CN113851253A - Magnetic resonance imaging compatible conductive paste compound and preparation method thereof - Google Patents
Magnetic resonance imaging compatible conductive paste compound and preparation method thereof Download PDFInfo
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- CN113851253A CN113851253A CN202110981747.XA CN202110981747A CN113851253A CN 113851253 A CN113851253 A CN 113851253A CN 202110981747 A CN202110981747 A CN 202110981747A CN 113851253 A CN113851253 A CN 113851253A
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- magnetic resonance
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- synthetic resin
- metal powder
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- 238000002595 magnetic resonance imaging Methods 0.000 title claims abstract description 39
- 150000001875 compounds Chemical class 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 30
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 19
- 239000000057 synthetic resin Substances 0.000 claims abstract description 19
- 150000003377 silicon compounds Chemical class 0.000 claims abstract description 18
- 229910052709 silver Inorganic materials 0.000 claims abstract description 17
- 239000004332 silver Substances 0.000 claims abstract description 17
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 17
- 239000010937 tungsten Substances 0.000 claims abstract description 17
- 238000007650 screen-printing Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 24
- 229910052751 metal Inorganic materials 0.000 claims description 21
- 239000002184 metal Substances 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 18
- 239000003085 diluting agent Substances 0.000 claims description 16
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 9
- 230000010358 mechanical oscillation Effects 0.000 claims description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 7
- 230000010355 oscillation Effects 0.000 claims description 7
- 230000001537 neural effect Effects 0.000 claims description 6
- 229920002379 silicone rubber Polymers 0.000 claims description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004944 Liquid Silicone Rubber Substances 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- 239000009719 polyimide resin Substances 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 239000004945 silicone rubber Substances 0.000 claims description 2
- 150000003961 organosilicon compounds Chemical class 0.000 claims 2
- 229920006337 unsaturated polyester resin Polymers 0.000 claims 1
- 238000003745 diagnosis Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 15
- 238000005303 weighing Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- -1 conductive silver paste compound Chemical class 0.000 description 4
- 230000005415 magnetization Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 3
- 239000007943 implant Substances 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910001260 Pt alloy Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000013528 metallic particle Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000012217 deletion Methods 0.000 description 1
- 230000037430 deletion Effects 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 238000013421 nuclear magnetic resonance imaging Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
Abstract
The invention discloses a magnetic resonance imaging compatible conductive paste compound and a preparation method thereof. The conductive paste compound compatible with magnetic resonance imaging is a compound of silver and tungsten nanoparticles and synthetic resin or organic silicon compound, wherein the magnetic resonance imaging compatibility means that after an 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 conductive paste compound formed by the invention can keep good conductive performance and biocompatibility while improving the magnetic resonance compatibility, can be placed on a required position by screen printing or dispensing and other methods, and can be cured according to the properties of synthetic resin or organic silicon compound materials, so that medical and electronic instruments applying the conductive paste compound do not interfere with related magnetic resonance imaging detection and diagnosis after being implanted.
Description
Technical Field
The invention relates to a conductive slurry compound in the technical field of medical instruments, biomedical engineering and micro-nano processing, in particular to a magnetic resonance imaging compatible conductive slurry applied to implantable medical electronic instruments and a preparation method thereof.
Background
In recent years, magnetic resonance imaging and implantable electronic devices have been developed into reliable medical diagnosis and auxiliary treatment means, respectively, but the application of the two devices can cause mutual influence due to electromagnetic induction and even cause safety problems. With the continuous and deep research on implantable medical devices, nerve interfaces and brain-computer interfaces compatible with magnetic resonance imaging, the safety risks such as torsion and thermal injury caused by implants are gradually reduced. However, the great difference between the magnetization properties of the implant and the biological tissue can cause the magnetic field distortion of the implant in the magnetic resonance imaging environment, thereby generating imaging artifacts and image deletion, which affect the clinical application of magnetic resonance imaging diagnosis. There have been some studies directed to optimizing implantable probes for medical devices to reduce the effects of magnetic resonance artifacts. Notably, the conductive paste composition used in the implanted electronics can also cause magnetic resonance imaging artifacts. The conductive paste composite is an important material for connecting conductive elements such as chips, devices and electrodes in implantable electronic devices, and is indispensable for implantable electronic devices. Therefore, there is a need for a magnetic resonance imaging compatible conductive paste composition for reducing artifacts in medical images of implantable medical devices.
