CN204883410U - A electrochemistry accuse oxygen device for water under high pressure hot body system - Google Patents
A electrochemistry accuse oxygen device for water under high pressure hot body system Download PDFInfo
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- CN204883410U CN204883410U CN201520602406.7U CN201520602406U CN204883410U CN 204883410 U CN204883410 U CN 204883410U CN 201520602406 U CN201520602406 U CN 201520602406U CN 204883410 U CN204883410 U CN 204883410U
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- round table
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- temperature
- inert metal
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Abstract
The utility model discloses an electrochemistry accuse oxygen device for water under high pressure hot body system, it is by the base, the resistant high temperature insulation awl of round platform form fills up, the taper sleeve of nai high temperature insulation, the resistant high temperature insulation pottery of round platform form, round platform form solid electrolyte ceramic pipe, spongy inert metal layer, constitutions such as inert metal piece and electrode lead, each spare part combination forms toper self -energized seal mechanism, the electrochemistry accuse oxygen device that from this constitutes is compared with the current all kinds of direct or indirect accuse oxygen device that is used for high temperature water under high pressure hot body system, the comprehensive compensation device is rapid in response speed, and stable and reliable in performance, and high reusage rate, can extensively be used for wideer warm -pressing scope (250 -700 DEG C, ordinary pressure - 100 MPa), hydrothermal system.
Description
Technical field
The utility model relates to a kind of galvanochemistry control oxygen device for High Temperature High Pressure hydrothermal system.
Background technology
Under high-temperature and high-pressure conditions, the oxygen fugacity/activity in hydrothermal system is one of very important the physical-chemical parameters of system, and it had both retrained other oxidations, the kind of reduction components and content, govern again the various processes of system.Oxygen fugacity/activity is great at High Temperature High Pressure field such as such as mineral dissolution, one-tenth oil cracking gas process, hydrothermal replacement, artificial lens synthesis, high-temperature boiler burn into thermal power generation/nuclear reactor equipment burn into overcritical refuse process.In-situ control is carried out to the oxygen fugacity/activity under High Temperature High Pressure thermal and hydric environment, can the clearly generation of the material composition of enzymatic hydrolysis system, character, state and process and development.Therefore, the oxygen fugacity/activity of in-situ control water under high pressure hot system has very important scientific meaning.
The method controlling High Temperature High Pressure hydrothermal system oxygen fugacity/activity at present in the world mainly adopts film osmosis process and the solid electrolyte film electrode methods such as Eugster two capsule method, Shaw membrane process, polytetrafluoroethylene film osmosis.Above-mentioned several film osmosis process is all by controlling hydrogen fugacity/activity, recycling 2H
2+ O
22H
2hydrogen fugacity/activity is converted into oxygen fugacity/activity by O balanced reaction.In conversion process, aqueous fluid is taken as Pure water preparation usually.But in fact, in many High Temperature High Pressure scientific experiments, industrial process, environments such as subsea detection, the strong solution system that what we often ran into is composition is complicated, if will the fugacity/activity of system water as the fugacity/activity of pure water, then can bring larger error to result undoubtedly.And the film osmosis process response time generally reaches a few hours to a couple of days, all difficulty is satisfied responds requirement fast.The response of solid electrolyte film electrode method is fast, and utilize the oxygen sensitivity characteristic of solid electrolyte directly to control system oxygen, but report and used solid electrolyte film electrode method to control in oxygen fugacity/activity document, because the restriction of structural design and encapsulant used is difficult to work more than 450 DEG C, be particularly respectively 400-700 DEG C at temperature, pressure, be difficult to use under the high temperature and high pressure environment of 40-100MPa.
In view of controlling the significance of oxygen fugacity/activity in high-temperature high pressure water science of heat and technical research, and the predicament run in work at present, require that a kind of energy of development quick in situ controls the sensor of oxygen fugacity/activity in High Temperature High Pressure hydrothermal system.
Utility model content
The technical problems to be solved in the utility model is: the device providing a kind of High Temperature High Pressure hydrothermal system electrochemical control oxygen, the original position that this device can be used for high temperature (250-700 DEG C) high pressure (normal pressure-100MPa) hydrothermal system oxygen fugacity or oxygen activity directly controls, long to solve the response time that the working temperature pressure that existing similar direct control oxygen technology exists not high (be difficult to simultaneously more than 400 DEG C, 40MPa) and existing indirect control oxygen technology face, the various difficult problems such as the institute's result reliability that obtains existence query.
