CN107561315B - The test device and method of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal - Google Patents
The test device and method of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal Download PDFInfo
- Publication number
- CN107561315B CN107561315B CN201710829523.0A CN201710829523A CN107561315B CN 107561315 B CN107561315 B CN 107561315B CN 201710829523 A CN201710829523 A CN 201710829523A CN 107561315 B CN107561315 B CN 107561315B
- Authority
- CN
- China
- Prior art keywords
- hydrogen
- sample
- tested
- probe
- environmental cabinet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The present invention relates to metal erosion research fields, it is desirable to provide the test device and method of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal.The device includes hollow sample stage, and internal cavities pass through piping connection to heat-exchange system;The top of flying-spot tube is fixedly connected with the downside of sample stage, and the sample to be tested of sheet is fixed to be loaded on sample stage upper surface;Only the environmental cabinet made of the light transmission organic glass of bottom opening is placed on sample to be tested, and the carrier gas inlet of side wall is connected to nitrogen cylinder group, and carrier gas outlet is connected to mass spectrograph;The laser emitter of laser system is located above environmental cabinet, and for probe by piezoelectric ceramics loaded on inside environmental cabinet, controller is respectively connected to laser system, flying-spot tube, mass spectrograph, piezoelectric ceramics and probe by signal wire.The present invention can be convenient, accurately can be carried out test to olefin hydrogen microcosmic in metal and the activation of hydrogen segregation.Being compared with the traditional method has many advantages, such as that spatial resolution is high, tests lossless, multiple functional, simple equipments.
Description
Technical field
The invention belongs to metal erosion research field, in particular to microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal
Test device and test method.
Background technique
Hydrogen embrittlement is one of the key factor for endangering high pressure hydrogen system safety, microcosmic part in the hydrogen embrittlement degree and material of material
Hydrogen concentration distribution and hydrogen segregation are directly related.The segregation of (dislocation, crystal boundary, phase boundary etc.) leads to material to hydrogen at microstructure in the material
Expect that microcosmic local hydrogen concentration increases, and then promotes the generation of hydrogen induced cracking.Hydrogen segregation activation energy is the weight for characterizing hydrogen segregation degree
Parameter is wanted, therefore is to disclose mechanism of hydrogen embrittlement and controlled material to the testing research of olefin hydrogen microcosmic in metal and hydrogen segregation activation energy
The important foundation of hydrogen embrittlement energy.But lack the effective means for microscopic hydrogen distribution tests in metal at present.
Related scholar also explores the method for olefin hydrogen test.The more method of early stage application is the microcosmic printing of hydrogen
And tritium tracer technique, but both methods can only characterize the discharging amount of different location hydrogen in metal, and non-hydrogen is real-time molten
Xie Liang.Ion microprobe technology is also used for the test of olefin hydrogen, but it substantially belongs to the scope for damaging test, and
The performances such as the spatial resolution of the device are to be improved.The spatial resolution that atom-probe chromatographs microscopy is higher, but its
The microscopic damage generated in test process to material makes the follow-on test in situ that cannot achieve microcosmic olefin hydrogen.
Scanning Kelvin Force probe is a kind of gaseous environment metal work function (Work Function) based on capacitance-type vibration
Measuring technique.It can be used for detecting in gaseous environment because of the dissimilar substances dissolution of metal, electricity, mechanics, crystal, absorption etc.
The minor change of material work functions caused by factor has outstanding advantages of spatial resolution is high, high sensitivity and test are lossless,
It is the method that can uniquely measure corrosion electrode potential in gaseous environment.But it is not yet used for microcosmic olefin hydrogen in metal at present
And the report of hydrogen segregation activation energy test.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of in currently existing technology, propose microcosmic in a kind of metal
Olefin hydrogen and hydrogen segregation activation energy test device and test method.