Based on a search of the prior art, Kodama T, Nakai R, Goto K et al, Magnetic Resonance Imaging, 44: 38-45,2017, written "Preparation of an Au-Pt alloy free from artifacts in Magnetic Resonance Imaging", indicated that homogeneous Au-Pt alloy cylinders 3mm in diameter and 8mm in length (Au: Pt = 65:35, wt%) produced negligible artifacts in Magnetic Resonance Imaging compared to other biocompatible metallic material cylinders such as pure gold, pure platinum, etc. The research indicates that bulk alloys (bulk materials) of different magnetizable materials can be prepared into magnetic resonance imaging compatible materials through high-temperature annealing and other processes. However, the research does not provide a corresponding preparation method for the conductive paste compound compatible with magnetic resonance imaging, and the practical application is limited.
In summary, although research on magnetic resonance compatible materials has been advanced, no conductive paste compound capable of achieving magnetic resonance imaging compatibility is reported in the literature.
Disclosure of Invention
Aiming at the actual requirements of an implanted electronic device and the defects in the prior art, the invention aims to provide a conductive paste compound which is compatible with magnetic resonance imaging and is applied to the implanted device and a preparation method thereof. Has better conductivity and biocompatibility and has no artifact 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 paste compound which comprises a metal powder material, wherein the metal powder material is composed of silver and tungsten, and the mass ratio of the silver to the tungsten is 1: 1-18: 1.
Preferably, the particle diameter of the silver and tungsten in the metal powder material is in the range of 0.1 to 10 μm.
Preferably, in the metal powder material, the ratio of the diameters of the silver particles to the tungsten particles is 1: 4-5: 1.
Preferably, the metal powder material further comprises synthetic resin or organic silicon compound, wherein the mass of the metal powder material is 10% -95%, and the mass of the synthetic resin or organic silicon compound is 5% -90%, based on 100% of the total mass of the metal powder material and the synthetic resin or organic silicon compound.
Preferably, the metal powder material also comprises a diluent, and the diluent accounts for 5-30% of the total mass of the metal powder material, the synthetic resin or the organic silicon compound and the diluent.
Preferably, the magnetic susceptibility is in the range of-70 to 60 ppm.
The invention also provides a preparation method of the conductive paste compound compatible with magnetic resonance imaging, which comprises the following specific steps:
(1) uniformly mixing the diluent with the synthetic resin or the organic silicon compound; the diluent comprises weak polar organic solvents such as n-heptane, n-hexane, cyclohexane and the like. Synthetic resins include epoxy resins, unsaturated polyesters, polyimide resins, and the like; the organic silicon compound includes silane coupling agent, silicone oil, high temperature vulcanized silicone rubber, liquid silicone rubber, etc.
(2) Mixing silver and tungsten nano metal powder, and adding the mixture into the mixture;
(3) uniformly mixing the mixture by ultrasonic oscillation or mechanical oscillation;
(4) the diluent was partially discharged to bring the mixture to a viscosity suitable for handling, in the range of 500-.
Preferably, in the step (3), the frequency range of the ultrasonic oscillation is 30-75 kHz, and the frequency range of the mechanical oscillation is 10-1000 Hz.
The invention further provides an implanted medical device, a neural interface or a brain-computer interface which is prepared by processing the conductive paste compound compatible with the magnetic resonance imaging. Preferably, the conductive paste compound compatible with magnetic resonance imaging is prepared by placing the conductive paste compound on a required position through screen printing or dispensing and curing according to the properties of the synthetic resin or the organic silicon compound material.
Compared with the prior art, the invention has the following beneficial effects:
the invention utilizes the opposite magnetization properties of different metal nano particles, and silver and tungsten nano particles in a certain proportion are mixed with synthetic resin or an organic silicon compound to form a conductive paste compound by optimizing the proportion, so that the magnetic resonance compatibility is improved, meanwhile, the good conductive performance and the biocompatibility are kept, the conductive paste compound can be placed on a required position by screen printing or dispensing and other methods, and the conductive paste compound can be solidified according to the material properties of the synthetic resin or the organic silicon compound, so that the medical electronic instrument applying the conductive paste compound does not interfere with the related magnetic resonance imaging detection and diagnosis after being implanted.
