CN107219296A - A kind of method of diffusible hydrogen content in quick and precisely measurement weld metal - Google Patents
A kind of method of diffusible hydrogen content in quick and precisely measurement weld metal Download PDFInfo
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- CN107219296A CN107219296A CN201710464661.3A CN201710464661A CN107219296A CN 107219296 A CN107219296 A CN 107219296A CN 201710464661 A CN201710464661 A CN 201710464661A CN 107219296 A CN107219296 A CN 107219296A
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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Abstract
The present invention relates to a kind of method of diffusible hydrogen content in quick and precisely measurement weld metal, belong to steel physical and chemical inspection technical field.This method is heated by the way that weld metal sample is placed in the electric furnace under high vacuum state, is heated according to the program of technological requirement, diffusible hydrogen in weld seam is obtained energy and is accelerated diffusion, while carrying out translocation with high-precision mass spectrograph.Realize quick and precisely efficiently measurement weld metal in diffusible hydrogen content, overcome before conventional method measurement the diffusible hydrogen content cycle length, precision is low, toxicity is big, pollute environment the shortcomings of.
Description
Technical field
The invention discloses a kind of method of diffusible hydrogen content in weld metal, belong to steel physical and chemical inspection technical field.
Background technology
Welding is a kind of method of the most frequently used connection metal in modern industry.In welding process, it can produce a certain amount of
Hydrogen, a portion can be escaped during the cooled and solidified of molten bath, had little time the hydrogen of effusion and can then be remained into weld seam.Retain
The hydrogen come exists with atom or ionic condition more, because its radius is relatively small, can be diffused in metal lattice, so
Referred to as diffusible hydrogen.
Postwelding can be escaped with the increase of standing time, a part of diffusible hydrogen from weld seam, and another part diffusible hydrogen then can
Diffusion aggregation is combined into hydrogen molecule, is changed into being difficult at the holes such as lattice defect, micro-flaw and non-metallic inclusion edge
Diffusible hydrogen, and constantly aggregation accumulation.Weld seam sensitive organization can be caused to produce hydrogen induced cracking under stress, influence welding connects
The mechanical property of head, butt welding binding is configured to potentially hazardous.Because the diffusion aggregation of hydrogen needs the time, diffusible hydrogen is caused to cause
Crackle delay occur, the welding structure often aligned under arms causes fatal harm.Diffusible hydrogen content, residual stress, weldering
It is the main cause for causing welding structure crackle to stitch sensitive organization three.Control diffusible hydrogen content is typically considered reduction hydrogen and caused
Crackle endangers maximally effective means.Based on above reason, quick and precisely measuring diffusible hydrogen content in weld metal becomes particularly
It is important.
Current many countries have all formulated the standard method for determining Diffusible Hydrogen In Deposited Metal, including International Welding
Meeting standard IIW/ISO 3690-2012, Unite States Standard AWS A4.3-1993, JISZ3113-2007D of Japan etc., we are national
The standard method of the measure Diffusible Hydrogen In Deposited Metal of newest formulation is GB/T3965-2012.The above standard is in weld seam
The continuous mode of diffusible hydrogen has all done specific regulation.On the whole, method determines diffusible hydrogen in weld metal in mainly having three,
Respectively glycerine method, mercury process and gas chromatography.But these three methods have its limitation and weak point.Glycerine method by
It is big in glycerine viscosity, cause hydrogen partial to be attached on sample and measurement tube wall or be suspended in glycerine, make measurement result relatively low,
Measuring result error is larger.Although mercury process is accurate compared with glycerine method measurement result, mercury pollutes the environment, harmful to human, real
Border application is very limited.Gas chromatography is it may be said that more more advanced than both the above method, although overcome both the above method
Weak point, be classified as standard by many countries, but gas chromatography also has that complex operation, instrument price be expensive, detection limit for height
Weak point.Other three of the above method also has the shortcomings that measurement period length, precision are low.Based on above reason, it is badly in need of seeking
Diffusible hydrogen content new method in a kind of quick and precisely measurement weld metal is looked for, the need for meeting welding development now.This patent
Diffusible hydrogen content new method in a kind of disclosed quick and precisely measurement weld metal, overcomes three of the above method not well
Foot part.