The technical solution of the utility model is: a kind of device for High Temperature High Pressure hydrothermal system electrochemical control oxygen, be made up of pedestal, round table-like high-temperature insulation cone pad, high-temperature insulation tapered sleeve, round table-like high-temperature insulation pottery, round table-like solid electrolyte ceramic pipe, spongy inert metal layer, inert metal sheet and contact conductor etc., it is characterized in that: described pedestal 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 is furnished with wherein in a taper hole, round table-like solid electrolyte ceramic pipe is provided with in this high-temperature insulation tapered sleeve, all there is spongy inert metal layer on the large disc of round table-like solid electrolyte ceramic pipe and the interior top of pipe, is positioned at the spongy inert metal layer on round table-like solid electrolyte ceramic pipe pipe top by contact conductor through hole extraction from below, round table-like high-temperature insulation pad is provided with 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 the inert metal sheet 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 is spongy inert metal layer, be positioned at the contact conductor of through hole below this taper hole through round table-like high-temperature insulation cone pad, the electric connection with the spongy inert metal layer on round table-like high-temperature insulation pottery large end face is realized by inert metal sheet and the contact conductor being arranged in round table-like high-temperature insulation pottery, and the spongy inert metal layer on round table-like high-temperature insulation pottery large end face realizes the electric connection with the spongy inert metal layer on round table-like solid electrolyte ceramic pipe large end face by contact conductor.
The material of described round table-like high-temperature insulation pad and high-temperature insulation tapered sleeve is pyrophyllite, mica or boron nitride.
The material of described round table-like high-temperature insulation pottery is corundum ceramic, and its axle center is containing the contact conductor that together sinter ceramic with round table-like high-temperature insulation.
Described inert metal sheet is platinum or gold sheet.
Described spongy inert metal layer material is Pt.
Described contact conductor is platinum filament.
Taper hole on described pedestal, and round table-like high-temperature insulation pad, high-temperature insulation tapered sleeve, round table-like solid electrolyte ceramic pipe and the round table-like high-temperature insulation pottery be installed in taper hole has identical cone angle, is 10-20
o, jointly form taper self-energized seal mechanism each other.
The material of preparing of described pedestal is nickel-base alloy or titanium alloy or stainless steel.
The material of described round table-like solid electrolyte ceramic pipe is YSZ pottery, and made by slip casting method, form through high temperature sintering, its preparation comprises following key step:
Step one: use the slurry that the material formulation solid contents such as YSZ ceramic powder, gum arabic, deionized water are 30-70%, and by slurry ball milling 1-5h on bowl mill;
Step 2: pour out the flowing slurry in grinding tool after dripping slurry certain hour in a mold, the demoulding after placement 5-20h, repaired biscuit, obtain tubulose YSZ biscuit of ceramics;
Step 3: in Si-Mo rod high temperature furnace, tubulose YSZ biscuit of ceramics is sintered, sintering temperature is 1300-1600 DEG C, and sintering time is 1-6h, obtains the tubulose YSZ pottery of tool high mechanical properties;
Step 4: on grinding machine, the tubulose YSZ Ceramic manufacturing of above-mentioned thermal sintering is become round table-like and the large end face of round platform of polishing with wafer lapping machine;
Step 5: the round table-like YSZ ceramic pipe of having polished is cleaned 10-20min in rare HCl, absolute ethyl alcohol or acetone, deionized water for ultrasonic successively, then dries in 100-150 DEG C of baking oven.
