CN117030431B - In-situ cleaning device and method for ultralow-temperature hydrate nano probe - Google Patents
In-situ cleaning device and method for ultralow-temperature hydrate nano probe Download PDFInfo
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- 239000000523 sample Substances 0.000 title claims abstract description 169
- 238000004140 cleaning Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 56
- 238000012360 testing method Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 12
- 238000007373 indentation Methods 0.000 claims description 94
- 230000001681 protective effect Effects 0.000 claims description 9
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 5
- 238000005259 measurement Methods 0.000 abstract description 3
- 238000013461 design Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- 239000012634 fragment Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/02—Details
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
- B08B7/0071—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating
- B08B7/0085—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating by pyrolysis
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Abstract
The invention discloses an in-situ cleaning device and method for an ultralow-temperature hydrate nano probe, and belongs to the technical field of hydrate microscopic testing. The in-situ cleaning device comprises a heating and dissolving mechanism and a residual stain erasing mechanism; the heating and dissolving mechanism is arranged at the root of the side diameter-changing part of the nano probe and used for automatically decomposing hydrate particles adhered to the probe of the nano probe by heating, and the residual water stain removing mechanism is used for removing residual water stains on the surface of the nano probe. In specific operation, firstly judging the adhesion condition of the surface of the nano probe; then the hydrate adhered on the probe is decomposed by heating by a heating and dissolving mechanism, and residual water stains on the probe are erased by a residual stain erasing mechanism. According to the scheme, on the premise that the environment temperature of the ultralow-temperature nanoindentation probe is not disturbed as much as possible, the hydrate particles adhered to the tip of the nanoprobe are cleaned, the influence of the adhered particles in the re-measurement process is avoided, and the accuracy of experimental results is improved.
Description
Technical Field
The invention belongs to the technical field of microscopic hydrate tests, and particularly relates to an in-situ cleaning device and method for a nano probe of an ultralow-temperature hydrate nano indentation instrument/scratch instrument.
Background
The nano indentation/scratch has wide application prospect in the aspect of testing the physical and mechanical properties of the natural gas hydrate sample. However, the natural gas hydrate sample can be tested only in an ultralow temperature environment due to the limitation of the characteristics of the natural gas hydrate.
In the prior art, a typical method for cleaning the nano indentation/scratch probe under normal temperature condition is to clean the probe with alcohol, such as using dust-free paper dipped with alcohol or dust-free cloth to gently wipe the pressure head; the ram is either rubbed against a soft but abrasive material, such as a clean room wet wipe. However, these methods are not suitable for hydrate nanoindentation testing at ultra-low temperatures. Because the mechanical process of cleaning the tip of the indenter may cause serious disturbances to the stable experimental environment, it may take hours or even longer to fully recover to the conditions required for the experiment, severely affecting the experimental progress.
The ultra-low temperature environment results in that during the hydrate indentation/scratch test, the indenter is often contaminated with fragments of the sample, and very small hydrate fragments often adhere to the indenter tip, which can affect the results of the later indentation test. And fragments of hydrates can often freeze on the tip of the low temperature ram creating strong adhesion and limited cleaning with physical abrasion. Moreover, the key point of the hydrate nano-indentation is that high temperature stability is required to minimize the influence caused by thermal drift. Such drift includes mechanical thermal expansion/contraction and changes in electrical properties due to temperature changes. In order to be able to perform accurate nanoindentation tests at low temperatures, it is often necessary to wait for a long period of time until the temperature of the system and the sample reaches a steady state before the indentation test can be performed.
Disclosure of Invention
Aiming at the defect that the traditional nano indentation/scratch probe cleaning method is not suitable for the hydrate nano indentation test in the ultralow temperature environment, the invention provides an in-situ cleaning device and method for the ultralow temperature hydrate nano probe, which can clean the hydrate particles adhered to the tip of the nano probe on the premise of not disturbing the environmental temperature of the ultralow temperature nano probe as much as possible, ensure that the influence of the adhered particles is avoided in the re-measurement process, and improve the accuracy of experimental results.
