CN102095746B - Micro solenoid radio frequency coil for microfluid nuclear magnetic resonance detection and manufacturing method thereof - Google Patents
Micro solenoid radio frequency coil for microfluid nuclear magnetic resonance detection and manufacturing method thereof Download PDFInfo
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- CN102095746B CN102095746B CN 201010589840 CN201010589840A CN102095746B CN 102095746 B CN102095746 B CN 102095746B CN 201010589840 CN201010589840 CN 201010589840 CN 201010589840 A CN201010589840 A CN 201010589840A CN 102095746 B CN102095746 B CN 102095746B
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Abstract
The invention relates to a micro solenoid radio frequency coil for microfluid nuclear magnetic resonance detection and a manufacturing method thereof. The micro solenoid radio frequency coil comprises a bottom slanted-bar coil, left and right rows of bottom coils, cylindrical coils, a microfluid passage and a top slanted-bar coil, wherein the bottom slanted-bar coil and the left and right rows ofbottom coils are positioned on an insulating substrate; the cylindrical coils are arranged on the top parts of the bottom coils; the mocrofluid passage is positioned between the left and right rows of bottom coils; the top slanted-bar coil is positioned above the microfluid passage; both ends of the bottom slanted-bar coil are respectively connected with the left and right rows of bottom coils ina staggered mode; both ends of the top slanted-bar coil are respectively connected with the cylindrical coils arranged on the top parts of the bottom coils in a staggered mode; and the inclination directions of the bottom slanted-bar coil and the top slanted-bar coil are opposite to each other. In the invention, the micro solenoid radio frequency coil is manufactured by a photoresist photoetchingtechnology and a copper electroplating coil technology; the defect that a micro-scale solenoid radio frequency coil is difficult to wind is overcome; and the micro solenoid radio frequency coil has the advantages of high uniformity of a radio frequency magnetic field and the like and can be used for nuclear magnetic resonance detection of rare and precious samples.
Description
Technical field
The present invention relates to a kind of radio-frequency coil for the microfluid magnetic resonance detection, particularly the uniform radio frequency miniature coils of solenoid type Distribution of Magnetic Field and manufacture method thereof.
Background technology
The nuclear magnetic resonance spectrum detection technique has non-destructive to sample, thereby is widely used in chemistry, biomedicine and material science.NMR RF coil can use the transmitting-receiving separate type or possess simultaneously the coil of transceiver, emission function is launch pulse sequence with the magnetization vector of excitation sample, and receiving function is to receive the free induction decay signal that excites spin and produce.Signal is carried out Fourier transform can obtain nuclear magnetic resonance spectrum figure, always obtain the one-tenth grading information of sample.According to different applications, general radio-frequency coil has solenoid coil, planar coil, saddle coil, birdcage coil, butterfly shaped coils and phase array coil etc.(Hoult, D.I.and R.E.Richards, SIGNAL-TO-NOISE RATIO OF NUCLEARMAGNETIC-RESONANCE EXPERIMENT.Journal of Magnetic Resonance, 1976.24 (1): p.71-85.) discussed in the document and compare the other types coil, solenoid has the advantages such as high sensitivity, Distribution of Magnetic Field be even, so the nuclear magnetic resonance spectrum detection technique of conventional commercial usefulness is that the employing aperture is the probe of 5mm now, namely adopts at glass capillary and twine wire formation solenoid coil.Its sample detection limit is approximately 5 * 10
