CN107561315A - 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
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Abstract
The present invention relates to metal erosion research field, 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 its internal cavities is connected to heat-exchange system by pipeline；The top of flying-spot tube is fixedly connected with the downside of sample stage, and the testing sample of sheet, which is fixed, is loaded on sample stage upper surface；Environmental cabinet made of printing opacity lucite only in bottom opening is positioned on testing sample, and the carrier gas inlet of its side wall is connected to nitrogen cylinder group, and carrier gas outlet is connected to mass spectrograph；The generating laser of laser system is located above environmental cabinet, and for probe by piezoelectric ceramics loaded on inside environmental cabinet, controller is respectively connecting to laser system, flying-spot tube, mass spectrograph, piezoelectric ceramics and probe by signal wire.The present invention can easily and accurately can be tested microcosmic olefin hydrogen in metal and the activation of hydrogen segregation.Have the advantages that spatial resolution is high, tests lossless, multiple functional, simple equipments compared with conventional method.
Description
Technical field
The invention belongs to metal erosion research field, microcosmic olefin hydrogen and hydrogen segregation activation energy in more particularly to a kind of metal
Test device and method of testing.
Background technology
Hydrogen embrittlement is to endanger one of an important factor for high pressure hydrogen system is safe, 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.) causes material to hydrogen at microstructure in the material
Expect microcosmic local hydrogen concentration rise, and then promote the generation of hydrogen induced cracking.The activation of hydrogen segregation can characterize the weight of hydrogen segregation degree
Parameter is wanted, therefore the testing research that energy is activated to microcosmic olefin hydrogen in metal and hydrogen segregation is to disclose mechanism of hydrogen embrittlement and controlled material
The important foundation of hydrogen embrittlement energy.But lack the effective means for being directed to microscopic hydrogen distribution tests in metal at present.
Related scholar is also explored to 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 approaches can only characterize the discharging amount of diverse 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 category for damaging test, and
The performances such as the spatial resolution of the device have much room for improvement.The spatial resolution of atom-probe chromatography microscopy is higher, but its
Cause the follow-on test in situ that can not realize microcosmic olefin hydrogen in test process to microscopic damage caused by material.
It is a kind of gaseous environment metal work function (Work Function) based on capacitance-type vibration to scan Kelvin Force probe
E measurement technology.It can be used for detecting in gaseous environment because of the dissimilar substances dissolving of metal, electricity, mechanics, crystal, absorption etc.
The minor variations of material work functions caused by factor, there is outstanding advantages of spatial resolution is high, high sensitivity and test are lossless,
It is the method that can uniquely determine corrosion electrode potential in gaseous environment.But not yet use it for microcosmic olefin hydrogen in metal at present
And the report that the activation of hydrogen segregation can be tested.
The content of the invention
The technical problem to be solved in the present invention is overcome the shortcomings of in currently existing technology, is proposed microcosmic in a kind of metal
Olefin hydrogen and the activation of hydrogen segregation can test device and method of testings.
To solve technical problem, solution of the invention is：
A kind of test device of microcosmic olefin hydrogen and hydrogen segregation activation energy in metal is provided, including for providing the nitrogen of carrier gas
Gas cylinders group；The device also includes the scanning Kelvin Force being made up of laser system, probe, piezoelectric ceramics, flying-spot tube and controller
Probe system；Sample stage is in hollow box-shaped, and its internal cavities is connected to heat-exchange system by pipeline；The top of the flying-spot tube
The downside of sample stage is fixedly connected with, the testing sample of sheet fixes the upper horizontal surface loaded on sample stage；
Only it is made up in the tubular environmental cabinet of bottom opening of printing opacity lucite, groove is set on the end face of its open side, it is recessed
O-ring is embedded with groove, environmental cabinet is positioned on testing sample and realized by O-ring and sealed；Carrier gas is set in 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 generating laser of system is located above environmental cabinet, probe by piezoelectric ceramics loaded on inside environmental cabinet, generating laser, probe and
The line of flying-spot tube is in vertical；The controller is respectively connecting to laser system, flying-spot tube, mass spectrograph, piezoelectricity by signal wire
Ceramics and probe.
In the present invention, the flying-spot tube possesses 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 its internal cavities is full of heating agent, and heating agent is set in cavity wall
Import and heating agent outlet.
In the present invention, the sample to be tested is the thin rounded flakes that thickness is 0.5~1mm, its surfacing and is thrown through metallographic
Light processing；The overall diameter of sample to be tested is more than the largest outer diameter of environmental cabinet.
In the present invention, the O-ring is the O-ring of graphite material, can be realized 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 brought into close contact with piezoelectric ceramics.
Invention further provides one kind to utilize microcosmic olefin hydrogen and hydrogen segregation activation energy in aforementioned means test metal
Method, comprise the following steps：
(1) metal material that thickness is 0.5~1mm is taken, to its surfacing and carries out metallurgical polishing processing；Cut out two
Block-shaped size identical thin rounded flakes, 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 positioned over sample to be tested
Upper surface, both relative positions of adjustment make the line of generating laser, probe and flying-spot tube in vertical, and ensure 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 of nitrogen cylinder group is opened, the inner chamber of environmental cabinet is continuously replaced, nitrogen is adjusted using flow control valve
Gas velocity keeps uniform and stable；After displacement is more than 0.5h, control heat-exchange system is with the constant heating rate φ not higher than 20 DEG C/h
500 DEG C are warming up to, while starts the hydrogen content in mass spectrograph continuous monitoring 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 closed successively；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 the carrier gas for measuring mass spectrograph integrates to the time, obtains total hydrogen in sample to be tested
Content Q1, identify temperature T corresponding at hydrogen content peak of curveP1；The work function regularity of distribution of sample to be tested and olefin hydrogen rule
It is mutually corresponding；Integral Processing is carried out to a series of work function distribution maps of sample to be tested, with reference to total hydrogen content Q1Treated
Olefin hydrogen rule in test specimens；
(7) second piece of sample to be tested is taken, identical test program is repeated by step (2)~(6), corresponding total hydrogen is obtained and contains
Measure Q2, and temperature T corresponding at hydrogen content peak of curveP2；In test process, except by the heating rate in step (4)
2 φ are changed into from φ, keep other test conditions to keep constant；
(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 scope 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 its mass number scope.
Inventive principle describes：
Found after applicant carries out a large amount of basic research, hydrogen dissolves in a metal can cause metal part work function
Change, and there is good corresponding relation between the change of work function and local hydrogen solubility.Based on this principle, the present invention proposes profit
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 of mass spectrograph acquisition that literary force probe technology obtains
Microcosmic olefin hydrogen in category, the caving law of hydrogen in sample to be tested under different heating rates is finally tested using mass spectrograph to be counted
Calculation obtains corresponding hydrogen segregation activation energy.
Compared with prior art, the beneficial effects of the invention are as follows：
Test device and method of testing proposed by the invention, can easily and accurately to microcosmic olefin hydrogen in metal and
The activation of hydrogen segregation can be tested.There is spatial resolution height compared with conventional method, test is lossless, multiple functional, equipment is simple
Just the advantages that.
Brief description of the drawings
Fig. 1 is the general arrangement schematic diagram of the present invention.
Reference in figure：Nitrogen cylinder group 1, flow control valve 2, carrier gas inlet 3, O-ring 4, environmental cabinet 5, laser system
6th, 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.
Embodiment
Microcosmic olefin hydrogen and hydrogen segregation activation energy test device is as shown in Figure 1 in metal in the present embodiment.
The device is included only in the tubular environmental cabinet 5 of bottom opening, is made up of printing opacity lucite, can high temperature resistant 600
℃.Gas cylinders group 1 proposes the carrier gas that is for experiment, the carrier gas inlet 3 being connected to by flow control valve 2 on environmental cabinet 5, on environmental cabinet 5
Carrier gas outlet 9 is additionally provided with, 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, its mass number scope 0
~50amu.Sample stage 14 is manufactured by the good metal of thermal conductivity factor, and be hollow structure, internal to be full of heating agent 15, heating agent 15 by
Heat-exchange system 18 is provided, and heating agent valve 17 is set in corresponding connecting line.The heat-exchange temperature scope 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 be thickness be 0.5~1mm thin rounded flakes, its surface
Smooth and progress metallurgical polishing processing, overall diameter are more than the overall diameter of environmental cabinet 5.Environmental cabinet 5 is positioned on sample to be tested 10
And sealed between the two by O-ring 4, relative slip 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 also 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 scope is not less than 30 μm, sample stage 14
It is positioned on flying-spot tube 16, and it is affixed with flying-spot tube 16.Piezoelectric ceramics 8 and probe 7 are fixed on inside environmental cabinet 5, the table of probe 7
There is conductive and reflecting coating in face, and laser system 6 is arranged in directly over probe 7, and by laser projection in the back side of probe 7 (laser system
The generating laser of system 6, the line of probe and flying-spot tube are in vertical).Controller 11 to probe 7, flying-spot tube 16, laser system 6,
Piezoelectric ceramics 8 and mass spectrograph 12 are controlled.In test process, piezoelectric ceramics 8 drives probe 7 regularly to be shaken
Dynamic, after being influenceed by the work function of sample to be tested 10, its vibration characteristics is changed probe 7, and these changes are carried on the back in probe 7
The laser system 6 of face reflecting coating projection laser is perceived, and signal is passed to controller 11 by laser system 6, the latter to signal at
The work function regularity of distribution of sample to be tested 10 can be obtained 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 microcosmic olefin hydrogen in aforementioned metal and the method for testing of hydrogen segregation activation energy test device, including following step
Suddenly：
First, the metal material that thickness is 0.5~1mm is taken, to its surfacing and carries out metallurgical polishing processing；Cut out
Two block-shaped size identical thin rounded flakes, then it is flushed with hydrogen simultaneously in 100~300 DEG C and 10~50MPa of hydrogen environment
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 placed environmental cabinet 5
In on the surface to be measured of sample to be tested 10, both relative positions of adjustment make the line of generating laser, probe 7 and flying-spot tube 16 be in
Vertically, and the sealed reliable of O-ring 4 is ensured；Each road pipeline and signal wire are connected, heating agent is filled into sample stage 14；
Gas in environmental cabinet 5 is continuously replaced using nitrogen cylinder group 1, nitrogen flow rate is adjusted using flow control valve 2
And make its holding uniform and stable；After displacement is more than 0.5h, opens controller 11 and rational test parameter is set, open mass spectrograph
Hydrogen content in 12 continuous monitoring carrier gas, adjustment heat-exchange system 18 are warming up to 500 DEG C with constant heating rate φ, 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 regular time section is spaced；
After the temperature of heat-exchange system 18 reaches 500 DEG C, mass spectrograph 12, controller 11 are closed successively, and the regulation temperature of heat-exchange system 18 is slow
Room temperature is down to, nitrogen cylinder group 1 is then closed and takes out sample to be tested 10；Hydrogen content curve in the carrier gas that mass spectrograph 12 is measured
Integration is carried out to the time can obtain total hydrogen content Q in sample to be tested 101, temperature corresponding at hydrogen content peak of curve is identified in addition
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 with reference to total hydrogen content Q1The olefin hydrogen rule in sample to be tested 10 can be obtained.
Second piece of sample to be tested 10 is taken, carries out above-mentioned identical test program.Except heating rate is changed into 2 from φ in experiment
φ, keep other test conditions to keep constant.Obtain corresponding total hydrogen content Q2, and corresponding at hydrogen content peak of curve
Temperature TP2；
Finally, the activation of hydrogen segregation can be equal in sample to be tested 10Wherein R
It is gas constant.
As described above, microcosmic olefin hydrogen and hydrogen segregation activation can test device and method of testing in metal proposed by the present invention
The microcosmic olefin hydrogen that can not only test exactly in metal, the hydrogen segregation activation in metal can be also easily tested out 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 (can be achieved continuously test same position and disclose the Evolution of olefin hydrogen), multiple functional, simple equipments.
It is described above, only it is the case study on implementation of the present invention, any formal limitation not is done to the present invention,
Although the present invention is disclosed as above with preferable case study on implementation, but is not limited to the present invention, any to be familiar with this professional skill
Art personnel, without departing from the scope of the present invention, when structure and technology contents using the disclosure above make it is some
Change or change and turn into the equivalence enforcement case of equivalent variations.Every content without departing from technical solution of the present invention, according to this
Any simple modification, equivalent change and modification that the technical spirit of invention is made to above case study on implementation, still falls within the present invention
In the range of technical scheme.