In addition, the investigative technique personnel of the present invention authorize the patent specification and right of Boeing Co. to disclosing
Claim（Patent publication No.：Hydrogen content system and method in the measurement samples of CN 103454125）Carry out after careful reading,
It is the remodeling upgrading in research measurement diffusible hydrogen field unanimously to think method of disclosure, is existed with the method disclosed in Boeing
In implementation process, using all different on field and mass spectrograph construction and detection algorithm.Wherein topmost distinguish is exactly：Ripple
Need to use inert gas in method implementation process disclosed in sound company and do carrier gas, carrier gas is mixed with the hydrogen diffused out, then
Detector is brought to be detected, this method detection noise it is very big, data accuracy is not high, specifically how examinations and calculation
Method is not disclosed.By comparison, biggest advantage is exactly without carrier gas in detection process to this method.Carrier gas can thus be avoided
Influence of the factor such as purity, air pressure back end to testing result.And simple to operate, can also reduce high-purity inert gas makes
With the financial cost brought.Method disclosed in Boeing is mainly used in structural material to prevent environmental corrosion from carrying out surface
Hydrogen in the hydrogen increased in processing procedure, mainly some weak traps.And method of disclosure is mainly measurement weld metal
In diffusible hydrogen, including the hydrogen in weak trap and deep trap, specific aim is stronger.
The method of diffusible hydrogen content, overcomes the above three well in the quick and precisely measurement weld metal of the application design
The weak point of the method for kind.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of quick and precisely measurement weld seam gold for above-mentioned prior art
The new method of diffusible hydrogen content in category, significantly improves detection speed, and detection limit is lower, and measurement accuracy is up to 0.01ppm.
The present invention the used technical scheme that solves the above problems is：Diffusible hydrogen in a kind of quick and precisely measurement weld metal
The method of content, comprises the following steps,
（1）Sampling and processing：Postwelding metal material is sampled in representative commissure, obtained during sampling with wire cutting method
Sample, removes surface oxide layer, whole sample pretreating process, specimen temperature with 1200 mesh with thin sand paper polishing sample afterwards
Room temperature scope is maintained at, in case temperature crosses the escape of high part diffusible hydrogen；
（2）Sample is cleaned：Sample is put into absolute ethyl alcohol, cleaned more than 10 minutes in ultrasonic washer, sample is taken out
Dried up with hair-dryer cold wind；
（3）Sample is weighed：Sample mass is weighed with high Accuracy Electronic Balance and is recorded, 0.0001 gram is accurate to；
（4）Cleaned sample in high pure nitrogen protection down enters high precision electro steam stove, close sample introduction storehouse and electric furnace it
Between connection valve, with two-stage vortex molecular pump electric furnace is evacuated, when vacuum reaches ultrahigh vacuum in electric furnace burner hearth
After state, the secondary vortices molecular pump being connected with electric furnace is closed, while opening the company between electric furnace and mass spectrograph detection storehouse
Valve is connect, mass spectrometric two-stage vortex molecular pump and one-level mechanical pump is opened, treats that the vacuum in mass spectrograph detection storehouse reaches 10- 10Below pa and stably one value it is constant after, carry out next step operation；
（5）Heating Dehydrogenation：Electric furnace firing rate and target temperature are set as needed, start to heat sample, sample
In diffusible hydrogen occur acceleration diffusional precipitation because obtaining certain energy；
（6）Diffusible hydrogen is determined：The vortex molecular pump extracting in the hydrogen mass spectrograph diffused out in electric furnace to high accuracy four
In heavy duty mass spectrograph, content is measured using mass spectrography, hydrogen is extracted into mass spectrograph, is first ionized, added in magnetic field
Speed, is then split into the mass detector of protium and detects, constantly keep track of the quality signal of the protium detected
Intensity, cumulative calculation goes out the gross mass of the hydrogen diffused out, algorithm：The quality for the hydrogen that computer recording every five seconds for example is diffused out, root
Time conversion is recorded as the corresponding change curve of diffusible hydrogen quality and temperature, to diffusible hydrogen curve into temperature according to the rate of heat addition
The definite integral for carrying out temperature range is that can calculate the diffusible hydrogen content of the temperature range；
（7）Data processing：The quality for the diffusible hydrogen quality combination sample that mass spectrograph is detected obtains diffusible hydrogen quality in sample
Fraction.