9Mol far is worse than other detection techniques such as Infrared spectroscopy, mass spectrophotometry etc.(Peck, T.L., R.L.Magin, and P.C.Lauterbur, DESIGN AND ANALYSIS OF MICROCOILS FOR NMRMICROSCOPY.Journal of Magnetic Resonance Series B, 1995.108 (2): p.114-124.) during theoretical in the document and the about 100um of experimental verification coil diameter, unit volume sample signal to noise ratio (S/N ratio) (S/N) is inversely proportional to coil diameter; During less than 100um, be inversely proportional to the square root of coil diameter, so occur using miniature coils to improve sensitivity in a lot of document.But winding method is difficult for realizing under microscale, thereby is difficult for making the Minitype solenoid coil.(Massin, C., et al., Planar microcoil-based microfluidic NMR probes.Journal ofMagnetic Resonance, 2003.164 (2): p.242-255.) document causes numerous focus of attentions, tells about in the document based on the micro-example solution in the nmr probe detection microchannel of little planar spiral winding.Proposing the earliest micro-planar coil is applied to the nuclear magnetic resonance spectrum detection technique is document (Peck, T.T., et al., NMRMICROSPECTROSCOPY USING 100-MU-M PLANAR RF-COILS FABRICATEDON GALLIUM-ARSENIDE SUBSTRATES.Ieee Transactions on BiomedicalEngineering, 1994.41 (7): p.706-709.).Sensitivity is low although plane micro coil has, the radio-frequency (RF) magnetic field lack of homogeneity, and below micron-scale, it can carry out the robotization mass production by little manufacturing photoetching technique of modern times; In addition, plane micro coil easily is combined with the microfluid system based on chip, so that operation microfluid and the integrated performance of increase.With Massin, the Ehrmann of the same research group of C., K. proposes to use MEMS fabrication techniques solenoid coil and Helmholtz coils at 2006-2007, and applies it to the nuclear magnetic resoance spectrum detection of mammalian cell.
Domestic researcher such as Wang Ming, Li Xiaonan etc. number are in 200610164809.3,200710179309.1,200910081526.6 etc. in Chinese patent application, and design and manufacturing nuclear magnetic resonance miniature planar helical RF coil in the document " receiving the design of the little detection of upgrading biological sample nuclear magnetic resonance with the high s/n ratio plane micro coil. ", " based on the high Q value nuclear magnetic resonance plane micro coil of MEMS " etc.What Chinese patent 200910091597.4 " a kind of nuclear magnetic resonance radio-frequency micro-coil and preparation method thereof " then related to is Helmholtz's type (saddle type) nuclear magnetic resonance radio-frequency micro-coil, but produce onesize radio-frequency (RF) magnetic field, the resistance of Helmholtz's type (saddle type) nuclear magnetic resonance radio-frequency micro-coil is larger than Minitype solenoid radio-frequency coil, thereby signal to noise ratio (S/N ratio) will less.
Summary of the invention
What the present invention will solve is that existing conventional microfluid detection is difficult for being fit to use micro-example to detect; Miniature planar spiral winding radio-frequency (RF) magnetic field is inhomogeneous and sensitivity is low; The Minitype solenoid coil is difficult for using conventional winding method manufacturing; And producing onesize radio-frequency (RF) magnetic field, the resistance of Helmholtz's type (saddle type) coil has reduced greatly the problems such as signal to noise ratio (S/N ratio).
For solving the problems of the technologies described above, the invention provides a kind of Minitype solenoid radio-frequency coil, being used for the nuclear magnetic resonance microfluid detects, this radio-frequency coil comprise the bottom oblique strip shaped coil that is positioned on the dielectric substrate, about two row's bottom coil, be arranged on the cylindrical solenoid at bottom coil top, about the microchannels of two rows between the bottom coil, and the top layer oblique strip shaped coil that is positioned at the microchannel top; The two ends of bottom oblique strip shaped coil respectively with about two row's bottom coil dislocation be connected, the two ends of top layer oblique strip shaped coil link to each other with the cylindrical solenoid dislocation that is arranged on the bottom coil top respectively, and the vergence direction of bottom oblique strip shaped coil and top layer oblique strip shaped coil is opposite.
Do signal to noise ratio (S/N ratio) of the present invention for carrying, above-mentioned bottom oblique strip shaped coil, bottom coil, cylindrical solenoid and top layer oblique strip shaped coil all adopt the Low ESR metal material to make, not only conductance is high and cheap owing to copper, excellent corrosion resistance, easily be combined with integrated circuit, so the coil method preferably copper.