In order to solve the technical problem, solution of the invention is:
The test device of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal is provided, including for providing the nitrogen of carrier gas
Gas cylinders group;The device further includes the scanning Kelvin Force being made of laser system, probe, piezoelectric ceramics, flying-spot tube and controller
Probe system;Sample stage is in hollow box-shaped, and internal cavities pass through piping connection to heat-exchange system;The top of the flying-spot tube
It is fixedly connected with the downside of sample stage, the fixed upper horizontal surface for being loaded on sample stage of the sample to be tested of sheet;
It is only made in the tubular environmental cabinet of bottom opening of light transmission organic glass, groove is set on the end face of open side, it is recessed
O-ring is embedded in slot, environmental cabinet is placed on sample to be tested and realizes by O-ring and seals;Carrier gas is set on the side wall of environmental cabinet
Inlet and outlet, carrier gas inlet are connected to nitrogen cylinder group by pipeline, and carrier gas outlet is connected to mass spectrograph by pipeline;The laser system
The laser emitter of system is located above environmental cabinet, probe by piezoelectric ceramics loaded on inside environmental cabinet, laser emitter, probe and
The line of flying-spot tube is in vertical;The controller is respectively connected to laser system, flying-spot tube, mass spectrograph, piezoelectricity by signal wire
Ceramics and probe.
In the present invention, the flying-spot tube has structure flexible up and down, and upper and lower telescopic extensions are not less than 30 μm, flying-spot tube
Scanning range is not less than 150 × 150 μm.
In the present invention, the sample stage is fabricated by heat-conducting metal, and internal cavities are full of heating agent, sets heating agent in cavity wall
Import and heating agent outlet.
In the present invention, the sample to be tested is the thin rounded flakes with a thickness of 0.5~1mm, surfacing and is thrown through metallographic
Light processing;The overall diameter of sample to be tested is greater than the largest outer diameter of environmental cabinet.
In the present invention, the O-ring is the O-ring of graphite material, is able to achieve between environmental cabinet and sample to be tested relatively sliding
It is dynamic.
In the present invention, there are conductive coating and reflecting coating in the upper surface of the probe, and probe is fitted closely with piezoelectric ceramics.
Microcosmic olefin hydrogen and hydrogen segregation activation energy in aforementioned device test metal are utilized invention further provides a kind of
Method, comprising the following steps:
(1) metal material with a thickness of 0.5~1mm is taken, to its surfacing and carries out metallurgical polishing processing;It is cut into two
The identical thin rounded flakes of block-shaped size, then carry out being flushed with hydrogen place simultaneously in 100~300 DEG C and 10~50MPa of hydrogen environment
Reason, obtains two pieces of samples to be tested;
(2) first piece of sample to be tested is taken, is pasted and fixed on sample stage;Then environmental cabinet is placed in sample to be tested
Upper surface, both adjustment relative position makes the line of laser emitter, probe and flying-spot tube in vertical, and ensures that O-ring is close
Envelope is reliable;
(3) each road pipeline and signal wire are connected, heating agent is filled into sample stage;
(4) valve for opening nitrogen cylinder group, continuously replaces the inner cavity of environmental cabinet, uses flow control valve regulation nitrogen
Gas velocity keeps uniform and stable;After displacement is more than 0.5h, heat-exchange system is controlled to be not higher than the constant heating rate φ of 20 DEG C/h
500 DEG C are warming up to, while starting mass spectrograph and continuously monitoring hydrogen content in carrier gas;Using controller control probe, piezoelectric ceramics,
Laser system and flying-spot tube, interval regular time section carry out the follow-on test of work function to the same area;
(5) after the temperature of heating agent in heat-exchange system reaches 500 DEG C, mass spectrograph, controller are successively closed;Control heat exchange system
After system is gradually cooled to room temperature, closes nitrogen cylinder group and remove sample to be tested;
(6) the hydrogen content curve in carrier gas that mass spectrograph measures integrates the time, obtains total hydrogen in sample to be tested
Content Q1, identify corresponding temperature T at hydrogen content peak of curveP1;The work function regularity of distribution and the olefin hydrogen rule of sample to be tested
It is mutual corresponding;Integral Processing is carried out to a series of work function distribution maps of sample to be tested, in conjunction with total hydrogen content Q1Obtain to
Olefin hydrogen rule in test specimens;
(7) second piece of sample to be tested is taken, repeats identical test program by step (2)~(6), corresponding total hydrogen is obtained and contains
Measure Q2And corresponding temperature T at hydrogen content peak of curveP2;During the test, in addition to by the heating rate in step (4)
2 φ are become from φ, other test conditions is kept to remain unchanged;
(8) hydrogen segregation activation energy in sample to be tested is obtained according to the following formula:
R is gas constant in formula.