Vacuum in electric furnace is up to 10-10Below pa.
Alternatively, 50 DEG C/h-100 DEG C/h of electric furnace firing rate in step 5,300 DEG C -600 DEG C of target temperature.
Compared with prior art, the advantage of the invention is that：
Solve diffusible hydrogen in current welding metal weld seam and be difficult to the problem quick and precisely measured, evaluated in metal weldability quality
In method, diffusible hydrogen content is a major parameter of weld seam cool attenuation.So diffusible hydrogen contains in measurement weld metal
Amount is particularly important.The application is placed to weld metal sample in the electric furnace under a kind of high vacuum state and heated, according to
The program heating of technological requirement, makes in weld seam diffusible hydrogen obtain energy and accelerates to spread according to rule, while with high accuracy mass spectrum
Instrument carries out translocation.Realize well and quick and precisely efficiently measure diffusible hydrogen content in weld metal.Tradition side before overcoming
Method measurement the diffusible hydrogen content cycle length, precision is low, toxicity is big, pollute environment the shortcomings of.
Embodiment
The present invention is described in further detail with reference to embodiments.
Example 1（Standard sample is verified）
Standard specimen is the hydrogen standard specimen of LECO companies production, and the numbering of standard specimen 1 is：PART NO 502-457 hydrogen contents are：0.9±
0.03ppm；Standard specimen 2 is numbered：PART NO 501-529 hydrogen contents are：5.7±0.06ppm.Both standard specimens take two respectively
, and it is encoded to 1,2,3,4.All washed respectively with ultrasonic washer in absolute alcohol after 15 minutes.Taking-up is blown with cold wind
It is dry, then weigh 1 respectively with balance, 2,3, No. 4 standard specimen quality and record.No. 1, No. 3 sample measuring methods of the present invention
Determine hydrogen content.No. 2, the EMGA-821 hydrogen determinators measurement of No. 4 samples.Measurement result is as shown in table 1：
Table 1
| Standard specimen is encoded | The present invention surveys hydrogen method | EMGA-821 hydrogen determinators | Standard value |
| Standard specimen 1 | 0.76 ppm | 1.37 ppm | 0.9±0.03ppm |
| Standard specimen 2 | 5.53 ppm | 6.18 ppm | 5.7±0.06ppm |
The hydrogen content that the inventive method measures can be seen that by above measurement result substantially more relatively low than standard value.This is
Because this method measurement is diffusible hydrogen content in sample, it is certain to lower than hydrogen total amount.And use the measurement of EMGA-821 hydrogen determinators
Principle is thermal conductivity method, and the result of the method measurement is hydrogen total amount in sample.But measured deviation is big, and the hydrogen content measured is not accurate
Diffusible hydrogen, data can only be used for refer to.Above example shows what this method measurement diffusible hydrogen content can be achieved on.
