CN106596729B - 2.25Cr-1Mo the monitoring of steel crack Propagation and hydrogen embrittlement evaluation method - Google Patents
2.25Cr-1Mo the monitoring of steel crack Propagation and hydrogen embrittlement evaluation method Download PDFInfo
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- CN106596729B CN106596729B CN201611197537.7A CN201611197537A CN106596729B CN 106596729 B CN106596729 B CN 106596729B CN 201611197537 A CN201611197537 A CN 201611197537A CN 106596729 B CN106596729 B CN 106596729B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/14—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object using acoustic emission techniques
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of monitoring of 2.25Cr-1Mo steel crack Propagation and hydrogen embrittlement evaluation method based on sound emission, belong to material non-destructive testing and Nondestructive Evaluation technical field.The present invention utilizes acoustic emission, by monitoring and analyzing the sound emission signal characteristic in 2.25Cr-1Mo steel Fatigue Cracks Propagation, the acoustic emission signal of original state material and hydrogen embrittlement state material is compared and analyzed, by 60dB or more signal accounting come the hydrogen embrittlement situation of assessment material.Present invention could apply to the on-line monitoring of hydrogenator and Nondestructive Evaluations, and relative to traditional material hydrogen embrittlement evaluation method, the present invention has the characteristics that at low cost, speed is fast (1 hour), have biggish application prospect.
Description
Technical field
The invention belongs to material non-destructive testings and Nondestructive Evaluation technical field, are related to a kind of by monitoring crack Propagation
Acoustic emission signal in the process is come the method for evaluating material hydrogen embrittlement situation, specifically, being a kind of 2.25Cr- based on sound emission
The monitoring of 1Mo steel crack Propagation and hydrogen embrittlement evaluation method.
Background technique
2.25Cr-1Mo steel is usually on active service in the case where facing hydrogen environment, inevitably will appear Hydrogen Brittleness Phenomena.Existing material
Hydrogen embrittlement evaluation method be all it is destructive, during sample preparation, the hydrogen of material internal has been escaped, can not accurate evaluation material
Hydrogen embrittlement degree.Therefore, it is necessary to develop Nondestructive Evaluation method, Real-Time Evaluation is carried out to the hydrogen embrittlement situation of material.
Past people are often evaluated with hydrogen embrittlement situation of the method for hanging block performance test to 2.25Cr-1Mo material.Such as Dong
The equality that continues (Dong Shaoping, Yang Huosheng, yellow spring mythical bird like the phoenix etc., domestic hot-wall hydrogenation reactor test plate (panel) dissection test and research [J] petroleum
Construction equipment, 1999,28 (4): 12-14.) by carrying out dissection processing, the impact of test material to the test plate (panel) in hydrogenator
Toughness and fracture toughness, to evaluate material hydrogen embrittlement situation.The disadvantages of the method are as follows heavy workload, and due to test plate (panel) and wall
The stress of material is different, and the result surveyed cannot really reflect the hydrogen embrittlement situation of wall material.
Summary of the invention
It is an object of the invention to propose it is a kind of based on sound emission 2.25Cr-1Mo steel crack Propagation monitoring and hydrogen
Crisp evaluation method, using acoustic emission, by monitoring and analyzing the hair of the sound in 2.25Cr-1Mo steel Fatigue Cracks Propagation
Signal characteristic is penetrated, the acoustic emission signal of original state material and hydrogen embrittlement state material is compared and analyzed, 60dB or more signal is passed through
Accounting carrys out the hydrogen embrittlement situation of assessment material.
A kind of monitoring of 2.25Cr-1Mo steel crack Propagation and hydrogen embrittlement evaluation side based on sound emission that the present invention improves
Method is achieved by the steps of:
2.25Cr-1Mo steel is cut into compact tensile specimen by the first step, is flushed with hydrogen 12~24 hours.Described is flushed with hydrogen use
The method that electrochemistry is flushed with hydrogen.
The electrochemistry is flushed with hydrogen method specifically: using platinized platinum as anode, using sample as cathode, and electrolyte 0.5mol/l
H2SO4 +3.1×10-3mol/l Na2S, being flushed with hydrogen electric current is 15mA/cm2。
Second step will be coupled between the sensor of sound emission instrument and sample with vacuum grease, and blend compounds band is fixed on
Sample side channel two sides.