In the present invention, the heat-exchange temperature range of heat-exchange system is -50 DEG C~500 DEG C.
In the present invention, mass spectrograph is triple quadrupole bar mass spectrum, 0~50amu of mass number range.
Inventive principle description:
It is found after applicant carries out a large amount of basic research, hydrogen dissolves in a metal will lead to metal part work function
Variation, and there is good corresponding relationship between the variation of work function and local hydrogen solubility.Based on this principle, the invention proposes benefits
It is right with scanning Kelvin Force probe technique (spatial resolution is high, can reach 20nm, tests lossless achievable follow-on test in situ)
The metal part work function regularity of distribution is tested, and the work function regularity of distribution characterizes the regularity of distribution of hydrogen, right in test process
Sample to be tested heat simultaneously while using the quantitative caving law of hydrogen in mass spectrograph monitoring sample, then combines by scanning Kai Er
The olefin hydrogen law of regularity and gold can be calculated by the hydrogen content quantitative data that mass spectrograph obtains that literary force probe technology obtains
Microcosmic olefin hydrogen in category can finally be counted using the caving law that mass spectrograph tests hydrogen in sample to be tested under different heating rates
Calculation obtains corresponding hydrogen segregation activation energy.
Compared with prior art, the beneficial effects of the present invention are:
Test device and test method proposed by the invention, can be convenient, accurately to olefin hydrogen microcosmic in metal and
The activation of hydrogen segregation can be carried out test.It is compared with the traditional method with spatial resolution is high, test is lossless, multiple functional, equipment is simple
Just the advantages that.
Detailed description of the invention
Fig. 1 is general arrangement schematic diagram of the invention.
Appended drawing reference in figure: nitrogen cylinder group 1, flow control valve 2, carrier gas inlet 3, O-ring 4, environmental cabinet 5, laser system
6, probe 7, piezoelectric ceramics 8, carrier gas outlet 9, sample to be tested 10, controller 11, mass spectrograph 12, mass spectrograph valve 13, sample stage 14,
Heating agent 15, flying-spot tube 16, heating agent valve 17, heat-exchange system 18.
Specific embodiment
Microcosmic olefin hydrogen and hydrogen segregation activation energy test device are as shown in Figure 1 in metal in the present embodiment.
The device includes the only tubular environmental cabinet 5 in bottom opening, is made of light transmission organic glass, can high temperature resistant 600
℃.Gas cylinders group 1 proposes the carrier gas that is for experiment, and the carrier gas inlet 3 on environmental cabinet 5 is connected to by flow control valve 2, on environmental cabinet 5
It is additionally provided with carrier gas outlet 9, carrier gas outlet 9 is connected to mass spectrograph 12 by mass spectrograph valve 13.Mass spectrograph 12 was mainly being tested
Monitoring flows through the hydrogen content in the carrier gas of environmental cabinet 5 in journey, and mass spectrograph 12 is triple quadrupole bar mass spectrum, mass number range 0
~50amu.Sample stage 14 is manufactured by the good metal of thermal coefficient, and is hollow structure, and inside is full of heating agent 15, heating agent 15 by
Heat-exchange system 18 provides, and heating agent valve 17 is arranged in corresponding connecting line.The heat-exchange temperature range of heat-exchange system 18 is -50 DEG C
~500 DEG C, affixed sample to be tested 10 on sample stage 14.Sample to be tested 10 is the thin rounded flakes with a thickness of 0.5~1mm, surface
Smooth and progress metallurgical polishing processing, overall diameter are greater than the overall diameter of environmental cabinet 5.Environmental cabinet 5 is placed on sample to be tested 10
And be sealed between the two by O-ring 4, opposite sliding can be achieved between environmental cabinet 5 and sample to be tested 10, O-ring 4 uses
The good graphite material of sliding capability.
