CN105067674A - Methane sensor for high-pressure hydrothermal system and manufacturing method of methane sensor - Google Patents
Methane sensor for high-pressure hydrothermal system and manufacturing method of methane sensor Download PDFInfo
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- CN105067674A CN105067674A CN201510490536.0A CN201510490536A CN105067674A CN 105067674 A CN105067674 A CN 105067674A CN 201510490536 A CN201510490536 A CN 201510490536A CN 105067674 A CN105067674 A CN 105067674A
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Abstract
The invention discloses a methane sensor for a high-pressure hydrothermal system and a manufacturing method of the methane sensor. The sensor comprises a base, a circular-truncated-cone-shaped high-temperature-resistant insulated taper pad, a high-temperature-resistant insulated taper sleeve, circular-truncated-cone-shaped high-temperature-resistant ceramic, circular-truncated-cone-shaped solid electrolyte ceramic, a spongy active electrode, a spongy inert electrode, a spongy inert metal layer, an inert metal piece, an electrode lead and the like, wherein the parts are combined into a conical self-tightening sealing mechanism; compared with existing various methane sensors, the manufactured methane sensor has the advantages of simple structure, high selectivity, high response speed, stable and reliable performance and the like, can be used for in-situ measurement of methane fugacity in a high-temperature and high-pressure hydrothermal system such as a crater on a seabed, hydrothermal fluid spouts and the like, provides a technological support for exploration of natural gas hydrate resources on the seabed and can also be applied to other high-temperature (300DEG C-700 DEG C) high-pressure (normal pressure-100 MPa) hydrothermal environments requiring on-site detection of methane gas.
Description
Technical field
The present invention relates to a kind of CH
4chemical sensor, particularly relates to and a kind ofly can be used for methane transducer of water under high pressure hot system and preparation method thereof.
Background technology
Along with the quick growth of global economy, the demand of people to oil, rock gas equal energy source is increasing.Under the background that land hydrocarbon resources is day by day exhausted, sight focuses in the exploitation of ocean resources by each coastal state, and Marine oil and gas resource is the natural gas hydrate resources emphasis that will be future world Exploration of Oil And Gas and exploitation especially.In gas hydrate, methane reserves are twices of explored coal, oil, rock gas summation.Research for gas hydrate is also mainly in the exploration stage within the scope of our times.Researchers are actively making great efforts to utilize various measurement means to find gas hydrate, detect its concrete distributing position in seabed, can exploit it in the near future, solve the energy crisis of the mankind.
At present, mainly use that such as earthquake geophysical exploration about exhausted, electromagnetic surveying, FLUID GEOCHEMICAL are detected in the world, the geophysics means such as oceanic heat flow is detected, sea-floor soil sampling and geochemical method explore cryogenic natural gas hydrate.Wherein seismic detection method application is maximum, and especially Bottom-simulating reflector (BSR) Detection Techniques, most sea bed gas hydrates is all found based on this technology.Then seldom detect for the thermogenic methane that gas hydrate form relevant submarine volcano and hydrothermal vent place.Therefore, how to develop the methane transducer that can be used for seabed with the methane at direct detection crater and hydrothermal vent place, to the distribution verifying gas hydrate, there is important directive significance.