The invention is realized by adopting the following technical scheme: an in-situ cleaning device for an ultralow-temperature hydrate nano probe comprises a heating and dissolving mechanism, a driving device and a residual stain erasing mechanism; the driving device is connected with the heating and dissolving mechanism through a lifting rope, the pretightening force of the lifting rope is equal to the weight of the heating and dissolving mechanism, the heating and dissolving mechanism is arranged at the root of the side diameter-changing part of the nano indentation probe and used for automatically decomposing hydrate particles adhered to the nano indentation probe, and the residual water stain erasing mechanism is used for removing residual water stains on the surface of the nano indentation probe;
the heating and dissolving mechanism comprises a flexible heat conduction component, a first thermistor and a controller, wherein the first thermistor is electrically connected with the controller, and the controller is also connected with a digital display screen; the flexible heat conduction component and the nano indentation probe are tightly attached to the side wall of the cambered surface of the flexible heat conduction component, the first thermistor is arranged on the periphery of the flexible heat conduction component, the controller controls the first thermistor to heat, and the heat is transmitted to the nano indentation probe through the flexible heat conduction component, so that the nano indentation probe is heated locally, and the hydrate is decomposed by the heating probe;
the residual stain erasing mechanism is arranged in parallel with the heating and dissolving mechanism, the residual stain erasing mechanism sequentially comprises a compact sponge, a second thermistor and a heat shield from inside to outside, the second thermistor is connected with a controller, the controller synchronously controls the temperatures of the first thermistor and the second thermistor, and the temperatures of the two sets of thermistors are always kept consistent.
Further, the outermost layer of the heating and dissolving mechanism is wrapped with a light insulating protective cover, so that heat generated by the first thermistor is transmitted to the flexible heat conduction component in the first thermistor in a directional manner, and the light insulating protective cover and the nano indentation probe are bonded by adopting a low-temperature compatible ceramic-based adhesive.
The invention further provides an in-situ cleaning method of the in-situ cleaning device for the ultralow-temperature hydrate nano probe, which comprises the following steps of:
step A, judging the adhesion condition of the surface of the nanoindentation probe by comparing the depth of the pressed compact sponge in the cleaning state of the probe with the force value in the state to be cleaned;
b, decomposing the hydrate adhered to the probe by heating by using a heating and dissolving mechanism, and determining the heating time according to the adhesion condition of the probe surface determined in the step A;
and C, utilizing a residual water stain erasing mechanism to erase residual water stains on the probe, and completing cleaning of the probe by inserting and extracting different contact points of the compact sponge for a plurality of times.
Further, the step a includes the following steps:
(1) In the whole testing and cleaning process, the external temperature environment of the nano indentation probe is ensured to be in an ultralow temperature state; before a test hydrate sample is developed, driving a nano indentation probe to press into a compact sponge at a set sample test pressing rate, and recording the pressing depth of the probe and the force value of the probe as initial values of the force value pressed into the compact sponge under the probe cleaning condition;
(2) Carrying out nano indentation/scratch test on a natural gas hydrate sample, and driving a nano indentation probe to enable the tip of the nano indentation probe to be in contact with compact sponge after finishing the previous round of nano indentation/scratch test; and pressing the dense sponge at the same pressing rate as the sample test pressing rate, synchronously recording the force value and pressing depth of the nano indentation probe at the moment, comparing with the initial value of the force value obtained in the step (1), and qualitatively judging the adhesion condition of the hydrate on the surface of the probe, wherein the larger the difference of the force value is, the more serious the surface adhesion condition is.