The conductive paste compound compatible with magnetic resonance imaging is prepared by using silver-tungsten-resin/organic silicon-diluent in a specific ratio, has better conductive property and lower manufacturing cost. The implanted medical device prepared by the conductive paste compound does not generate artifacts in magnetic resonance imaging.
Drawings
Fig. 1 is a graph of representative magnetic field strength versus magnetization for an organosilicon composite of nano-metallic particles of silver and tungsten.
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 spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment provides a conductive silver paste compound compatible with magnetic resonance imaging and applied to an implanted neural electrode, namely an organic silicon compound containing nano metal particles of silver and tungsten, specifically:
(1) weighing 60 parts of cyclohexane and 30 parts of polydimethylsiloxane in parts by weight, and uniformly stirring and mixing;
(2) weighing 45 parts of silver powder with the particle size of 500 nanometers and 15 parts of tungsten powder with the particle size of 400 nanometers in parts by weight,
fully shaking and mixing the metal powder;
(3) uniformly mixing the mixture in a mechanical oscillation and ultrasonic oscillation mode;
(4) vacuumizing, and discharging the cyclohexane part to ensure that the mixture reaches the viscosity suitable for operation;
(5) storing at 0-4 deg.C.
As shown in fig. 1, which is a representative magnetic field strength versus magnetization curve for an organosilicon composite of nano-metallic particles of silver and tungsten, the test data is from example 1 and has a magnetic susceptibility of-8.98 ppm. According to different mixing degrees and the residual quantity of the diluent, the line width of the screen printing of the compound is 50-1000 microns, and the square resistance of the compound is 0.1-50 ohms.
Example 2
The embodiment provides a conductive silver paste compound compatible with magnetic resonance imaging and applied to an implanted neural electrode, namely a synthetic resin compound containing nano metal particles of silver and tungsten, specifically:
(1) weighing 60 parts of n-heptane and 30 parts of epoxy resin by weight, and uniformly stirring and mixing;
(2) weighing 45 parts of silver powder with the particle size of 2500 nanometers and 15 parts of tungsten powder with the particle size of 10000 nanometers in parts by weight,
fully shaking and mixing the metal powder;
(3) uniformly mixing the mixture in a mechanical oscillation and ultrasonic oscillation mode;
(4) vacuumizing, and discharging a part of n-heptane to enable the mixture to reach a viscosity suitable for operation;
(5) storing at 0-4 deg.C.
The magnetic susceptibility of example 2 was-10.52 ppm. According to different mixing degrees and the residual quantity of the diluent, the compound silk
The screen printed line width was 100-1000 microns and the square resistance of the composite was 0.25-200 ohms.
Example 3
The embodiment provides a conductive silver paste compound compatible with magnetic resonance imaging and applied to an implanted neural electrode, namely an organic silicon compound containing nano metal particles of silver and tungsten, specifically:
(1) weighing 60 parts of normal hexane and 30 parts of liquid silicone rubber in parts by weight, and uniformly stirring and mixing;
(2) weighing 45 parts of silver powder with the grain diameter of 10000 nanometers and 15 parts of tungsten powder with the grain diameter of 2000 nanometers in parts by weight,
fully shaking and mixing the metal powder;
(3) uniformly mixing the mixture in a mechanical oscillation and ultrasonic oscillation mode;
(4) vacuumizing, and partially discharging n-hexane to ensure that the mixture reaches a viscosity suitable for operation;
(5) storing at 0-4 deg.C.
The magnetic susceptibility of example 3 was-18.65 ppm. According to different mixing degrees and the residual quantity of the diluent, the compound silk
The screen printed line width was 200-1000 microns and the square resistance of the composite was 0.5-500 ohms.