The device further includes scanning Kelvin Force probe system, by laser system, probe, piezoelectric ceramics, flying-spot tube and control
Device composition processed.The scanning range of flying-spot tube 16 is not less than 150 × 150 μm, and upper and lower scalable range is not less than 30 μm, sample stage 14
It is placed on flying-spot tube 16, and affixed with flying-spot tube 16.Piezoelectric ceramics 8 and probe 7 are fixed on inside environmental cabinet 5,7 table of probe
There is conductive and reflecting coating in face, and laser system 6 is arranged in right above probe 7, and by laser projection in 7 back side of probe (laser system
The laser emitter of system 6, probe and flying-spot tube line in vertical).Controller 11 to probe 7, flying-spot tube 16, laser system 6,
Piezoelectric ceramics 8 and mass spectrograph 12 are controlled.During the test, piezoelectric ceramics 8 drives probe 7 regularly to shake
Dynamic, after being influenced by 10 work function of sample to be tested, vibration characteristics changes probe 7, these variations are carried on the back in probe 7
The laser system 6 that face reflecting coating projects laser perceives, and signal is passed to controller 11 by laser system 6, the latter to signal at
It can be obtained the work function regularity of distribution of sample to be tested 10 after reason, flying-spot tube 16 drives sample to be tested 10 and probe in the process
The relative movement of position occurs between 7 to complete scanning process.
Utilize olefin hydrogen microcosmic in aforementioned metal and the test method of hydrogen segregation activation energy test device, including following step
It is rapid:
Firstly, taking the metal material with a thickness of 0.5~1mm, to its surfacing and metallurgical polishing processing is carried out;It is cut into
The identical thin rounded flakes of two block-shaped sizes, are then flushed with hydrogen in 100~300 DEG C and 10~50MPa of hydrogen environment simultaneously
Processing, obtains two pieces of samples to be tested 10;
First piece of sample to be tested 10 is fixed on sample stage 14 using high temperature resistant alite paste, then places environmental cabinet 5
In on the surface to be measured of sample to be tested 10, both adjustment relative position makes the line of laser emitter, probe 7 and flying-spot tube 16 be in
Vertically, and ensure 4 sealed reliable of O-ring;Each road pipeline and signal wire are connected, fills heating agent into sample stage 14;
Gas in environmental cabinet 5 is continuously replaced using nitrogen cylinder group 1, adjusts nitrogen flow rate using flow control valve 2
And keep its holding uniform and stable;After displacement is more than 0.5h, opens controller 11 and reasonable test parameter is set, open mass spectrograph
Hydrogen contents in 12 continuous monitoring carrier gas, adjust heat-exchange system 18 with constant heating rate φ and are warming up to 500 DEG C, and wherein φ is not
Higher than 20 DEG C/h, probe 7, piezoelectric ceramics 8, laser system 6 and flying-spot tube 16 then are controlled to realize using controller 11 at once
The test of the work function of sample to be tested 10, and work function test continuously is carried out to the same area after being spaced regular time section;
After 18 temperature of heat-exchange system reaches 500 DEG C, mass spectrograph 12, controller 11 are successively closed, it is slow to adjust 18 temperature of heat-exchange system
It is down to room temperature, then close nitrogen cylinder group 1 and takes out sample to be tested 10;Hydrogen content curve in the carrier gas that mass spectrograph 12 is measured
Time is carried out to integrate total hydrogen content Q in available sample to be tested 101, furthermore identify corresponding temperature at hydrogen content peak of curve
TP1;The work function regularity of distribution of sample to be tested 10 is corresponding with olefin hydrogen rule, to a series of work functions point of sample to be tested 10
Butut carries out Integral Processing, then combines total hydrogen content Q1It can get the olefin hydrogen rule in sample to be tested 10.
Second piece of sample to be tested 10 is taken, above-mentioned identical test program is carried out.In addition to heating rate from φ becomes 2 in test
φ, keep other test conditions to remain unchanged.Obtain corresponding total hydrogen content Q2And it is corresponding at hydrogen content peak of curve
Temperature TP2;
Finally, hydrogen segregation activation energy is equal in sample to be tested 10Wherein R
It is gas constant.