Further, the step B specifically includes the following steps:
the tip of the nano indentation probe is driven to contact with the compact sponge, the controller is started to synchronously heat the first thermistor and the second thermistor, and when the temperature of the digital display screen reaches more than 0 ℃, the hydrate and ice particles on the surface of the nano indentation probe are automatically dissolved, and the dissolved water is automatically dripped into the compact sponge and absorbed by the sponge.
Further, in the step C, after the step B is completed, the controller is continuously maintained to heat, the contact position of the nanoindentation probe and the dense sponge is replaced, and the dense sponge is inserted and pulled out for several times, so that the residual water stain at the tip of the nanoprobe is absorbed by the dense sponge.
Further, in the step C, after the cleaning of the probe is completed, the cleaning state is judged:
and continuously replacing the contact position of the nano indentation probe and the compact sponge, synchronously recording the force value and the indentation depth of the nano indentation probe by the nano indentation probe pressed into the compact sponge at the same indentation rate as that of the pressed sample for test, and cleaning the probe when the force value and the initial value of the force value are all the time, otherwise, repeating the heating and cleaning operations.
Compared with the prior art, the invention has the advantages and positive effects that:
according to the scheme, the tip of the nanoindentation probe is heated locally through the thermistor with special design, so that hydrate particles adhered to the probe are automatically decomposed, and the residual water stain on the surface of the nanoindentation probe is removed by combining the dense sponge with special design. The whole cleaning process is carried out in a closed ultralow-temperature environment, and operators do not contact with the probe, so that the disturbance of the ambient temperature is avoided. And the probe with local heating can recover the ultralow temperature state in a short period under the control of the ambient temperature, so that the next round of nanometer indentation/scratch experiment is conveniently developed, a better cleaning effect is achieved, and the experiment efficiency is improved.
Drawings
FIG. 1 is a schematic view of a cleaning device according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart of a cleaning method according to an embodiment of the invention;
wherein: 1. a nanoindentation probe; 2. a driving device; 3. heating and dissolving mechanism; 4. a hanging rope; 3-1, a flexible heat conduction member; 3-2, a thermistor; 3-3, insulating protective cover; 3-4, a ceramic-based adhesive; 3-5, teflon wires; 3-6, a controller; 3-7, a digital display screen; 5-1, compact sponge; 5-2, a heat shield; 5-3, thermistor.
Detailed Description
In order that the above objects, features and advantages of the invention will be more readily understood, a further description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as described herein, and thus the present invention is not limited to the specific embodiments disclosed below, it being noted that the nanoprobes described herein comprise nanoindentation probes and nanoscoring probes.
Embodiment 1, an in-situ cleaning device for ultra-low temperature hydrate nano-probes, as shown in fig. 1, comprises a heating and dissolving mechanism 3, a residual stain erasing mechanism and a driving device 2; the heating and dissolving mechanism 3 is arranged at the root of the side diameter-changing part of the nano indentation probe 1, the driving device 2 is arranged at the top end of the nano indentation probe 1, and the driving device 2 is connected with the heating and dissolving mechanism 3 through a lifting rope 4;
the heating and dissolving mechanism 3 comprises a flexible heat conduction component 3-1, a first thermistor 3-2, a controller 3-6 and a digital display screen 3-7, wherein the flexible heat conduction component 3-1 is tightly attached to and contacted with the nano indentation probe 1, and the adoption of the flexible heat conduction component 3-1 can effectively avoid the direct contact of the rigid thermistor and the nano indentation probe, thereby being beneficial to protecting the probe from being damaged by the rigid contact. The first thermistor 3-2 is arranged on the periphery of the flexible heat conduction component 3-1, the first thermistor 3-2 is respectively connected with a controller 3-6 and a digital display screen 3-7 outside the ultralow temperature environment through two superfine Teflon wires 3-5, the controller 3-6 controls the first thermistor 3-2 to generate heat and transmits the heat to the nano indentation probe 1 through the flexible heat conduction component 3-1, so that local heating of the nano indentation probe 1 is realized, hydrate particles are heated by the heating probe to be automatically decomposed, and the specific temperature value is read by the digital display screen 3-7.
