CN102518434B - Micro-detection probe for nuclear magnetic resonance analysis of fluid - Google Patents

Micro-detection probe for nuclear magnetic resonance analysis of fluid Download PDF

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CN102518434B
CN102518434B CN201110409749.8A CN201110409749A CN102518434B CN 102518434 B CN102518434 B CN 102518434B CN 201110409749 A CN201110409749 A CN 201110409749A CN 102518434 B CN102518434 B CN 102518434B
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copper layer
micro
fluid
strip line
detection probe
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CN102518434A (en
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肖立志
吴保松
李晓南
郭葆鑫
安天琳
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China University of Petroleum Beijing
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China University of Petroleum Beijing
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Abstract

The invention provides a micro-detection probe for nuclear magnetic resonance analysis of fluid. The probe comprises a ring permanent magnet, and a high-permeability shell fitted over the outer wall of the ring permanent magnet. A strip micro-coil structure is arranged at the middle part of the ring permanent magnet, and is sleeved with a gradient coil. The strip micro-coil structure comprises an upper shielding copper layer, an upper substrate, a strip line copper layer, a lower substrate and a lower shielding copper layer. The upper substrate and the lower substrate are provided thereon with a fluid channel, respectively. The strip line copper layer is sandwiched between the upper substrate and the lower substrate, for forming a radio-frequency magnetic field in the fluid channels under the action of applying current. The upper shielding copper layer is arranged on the surface of the upper substrate opposite to the strip line copper layer. The lower shielding copper layer is arranged on the surface of the lower substrate opposite to the strip line copper layer. The strip coil micro-detection probe of the invention has small volume, and the generated magnetic field has uniform intensity.

Description

Micro-detection probe for nuclear magnetic resonance analysis of fluid
Technical field
The present invention relates to formation fluid parameter detecting technology, relate in particular to a kind of micro-detection probe for nuclear magnetic resonance analysis of fluid.
Background technology
In oil field operation development process, need to use modular formation tester to get liquid to stratum to formation fluid pollution condition and fluid behaviour are carried out to Real-Time Evaluation analysis, for Petroleum Production provides important reference data.Wherein, down-hole optical fluid analysis module and downhole NMR fluid analysis module are two kinds of common bottom fluid parameter detection equipments, optical fluid analysis module is gas and the fluid properties based in reflection of light and transmission principle identification fluid line, and the content of definite fluid; Nuclear magnetic resonance analysis of fluid module is to utilize nuclear magnetic resonance principle to measure fluid parameter T 1, to evaluate formation fluid pollution condition, and measurement parameter T 2obtain the parameter such as fluid viscosity, gas-oil ratio with D.
Nuclear magnetic resonance analysis of fluid module is to provide required magnetic field by detection probe for testing, to utilize nmr phenomena test fluid flow parameter T 1, T 2and D.Along with hardware technology and MEMS (Micro-Electro-Mechanical Systems, MEMS) development of technology, a kind of micro-detection probe for nuclear magnetic resonance analysis of fluid has been proposed, it can utilize micro-coil probe incorporated small low-cost spectrometer, particularly can combine with the ripe microflow control technique such as Capillary Electrophoresis or fluid separation applications and form micro-total analysis system on sheet, convection cell parameter is measured.Adopt micro-detection probe of micro-coil form, have low in energy consumption, volume is little and detection sensitivity high, can be applied to oil field, be particularly suitable for boring the measurement requirement of low-power consumption.
Micro-detection probe for nuclear magnetic resonance analysis of fluid is based on nuclear magnetic resonance spectroscopy principle, utilize existence or the molecular structure of nmr phenomena and chemical shift effect research compound thereof, because the varying environment variations in temperature along with depth of stratum under oil well is very large, the requirement that the downhole NMR magnetostatic field uniformity does not reach NMR spectrum, therefore, can be test fluid by micro-detection probe required magnetic field is provided, with convection cell parameter T 1, T 2measure with D.At present, adopt in micro-detection probe for nuclear magnetic resonance analysis of fluid, conventionally adopt the micro-coil of snail and toroidal winding, it utilizes the micro-coil of snail and toroidal winding structure, fluid channel and magnetic field are provided, for providing and measure required magnetic field through the fluid of fluid channel, but the RF magnetic field uniformity of its formation is poor.
Summary of the invention
The invention provides a kind of micro-detection probe for nuclear magnetic resonance analysis of fluid, can effectively overcome the problem that prior art exists.