Example 2
After Q690 steel plates cold crack sensitivity soldering test, before Dehydroepiandrosterone derivative is carried out, taken respectively at three diverse locations of weld seam
Two samples, altogether 6 samples；Numbering is：1st, 1,2,2,3,3；Again after Dehydroepiandrosterone derivative, in three diverse location punishment of weld seam
Two samples are not taken, are total up to 6 samples；Numbering is：4th, 4,5,5,6,6；It is 10 × 10 that above sample, which is all processed into size,
×30mm.Surface oxide layer is gently polished off with 1200 mesh sand paper, is cleaned in ultrasonic washer with absolute alcohol 15 minutes,
Take out sample to be dried up with cold wind, use electronic balance（It is accurate to 0.0001g）Weigh sample mass and record.One of which is tried
Sample is to determine diffusible hydrogen content with the inventive method.Sample is specifically put into sample introduction storehouse, sample imported with magnetic coupling guide rod
Electric furnace, each parameter of setting heating.Treat vacuum up to 10-10Electric furnace is opened when following, at the same open mass spectrograph carry out constantly with
Track translocation, according to certain rate of heat addition（The optimal rate of heat addition that test of many times is found out）Stop during the target temperature for reaching setting
Heating.The diffusible hydrogen accumulated quality combination sample mass that mass spectrograph is detected calculates diffusible hydrogen mass fraction in sample.Separately
One group of sample determines hydrogen content using mercury process.Measurement result such as table 2, table 3.
Diffusible hydrogen content before the Dehydroepiandrosterone derivative of table 2
Diffusible hydrogen content after the Dehydroepiandrosterone derivative of table 3
By above example analysis result, table 2 this it appears that present invention measurement diffusible hydrogen content result is surveyed with traditional mercury process
Amount result is consistent substantially.It is accurate to illustrate this method measurement result.The result of table 3 shows that this patent measuring method can be surveyed
Measure the diffusible hydrogen of low content and traditional mercury process cannot measure low content diffusible hydrogen.Present invention measurement diffusion hydrogen methods detection limit
It is low, the weak point that conventional method detects limit for height is overcome well.
In addition to the implementation, present invention additionally comprises have other embodiment, all use equivalent transformation or equivalent replacements
The technical scheme that mode is formed, all should fall within the scope of the hereto appended claims.
Claims (3)
1. a kind of method of diffusible hydrogen content in quick and precisely measurement weld metal, it is characterised in that：Comprise the following steps,
（1）Sampling and processing：Postwelding metal material is sampled in representative commissure, obtained during sampling with wire cutting method
Sample, removes surface oxide layer, whole sample pretreating process, specimen temperature with 1200 mesh with thin sand paper polishing sample afterwards
Room temperature scope is maintained at, in case temperature crosses the escape of high part diffusible hydrogen；
（2）Sample is cleaned：Sample is put into absolute ethyl alcohol, cleaned more than 10 minutes in ultrasonic washer, sample is taken out
Dried up with hair-dryer cold wind；
（3）Sample is weighed：Sample mass is weighed with high Accuracy Electronic Balance and is recorded, 0.0001 gram is accurate to；
（4）Cleaned sample in high pure nitrogen protection down enters high precision electro steam stove, close sample introduction storehouse and electric furnace it
Between connection valve, with two-stage vortex molecular pump electric furnace is evacuated, when vacuum reaches ultrahigh vacuum in electric furnace burner hearth
After state, the secondary vortices molecular pump being connected with electric furnace is closed, while opening the company between electric furnace and mass spectrograph detection storehouse
Valve is connect, mass spectrometric two-stage vortex molecular pump and one-level mechanical pump is opened, treats that the vacuum in mass spectrograph detection storehouse reaches 10- 10Below pa and stably one value it is constant after, carry out next step operation；
（5）Heating Dehydrogenation：Electric furnace firing rate and target temperature are set as needed, start to heat sample, sample
In diffusible hydrogen occur acceleration diffusional precipitation because obtaining certain energy；
（6）Diffusible hydrogen is determined：The vortex molecular pump extracting in the hydrogen mass spectrograph diffused out in electric furnace to high accuracy four
In heavy duty mass spectrograph, content is measured using mass spectrography, hydrogen is extracted into mass spectrograph, is first ionized, added in magnetic field
Speed, is then split into the mass detector of protium and detects, constantly keep track of the quality signal of the protium detected
Intensity, cumulative calculation goes out the gross mass of the hydrogen diffused out, algorithm：The quality for the hydrogen that computer recording every five seconds for example is diffused out, root
Time conversion is recorded as the corresponding change curve of diffusible hydrogen quality and temperature, to diffusible hydrogen curve into temperature according to the rate of heat addition
The definite integral for carrying out temperature range is that can calculate the diffusible hydrogen content of the temperature range；
（7）Data processing：The quality for the diffusible hydrogen quality combination sample that mass spectrograph is detected obtains diffusible hydrogen quality in sample
Fraction.