The beneficial effects of the utility model:
Substantivity in the superiority of the utility model galvanochemistry control oxygen device in structural design, control oxygen principle and the dirigibility in configuration design, make the existing various such as similar direct control oxygen technical work temperature, pressure faced for the control oxygen device of water under high pressure hot system not high (be difficult to simultaneously more than 400 DEG C, 40MPa) and the existing indirect control oxygen technology response time long, there is the various difficult problems such as query and almost obtain comprehensive solution in institute's result reliability that obtains.Main beneficial effect comprises:
1, be used for making the encapsulant such as high-temperature insulation tapered sleeve (5) and the pyrophyllite of round table-like high-temperature insulation pad (8), mica or boron nitride in the utility model 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; YSZ powder is used directly to contact with the high-temperature high pressure water fluid sample in high temperature pressure vessel through continuous shape inert metal layer (1) in its large disc Shanghai of round table-like solid electrolyte ceramic (2) that slip casting method sintering makes; Use Al
2o
3powder and platinum go between, and to make contact conductor that integral sintered round table-like its axle center of high-temperature insulation pottery (4) 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 (9) of installing electrodes is that nickel-base alloy or the high temperature alloy such as titanium alloy or stainless steel are made in the utility model, 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 (5), round table-like high-temperature insulation pad (8), round table-like solid electrolyte ceramic pipe (2)/round table-like high-temperature insulation pottery (4) and pedestal (9) makes the utility model device can use at very high temperature (such as: 700 DEG C) with pressure (such as: 100MPa) condition.
2, the aforementioned round table-like high-temperature insulation pad (8) in the utility model, high-temperature insulation tapered sleeve (5), round table-like solid electrolyte ceramic pipe (2), round table-like high-temperature insulation pottery (4), inert metal sheet (6) and contact conductor (3) 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 the utility model device can be repeatedly used.
3, the biscuit platinum layer in the utility model, the large disc of round table-like solid electrolyte ceramic pipe (2) made through brushing-sintering process, 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, the utility model device compared with the existing all kinds of direct or indirect control oxygen device for High Temperature High Pressure hydrothermal system, fast response time, stable and reliable for performance, repeat usage is high, can be widely used in the hydrothermal system of wider temperature and pressure scope (250-700 DEG C, normal pressure-100MPa).
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
Embodiment
For making the purpose of this utility model, technical scheme and advantage clearly, below in conjunction with accompanying drawing, the utility model is described in further detail.
1, the composition of each parts of galvanochemistry control oxygen device and making.
As shown in Figure 1, in the present embodiment, the parts of device bore the compositions such as pad 8, high-temperature insulation tapered sleeve 5, round table-like solid electrolyte ceramic pipe 2, round table-like high-temperature insulation pottery 4, spongy inert metal layer 1, inert metal sheet 6 and contact conductor 3 primarily of pedestal 9, 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 8 and high-temperature insulation tapered sleeve 5, and round table-like high-temperature insulation pad 8 axially have a through hole; Select corundum ceramic to make round table-like high-temperature insulation pottery 4, its axle center platinum electrode lead-in wire 3 and ceramic body form through slip casting method is integral sintered; Select YSZ ceramic making round table-like solid electrolyte ceramic pipe 2 bearing; Platinum wire is adopted to make contact conductor 3; Select platinum slurry to make on the large disc of round table-like solid electrolyte ceramic pipe 2 and manage the spongy inert metal layer 1 on interior top and round table-like high-temperature insulation pottery 4 large discs, it is made through brushing-sintering process; Metal platinum is adopted to make inert metal sheet 6; The angle of release of two taper holes on nickel-base alloy pedestal 9, round table-like high-temperature insulation pad 8, high-temperature insulation tapered sleeve 5, round table-like solid electrolyte ceramic 2 and round table-like high-temperature insulation pottery 4 is 15
o.
Concrete aforementioned round table-like solid electrolyte ceramic pipe 2 is made by slip casting method, forms through high temperature sintering, and its preparation comprises following key step:
Step one: use the material formulation solid contents such as YSZ ceramic powder, gum arabic, deionized water to be the slurry of 40%, and by slurry ball milling 2h on bowl mill;
Step 2: pour out the flowing slurry in grinding tool after dripping slurry certain hour in a mold, the demoulding after placement 10h, repaired biscuit, obtain tubulose YSZ biscuit of ceramics;
Step 3: in Si-Mo rod high temperature furnace, tubulose YSZ biscuit of ceramics is sintered, sintering temperature is 1500 DEG C, and sintering time is 1h, obtains the tubulose YSZ pottery of tool high mechanical properties;
Step 4: on grinding machine, the tubulose YSZ Ceramic manufacturing of above-mentioned thermal sintering is become round table-like and the large end face of round platform of polishing with wafer lapping machine;
Step 5: the round table-like YSZ ceramic pipe of having polished is cleaned 10min in rare HCl, absolute ethyl alcohol or acetone, deionized water for ultrasonic successively, then dries in 120 DEG C of baking ovens.