As described above, microcosmic olefin hydrogen and hydrogen segregation activation energy test device and test method in metal proposed by the present invention
The microcosmic olefin hydrogen in metal not only can be accurately tested, can also easily test out the hydrogen segregation activation in metal simultaneously
Energy.Have spatial resolution high (test space resolution ratio of probe 7 is up to 20nm), test lossless compared with traditional test means
The advantages that Evolution of olefin hydrogen (can be achieved same position is continuously tested and is disclosed), multiple functional, simple equipments.
The above is only a case study on implementation of the invention, not does limitation in any form to the present invention,
Although the present invention is disclosed as above with preferable case study on implementation, however, it is not intended to limit the invention, any skill for being familiar with this profession
Art personnel, without departing from the scope of the present invention, when the structure and technology contents using the disclosure above make it is certain
Change or modify and become the equivalence enforcement case of equivalent variations.Anything that does not depart from the technical scheme of the invention, according to this
The technical spirit of invention still falls within the present invention to any simple modification, equivalent change and modification made by the above case study on implementation
In technical proposal scope.
Claims (9)
1. the test device of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal, including for providing the nitrogen cylinder of carrier gas
Group;It is characterized in that, the device sample stage is in hollow box-shaped, internal cavities pass through piping connection to heat-exchange system;Scanning
The top of pipe is fixedly connected with the downside of sample stage, the fixed upper horizontal surface for being loaded on sample stage of the sample to be tested of sheet;
It is only made in the tubular environmental cabinet of bottom opening of light transmission organic glass, sets groove on the end face of open side, in groove
Embedded with O-ring, environmental cabinet is placed on sample to be tested and is realized by O-ring and sealed;Carrier gas disengaging is set on the side wall of environmental cabinet
Mouthful, carrier gas inlet is connected to nitrogen cylinder group by pipeline, and carrier gas outlet is connected to mass spectrograph by pipeline;The laser of laser system
Transmitter is located above environmental cabinet, probe by piezoelectric ceramics loaded on inside environmental cabinet, laser emitter, probe and flying-spot tube
Line is in vertical;Controller is respectively connected to laser system, flying-spot tube, mass spectrograph, piezoelectric ceramics and probe by signal wire.
2. the apparatus according to claim 1, which is characterized in that the flying-spot tube has structure flexible up and down, stretches up and down
Contracting range is not less than 30 μm, and the scanning range of flying-spot tube is not less than 150 × 150 μm.
3. the apparatus according to claim 1, which is characterized in that the sample stage is fabricated by heat-conducting metal, inside
Cavity is full of heating agent, sets heat medium import and heat medium export in cavity wall.
4. the apparatus according to claim 1, which is characterized in that the sample to be tested is thin with a thickness of the circle of 0.5~1mm
Piece, surfacing and is handled through metallurgical polishing;The overall diameter of sample to be tested is greater than the largest outer diameter of environmental cabinet.
5. the apparatus according to claim 1, which is characterized in that the O-ring is the O-ring of graphite material, environmental cabinet with
Opposite sliding is able to achieve between sample to be tested.
6. the apparatus according to claim 1, which is characterized in that there are conductive coating and reflective painting in the upper surface of the probe
Layer, probe are fitted closely with piezoelectric ceramics.