Above-mentioned microchannel adopts glass capillary, and its cross sectional shape is preferably square, is used for placing sample.
Because traditional silicon substrate mechanical property is more crisp and cost is expensive, therefore the dielectric substrate of stating of the present invention selects pyroceram or other stable on heating polymeric materials that insulate to make, the insulation lining substrate that adopts previous materials to make has bio-compatibility, cost is low, and the capacitance to substrate that produces between the coil (substrate capacitance) is less, thereby and on the less power consumption penalty that reduces of the impact of the conduction current in the coil.
Above-mentioned bottom coil is identical with the every row's of cylindrical solenoid quantity, is n, and bottom oblique strip shaped coil is identical with the quantity of top layer oblique strip shaped coil, is n-1, and n is the natural number greater than 1.
Manufacture method of the present invention is mainly electroplated Coil technique based on photoresist photoetching technique and copper, specifically comprises the steps:
1, at dielectric substrate precipitation one deck photoresist;
2, settled photoresist is carried out the ultraviolet lithography irradiation, two row's grooves are filled the Low ESR metal material with plating mode again about formation in groove, two row's bottom coil about formation;
3, to about the photoresist of two rows in the middle of the bottom coil carry out photoetching, form the oblique strip shaped groove, then in groove, fill the Low ESR metal material with plating mode, form bottom oblique strip shaped coil;
4, do not precipitate again one deck photoresist on the photoresist of photoetching in the bottom coil of having plated and bottom coil both sides;
5, the ultraviolet lithography irradiation is carried out in the photoresist of step 4 precipitation, form cylindrical groove, in groove, fill the Low ESR metal material with plating mode again, form two organ timbering shape coils;
6, the photoresist between the two organ timbering line coils is carried out the ultraviolet lithography irradiation, form the oblique strip shaped groove, then in groove, fill the Low ESR metal material with plating mode, form top layer oblique strip shaped coil;
7, from a side photoresist that is positioned at bottom oblique strip shaped coil and top layer oblique strip shaped coil is carried out the ultraviolet lithography irradiation, form a center line perpendicular to the through hole of cylindrical solenoid, again microchannel is placed aforementioned through-hole, namely make finished product.
The present invention can also adopt the following steps manufacturing:
1, at dielectric substrate precipitation one deck photoresist;
2, settled photoresist is carried out the ultraviolet lithography irradiation, two row's grooves are filled the Low ESR metal material with plating mode again about formation in groove, two row's bottom coil about formation;
3, to about the photoresists of two rows in the middle of the bottom coil carry out photoetching, forms six oblique strip shaped grooves, then in groove, fill the Low ESR metal material with plating mode, formation bottom oblique strip shaped coil;
4, do not precipitate again one deck photoresist on the photoresist of photoetching in the bottom coil of having plated and bottom coil both sides;
5, the ultraviolet lithography irradiation is carried out in the photoresist of step 4 precipitation, form cylindrical groove, in groove, fill the Low ESR metal material with plating mode again, form two organ timbering shape coils;
6, microchannel is placed between the two organ timbering shape coils, then parallel with the top of post line coil to its top at microchannel precipitation photoresist, again photoresist is carried out the ultraviolet lithography irradiation, form the oblique strip shaped groove, then in groove, fill the Low ESR metal material with plating mode, form top layer oblique strip shaped coil, namely make finished product.
Microchannel should adopt heat-resisting capillary glass material when adopting this method.
Because the SU-8 photoresist is compared with the other types photoresist, can make the MEMS microstructure (namely referring to coil among the present invention) of high-aspect-ratio; Have good mechanical property and thermal stability; Non-conductive, when electroplating, can directly insulate.Therefore the photoresist that adopts in two kinds of methods is preferred SU-8 photoresist all
The present invention can carry out the robotization mass production with photoetching and electroplating technology in little manufacturing of modern times, can produce uniform radio-frequency (RF) magnetic field, and its coil section size is particularly suitable for the detection of rare and valuable sample tens to the hundreds of micron dimension.