The invention provides a kind of micro-detection probe for nuclear magnetic resonance analysis of fluid, comprising: annular permanent magnet, and be set in the high magnetic conductive shell on described annular permanent magnet outer wall;
The middle part of described annular permanent magnet is provided with banded micro-loop construction, and is arranged with gradient coil on the micro-loop construction of described band shape;
The micro-loop construction of described band shape comprises shielding copper layer, upper substrate, strip line copper layer, infrabasal plate and lower shielding copper layer;
On described upper substrate and infrabasal plate, be respectively arranged with fluid passage;
Described strip line copper layer is folded between described upper substrate and infrabasal plate, for forming RF magnetic field applying under the function of current in described fluid passage;
Described upper shielding copper layer is arranged on described upper substrate, with described strip line copper layer back to surface;
Described lower shielding copper layer is arranged on described infrabasal plate, with described strip line copper layer back to surface.
In above-mentioned micro-detection probe for nuclear magnetic resonance analysis of fluid, described strip line copper layer comprises effective strip line copper layer and edge copper layer;
The middle part width of described effective strip line copper layer is less than the width of end, forms at the middle part of described effective strip line copper layer the groove being caved inward by both sides;
Described edge copper layer is arranged in described groove, and has gap between described edge copper layer and described effective strip line copper layer.
In above-mentioned micro-detection probe for nuclear magnetic resonance analysis of fluid, the shape of described groove and edge copper layer is trapezoidal.
In above-mentioned micro-detection probe for nuclear magnetic resonance analysis of fluid, described upper shielding copper layer, strip line copper layer and lower screen layer form by MEMS fabrication techniques.
In above-mentioned micro-detection probe for nuclear magnetic resonance analysis of fluid, described fluid passage is oval fluid passage.
In above-mentioned micro-detection probe for nuclear magnetic resonance analysis of fluid, described upper substrate and infrabasal plate are borate glass substrate.
In above-mentioned micro-detection probe for nuclear magnetic resonance analysis of fluid, the two ends of described fluid passage are connected with respectively capillary tube, for external fluid being imported to described fluid passage.
In above-mentioned micro-detection probe for nuclear magnetic resonance analysis of fluid, described capillary tube is to adopt polyether-ether-ketone resin to make the capillary tube obtaining.
The micro-detection probe of nuclear magnetic resonance analysis of fluid instrument provided by the invention, in utilization, shielding copper layer, strip line copper layer and lower shielding copper layer form the micro-loop construction of strip line, can provide required magnetic field for two fluid passages that are formed on upper substrate and infrabasal plate, make to detect in same volume sample situation, the probe of relatively existing toroidal winding structure, has less volume; Meanwhile, more even by the magnetic field that adopts the micro-loop construction of strip line to form, the magnetostatic field B that annular permanent magnet is produced 0disturb little, make fluid parameter detect more accurate.Micro-detection probe volume provided by the invention is little, low in energy consumption, can be combined in convection cell parameter in earth layer measuring instrument and measure, and can effectively reduce the size of whole earth layer measuring instrument.
Brief description of the drawings
The structural representation of the micro-detection probe for nuclear magnetic resonance analysis of fluid that Fig. 1 provides for the embodiment of the present invention in the time that formation tester is combined;
The structural representation of the micro-detection probe for nuclear magnetic resonance analysis of fluid that Fig. 2 provides for the embodiment of the present invention;
Fig. 3 A is the perspective structure schematic diagram of banded micro-coil in the embodiment of the present invention;
Fig. 3 B is the package assembly schematic diagram of banded micro-coil in the embodiment of the present invention;
Fig. 4 is the structural representation of strip line copper layer in the embodiment of the present invention;
Fig. 5 is the magnetic field schematic diagram that the cross-sectional structure of Fig. 3 A and strip line copper layer produce while being applied with electric current;
Fig. 6 is the RF magnetic field changes in amplitude curve synoptic diagram of the embodiment of the present invention along direction of fluid;
Fig. 7 is the structural representation of gradient coil in the embodiment of the present invention;
Fig. 8 carries out the pulse train schematic diagram of fluid parameter while measuring for the micro-detection probe for nuclear magnetic resonance analysis of fluid that utilizes the embodiment of the present invention and provide.