The more chemical sensor being used for detecting methane gas is used to have electromotive force type sensor, amperometric sensor and oxide semiconductor-type sensor now.In a few class methane transducer, oxide semiconductor-type sensor is owing to being widely used in CH to the height detection sensitivity of micro-object gas
4the detection of gas.This type sensor is the main flow that current methane transducer is developed, and is used for colliery, pipeline warning device.But it is poor to the gas-selectively that chemical property is similar, measurement result is difficult to meet the measurement requirement for composition complex detection atmosphere, and hydrone is to its accuracy of detection serious interference.(the Wang Weixi such as Wang Weixi, Sun Chunyan, Yang Hui etc. the development of high sensitivity gaseous hydrocarbon in-situ measurement system in gas and oil in sea. geoscience---China University of Geosciences's journal, 2004,29:163-168.) once report utilize this principle successfully to develop a set of sensing device for surveying gaseous hydrocarbon in gas and oil in sea.This gaseous hydrocarbon sensing device is made up of chemical sensor, chromatography column, E-signal processor, Data Processing in Chromatography Workstation etc., marine bottom sediment from collection in worksite can be taken off after treatment the hydrocarbon gas solved aboard ship to be injected by injection port, after chromatographic column is separated, enter chemical sensor analysis.Amperometric sensor structure is relatively complicated, and the reappearance of measurement result is relatively poor, limits its application to a certain extent.Electromotive force type sensor construction is relatively simple, can carry out quick, high-precision measurement.A few class sensor is mainly for detection of the methane in gas atmosphere above, seldom has and is respectively 300-700 DEG C, the high temperature and high pressure environment of 30-100MPa about the report, particularly temperature that detect High Temperature High Pressure thermal and hydric environment methane, pressure.The present invention is directed to this demand propose development one can in high temperature (300-700 DEG C) high pressure (normal pressure-100MPa) hydrothermal system fast, the chemical sensor of Measurement accuracy methane.
Summary of the invention
The technical problem to be solved in the present invention: a kind of methane transducer for water under high pressure hot system and preparation method thereof is provided, can not be respectively 300-700 DEG C at temperature, pressure with what solve that prior art exists in use, work in the water under high pressure thermal environment of 30-100MPa, and precision is low, the problem of unstable properties.
Technical scheme of the present invention: a kind of methane transducer for water under high pressure hot system, bore pad, high-temperature insulation tapered sleeve, round table-like high-temperature insulation pottery, round table-like solid electrolyte ceramic, spongy active electrode, spongy inert electrode, spongy inert metal layer, inert metal sheet and contact conductor etc. by pedestal, round table-like high-temperature insulation to form, described pedestal is provided with two taper holes, and the convergence end of two taper holes is communicated with two through holes respectively, be furnished with high-temperature insulation tapered sleeve in a taper hole wherein, in this high-temperature insulation tapered sleeve, have round table-like solid electrolyte ceramic, the large end face of round table-like solid electrolyte ceramic has non-touching spongy active electrode and spongy inert electrode, round table-like high-temperature insulation is had to bore pad at the convergence end of another taper hole, round table-like high-temperature insulation tapered sleeve is had on the large disc of round table-like high-temperature insulation cone pad, and two the non-touching inert metal sheets be arranged on successively from top to bottom in round table-like high-temperature insulation tapered sleeve and round table-like high-temperature insulation pottery, round table-like high-temperature insulation pottery large end face there are two non-touching spongy inert metal layers, be positioned at two contact conductors of through hole below this taper hole through round table-like high-temperature insulation cone pad, the electric connection with two spongy inert metal layers on round table-like high-temperature insulation pottery large end face is realized by non-touching two inert metal sheets and two contact conductors being arranged in round table-like high-temperature insulation pottery, and two spongy inert metal layers on round table-like high-temperature insulation pottery large end face realize the electric connection of non-touching spongy active electrode and spongy inert electrode on the large end face with round table-like solid electrolyte ceramic by two contact conductors.
The material of described round table-like high-temperature insulation cone pad and high-temperature insulation tapered sleeve is pyrophyllite, mica or boron nitride.
The material of described round table-like solid electrolyte ceramic is YSZ pottery.
The material of described round table-like high-temperature insulation pottery is corundum ceramic, its containing two that together sinter into round table-like high-temperature insulation pottery along round table-like high-temperature insulation ceramic shaft to through and non-touching contact conductor.
The material of preparing of described pedestal is nickel-base alloy or titanium alloy or stainless steel.
Described inert metal sheet is platinum or gold sheet.
Described spongy inert metal layer and contact conductor material are Pt.
Described spongy active electrode is Pt, Pd or the Ru methane oxidation to catalytic activity.
Described spongy inert electrode is Au, the La methane oxidation to inertia
0.8sr
0.2mnO
3or (La
0.75sr
0.25)
0.9cr
0.5mn
0.5o
3.