2, the assembling of each parts of galvanochemistry control oxygen device.As shown in Figure 1, comprise the steps:
Step one: the through hole of contact conductor 3 along round table-like high-temperature insulation pad 8 is passed.
Step 2: the convergence end round table-like high-temperature insulation pad 8 being installed with contact conductor 3 being pressed into one of them taper hole on nickel-base alloy pedestal 9, wherein retains a fixed gap between the little disc of round table-like high-temperature insulation pad 8 and the little disc of taper hole.
Step 3: in step 2 round table-like high-temperature insulation pad 8 large disc on place high-temperature insulation tapered sleeve 5 and there is the inert metal sheet 6 of suitable thickness.
Step 4: be pressed into large disc having spongy inert metal platinum layer 1 and platinum electrode lead-in wire 3, axle center in high-temperature insulation tapered sleeve 5 described in step 3 containing the round table-like high-temperature insulation pottery 4 of platinum electrode lead-in wire 3 with hydraulic jack.The resistance that contact conductor 3-inert metal sheet 6-round table-like high-temperature insulation pottery 4 axle center platinum electrodes lead-in wire 3-spongy inert metal layer 1-spongy inert metal layer 1 top electrode measuring the round table-like high-temperature insulation pad 8 of insertion goes between 3, confirms to contact with each other well.Measure resistance between spongy inert metal layer 1 and pedestal 9, confirm well insulated from each other.
Step 5: put into high-temperature insulation tapered sleeve 5 in another taper hole of nickel-base alloy pedestal 9, be pressed on large disc with hydraulic jack in high-temperature insulation tapered sleeve 5 and have the round table-like solid electrolyte ceramic pipe 2 of spongy inert metal platinum layer 1 and platinum electrode lead-in wire 3 with top in pipe, confirm that the platinum electrode in round table-like solid electrolyte ceramic pipe 2 large disc top electrode lead-in wire 3, round table-like solid electrolyte ceramic pipe 2 pipe goes between well insulated from each other between 3 and pedestal 9 by resistance measurement.
Step 6: connect round table-like solid electrolyte ceramic pipe 2 and the contact conductor 3 on the spongy inert metal layer 1 of round table-like high-temperature insulation pottery 4 large disc, make it contact and well form electric pathway.
So far, the assembling of each parts of galvanochemistry control oxygen device completes.
3, the integral installation of galvanochemistry control oxygen device.By profile and the size of change nickel-base alloy pedestal 9, nickel-base alloy pedestal 9 can be installed on dissimilar high temperature pressure vessel, installs two spongy inert metal layers 1 in rear the utility model device taper hole and directly contacts with the high-temperature high pressure water fluid sample in high temperature pressure vessel.Adopt air as oxygen storehouse atmosphere 7 in the course of work, select constant current supply as control oxygen external circuit, while continuously passing into air 7 in round table-like solid electrolyte ceramic pipe 2, by changing the direction and time that in nickel-base alloy pedestal 9 two through holes, between two contact conductors 3, impressed current applies, reach the object of the oxygen fugacity in High Temperature High Pressure hydrothermal system or activity being carried out to in-situ control.
In the utility model, oxygen storehouse atmosphere 7 also can select CO/ air Mixture or CO/ oxygen mixture etc.