Acoustic emission detection system parameter setting in setting sound emission instrument: peak value defines time 300us, hits the definition time
600us, blocking time 1000us, sampling length 2k, sample rate 1MSPS are hit.
Third step is acquired acoustic emission signal and is filtered while crack Propagation.
4th step handles the amplitude of filtered acoustic emission signal: calculating amplitude is that 60dB or more (is free of
Number of signals 60dB) accounts for the ratio of whole number of signals.
5th step is flushed with hydrogen the sample of time to difference respectively using Charpy-type test method and tests, passes through sample 54J
The raised numerical value △ VTr54 (DEG C) of ballistic work evaluates the hydrogen embrittlement degree of material.
6th step, according to the 4th step and the 5th step as a result, drawing △ VTr54 (DEG C)-by way of Smoothing fit
60dB or more signal accounting (%) curve.For the material of unknown hydrogen embrittlement degree, by measure in its acoustic emission signal 60dB with
The accounting of upper signal can push away its hydrogen embrittlement degree by the way that the curve is counter.
The beneficial effects of the present invention are:
Present invention could apply to the on-line monitoring of hydrogenator and Nondestructive Evaluations, comment relative to traditional material hydrogen embrittlement
Valence method, the present invention have the characteristics that at low cost, speed is fast (1 hour), have biggish application prospect.
Detailed description of the invention
Fig. 1 is the compact test size of stretching used in the present invention and structural schematic diagram.
Fig. 2 is original state sample acoustic emission signal amplitude situation of change.
Fig. 3 is to be flushed with hydrogen 12 hours sample acoustic emission signal amplitude situations of change.
Fig. 4 is to be flushed with hydrogen 24 hours sample acoustic emission signal amplitude situations of change.
Fig. 5 is the Charpy bar size and result schematic diagram that the present invention uses.
Fig. 6 is the ductile-brittle transiton curve of material.
Fig. 7 is above acoustic emission signal accounting (%) curve of △ VTr54 (DEG C) -60dB.
Fig. 8 is to be flushed with hydrogen 18 hours sample acoustic emission signal amplitude situations of change.
Specific embodiment
Below in conjunction with drawings and examples, the present invention is described in further detail.
The present invention proposes a kind of monitoring of 2.25Cr-1Mo steel crack Propagation and hydrogen embrittlement evaluation method based on sound emission,
Each chemical component of 2.25Cr-1Mo steel is shown in Table 1.
1 2.25Cr-1Mo chemical component of table
Material preparation, and normalizing+tempering are carried out according to said ratio, obtains the 2.25Cr-1Mo steel.
Using the 2.25Cr-1Mo steel crack Propagation monitoring provided by the invention based on sound emission and hydrogen embrittlement evaluation side
Method carries out crack Propagation monitoring to the 2.25Cr-1Mo steel and hydrogen embrittlement is evaluated, the specific steps are as follows:
2.25Cr-1Mo steel is cut into compact tensile specimen by the first step, is flushed with hydrogen 12~24 hours.Described is flushed with hydrogen use
The method that electrochemistry is flushed with hydrogen.
The electrochemistry is flushed with hydrogen method specifically: using platinized platinum as anode, using sample as cathode, and electrolyte 0.5mol/l
H2SO4 +3.1×10-3mol/l Na2S, being flushed with hydrogen electric current is 15mA/cm2。
Second step will be coupled between the sensor of sound emission instrument and sample with vacuum grease, and blend compounds band is fixed on
Sample side channel two sides.
Acoustic emission detection system parameter setting in setting sound emission instrument: peak value defines time 300us, hits the definition time
600us, blocking time 1000us, sampling length 2k, sample rate 1MSPS are hit.
Third step is acquired acoustic emission signal and is filtered while crack Propagation.
4th step handles the amplitude of filtered acoustic emission signal: calculating amplitude is that 60dB or more (is free of
Number of signals 60dB) accounts for the ratio of whole number of signals.