In addition, the light insulating protective cover 3-3 is wrapped on the outermost layer of the heating and dissolving mechanism 3, and the light insulating protective cover 3-3 is used for isolating the first thermistor 3-2 and the ultralow temperature environment originally existing around the probe, so that heat generated by the first thermistor 3-2 is guided to the flexible heat conducting component 3-1 in the probe to be conveyed, the heating efficiency of the probe is improved, and the cleaning efficiency of the probe is improved.
The light insulating protective cover 3-3 and the nano indentation probe 1 are adhered together by adopting a ceramic-based adhesive 3-4 compatible with low temperature, so that the relative fixation between the heating and dissolving mechanism 3 and the nano indentation probe 1 in the nano indentation process is ensured, and the disturbance on the nano measurement result is reduced as much as possible.
The main purpose of the lifting rope 4 is to support the weight of the heating and dissolving mechanism 3, the lower end of the lifting rope 4 is connected with the light insulating protective cover 3-3, the upper end of the lifting rope 4 is connected with the nano indentation probe driving device 2, the pretightening force of the lifting rope 4 is equal to the weight of the heating and dissolving mechanism 3, the lifting rope can completely support the weight of the heating and dissolving mechanism 3 under the ultralow temperature condition once the ceramic-based adhesive 3-4 fails, the nano indentation probe 1 is guaranteed not to bear the weight of the heating and dissolving mechanism 3, and the accuracy of the nano indentation test result is guaranteed.
With continued reference to fig. 1, the residual stain erasing mechanism is arranged in parallel with the heating and dissolving mechanism 3, and sequentially comprises a compact sponge 5-1, a second thermistor 5-3 and a heat shield 5-2 from inside to outside. The second thermistor 5-3 is connected with the controller 3-6 through an ultrafine Teflon wire, and the controller 3-6 synchronously controls the temperature of the second thermistor 5-3 in the residual erasing mechanism when controlling the temperature of the first thermistor 3-2 in the heating and dissolving mechanism, so that the temperatures of the two sets of thermistors are always consistent (equal). The second thermistor 5-3 transmits the temperature to the inside compact sponge 5-1, and the heat shield 5-2 outside the second thermistor mainly plays a role in isolating the surrounding ultra-low temperature environment, so that the surrounding environment is not influenced by the heating of the second thermistor 5-3 as much as possible, and the heating efficiency of the inside compact sponge 5-1 is improved.
It should be noted that in the above structural design, the heating and dissolving mechanism 3 is fixed on the nanoindentation probe 1 in the form of an auxiliary structure, and always moves synchronously with the nanoindentation probe during the nanoindentation/scratch test. The main reason for this is: the nano indentation probe has very small size and high sensitivity, and the whole cleaning process is carried out in an ultralow temperature environment which is not directly contacted by manpower. The heating and dissolving mechanism 3 and the nano indentation probe 1 are integrally designed, so that the frequency of manual contact of the probe is reduced, the sensitivity of the probe is protected, and the residual erasing mechanism does not belong to an accessory mechanism of the nano indentation probe and is independently arranged in a range which can be reached by a nano indentation probe driving device.