In conclusion, the conductive silver paste compatible with nuclear magnetic resonance imaging, which is prepared by using the materials in the proportion and the preparation method thereof, has better conductive property and is free from artifacts in the magnetic resonance imaging.
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 (10)
1. The conductive paste compound compatible with magnetic resonance imaging is characterized by comprising a metal powder material, wherein the metal powder material is composed of silver and tungsten, and the mass ratio of the silver to the tungsten is 1: 1-18: 1.
2. The conductive paste composition according to claim 1, wherein the particle diameters of the silver and the tungsten in the metal powder material are in the range of 0.1 to 10 μm.
3. The conductive paste composition according to claim 1, wherein the ratio of the silver to tungsten particles in the metal powder material is between 1:4 and 5: 1.
4. The electroconductive paste composition according to claim 1, further comprising a synthetic resin or an organic silicon compound, wherein the mass of the metal powder material is 10% to 95% and the mass of the synthetic resin or the organic silicon compound is 5% to 90%, based on 100% of the total mass of the metal powder material and the synthetic resin or the organic silicon compound.
5. The electroconductive paste composition according to claim 1, further comprising a diluent, wherein the diluent accounts for 5 to 30% of the total mass of the metal powder material, the synthetic resin or the organosilicon compound and the diluent.
6. The electroconductive paste composition according to claim 1, wherein the magnetic susceptibility is in the range of-70 to 60 ppm.
7. The preparation method of the conductive paste composition according to claim 1, comprising the following steps:
(1) uniformly mixing the diluent with the synthetic resin or the organic silicon compound;
(2) mixing silver and tungsten nano metal powder, and adding the mixture into the mixture;
(3) uniformly mixing the mixture by ultrasonic oscillation or mechanical oscillation;
(4) the diluent is partially drained to bring the mixture to a viscosity suitable for handling.
8. The preparation method according to claim 7, wherein in the step (1), the diluent is selected from one or more of n-heptane, n-hexane and cyclohexane; the synthetic resin is selected from one or more of epoxy resin, unsaturated polyester or polyimide resin; the organic silicon compound is selected from any one or more of silane coupling agent, silicone oil, high-temperature vulcanized silicone rubber or liquid silicone rubber; in the step (3), the frequency range of ultrasonic oscillation is 30-75 kHz, and the frequency range of mechanical oscillation is 10-1000 Hz.
9. An implantable medical device, a neural interface, or a brain-computer interface fabricated based on the magnetic resonance imaging compatible electroconductive paste composition of claim 1.
10. The implantable medical device, neural interface or brain-computer interface according to claim 9, wherein the mri compatible conductive paste composition is prepared by placing it on a desired site by screen printing or dispensing, and curing it according to the properties of the synthetic resin or organosilicon compound material.
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JPH11111052A (en) * | 1997-10-07 | 1999-04-23 | Ngk Spark Plug Co Ltd | Conductive paste composition, manufacture of conductive paste composition, surface layer conductor forming method, and ceramic multi-layer substrate |
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US20110130807A1 (en) * | 2009-12-01 | 2011-06-02 | Nidek Co., Ltd. | Vision regeneration assist apparatus and implantable apparatus |
WO2017006714A1 (en) * | 2015-07-03 | 2017-01-12 | 株式会社村田製作所 | Electroconductive paste, and glass article |
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CN113025230A (en) * | 2021-03-10 | 2021-06-25 | 中国电子科技集团公司第三十八研究所 | Heat-conducting and electric-conducting copper paste, preparation method and application thereof |
CN113099603A (en) * | 2017-12-29 | 2021-07-09 | 深圳硅基仿生科技有限公司 | Ceramic substrate for implantable medical device and method for manufacturing same |
WO2021141163A1 (en) * | 2020-01-09 | 2021-07-15 | 서울시립대학교 산학협력단 | Deep brain stimulation transparent electrode array and neural signal detection method using same |
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2021
- 2021-08-25 CN CN202110981747.XA patent/CN113851253A/en active Pending
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JPH11111052A (en) * | 1997-10-07 | 1999-04-23 | Ngk Spark Plug Co Ltd | Conductive paste composition, manufacture of conductive paste composition, surface layer conductor forming method, and ceramic multi-layer substrate |
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