Taper hole on described pedestal, and the round table-like high-temperature insulation be installed in taper hole bores pad, high-temperature insulation tapered sleeve, round table-like solid electrolyte ceramic and round table-like high-temperature insulation pottery has identical cone angle, is 10-20
o, jointly form taper self-energized seal mechanism each other.
Beneficial effect of the present invention:
1, be used for making the encapsulant such as pyrophyllite, mica or boron nitride of high-temperature insulation tapered sleeve and round table-like high-temperature insulation cone pad in the present invention hardness be moderate under High Temperature High Pressure thermal and hydric environment, thermo-chemical stability good, anticorrosive, and the good high temperature insulation characteristic of tool; The spongy active electrode of YSZ powder on its large disc of round table-like solid electrolyte ceramic that slip casting method sintering makes is used directly to contact with the high-temperature high pressure water fluid sample in high temperature pressure vessel with spongy inert electrode; Use Al
2o
3powder and platinum go between, and to make contact conductor that integral sintered its axle center of round table-like high-temperature insulation pottery be made into the embeds environment that insulate good, and the globality between ceramic body is strong, even if whole round table-like high-temperature insulation pottery also has good corrosion resistivity, high temperature mechanical strength in High Temperature High Pressure hydrothermal system.Moreover, be used for carrying and the pedestal system nickel-base alloy of installing electrodes or the high temperature alloy such as titanium alloy or stainless steel are made in the present invention, such material also has good corrosion resistivity and high temperature mechanical strength in High Temperature High Pressure thermal and hydric environment.Therefore, the taper self-energized seal mechanism formed by the taper hole on aforementioned high-temperature insulation tapered sleeve, round table-like high-temperature insulation cone pad, round table-like solid electrolyte ceramic/round table-like high-temperature insulation pottery and pedestal makes apparatus of the present invention can use at very high temperature (such as: 700 DEG C) with pressure (such as: 100MPa) condition.
2, aforementioned round table-like high-temperature insulation cone pad, high-temperature insulation tapered sleeve, round table-like solid electrolyte ceramic, round table-like high-temperature insulation pottery, inert metal sheet and contact conductor in the present invention are after the taper hole being assembled to said apparatus pedestal, close contact between each building block, the good globality of tool, not easily be scattered and damage, thus apparatus of the present invention can be repeatedly used.
3, the spongy layers of active electrodes in the present invention, the large disc of round table-like solid electrolyte ceramic made through brushing-sintering process and spongy inert electrode layer, greatly can increase the effective length of hydro-thermal sample-YSZ-platinum three-phase line of contact and effective contact area of platinum electrode and hydro-thermal sample, thus increase substantially the speed of response of this device.
4, the configuration design of this device is flexible and changeable, therefore can select not cause the position of obviously impact to install this device on high temperature pressure vessel mechanical strength on high temperature pressure vessel, thus decrease the negative effect that the installation because of this device brings high temperature pressure vessel working temperature and pressure to greatest extent.
In a word, methane transducer of the present invention is compared with existing all types of methane transducer, structure is simple, selectivity is high, it is rapid, stable and reliable for performance to respond, not only can be used for the in site measurement of methane fugacity in the high-temperature high pressure water hot system such as submarine volcano mouth, hydrothermal vent, for detection sea bed gas hydrate resource provides technical support, also can be applicable to the High Temperature High Pressure thermal and hydric environment that other need to carry out methane gas Site Detection.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, the present invention is described in further detail.
1, the composition of each parts of methane transducer and making.