7. it is a kind of using the method for microcosmic olefin hydrogen and hydrogen segregation activation energy in claim 1 described device test metal, it is special
Sign is, comprising the following steps:
(1) metal material with a thickness of 0.5~1mm is taken, to its surfacing and carries out metallurgical polishing processing;It is cut into two pieces of shapes
Then the identical thin rounded flakes of shape size are carried out being flushed with hydrogen processing, be obtained simultaneously in 100~300 DEG C and 10~50MPa of hydrogen environment
To two pieces of samples to be tested;
(2) first piece of sample to be tested is taken, is pasted and fixed on sample stage;Then environmental cabinet is placed in the upper of sample to be tested
Surface, both adjustment relative position makes the line of laser emitter, probe and flying-spot tube be in vertical, and ensures that O-ring sealing can
It leans on;
(3) each road pipeline and signal wire are connected, heating agent is filled into sample stage;
(4) valve for opening nitrogen cylinder group, continuously replaces the inner cavity of environmental cabinet, uses flow control valve regulation nitrogen stream
Speed keeps uniform and stable;After displacement is more than 0.5h, controls heat-exchange system and heated up with the constant heating rate φ not higher than 20 DEG C/h
To 500 DEG C, while starting mass spectrograph and continuously monitoring hydrogen content in carrier gas;Probe, piezoelectric ceramics, laser are controlled using controller
System and flying-spot tube, interval regular time section carry out the follow-on test of work function to the same area;
(5) after the temperature of heating agent in heat-exchange system reaches 500 DEG C, mass spectrograph, controller are successively closed;Control heat-exchange system by
After being gradually cooled to room temperature, closes nitrogen cylinder group and remove sample to be tested;
(6) the hydrogen content curve in carrier gas that mass spectrograph measures integrates the time, obtains total hydrogen content in sample to be tested
Q1, identify corresponding temperature T at hydrogen content peak of curveP1;The work function regularity of distribution of sample to be tested and olefin hydrogen rule are phases
It is mutually corresponding, Integral Processing is carried out to a series of work function distribution maps of sample to be tested, in conjunction with total hydrogen content Q1Obtain hydrogeneous examination
Olefin hydrogen rule in sample;
(7) second piece of sample to be tested is taken, identical test program is repeated by step (2)~(6), obtains corresponding total hydrogen content Q2,
And corresponding temperature T at hydrogen content peak of curveP2;During the test, in addition to becoming the heating rate in step (4) by φ
For 2 φ, other test conditions is kept to remain unchanged;
(8) hydrogen segregation activation energy in hydrogeneous sample is obtained according to the following formula:
R is gas constant in formula.
8. the method according to the description of claim 7 is characterized in that the heat-exchange temperature range of heat-exchange system is -50 DEG C~500
℃。
9. the method according to the description of claim 7 is characterized in that mass spectrograph is triple quadrupole bar mass spectrum, mass number range 0
~50amu.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710829523.0A CN107561315B (en) | 2017-09-14 | 2017-09-14 | The test device and method of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710829523.0A CN107561315B (en) | 2017-09-14 | 2017-09-14 | The test device and method of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal |
Publications (2)
Publication Number | Publication Date |
---|---|
CN107561315A CN107561315A (en) | 2018-01-09 |
CN107561315B true CN107561315B (en) | 2019-08-30 |
Family
ID=60980961
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201710829523.0A Active CN107561315B (en) | 2017-09-14 | 2017-09-14 | The test device and method of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107561315B (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109001292A (en) * | 2018-08-23 | 2018-12-14 | 浙江大学 | A kind of test device and test method of high-strength steel hydrogen segregation activation energy |
CN109668823B (en) * | 2019-01-11 | 2021-05-14 | 中国石油大学(华东) | In-situ online collection and electrochemical detection system for erosion corrosion morphology of bent pipe |
CN110954714B (en) * | 2019-12-20 | 2021-10-19 | 江苏集萃微纳自动化系统与装备技术研究所有限公司 | Real-time rigidity adjusting method for probe of atomic force microscope |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1039304A (en) * | 1988-07-12 | 1990-01-31 | 中国科学院北京真空物理开放实验室 | The reaction and the thermal desorption spec-troscopy (TDS) analytical approach of dissociating |
JP2001255290A (en) * | 2000-03-09 | 2001-09-21 | Toyota Motor Corp | Analysis method of solid substance surface |