Claims (8)
1. the device for High Temperature High Pressure hydrothermal system electrochemical control oxygen, bore pad (8), high-temperature insulation tapered sleeve (5), round table-like high-temperature insulation pottery (4), round table-like solid electrolyte ceramic pipe (2), spongy inert metal layer (1), inert metal sheet (6) and contact conductor (3) etc. by pedestal (9), round table-like high-temperature insulation to form, it is characterized in that: described pedestal (9) 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 (5) is furnished with wherein in a taper hole, round table-like solid electrolyte ceramic pipe (2) is provided with in this high-temperature insulation tapered sleeve (5), all there is spongy inert metal layer (1) on top on the large disc of round table-like solid electrolyte ceramic pipe (2) and in pipe, is positioned at the spongy inert metal layer (1) on round table-like solid electrolyte ceramic pipe (2) pipe top by contact conductor through hole extraction from below, round table-like high-temperature insulation pad (8) is provided with at the convergence end of another taper hole, round table-like high-temperature insulation tapered sleeve (5) is had on the large disc of round table-like high-temperature insulation cone pad (8), and the inert metal sheet (6) be arranged on successively from top to bottom in round table-like high-temperature insulation tapered sleeve (5) and round table-like high-temperature insulation pottery (4), round table-like high-temperature insulation pottery (4) large end face there is spongy inert metal layer (1), be positioned at the contact conductor (3) of through hole below this taper hole through round table-like high-temperature insulation cone pad (8), realize and the electric connection of spongy inert metal layer (1) on round table-like high-temperature insulation pottery (4) large end face by inert metal sheet (6) and the contact conductor (3) that is arranged in round table-like high-temperature insulation pottery (4), and the spongy inert metal layer (1) on round table-like high-temperature insulation pottery (4) large end face realizes the electric connection with the spongy inert metal layer (1) on round table-like solid electrolyte ceramic pipe (2) large end face by contact conductor (3).
2. the device for High Temperature High Pressure hydrothermal system electrochemical control oxygen according to claim 1, is characterized in that: the material of described round table-like high-temperature insulation pad (8) and high-temperature insulation tapered sleeve (5) is pyrophyllite, mica or boron nitride.
3. the device for High Temperature High Pressure hydrothermal system electrochemical control oxygen according to claim 1, it is characterized in that: the material of described round table-like high-temperature insulation pottery (4) is corundum ceramic, its axle center contains the contact conductor (3) together sintered into round table-like high-temperature insulation pottery (4).
4. the device for High Temperature High Pressure hydrothermal system electrochemical control oxygen according to claim 1, is characterized in that: described inert metal sheet (6) is platinum or gold sheet.
5. the device for High Temperature High Pressure hydrothermal system electrochemical control oxygen according to claim 1, is characterized in that: described spongy inert metal layer (1) material is Pt.
6. the device for High Temperature High Pressure hydrothermal system electrochemical control oxygen according to claim 1, is characterized in that: described contact conductor (3) is platinum filament.
7. the device for High Temperature High Pressure hydrothermal system electrochemical control oxygen according to claim 1, it is characterized in that: the taper hole on described pedestal (9), and be installed on round table-like high-temperature insulation pad (8) in taper hole, high-temperature insulation tapered sleeve (5), round table-like solid electrolyte ceramic pipe (2) and round table-like high-temperature insulation pottery (4) there is identical cone angle, be 10-20
o, jointly form taper self-energized seal mechanism each other.
8. the device for High Temperature High Pressure hydrothermal system electrochemical control oxygen according to claim 1, is characterized in that: the material of preparing of described pedestal (9) is nickel-base alloy or titanium alloy or stainless steel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520602406.7U CN204883410U (en) | 2015-08-12 | 2015-08-12 | A electrochemistry accuse oxygen device for water under high pressure hot body system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520602406.7U CN204883410U (en) | 2015-08-12 | 2015-08-12 | A electrochemistry accuse oxygen device for water under high pressure hot body system |
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| Publication Number | Publication Date |
|---|---|
| CN204883410U true CN204883410U (en) | 2015-12-16 |
Family
ID=54827766
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201520602406.7U Withdrawn - After Issue CN204883410U (en) | 2015-08-12 | 2015-08-12 | A electrochemistry accuse oxygen device for water under high pressure hot body system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105159343A (en) * | 2015-08-12 | 2015-12-16 | 中国科学院地球化学研究所 | Electrochemical oxygen control device applied to high pressure hydrothermal system and preparation method thereof |
-
2015
- 2015-08-12 CN CN201520602406.7U patent/CN204883410U/en not_active Withdrawn - After Issue
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105159343A (en) * | 2015-08-12 | 2015-12-16 | 中国科学院地球化学研究所 | Electrochemical oxygen control device applied to high pressure hydrothermal system and preparation method thereof |
| CN105159343B (en) * | 2015-08-12 | 2017-06-16 | 中国科学院地球化学研究所 | A kind of electrochemistry control oxygen device for high pressure hydrothermal system and preparation method thereof |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20151216 Effective date of abandoning: 20170616 |
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| AV01 | Patent right actively abandoned |
Granted publication date: 20151216 Effective date of abandoning: 20170616 |