Description of drawings
Describe the present invention below in conjunction with accompanying drawing and instantiation, but not as a limitation of the invention.
Fig. 1 is structural representation of the present invention.
Fig. 2 a is the schematic diagram of method for making step 1 of the present invention.
Fig. 2 b and Fig. 2 c are the schematic diagram of method for making step 2 of the present invention.
Fig. 2 d is the schematic diagram of method for making step 3 of the present invention.
Fig. 2 e is the schematic diagram of method for making step 4 of the present invention.
Fig. 2 f and Fig. 2 g are the schematic diagram of method for making step 5 of the present invention.
Fig. 2 h and Fig. 2 i are the schematic diagram of method for making step 6 of the present invention and 7.
Embodiment
Referring to Fig. 1, the dielectric substrate of the present embodiment (1) is a rectangle thin plate, adopt the pyroceram material, the microchannel (4) that is used for the placement sample is square glass capillary, about two row bottom coil (7) every rows have 7, the every row of cylindrical solenoid (3) who is arranged on accordingly bottom coil (7) top also is 7, the bottom oblique strip shaped coil (2) that connects two row's bottom coil (7) is 6 with the top layer oblique strip shaped coil (5) that is connected two organ timbering shape coils (3), and wherein the vergence direction of bottom oblique strip shaped coil (2) and top layer oblique strip shaped coil (5) is opposite.The material of above-mentioned coil adopts copper, and number of turn of the rear formation that is connected to each other is six solenoid coil.
Referring to Fig. 2 a--2i, the manufacture method of the present embodiment is as follows:
1, the SU-8 photoresist (6) with 20 micron thick is deposited to dielectric substrate (1) upward (referring to Figure 42 a);
2, settled photoresist is carried out the ultraviolet lithography irradiation, totally seven pairs groove (referring to Fig. 2 b) about formation, fill the Low ESR metal material with plating mode in groove again, form 20 microns high left and right sides bottom coil (7), totally seven to (in Fig. 2 c);
3, to about photoresists in the middle of two rows bottom coil (7) carry out photoetching, form six oblique strip shaped grooves, then in groove, fill the Low ESR metal material with plating mode, form six bottom oblique strip shaped coils (2) (referring to Fig. 2 d) of 20 microns high;
4, do not precipitate again the SU-8 photoresist (referring to Fig. 2 e) of one deck 80 micron thick on the photoresist of photoetching in the bottom coil of having plated (7), oblique strip shaped coil (2) and bottom coil (7) both sides;
5, the photoresist of step 4 precipitation carried out the ultraviolet lithography irradiation, form 80 microns dark cylindrical groove referring to (Fig. 2 f), fill the Low ESR metal material with plating mode in groove again, form two row's 80 microns high cylindrical solenoids (3), totally seven to (referring to Fig. 2 g);
6, the SU-8 photoresist between the two organ timbering line coils (3) is carried out the ultraviolet lithography irradiation, form six oblique strip shaped grooves (referring to Fig. 2 h), then in groove, fill the Low ESR metal material with plating mode, form six top layer oblique strip shaped coils (5) (referring to Fig. 2 i);
Seven pairs of left and right sides bottom coil in the step (2), six oblique strip shaped coils in the step (3), seven pairs of cylindrical solenoids about step (5), and six top layer oblique strip shaped coils in the step (6) are around the solenoid coil that forms six circles;
7, referring to Fig. 2 i, from positive (or back side) direction six circle solenoids are carried out the ultraviolet lithography irradiation around the photoresist that the photoresist that surrounds is positioned at bottom oblique strip shaped coil (2) and top layer oblique strip shaped coil (5), form a center line perpendicular to the square hole of cylindrical solenoid (3), again square glass capillary is inserted in the square through hole, form microchannel (4), namely make finished product.
Principle of work of the present utility model is:
Sample in the microchannel (4) is placed main field, and sample shows magnetization vector just by magnetic polarization on the macroscopic view; Apply electric current to Minitype solenoid radio-frequency coil again, generation is perpendicular to main field and uniformity coefficient radio-frequency (RF) magnetic field preferably, radio-frequency (RF) magnetic field makes the atomic nucleus in the sample produce consistent flip angle uniformly, be that atomic nucleus in the sample carries out synchronous precession, synchronously precession makes sample show Mxy in macroscopic view, Mxy produces induction electromotive force in Minitype solenoid radio-frequency coil, obtain free induction decay signal after record a period of time, again free induction decay signal is carried out Fourier transform, obtain nuclear magnetic resonance spectrum figure.
Claims (8)
1. Minitype solenoid radio-frequency coil that is used for the microfluid magnetic resonance detection, it is characterized in that comprising the bottom oblique strip shaped coil (2) that is positioned on the dielectric substrate (1), about two row's bottom coil (7), be arranged on the cylindrical solenoid (3) at bottom coil (7) top, microchannel (4) about being positioned between two row's bottom coil (7), and the top layer oblique strip shaped coil (5) that is positioned at microchannel (4) top; The two ends of bottom oblique strip shaped coil (2) respectively with about two row bottom coil (7) dislocation be connected, the two ends of top layer oblique strip shaped coil (5) link to each other with cylindrical solenoid (3) dislocation that is arranged on bottom coil (7) top respectively, and the vergence direction of bottom oblique strip shaped coil (2) and top layer oblique strip shaped coil (5) is opposite.
2. the Minitype solenoid radio-frequency coil for the microfluid magnetic resonance detection according to claim 1 is characterized in that described bottom oblique strip shaped coil (2), bottom coil (7), cylindrical solenoid (3) and top layer oblique strip shaped coil (5) all adopt the Low ESR metal material to make.
3. the Minitype solenoid radio-frequency coil for the microfluid magnetic resonance detection according to claim 1 is characterized in that described microchannel (4) is glass capillary.
4. the Minitype solenoid radio-frequency coil for the microfluid magnetic resonance detection according to claim 1 is characterized in that described dielectric substrate (1) is made of pyroceram or other stable on heating polymeric materials that insulate.
5. such as the described Minitype solenoid radio-frequency coil for the microfluid magnetic resonance detection of claim 1 to 4 any one, it is characterized in that every row's bottom coil (7) is identical with the quantity of cylindrical solenoid (3), be n, bottom oblique strip shaped coil (2) is identical with the quantity of top layer oblique strip shaped coil (5), be n-1, aforementioned n is the natural number greater than 1.
6. the Minitype solenoid radio-frequency coil for the microfluid magnetic resonance detection as claimed in claim 5, the quantity that it is characterized in that every row's bottom coil (7) and cylindrical solenoid (3) is 7, the quantity of bottom oblique strip shaped coil (2) and top layer oblique strip shaped coil (5) is 6, jointly consists of a number of turn and be six solenoid coil.
7. the manufacture method of the described Minitype solenoid radio-frequency coil for the microfluid magnetic resonance detection of claim 1 to 6 any one is characterized in that comprising the steps:
(1) at dielectric substrate (1) precipitation one deck photoresist (6);
(2) settled photoresist is carried out the ultraviolet lithography irradiation, two row's grooves are filled the Low ESR metal material with plating mode again about formation in groove, two row's bottom coil (7) about formation;
(3) to about photoresists in the middle of two rows bottom coil (7) carry out photoetching, forms six oblique strip shaped grooves, then in groove, fill the Low ESR metal material with plating mode, formation bottom oblique strip shaped coil (2);
(4) do not precipitate again one deck photoresist on the photoresist of photoetching in the bottom coil of having plated (7) and bottom coil (7) both sides;
(5) the ultraviolet lithography irradiation is carried out in the photoresist of step (4) precipitation, form cylindrical groove, in groove, fill the Low ESR metal material with plating mode again, form two organ timbering shape coils (3);
(6) photoresist between the two organ timbering line coils (3) is carried out the ultraviolet lithography irradiation, form the oblique strip shaped groove, then in groove, fill the Low ESR metal material with plating mode, form top layer oblique strip shaped coil (5);
(7) from a side photoresist that is positioned at bottom oblique strip shaped coil (2) and top layer oblique strip shaped coil (5) is carried out the ultraviolet lithography irradiation, form a center line perpendicular to the through hole of cylindrical solenoid (3), again microchannel (4) is placed aforementioned through-hole, namely make finished product.