WO2006031905A1 (en) * | 2004-09-14 | 2006-03-23 | Midwest Instrument Company, Inc. | Molten metal gas sampling |
JP2008215995A (en) * | 2007-03-02 | 2008-09-18 | Canon Inc | Mass spectroscope and analysis method |
CN103424518A (en) * | 2013-08-02 | 2013-12-04 | 浙江工业大学 | Device and method for testing hydrogen release of temperature-adjustable material |
CN103592206A (en) * | 2013-11-19 | 2014-02-19 | 中国科学院金属研究所 | Method for testing hydrogen diffusivity or permeability in metal and specific device therefor |
CN105842271A (en) * | 2016-05-17 | 2016-08-10 | 江阴兴澄特种钢铁有限公司 | Method for accurately measuring steel hydrogen evolution temperature range |
CN106645808A (en) * | 2017-02-21 | 2017-05-10 | 哈尔滨工业大学 | Kelvin probe force microscope synchronously measuring multiple parameters |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8691590B2 (en) * | 2011-03-02 | 2014-04-08 | Yuan Ze University | Method for evaluating extrinsic hydrogenation degradation of hydrogen storage material |
-
2017
- 2017-09-14 CN CN201710829523.0A patent/CN107561315B/en active Active
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1039304A (en) * | 1988-07-12 | 1990-01-31 | 中国科学院北京真空物理开放实验室 | The reaction and the thermal desorption spec-troscopy (TDS) analytical approach of dissociating |
JP2001255290A (en) * | 2000-03-09 | 2001-09-21 | Toyota Motor Corp | Analysis method of solid substance surface |
WO2006031905A1 (en) * | 2004-09-14 | 2006-03-23 | Midwest Instrument Company, Inc. | Molten metal gas sampling |
JP2008215995A (en) * | 2007-03-02 | 2008-09-18 | Canon Inc | Mass spectroscope and analysis method |
CN103424518A (en) * | 2013-08-02 | 2013-12-04 | 浙江工业大学 | Device and method for testing hydrogen release of temperature-adjustable material |
CN103592206A (en) * | 2013-11-19 | 2014-02-19 | 中国科学院金属研究所 | Method for testing hydrogen diffusivity or permeability in metal and specific device therefor |
CN105842271A (en) * | 2016-05-17 | 2016-08-10 | 江阴兴澄特种钢铁有限公司 | Method for accurately measuring steel hydrogen evolution temperature range |
CN106645808A (en) * | 2017-02-21 | 2017-05-10 | 哈尔滨工业大学 | Kelvin probe force microscope synchronously measuring multiple parameters |
Also Published As
Publication number | Publication date |
---|---|
CN107561315A (en) | 2018-01-09 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN107561315B (en) | The test device and method of microcosmic olefin hydrogen and hydrogen segregation activation energy in a kind of metal | |
CN107966398B (en) | Test device for simulating high-temperature corrosion | |
WO2019109381A1 (en) | Rapid heating wide range thermogravimetric analyzer | |
CN103983660B (en) | A kind of indoor rock sample test device of thermal conductivity coefficient | |
CN106770440B (en) | A kind of Ceramic Balls bed efficient thermal conductivity test platform | |
McGaughey et al. | Temperature discontinuity at the surface of an evaporating droplet | |
CN101694477B (en) | Experimental device of gas-sensitive temperature property test of carbon nano tube sensor and method | |
CN109030318A (en) | A kind of pressure chamber structure and permeability test macro | |
WO2020177259A1 (en) | Aerosol quenching device, and test system and test method for interfacial heat transfer coefficient of part | |
CN103592206B (en) | A kind of hydrogen in metal diffusion or permeance property method of testing and special purpose device thereof | |
CN105588854A (en) | Quick temperature scanning screening calorimeter | |
CN103234971A (en) | Acidic etching instrument and operation method thereof | |
WO2021035765A1 (en) | Method for neutron imaging during triaxial mechanical test of sediment of natural gas hydrate | |
CN203849193U (en) | Indoor rock sample heat conduction coefficient testing device | |
CN108489855A (en) | A kind of sound-absorbing material flow resistance measuring instrument of temperature-controllable | |
CN101694448A (en) | Vapor pressure testing device and method for easy-sublimation solid energetic materials | |
CN108279187A (en) | The test device and test method of fluid viscosity | |
CN203299283U (en) | An apparatus for measuring the conductivity of high-temperature fused salt | |
RU2454659C2 (en) | Method of evaluating thermal and physical characteristics of building enclosures made from bricks in winter season based on full-scale test results | |
CN203838090U (en) | Thermal expansion material performance testing device | |
CN110793886A (en) | Device and method for measuring reaction rate of liquid alkali metal-water vapor interface | |
CN104819993A (en) | Device and method for testing heat exchange coefficient of cooling water pipe walls | |
CN202814901U (en) | Device for testing thermophysical parameters of asphalt materials by differential scanning calorimetry | |
CN210604475U (en) | Heat conductivity coefficient testing device | |
CN206557136U (en) | A kind of small-sized heater tested for metal micro sample high temperature |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |