sputtering chamber;
(2) Introducing argon, and controlling the pressure of the argon to be stable;
(3) Respectively adjusting the parameters of the sputtering current intensity, voltage, incident power and reflected power of paramagnetic substances and diamagnetic substances to ionize and glow argon, opening a baffle after the sputtering parameters are stable, and starting the magnetron sputtering process;
(4) Turning off the sputtering power supply and finishing the magnetron sputtering process; wherein:
in the step (1), the sputtering chamber is vacuumized to 5 x 10 -4 Pascal or less; in the step (2), the flow rate of the introduced argon is controlled to be 10-25cm 3 In the range of/min, the pressure of argon is controlled between 0.05 and 0.5 pascal; in the step (3), in the magnetron sputtering process, the incident sputtering power ratio of the diamagnetic substance to the paramagnetic substance is 1:5-1, the reflection power is less than 10% of the corresponding incident power, the rotation speed of the sample stage is 5-10 r/min, and the temperature range of the sample stage is 10-60 ℃; wherein:
the paramagnetic substance is platinum and the diamagnetic substance is gold.
5. The production method according to claim 4, wherein in the step (3), the film sputtering rate is 15 to 80nm/min.
6. An implantable medical device, neural interface or brain-computer interface having a coating of the conductive thin film alloy material of any one of claims 1-3.
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| US20050149002A1 (en) * | 2003-04-08 | 2005-07-07 | Xingwu Wang | Markers for visualizing interventional medical devices |
| US20050182482A1 (en) * | 2003-04-08 | 2005-08-18 | Xingwu Wang | MRI imageable medical device |
| JP5582484B1 (en) * | 2013-12-20 | 2014-09-03 | 田中貴金属工業株式会社 | Medical alloy and method for producing the same |
| CN104873215A (en) * | 2015-05-26 | 2015-09-02 | 上海奕瑞光电子科技有限公司 | Flat panel detector eliminating press image artifacts and manufacturing method thereof |
| CN105063427B (en) * | 2015-08-28 | 2017-03-22 | 中国科学院金属研究所 | Magnetic compatibility zinc alloy and application thereof |
| CN108183143A (en) * | 2017-12-27 | 2018-06-19 | 四川大学 | The technology of ultra-thin CdTe solar cells is prepared with more target radio frequency magnetron sputtering methods |
| CN113528883B (en) * | 2021-07-13 | 2022-05-20 | 上海理工大学 | Copper-niobium alloy for medical biopsy puncture needle |
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| MRI磁兼容合金研究;任伊宾等;《金属学报》;20171011(第10期);第175-182页 * |
| Reduction of magnetic resonance image artifacts of NiTi implant by carbon coating;Taeyang Han et al.;《Materials Science & Engineering C》;20181222;第1-8页 * |
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