Detailed description of the invention
The structural representation of the micro-detection probe for nuclear magnetic resonance analysis of fluid that Fig. 1 provides for the embodiment of the present invention in the time that formation tester is combined; The structural representation of the micro-detection probe for nuclear magnetic resonance analysis of fluid that Fig. 2 provides for the embodiment of the present invention; Fig. 3 A is the perspective structure schematic diagram of banded micro-coil in the embodiment of the present invention; Fig. 3 B is the package assembly schematic diagram of banded micro-coil in the embodiment of the present invention.As shown in Figure 1, earth layer measuring instrument is arranged on the schematic diagram under oil well, this earth layer measuring instrument comprises hydraulic module 1, probe module 2, micro-detection probe 3, measures and finish sampling module 4 and pump module 5, wherein, hydraulic module 1 can be introduced instrument internal by probe module 2 by formation fluid; Micro-detection probe 3, is also the micro-detection probe for nuclear magnetic resonance analysis of fluid that the embodiment of the present invention provides, and can carry out NMR relaxation time and propagation measurement to formation fluid; Measure finish sampling module 4 can be by fluid sampling, or by pumping module 5, fluid is drained into well 6.
As shown in Figure 2, for the structure for amplifying schematic diagram of micro-detection probe 3 in Fig. 1, this micro-detection probe 3 specifically can comprise: annular permanent magnet 31, high magnetic conductive shell 32, banded micro-loop construction 33 and gradient coil 34, and wherein, high magnetic conductive shell 32 is set on the outer wall of annular permanent magnet 1; Banded micro-loop construction 33 is arranged on the middle part of annular permanent magnet 31, and gradient coil 34 is set on banded micro-loop construction 33.In the present embodiment, annular permanent magnet 31 can form in central area even magnetostatic field B 0, high magnetic conductive shell 32 maskable magnetic fields, to external radiation, also provide a closed magnetic circuit, thereby can improve uniformity and the stability in the magnetic field that is formed on central area simultaneously.
As shown in Figure 3 A and Figure 3 B, banded micro-loop construction 33 comprises upper substrate 331, infrabasal plate 332, strip line copper layer 333, upper shielding copper layer 334 and lower shielding copper layer 335, wherein, upper substrate 331 and infrabasal plate 332 are oppositely arranged, on upper substrate 331 and infrabasal plate 332, be respectively arranged with fluid passage C, this fluid passage C runs through the fluid passage of substrate; Strip line copper layer 333 is folded between upper substrate 331 and infrabasal plate 332, and this strip line copper layer 333 for forming RF magnetic field applying under the function of current in fluid passage; Upper shielding copper layer 334 be arranged on upper substrate 331 with strip line copper layer 333 back to surface, the i.e. upper surface of upper substrate 331 as shown in Figure 3 B, lower shielding copper layer 335 arrange on infrabasal plate 332 with strip line copper layer 333 back to surface, i.e. the soffit of infrabasal plate 332 as shown in Figure 3 B.
In the present embodiment, upper shielding copper layer 334, strip line copper layer 333 and lower shielding copper layer 335 form banded micro-coil, for fluid parameter measurement provides required RF magnetic field, it specifically can be formed on glass substrate by MEMS fabrication techniques, particularly, can adopt the MEMS technique such as photoresist mask, copper plating to be produced on glass substrate; Strip line copper layer 333 can apply electric current, to produce required magnetic field, can receive again signal, thereby can measure fluid parameter by strip line copper layer 333 simultaneously.Can find out, in the present embodiment, current channel is made up of strip line copper layer 333, upper shielding copper layer 334 and lower shielding copper layer 335, wherein, electric current can flow through from strip line copper layer 333, upper shielding copper layer 334 and lower shielding copper layer 335 are screen layer, are also loops, can make electric current through strip line copper layer 333 time, the RF magnetic field forming in fluid passage on upper substrate 331 and infrabasal plate 332 is more even, and the region of uniform magnetic field is larger.
While it will be understood by those skilled in the art that actual measurement, upper shielding copper layer 334 and lower shielding copper layer 335 are all grounding copper layers, and with the earth terminal of strip line copper layer 333 altogether, thereby can utilize this three copper layers, produce banded micro-loop construction, think that fluid measurement provides required RF magnetic field.
In the present embodiment, the fluid passage being formed on upper substrate 331 and infrabasal plate 332 is oval fluid passage, the oval fluid passage arranging, can make strip line copper layer 333 apply electric current time, in this fluid passage, form magnetic field more uniformly, the suffered magnetic field of the fluid of this fluid passage of flowing through is also more even, can effectively improve the accuracy that fluid parameter is measured.
In the present embodiment, upper substrate 331 and infrabasal plate 332 are borate glass substrate, and like this, upper shielding copper layer 334, strip line copper layer 333 and lower shielding copper layer 335 are separated by borate glass substrate.
Fig. 4 is the structural representation of strip line copper layer in the embodiment of the present invention.In the present embodiment, as shown in Figure 4, strip line copper layer 333 comprises effective strip line copper layer 3331 and two edge copper layers 3332, wherein, effectively the middle part width of strip line copper layer 3331 is less than its end width, thereby forms at the middle part of effective strip line copper layer 333 the groove A being caved inward by both sides, and edge copper layer 3332 is arranged in this groove A, and between edge copper layer 3332 and effective strip line copper layer 3331, there is gap B, edge copper layer 3332 is not connected with effective strip line copper layer 3331.By the groove structure that both sides cave inward is arranged to in the middle part of effective strip line copper layer 3331, make the middle part of effective strip line copper layer 3331 narrower, like this, in the time that electric current passes through, the current density at the narrower place of width, middle part increases, the magnetic field intensity B that it produces in fluid passage in upper substrate 331 and infrabasal plate 332 1will strengthen, thereby improve the magnetic field intensity that is applied to fluid passage inner fluid.
In the present embodiment, above-mentioned groove A and the trapezium structure of edge copper layer 3332 for cooperatively interacting, like this, can make can produce stronger magnetic field intensity at the middle part of effective strip line copper layer 3331.
In the present embodiment, for ease of the fluid entering in earth layer measuring instrument is entered to fluid passage, can be connected with respectively capillary tube at the two ends of fluid passage, for external fluid is imported to fluid passage, particularly, this capillary tube specifically can be and adopts polyether-ether-ketone (Poly-Ether-Ether-Ketone, PEEK) resin to make the capillary tube obtaining.
Fig. 5 is the magnetic field schematic diagram that the cross-sectional structure of Fig. 3 A and strip line copper layer produce while applying electric current.As shown in Figure 5, upper shielding copper layer 334 and lower shielding copper layer 335 are two screen layers, can shield magnetic field; The current density at strip line copper layer 333 middle part is larger, and the magnetic field that strip line copper layer 333 produces can be bound in the central region of whole micro-detection probe, wherein, and the magnetostatic field B that the annular permanent magnet 31 in Fig. 2 produces 0as shown in Figure 5, strip line copper layer 333 applies the magnetic field B forming after electric current to direction 1direction as shown in Figure 5, can be found out two B that oval fluid channel C forms in upper substrate 331 and infrabasal plate 332 1opposite direction.Like this, the micro-loop construction forming by strip line copper layer, and annular permanent magnet, can be fluid parameter measurement required B be provided 0and B 1magnetic field, has reached test needs.
Fig. 6 is the RF magnetic field changes in amplitude curve synoptic diagram of the embodiment of the present invention along direction of fluid.As shown in Figure 6, when strip line copper layer 333 applies electric current, the RF magnetic field changes in amplitude schematic diagram producing along the direction of fluid of upper substrate or infrabasal plate, wherein, Fig. 6 abscissa is the length of strip line copper layer, ordinate is the magnetic field intensity of the RF magnetic field of strip line copper layer generation, can find out, position-4mm to 4mm at strip line copper layer locates, the magnetic field intensity producing is about 2.04 Gausses (Gauss), therefore, the effective length of strip line copper layer is 8mm, and the oval fluid passage length being formed on upper substrate and infrabasal plate should be at least 8mm.
Fig. 7 is the structural representation of gradient coil in the embodiment of the present invention.As shown in Figure 7, gradient coil 34 can form magnetic field gradient, to complete the measurement of diffusion, particularly, this gradient coil 34 can comprise upper and lower two parts coil, in the time measuring diffuse fluid coefficient D, can apply certain electric current for gradient coil 34, and the sense of current as shown by the arrows in Figure 7, thereby can form gradient magnetic, with convection cell parameter, D measures.There is linear gradient in the magnetic field that gradient coil 34 forms in z direction, and parallel and magnetostatic field B 0direction, is superimposed upon magnetostatic field B 0upper, both form a new gradient magnetic.
In the present embodiment, micro-detection probe for nuclear magnetic resonance analysis of fluid can apply certain magnetic field to the fluid entering in fluid passage, thereby convection cell carries out NMR relaxation time and propagation measurement, thereby obtains fluid parameter T 1, T 2and D.Wherein, spin spinrelaxation T 2a measurement parameter the most frequently used in nuclear magnetic resonance log, by T 2analysis, can effectively obtain the geological information such as fluid type, fluid content, particularly, spin spinrelaxation T 2when measurement, conventionally complete with CPMG pulse train a as shown in Figure 8, it is taking self-rotary echo-pulse series as basis, determines transverse relaxation by the attenuation process of the spin echo string observed; Longitudinal relaxation time T 1be an amount that characterizes magnetization vector recovery extent, and the geological information such as fluid type, fluid content has contact closely, its fundamental method of measurement is to complete by saturation recovery pulse train b as shown in Figure 8; Diffusion coefficient D is an amount that characterizes fluid viscosity, and its fundamental method of measurement is to complete by pulse train c as shown in Figure 8.Fluid parameter T in the present embodiment 1, T 2with the concrete measuring process of D similarly to the prior art, no longer describe in detail at this.
Embodiment of the present invention nuclear magnetic resonance analysis of fluid probe can be used in petroleum underground nuclear magnetic resonance fluid analysis, characteristic nmr and constituent for fluid detect, this nuclear magnetic resonance analysis of fluid can be used in combination with cable or with boring formation tester, under reservoir conditions environment, obtain the information of formation fluid characteristics, for open hole well or perforation rear sleeve well.
Finally it should be noted that: above embodiment only, in order to technical scheme of the present invention to be described, is not intended to limit; Although the present invention is had been described in detail with reference to previous embodiment, those of ordinary skill in the art is to be understood that: its technical scheme that still can record aforementioned each embodiment is modified, or part technical characterictic is wherein equal to replacement; And these amendments or replacement do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.

Claims (7)

1. a micro-detection probe for nuclear magnetic resonance analysis of fluid, is characterized in that, comprising: annular permanent magnet, and be set in the high magnetic conductive shell on described annular permanent magnet outer wall;
The middle part of described annular permanent magnet is provided with banded micro-loop construction, and is arranged with gradient coil on the micro-loop construction of described band shape;
The micro-loop construction of described band shape comprises shielding copper layer, upper substrate, strip line copper layer, infrabasal plate and lower shielding copper layer;
On described upper substrate and infrabasal plate, be respectively arranged with fluid passage;
Described strip line copper layer is folded between described upper substrate and infrabasal plate, for forming RF magnetic field applying under the function of current in described fluid passage;
Described upper shielding copper layer is arranged on described upper substrate, with described strip line copper layer back to surface;
Described lower shielding copper layer is arranged on described infrabasal plate, with described strip line copper layer back to surface;
Described strip line copper layer comprises effective strip line copper layer and edge copper layer;
The middle part width of described effective strip line copper layer is less than the width of end, forms at the middle part of described effective strip line copper layer the groove being caved inward by both sides;
Described edge copper layer is arranged in described groove, and has gap between described edge copper layer and described effective strip line copper layer.
2. micro-detection probe for nuclear magnetic resonance analysis of fluid according to claim 1, is characterized in that, the shape of described groove and edge copper layer is trapezoidal.
3. micro-detection probe for nuclear magnetic resonance analysis of fluid according to claim 1 and 2, is characterized in that, described upper shielding copper layer, strip line copper layer and lower shielding copper layer form by MEMS fabrication techniques.
4. micro-detection probe for nuclear magnetic resonance analysis of fluid according to claim 1 and 2, is characterized in that, described fluid passage is oval fluid passage.
5. micro-detection probe for nuclear magnetic resonance analysis of fluid according to claim 1, is characterized in that, described upper substrate and infrabasal plate are borate glass substrate.
6. micro-detection probe for nuclear magnetic resonance analysis of fluid according to claim 1, is characterized in that, the two ends of described fluid passage are connected with respectively capillary tube, for external fluid being imported to described fluid passage.
7. micro-detection probe for nuclear magnetic resonance analysis of fluid according to claim 6, is characterized in that, described capillary tube is to adopt polyether-ether-ketone resin to make the capillary tube obtaining.
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CN102540117B (en) * 2011-12-26 2014-07-02 中国石油大学(北京) Strip line nuclear magnetic resonance detecting device and processing method thereof
US20180292476A1 (en) * 2017-04-10 2018-10-11 Battelle Memorial Institute Nuclear magnetic resonance microprobe detectors and method for detection of low-volume samples
DE102017208841B3 (en) * 2017-05-24 2018-10-04 Bruker Biospin Ag NMR probe head with detachable HF seal

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