5th step is flushed with hydrogen the sample of time to difference respectively using Charpy-type test method and tests, passes through sample 54J
The raised numerical value △ VTr54 (DEG C) of ballistic work evaluates the hydrogen embrittlement degree of material.
6th step, according to the 4th step and the 5th step as a result, drawing △ VTr54 (DEG C)-by way of Smoothing fit
60dB or more signal accounting (%) curve.For the material of unknown hydrogen embrittlement degree, by measure in its acoustic emission signal 60dB with
The accounting of upper signal can push away its hydrogen embrittlement degree by the way that the curve is counter.
Below simultaneously verification experimental verification method of the invention effect.2.25Cr-1Mo steel curved beam three are prepared first, sample
State is respectively original state and is flushed with hydrogen 12 hours, 24 hours states, is introduced the hydrogen into sample using the method that electrochemistry is flushed with hydrogen
Portion.Using platinized platinum as anode, using sample as cathode, electrolyte is 0.5mol/l H2SO4+3.1×10-3mol/l Na2S is flushed with hydrogen electricity
Stream is 15mA/cm2.To avoid the too long a large amount of evolutions for causing hydrogen of test period, tired examination is carried out immediately after being flushed with hydrogen
It tests.This test uses low-cycle fatigue method, and by test period control within 1 hour, fatigue testing specimen is compact tensile specimen, such as
Shown in Fig. 1, specimen width 50mm, thickness 12.5mm, effective thickness 10.7mm, Initial crack length 18mm.Using MTS-880
Fatigue tester, maximum load are selected as 15kN, and cycle stress ratio selection 0.1, loading frequency selects 10Hz, is measured using extensometer
Notch opening displacement.
While crack Propagation, acoustic emission signal is monitored.The Disp produced using PAC company, the U.S.
16 channel acquisition system of with AEwin v2.19 type sound emission instrument, is acquired acoustic emission signal and handles.Select WD
Broadband sensor, 100~900kHz of response frequency, gain 40dB.Acoustic emission detection system parameter setting: peak value defines the time
300us, it hits definition time 600us, hit blocking time 1000us, sampling length 2k, sample rate 1MSPS.Sensor and examination
It is coupled between sample with vacuum grease, blend compounds band is fixed on sample side channel two sides, as shown in Figure 1, to reduce noise signal pair
Energy is that 10 signals below filter in signal acquisition using the method for energy filter by the interference of subsequent analysis bring.
The amplitude of acoustic emission signal is analyzed.Calculating amplitude is that the number of signals of 60dB or more (being free of 60dB) accounts for entirely
The ratio of portion's number of signals.Sample is under the action of pulsating stress, the plastic deformation of the material internal generation in peak stress
The acoustic emission signal of higher magnitude can be generated with crack propagation；And when stress level reduces, crack tip there are shear-deformable,
Crackle can be closed simultaneously, and fracture surface can generate fine motion friction at this time, can generate compared with low amplitude value acoustic emission signal.Material hair
After raw hydrogen embrittlement, crack closure effect is reduced, therefore amplitude signal proportion rises.
Experimental result shows that 60dB or more the signal accounting of original state material is 4.38% (see Fig. 2), is flushed with hydrogen 12 hours materials
60dB or more the signal accounting 7.28% (see Fig. 3) of material, be flushed with hydrogen 24 hours materials 60dB or more signal accounting 11.26% (see
Fig. 4).
Original state is chosen, be flushed with hydrogen 12 hours and is flushed with hydrogen 24 hours state materials, Charpy punching is carried out between -196 DEG C-room temperature
Test is hit, specimen size is as shown in Figure 5.Each temperature spot does 2~3 impact tests, then draws temperature-ballistic work curve,
Determine the ductile-brittle transition temperature of material.Obtained ductile-brittle transiton curve is as shown in Figure 6.The 54J ballistic work temperature of three kinds of state materials
Degree is as shown in table 2.From Table 2, it can be seen that embrittlement has occurred in material after being flushed with hydrogen, 54J ballistic work temperature increases 16.10 respectively
DEG C and 24.74 DEG C.The above sound of △ VTr54 (DEG C) -60dB is drawn according to acoustic emission signal result and Charpy-type test result to send out
Signal accounting (%) curve is penetrated, as shown in Figure 7.It thus can be according to Fig. 7's as a result, in conjunction with sound emission measurement result, to comment
The hydrogen embrittlement degree of valence material.