2. the method for diffusible hydrogen content in quick and precisely measurement weld metal according to claim 1, it is characterised in that：Electricity
Vacuum in steam stove is up to 10-10Below pa.
3. the method for diffusible hydrogen content in quick and precisely measurement weld metal according to claim 1, it is characterised in that：Step
50 DEG C/h-100 DEG C/h of electric furnace firing rate in rapid 5,300 DEG C -600 DEG C of target temperature.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111721663A (en) * | 2019-03-21 | 2020-09-29 | 宝山钢铁股份有限公司 | Method for evaluating fish scaling performance of steel for enamel |
| CN112986523A (en) * | 2021-03-08 | 2021-06-18 | 辽宁石油化工大学 | Method for displaying existence of diffusible hydrogen in welding seam on production site |
| CN113495021A (en) * | 2020-03-19 | 2021-10-12 | 宝山钢铁股份有限公司 | Surface treatment process method for diffusible hydrogen analysis sample |
| CN114414422A (en) * | 2022-03-31 | 2022-04-29 | 天津市特种设备监督检验技术研究院(天津市特种设备事故应急调查处理中心) | Method and device for measuring content of diffusible hydrogen in welding material deposited metal |
| US20220221439A1 (en) * | 2021-01-13 | 2022-07-14 | The Boeing Company | Systems and methods for determining concentrations of mobile hydrogen of metallic objects and/or reducing concentrations of mobile hydrogen of metallic objects |
-
2017
- 2017-06-19 CN CN201710464661.3A patent/CN107219296A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 武光宗: ""高强度传动轴用钢的氢脆敏感性"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111721663A (en) * | 2019-03-21 | 2020-09-29 | 宝山钢铁股份有限公司 | Method for evaluating fish scaling performance of steel for enamel |
| CN113495021A (en) * | 2020-03-19 | 2021-10-12 | 宝山钢铁股份有限公司 | Surface treatment process method for diffusible hydrogen analysis sample |
| US20220221439A1 (en) * | 2021-01-13 | 2022-07-14 | The Boeing Company | Systems and methods for determining concentrations of mobile hydrogen of metallic objects and/or reducing concentrations of mobile hydrogen of metallic objects |
| US11953488B2 (en) * | 2021-01-13 | 2024-04-09 | The Boeing Company | Systems and methods for determining concentrations of mobile hydrogen of metallic objects and/or reducing concentrations of mobile hydrogen of metallic objects |
| CN112986523A (en) * | 2021-03-08 | 2021-06-18 | 辽宁石油化工大学 | Method for displaying existence of diffusible hydrogen in welding seam on production site |
| CN114414422A (en) * | 2022-03-31 | 2022-04-29 | 天津市特种设备监督检验技术研究院(天津市特种设备事故应急调查处理中心) | Method and device for measuring content of diffusible hydrogen in welding material deposited metal |
| CN114414422B (en) * | 2022-03-31 | 2022-07-26 | 天津市特种设备监督检验技术研究院(天津市特种设备事故应急调查处理中心) | Method and device for measuring content of diffusible hydrogen in welding material deposited metal |
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Application publication date: 20170929 |