Embodiment 2, based on the in-situ cleaning device for ultra-low temperature hydrate nano probe set forth in embodiment 1, based on the above design, the present embodiment provides a corresponding nano indentation probe in-situ cleaning method, mainly including two steps of hydrate decomposition and residual water stain erasure, as shown in fig. 2, including the following steps:
step A, judging the surface adhesion condition of the nano indentation probe;
(1) Pre-installing: before the experiment starts, a fixed heating dissolving structure and a residual stain erasing mechanism are installed, so that the nano heating dissolving structure and the residual stain erasing mechanism are connected with a controller and a digital display screen, the contact is good, and the temperature environment where a nano indentation probe is positioned is always maintained at ultralow temperature (lower than-100 ℃) in the whole nano indentation/scratch testing process and the probe cleaning process;
(2) When the external temperature environment where the nano indentation probe is located reaches an ultralow temperature state, before a hydrate sample is tested by nano indentation/scratch (namely the nano indentation probe is in a clean state), rotating a nano indentation probe driving device to enable the nano indentation probe to be positioned right above a hard compact sponge, pressing the nano indentation probe into the hard compact sponge at a set sample test pressing-in rate, and recording the pressing-in depth and the force value of the probe as initial values of the force value pressed into the hard compact sponge under the probe cleaning condition;
(3) After the nanoindentation/scratch test of the natural gas hydrate sample is finished, a nanoindentation probe driving device is driven to pull the nanoindentation probe out of the sample, and the nanoindentation probe is driven to enable the tip of the nanoindentation probe to be in contact with the hard compact sponge;
(4) Driving a nano indentation probe, synchronously recording the force value and the indentation depth of the nano indentation probe by using the indentation probe to indentation into a compact sponge at the same indentation rate as the indentation sample for test, comparing the indentation force value at the moment with the initial value of the force value obtained in the step (2), qualitatively judging the adhesion condition of the hydrate on the surface of the probe, wherein the larger the difference of the force values is, the more serious the adhesion condition of the hydrate on the surface of the probe is, and the longer the required heating dissolution time is;
step B, hydrate decomposition
(4) Dissolving: and (3) pulling back the nanoindentation probe, enabling the tip of the nanoindentation probe to be in contact with the hard compact sponge, starting the controller, and synchronously heating the first thermistor and the second thermistor. When the temperature of the digital display screen reaches more than 0 ℃, the hydrate and ice particles on the surface of the nano indentation probe are automatically dissolved, and the dissolved water is automatically dripped into the compact sponge and absorbed by the sponge;
step C, residual water stain erasure
(5) And (3) erasure: and (3) after the step (4) is finished, continuously maintaining the controller to heat, replacing the contact position of the nanoindentation probe and the compact sponge, inserting and extracting the nanoprobe into and from the compact sponge for a plurality of times, and absorbing residual water stains at the tip of the nanoprobe by the compact sponge.
(6) Cleaning state confirmation: and continuously replacing the contact position of the nano indentation probe and the compact sponge, and synchronously recording the force value and the indentation depth of the nano indentation probe by pressing the nano indentation probe into the compact sponge at the same indentation rate as that of the indentation sample for test. And (3) when the force value is consistent with the initial value of the force value obtained in the step (2), cleaning the probe is completed.
Wherein, it is emphasized that before installing the fixed heating and dissolving mechanism and the residual wiping mechanism, the hard compact sponge must be ensured to be in a dry state, otherwise, the compact sponge is frozen under the ultralow temperature condition, and the cleaning effect is affected; in addition, in the cleaning process, the contact points of the nanoindentation probe and the compact sponge in the steps (2) to (4) can be the same, but the contact points are necessarily different from those in the steps (5) and (6), and in the steps (5) and (6), the positions which are dry and not inserted by the nanoprobe should be selected as much as possible for erasure and verification.
The present invention is not limited to the above-mentioned embodiments, and any equivalent embodiments which can be changed or modified by the technical content disclosed above can be applied to other fields, but any simple modification, equivalent changes and modification made to the above-mentioned embodiments according to the technical substance of the present invention without departing from the technical content of the present invention still belong to the protection scope of the technical solution of the present invention.