2 three kinds of state material 54J ballistic work temperature of table
The hydrogen embrittlement degree of 18 hours materials is flushed with hydrogen using Charpy-type test evaluation, as a result as shown in figure 8, its △ VTr54
=16.76 DEG C.
Be flushed with hydrogen 18 hours according to preceding method and handle, and to the acoustic emission signal in its Fatigue Cracks Propagation into
Row test, measuring its 60dB or more signal accounting is 7.57%, and the anti-knot fruit by Fig. 7 is △ VTr54=17.49 DEG C.With
Charpy-type test result difference 4.36%, illustrates that this method accuracy is higher.
Claims (4)
1. the monitoring of 2.25Cr-1Mo steel crack Propagation and hydrogen embrittlement evaluation method based on sound emission, it is characterised in that:
2.25Cr-1Mo steel is cut into compact tensile specimen by the first step, is flushed with hydrogen 12 ~ 24 hours；
Second step will be coupled between the sensor of sound emission instrument and sample with vacuum grease, and blend compounds band is fixed on sample
Side channel two sides；
Third step is acquired acoustic emission signal and is filtered while crack Propagation；
4th step handles the amplitude of filtered acoustic emission signal: calculating amplitude is that the number of signals greater than 60dB accounts for
The ratio of whole number of signals；
5th step is flushed with hydrogen the sample of time to difference respectively using Charpy-type test method and tests, impacted by sample 54J
The raised numerical value △ VTr54 of function evaluates the hydrogen embrittlement degree of material；
6th step, according to believing as a result, drawing △ VTr54-60dB or more by way of Smoothing fit for the 4th step and the 5th step
Number accounting curve；For the material of unknown hydrogen embrittlement degree, it is greater than the accounting of 60dB signal in its acoustic emission signal by measuring, leads to
Cross that the curve is counter to push away its hydrogen embrittlement degree.
2. the monitoring of 2.25Cr-1Mo steel crack Propagation and hydrogen embrittlement evaluation side according to claim 1 based on sound emission
Method, it is characterised in that: described is flushed with hydrogen the method being flushed with hydrogen using electrochemistry, specifically:
Using platinized platinum as anode, using sample as cathode, electrolyte is 0.5 mol/l H2SO4 + 3.1 × 10-3 mol/ l
Na2S, being flushed with hydrogen current density is 15mA/cm2。
3. the monitoring of 2.25Cr-1Mo steel crack Propagation and hydrogen embrittlement evaluation side according to claim 1 based on sound emission
Method, it is characterised in that: acoustic emission detection system parameter setting is as follows in setting sound emission instrument in second step: peak value defines the time
300 μ s, it hits definition 600 μ s of time, hit 1000 μ s of blocking time, sampling length 2k, sample rate 1MSPS.
4. the monitoring of 2.25Cr-1Mo steel crack Propagation and hydrogen embrittlement evaluation side according to claim 1 based on sound emission
Method, it is characterised in that: compact tensile specimen the width 50mm, thickness 12.5mm, effective thickness 10.7mm, initial crack are long
Spend 18mm.
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| CN108956287A (en) * | 2018-05-21 | 2018-12-07 | 国网甘肃省电力公司电力科学研究院 | A kind of detection method for power grid iron fitting drawing process |
| CN109470188B (en) * | 2018-11-28 | 2021-03-23 | 北京航空航天大学 | High-temperature ultrasonic wall thickness monitor |
| CN110333331B (en) * | 2019-06-24 | 2021-09-10 | 江阴兴澄特种钢铁有限公司 | Method for evaluating effectiveness of hydrogen induced crack resistance test of metal material |
| CN110470725A (en) * | 2019-07-31 | 2019-11-19 | 广州大学 | A kind of detection method detecting metal material tough transition temperature |
| WO2023203592A1 (en) * | 2022-04-18 | 2023-10-26 | 日本電信電話株式会社 | Hydrogen detection method |
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