As shown in Figure 1, in the present embodiment, the parts of device bore the compositions such as pad 9, high-temperature insulation tapered sleeve 7, round table-like solid electrolyte ceramic 5, round table-like high-temperature insulation pottery 6, spongy inert metal layer 3, spongy active electrode 1, spongy inert electrode 2, inert metal sheet 8 and contact conductor 4 primarily of pedestal 10, round table-like high-temperature insulation.Wherein adopt high-temperature nickel-base alloy to make pedestal 9, there are two taper holes one end of nickel-base alloy pedestal 9, and the other end has two through holes to be communicated with taper hole respectively; Adopt pyrophyllite to make round table-like high-temperature insulation cone pad 9 and high-temperature insulation tapered sleeve 7, and round table-like high-temperature insulation cone pad 9 axially have two through holes; Select corundum ceramic to make round table-like high-temperature insulation pottery 6, axially two non-touching platinum electrodes lead-in wires 4 and ceramic body form through slip casting method is integral sintered for they; Select the round table-like solid electrolyte ceramic 5 of YSZ ceramic making, it is made by slip casting method, forms through high temperature sintering, its large end face has non-touching spongy active Pt electrode and spongy inertia Au electrode; Platinum wire is adopted to make contact conductor 4; Select platinum slurry to make two non-touching spongy inert metal layers 3 on round table-like high-temperature insulation pottery 6 large discs, it is made through brushing-sintering process; Metal platinum is adopted to make inert metal sheet 8; The angle of release of two taper holes on nickel-base alloy pedestal 10, round table-like high-temperature insulation cone pad 9, high-temperature insulation tapered sleeve 7, round table-like solid electrolyte ceramic 5 and round table-like high-temperature insulation pottery 6 is 15
o.
2, the assembling of each parts of methane transducer.As shown in Figure 1, comprise the steps:
Step one: two contact conductors 4 are passed along two through holes of round table-like high-temperature insulation cone pad 9 respectively.
Step 2: the convergence end round table-like high-temperature insulation cone pad 9 being installed with two contact conductors being pressed into one of them taper hole on nickel-base alloy pedestal 10, wherein round table-like high-temperature insulation is bored between the little disc of pad 9 and the little disc of taper hole and retained a fixed gap.
Step 3: place high-temperature insulation tapered sleeve 7 and the two non-touching inert metal sheets 8 with suitable thickness on the large disc of round table-like high-temperature insulation cone pad 9.
Step 4: with hydraulic jack by large disc has two be not in contact with each other spongy inert metal layer 3 and contact conductor 4, longitudinally containing in the high-temperature insulation tapered sleeve 7 in the round table-like high-temperature insulation pottery 6 press-in abovementioned steps three of two contact conductors 4.Then measure the resistance between two groups of contact conductor 4-inert metal sheet 8-round table-like high-temperature insulation pottery 6 longitudinal electrode lead-in wire 4-spongy inert metal layer 3-spongy inert metal layer 3 top electrode lead-in wires 4 independently inserting round table-like high-temperature insulation cone pad 9 respectively, confirmation contacts with each other good; And it is well insulated from each other between two groups spongy inert metal layer 3 top electrode lead-in wires 4.Measure resistance between two groups spongy inert metal layers 3 and nickel-base alloy pedestal 10 respectively, confirm well insulated from each other.
Step 5: put into high-temperature insulation tapered sleeve 7 in another taper hole of nickel-base alloy pedestal 10, round table-like solid electrolyte ceramic 5 is pressed into hydraulic jack in high-temperature insulation tapered sleeve 7, the large disc of round table-like solid electrolyte ceramic 5 there are two non-touching spongy active electrode 1 and spongy inert electrodes 2, spongy active electrode 1 and spongy inert electrode 2 have contact conductor 4.Confirm that on the large disc of round table-like solid electrolyte ceramic 5, two contact conductors 4 are insulated from each other by resistance measurement, and and insulate good between nickel-base alloy pedestal 10.
Step 6: two non-touching spongy active electrodes 1 on two contact conductors 4 be not in contact with each other on spongy inert metal layer 3 on round table-like high-temperature insulation pottery 6 large discs respectively disc large with round table-like solid electrolyte ceramic 5 are connected with the contact conductor 4 on spongy inert electrode 2, make it contact between two and well form electric pathway.
So far, the assembling of each parts of methane transducer completes.
3, the integral installation of methane transducer.Methane transducer prepared by the present invention both can be installed on the in site measurement for methane in laboratory high pressure hydrothermal system on autoclave, also by the profile of sensor nickel-base alloy pedestal 10 and the change of size, be installed on dissimilar high temperature pressure vessel by sensor nickel-base alloy pedestal 10, the spongy active electrode 1 installed in rear apparatus of the present invention taper hole directly contacts with the methane in high temperature pressure vessel with spongy inert electrode 2 and two spongy inert metal layers 3.