Claims (10)
1. An in-situ cleaning device of an ultralow-temperature hydrate nano probe is characterized by comprising a heating and dissolving mechanism (3) and a residual stain erasing mechanism; the heating and dissolving mechanism (3) is arranged at the root of the side diameter-changing part of the nano indentation probe (1) and used for automatically decomposing hydrate particles adhered to the probe of the nano indentation probe (1) by heating, and the residual water stain erasing mechanism is used for removing residual water stains on the surface of the nano indentation probe;
the heating and dissolving mechanism (3) comprises a flexible heat conduction component (3-1), a first thermistor (3-2) and a controller (3-6), wherein the first thermistor (3-2) is electrically connected with the controller (3-6), and the controller (3-6) is also connected with a digital display screen (3-7); the flexible heat conduction component (3-1) is tightly attached to the cambered surface side wall of the nano indentation probe (1), the first thermistor (3-2) is arranged on the periphery of the flexible heat conduction component (3-1), the controller (3-6) controls the first thermistor (3-2) to generate heat, and the heat is transmitted to the nano indentation probe (1) through the flexible heat conduction component (3-1), so that the nano indentation probe (1) is locally heated, and the hydrate is decomposed by the heating probe.
2. The ultra-low temperature hydrate nanoprobe in-situ cleaning device according to claim 1, wherein: the residual stain erasing mechanism is arranged in parallel with the heating and dissolving mechanism (3), the residual stain erasing mechanism sequentially comprises a compact sponge (5-1), a second thermistor (5-3) and a heat shield (5-2) from inside to outside, the second thermistor (5-3) is connected with a controller (3-6), and the controller (3-6) synchronously controls the temperatures of the first thermistor (3-2) and the second thermistor (5-3), and the temperatures of the two sets of thermistors are always kept consistent.
3. The ultra-low temperature hydrate nanoprobe in-situ cleaning device according to claim 1, wherein: the outermost layer of the heating and dissolving mechanism (3) is wrapped with a light insulating protective cover (3-3), so that heat generated by the first thermistor (3-2) is directionally transferred to the flexible heat conducting component (3-1) inside the first thermistor.
4. The ultra-low temperature hydrate nanoprobe in-situ cleaning device according to claim 3, wherein: the light insulating protective cover (3-3) and the nano indentation probe (1) are bonded by adopting a low-temperature compatible ceramic-based adhesive (3-4).
5. The ultra-low temperature hydrate nanoprobe in-situ cleaning device according to claim 1, wherein: the top end of the nanometer indentation probe (1) is also provided with a driving device (2), the driving device (2) is connected with the heating and dissolving mechanism (3) through a lifting rope (4), and the pretightening force of the lifting rope (4) is equal to the weight of the heating and dissolving mechanism (3).
6. A method for cleaning in situ of a cleaning in situ device based on ultra low temperature hydrate nanoprobes according to claim 2, comprising the steps of:
step A, judging the adhesion condition of the surface of the nanoindentation probe by comparing the depth of the pressed compact sponge in the cleaning state of the probe with the force value in the state to be cleaned;
b, decomposing the hydrate adhered to the probe by heating by using a heating and dissolving mechanism, and determining the heating time according to the adhesion condition of the probe surface determined in the step A;
and C, utilizing a residual water stain erasing mechanism to erase residual water stains on the probe, and completing cleaning of the probe by inserting and extracting different contact points of the compact sponge for a plurality of times.
7. The clean-in-place method of claim 6, wherein: the step A comprises the following steps:
(1) In the whole testing and cleaning process, the external temperature environment of the nano indentation probe is ensured to be in an ultralow temperature state; before a test hydrate sample is developed, driving a nano indentation probe to press into a compact sponge at a set sample test pressing rate, and recording the pressing depth of the probe and the force value of the probe as initial values of the force value pressed into the compact sponge under the probe cleaning condition;
(2) Carrying out nano indentation/scratch test on a natural gas hydrate sample, and driving a nano indentation probe to enable the tip of the nano indentation probe to be in contact with compact sponge after finishing the previous round of nano indentation/scratch test; and pressing the dense sponge at the same pressing rate as the sample test pressing rate, synchronously recording the force value and pressing depth of the nano indentation probe at the moment, comparing the force value with the initial value of the force value obtained in the step (1), and qualitatively judging the adhesion condition of the hydrate on the surface of the probe, wherein the larger the difference of the force values is, the more serious the adhesion condition of the hydrate on the surface of the probe is.