8. the manufacture method of the described Minitype solenoid radio-frequency coil for the microfluid magnetic resonance detection of claim 1 to 6 any one is characterized in that comprising the steps:
(1) at dielectric substrate (1) precipitation one deck photoresist (6);
(2) settled photoresist is carried out the ultraviolet lithography irradiation, two row's grooves are filled the Low ESR metal material with plating mode again about formation in groove, two row's bottom coil (7) about formation;
(3) to about photoresist in the middle of two rows bottom coil (7) carry out photoetching, form the oblique strip shaped groove, then in groove, fill the Low ESR metal material with plating mode, form bottom oblique strip shaped coil (2);
(4) do not precipitate again one deck photoresist on the photoresist of photoetching in the bottom coil of having plated (7) and bottom coil (7) both sides;
(5) the ultraviolet lithography irradiation is carried out in the photoresist of step (4) precipitation, form cylindrical groove, in groove, fill the Low ESR metal material with plating mode again, form two organ timbering shape coils (3);
(6) microchannel (4) is placed between the two organ timbering shape coils (3), then parallel with the top of post line coil (3) to its top at microchannel (4) precipitation photoresist, again photoresist is carried out the ultraviolet lithography irradiation, form the oblique strip shaped groove, then in groove, fill the Low ESR metal material with plating mode, form top layer oblique strip shaped coil (5), namely make finished product.
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| CN103674997B (en) * | 2013-12-06 | 2015-12-02 | 东南大学 | Based on the low-field nuclear magnetic resonance probe of printed circuit board (PCB) solenoid coil |
| CN104199392A (en) * | 2014-07-28 | 2014-12-10 | 盐城工学院 | Gallium solenoid micro-coil with circular cross section based on bonding of capillary tube and double-faced adhesive tape and preparation method of micro-coil |
| CN107607894B (en) * | 2017-11-06 | 2019-06-04 | 厦门大学 | It is applicable in miniature malcoils and its preparation associated with HPLC-NMR |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6751847B1 (en) * | 1999-11-04 | 2004-06-22 | Fsu Research Foundation, Inc. | Laser-assisted fabrication of NMR resonators |
| CN101460860A (en) * | 2006-05-03 | 2009-06-17 | 普拉德研究及开发股份有限公司 | Downhole micro magnetic resonance analyzer |
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| JP2007128952A (en) * | 2005-11-01 | 2007-05-24 | Hst Kk | Coil body of three-dimensional structure and method of manufacturing same, magnetic sensor and method of manufacturing same |
| CN201993326U (en) * | 2010-12-15 | 2011-09-28 | 东南大学 | Minitype solenoid radio-frequency coil used for microfluid nuclear magnetic resonance detection |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6751847B1 (en) * | 1999-11-04 | 2004-06-22 | Fsu Research Foundation, Inc. | Laser-assisted fabrication of NMR resonators |
| CN101460860A (en) * | 2006-05-03 | 2009-06-17 | 普拉德研究及开发股份有限公司 | Downhole micro magnetic resonance analyzer |
Non-Patent Citations (3)
| Title |
|---|
| JP特开2007-128952A 2007.05.24 |
| 台式核磁共振成像仪高灵敏微型射频线圈的研制;汪红志等;《中国医疗器械杂志》;20081231;第32卷(第1期);35-39 * |
| 汪红志等.台式核磁共振成像仪高灵敏微型射频线圈的研制.《中国医疗器械杂志》.2008,第32卷(第1期),35-39. |
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