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；Characterized in that, the device sample stage is in hollow box-shaped, its internal cavities is connected to heat-exchange system by pipeline；It is described
The top of flying-spot tube is fixedly connected with the downside of sample stage, and the testing sample of sheet fixes the upper horizontal surface loaded on sample stage；
Only it is made up in the tubular environmental cabinet of bottom opening of printing opacity lucite, sets groove on the end face of its open side, in groove
Embedded with O-ring, environmental cabinet is positioned on testing sample and realized by O-ring and sealed；Carrier gas disengaging is set in 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 system
Generating laser is located above environmental cabinet, and probe is loaded on inside environmental cabinet by piezoelectric ceramics, generating laser, probe and scanning
The line of pipe is in vertical；The controller is respectively connecting to laser system, flying-spot tube, mass spectrograph, piezoelectric ceramics by signal wire
And probe.
2. device according to claim 1, it is characterised in that the flying-spot tube possesses structure flexible up and down, stretches up and down
Contracting scope is not less than 30 μm, and the scanning range of flying-spot tube is not less than 150 × 150 μm.
3. device according to claim 1, it is characterised in that the sample stage is fabricated by heat-conducting metal, inside it
Cavity is full of heating agent, and Heating medium and heating agent outlet are set in cavity wall.
4. device according to claim 1, it is characterised in that the sample to be tested is that thickness is the circular thin of 0.5~1mm
Piece, its surfacing and is handled through metallurgical polishing；The overall diameter of sample to be tested is more than the largest outer diameter of environmental cabinet.
5. device according to claim 1, it is characterised in that the O-ring is the O-ring of graphite material, environmental cabinet with
Relative slip can be realized between sample to be tested.
6. device according to claim 1, it is characterised in that there are conductive coating and reflective painting in the upper surface of the probe
Layer, probe are brought into close contact with piezoelectric ceramics.
7. a kind of test the method that microcosmic olefin hydrogen and hydrogen segregation activates energy in metal using claim 1 described device, it is special
Sign is, comprises the following steps：
(1) metal material that thickness is 0.5~1mm is taken, to its surfacing and carries out metallurgical polishing processing；Cut out two pieces of shapes
Shape size identical thin rounded flakes, then carry out being flushed with hydrogen processing simultaneously in 100~300 DEG C and 10~50MPa of hydrogen environment, obtain
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 positioned over the upper of sample to be tested
Surface, both relative positions of adjustment make the line of generating laser, probe and flying-spot tube be in vertical, and ensure that O-ring sealing can
Lean on；
(3) each road pipeline and signal wire are connected, heating agent is filled into sample stage；
(4) valve of nitrogen cylinder group is opened, the inner chamber of environmental cabinet is continuously replaced, nitrogen stream is adjusted using flow control valve
Speed keeps uniform and stable；After displacement is more than 0.5h, control heat-exchange system is heated up with the constant heating rate φ not higher than 20 DEG C/h
To 500 DEG C, while start the hydrogen content in mass spectrograph continuous monitoring carrier gas；Utilize 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 closed successively；Control heat-exchange system by
After being gradually cooled to room temperature, close nitrogen cylinder group and remove sample to be tested；
(6) the hydrogen content curve in the carrier gas for measuring mass spectrograph integrates to the time, obtains total hydrogen content in sample to be tested
Q1, identify temperature T corresponding at hydrogen content peak of curveP1；The work function regularity of distribution of sample to be tested and olefin hydrogen rule are phases
Corresponding to mutually, Integral Processing is carried out to a series of work function distribution maps of sample to be tested, with reference to 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 temperature T corresponding at hydrogen content peak of curveP2；In test process, except the heating rate in step (4) is become by φ
For 2 φ, other test conditions are kept to keep constant；
(8) hydrogen segregation in hydrogeneous sample is obtained according to the following formula activates energy：
R is gas constant in formula.
8. device according to claim 1, it is characterised in that the heat-exchange temperature scope of heat-exchange system is -50 DEG C~500
℃。
9. device according to claim 1, it is characterised in that mass spectrograph is triple quadrupole bar mass spectrum, its mass number scope 0
~50amu.
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| 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 |
| CN109668823A (en) * | 2019-01-11 | 2019-04-23 | 中国石油大学(华东) | A kind of bend pipe erosion corrosion pattern original position online acquisition and electrochemical detection system |
| CN110954714A (en) * | 2019-12-20 | 2020-04-03 | 江苏集萃微纳自动化***与装备技术研究所有限公司 | Real-time rigidity adjusting method for probe of atomic force microscope |
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|---|---|
| CN107561315B (en) | 2019-08-30 |
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