Claims (10)
1. the methane transducer for water under high pressure hot system, bore pad (9), high-temperature insulation tapered sleeve (7), round table-like high-temperature insulation pottery (6), round table-like solid electrolyte ceramic (5), spongy active electrode (1), spongy inert electrode (2), spongy inert metal layer (3), inert metal sheet (8) and contact conductor (4) etc. by pedestal (10), round table-like high-temperature insulation to form, it is characterized in that: described pedestal (10) is provided with two taper holes, the convergence end of two taper holes is communicated with two through holes respectively, high-temperature insulation tapered sleeve (7) is furnished with wherein in a taper hole, in this high-temperature insulation tapered sleeve (7), there is round table-like solid electrolyte ceramic (5), the large end face of round table-like solid electrolyte ceramic (5) has non-touching spongy active electrode (1) and spongy inert electrode (2), round table-like high-temperature insulation is had to bore pad (9) at the convergence end of another taper hole, round table-like high-temperature insulation tapered sleeve (7) is had on the large disc of round table-like high-temperature insulation cone pad (9), and two the non-touching inert metal sheets (8) be arranged on successively from top to bottom in round table-like high-temperature insulation tapered sleeve (7) and round table-like high-temperature insulation pottery (6), round table-like high-temperature insulation pottery (6) large end face there are two non-touching spongy inert metal layers (3), be positioned at two contact conductors (4) of through hole below this taper hole through round table-like high-temperature insulation cone pad (9), the electric connection with two spongy inert metal layers (3) on round table-like high-temperature insulation pottery (6) large end face is realized by non-touching two inert metal sheets (8) and two contact conductors (4) being arranged in round table-like high-temperature insulation pottery (6), and two spongy inert metal layers (3) on round table-like high-temperature insulation pottery (6) large end face realize the electric connection of non-touching spongy active electrode (1) and spongy inert electrode (2) on the large end face with round table-like solid electrolyte ceramic (5) by two contact conductors (4).
2. the methane transducer for water under high pressure hot system according to claim 1, is characterized in that: the material of described round table-like high-temperature insulation cone pad (9) and high-temperature insulation tapered sleeve (7) is pyrophyllite, mica or boron nitride.
3. the methane transducer for water under high pressure hot system according to claim 1, is characterized in that: the material of described round table-like solid electrolyte ceramic (5) is YSZ pottery.
4. the methane transducer for water under high pressure hot system according to claim 1, it is characterized in that: the material of described round table-like high-temperature insulation pottery (6) is corundum ceramic, its containing two that together sinter into round table-like high-temperature insulation pottery (6) along the axially through and non-touching contact conductor (4) of round table-like high-temperature insulation pottery (6).
5. the methane transducer for water under high pressure hot system according to claim 1, is characterized in that: the material of preparing of described pedestal (10) is nickel-base alloy or titanium alloy or stainless steel.
6. the methane transducer for water under high pressure hot system according to claim 1, is characterized in that: described inert metal sheet (8) is platinum or gold sheet.
7. the methane transducer for water under high pressure hot system according to claim 1, is characterized in that: described spongy inert metal layer (3) and contact conductor (4) material are Pt.
8. the methane transducer for water under high pressure hot system according to claim 1, is characterized in that: described spongy active electrode (1) is Pt, Pd or the Ru methane oxidation to catalytic activity.
9. the methane transducer for water under high pressure hot system according to claim 1, is characterized in that: described spongy inert electrode (2) is Au, the La methane oxidation to inertia
0.8sr
0.2mnO
3or (La
0.75sr
0.25)
0.9cr
0.5mn
0.5o
3.
10. the methane transducer for water under high pressure hot system according to claim 1, it is characterized in that: the taper hole on described pedestal (10), and be installed on round table-like high-temperature insulation cone pad (9), high-temperature insulation tapered sleeve (7) in taper hole, round table-like solid electrolyte ceramic (5) and round table-like high-temperature insulation pottery (6) there is identical cone angle, be 10-20
o, jointly form taper self-energized seal mechanism each other.
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