8. The cleaning-in-place method according to claim 6, wherein the step B specifically comprises the following steps:
the tip of the nano indentation probe is driven to contact with the compact sponge, the controller is started to synchronously heat the first thermistor and the second thermistor, and when the temperature of the digital display screen reaches more than 0 ℃, the hydrate and ice particles on the surface of the nano indentation probe are automatically dissolved, and the dissolved water is automatically dripped into the compact sponge and absorbed by the sponge.
9. The cleaning in situ method according to claim 6, wherein in the step C, after the step B is completed, the controller is continuously maintained to heat, the contact position of the nanoindentation probe and the compact sponge is replaced, and the compact sponge is inserted and pulled out for a plurality of times, so that the residual water stain at the tip of the nanoprobe is absorbed by the compact sponge.
10. The cleaning-in-place method according to claim 6, wherein in the step C, after the probe cleaning is completed, the cleaning state is judged:
and continuously replacing the contact position of the nano indentation probe and the compact sponge, synchronously recording the force value and the indentation depth of the nano indentation probe by the nano indentation probe pressed into the compact sponge at the same indentation rate as that of the pressed sample for test, and cleaning the probe when the force value and the initial value of the force value are all the time, otherwise, repeating the heating and cleaning operations.
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| CN202310982434.5A CN117030431B (en) | 2023-08-04 | 2023-08-04 | In-situ cleaning device and method for ultralow-temperature hydrate nano probe |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4138878A (en) * | 1976-12-03 | 1979-02-13 | Rohrback Corporation | Method and apparatus for detecting and measuring scale |
| CN108321098A (en) * | 2017-01-18 | 2018-07-24 | 中芯长电半导体（江阴）有限公司 | Cleaning solution, cleaning device and the method for a kind of probe tip for wafer test |
| CN208013259U (en) * | 2018-01-18 | 2018-10-26 | 德淮半导体有限公司 | A kind of high temperature test probe card heating control system |
| CN112649465A (en) * | 2020-11-20 | 2021-04-13 | 吉林大学 | Method for testing low-temperature thermal shrinkage coefficient of material by utilizing residual indentation morphology |
| CN114739842A (en) * | 2022-02-23 | 2022-07-12 | 深圳大学 | Atomic force microscope-based method for measuring mechanical properties of micro-plastics |
| CN116099819A (en) * | 2022-11-10 | 2023-05-12 | 浙江海洋大学 | Semiconductor testing machine capable of automatically cleaning probe |
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| US7161492B2 (en) * | 2004-12-02 | 2007-01-09 | Itt Industries | Mechanical self-cleaning probe via a jiggler |
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| US4138878A (en) * | 1976-12-03 | 1979-02-13 | Rohrback Corporation | Method and apparatus for detecting and measuring scale |
| CN108321098A (en) * | 2017-01-18 | 2018-07-24 | 中芯长电半导体（江阴）有限公司 | Cleaning solution, cleaning device and the method for a kind of probe tip for wafer test |
| CN208013259U (en) * | 2018-01-18 | 2018-10-26 | 德淮半导体有限公司 | A kind of high temperature test probe card heating control system |
| CN112649465A (en) * | 2020-11-20 | 2021-04-13 | 吉林大学 | Method for testing low-temperature thermal shrinkage coefficient of material by utilizing residual indentation morphology |
| CN114739842A (en) * | 2022-02-23 | 2022-07-12 | 深圳大学 | Atomic force microscope-based method for measuring mechanical properties of micro-plastics |
| CN116099819A (en) * | 2022-11-10 | 2023-05-12 | 浙江海洋大学 | Semiconductor testing machine capable of automatically cleaning probe |
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| CN117030431A (en) | 2023-11-10 |
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