CN106323978A - Test method of metallographic structure of austenitic stainless steel pipe for nuclear power - Google Patents
Test method of metallographic structure of austenitic stainless steel pipe for nuclear power Download PDFInfo
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- CN106323978A CN106323978A CN201610709233.8A CN201610709233A CN106323978A CN 106323978 A CN106323978 A CN 106323978A CN 201610709233 A CN201610709233 A CN 201610709233A CN 106323978 A CN106323978 A CN 106323978A
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- stainless steel
- steel pipe
- austenitic stainless
- nuclear power
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- 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
- G01N2001/2866—Grinding or homogeneising
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a test method of metallographic structure of austenitic stainless steel pipe for nuclear power. It is as follows: I. produce the metallographic observation plane by machining on the austenitic stainless steel pipe for nuclear power and grinding; II. conduct mechanical polishing on the plane by a polisher; III. Carry out electrolytic corrosion with the electrolyte the mixture of HNO3 and HCL and H2O [volume ratio, 10:1: (2 - 5)]; IV. Observe and measure the alpha phase of metallographic structure under the microscope; V. Maintain the electrolytic corrosion for another 5s-10s; VI. Observe the austenite grains under the microscope. The invention adopts the mixture of HNO3 and HCL and H2O as the electrolyte in the electrolytic corrosion. Together with the proper voltage, the phase of ferrite would not be affected by heavy corrosion while organization structures of ferrite and austenitic grains with clear levels can be obtained.
Description
Technical field
The invention belongs to material surface structure determination technical field, be specifically related to a kind of nuclear power Austenitic stainless steel pipe gold
The method of inspection of phase constitution.
Background technology
Widely, owing to steel and nickel-base alloy production technology are ripe, source is relatively wide, valency for the Material Field that nuclear power station relates to
Lattice relative moderate and become the main separation target of nuclear power station structural material.
Stainless steel material relates generally to the reactor pressure vessel of nuclear power station；Reactor core, in-pile component, control rod drive machine
Structure；Go the same way pipeline and cool down pump processed；Steam generator and heat exchanger；
Nuclear power stainless steel material has special requirement to composition, performance: 1, the control of neutron absorption element, material is wanted
Asking boron content the lowest, French Standard B content is 0.0015～0.0018%；2, artificial radioactivity Elements C o constituent content
Control, general require less than 0.05%；3, the requirement of anti-radiation performance: 1) control the content of the elements such as extraneous copper phosphorus in steel,
Reduce carbon content, control manganese, nickel content etc.；2) to grain size requirement；3) reduce Cu, As, Sn impurity content, reduce N, S, P, H,
O content；4) segregation and white-spot defects are reduced；5) use heat treatment heat processing technique to improve material property to contain as controlled ferrite
Amount.
As nuclear heat exchanger Austenitic stainless steel pipe
The grain size of product and ferritic phase inspection particularly important, with stainless routine microstructure examination caustic solution, due to
The existence of residual ferrite phase, makes us can not obtain austenite (γ) equi-axed crystal tissue and surveying with Quantitative metallography clearly
Ferrite (α) phase of amount.
Summary of the invention
The technical problem to be solved is for above-mentioned the deficiencies in the prior art, it is provided that one can effectively solve
Austenitic stainless steel pipeIt is difficult to obtain clear austenite etc.
Axialite grain and ferritic phase organisational issues, make Austenitic stainless steel pipe γ crystal grain nuclear power apparent with α phase austenite not
The method of inspection of rust steel pipe metallographic structure.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of nuclear power Austenitic stainless steel pipe gold
The method of inspection of phase constitution, it is characterised in that comprise the following steps:
Step one, on nuclear power Austenitic stainless steel pipe, it is machined into metallographic observation plane, then by machining
The metallographic observation plane gone out is ground on metallographic grinder, grinds backlash and washes the sand grains in metallographic observation plane off；
Step 2, the metallographic observation plane rinsing out the nuclear power Austenitic stainless steel pipe of sand grains in step one is placed in throwing
Mechanically polish on ray machine, until metallographic observation plane surface no marking and pulling；
Step 3, will in step 2 mechanical polishing after nuclear power Austenitic stainless steel pipe be placed in electrolytic etching as anode
Carrying out electrolytic etching in device, the cathode material of electrolytic etching is corrosion resistant plate, and electrolyte is HNO3, HCL and H2O is according to 10:1:
The mixed solution of the volume ratio mixing of (2～5), the voltage of electrolytic etching is 2V～5V, and electric current is 0.3A～0.5A, electrolytic etching
Time be 2s；
Step 4, the metallographic observation plane of nuclear power Austenitic stainless steel pipe after electrolytic etching in step 3 is placed in
Observation and the measurement of α phase metallographic structure is carried out under microscope；
Step 5, will in step 4 observation after nuclear power Austenitic stainless steel pipe be replaced in step 3 as anode
Described electrolyzing and corroding device continues electrolytic etching 5s～10s；
Step 6, the metallographic observation plane of nuclear power Austenitic stainless steel pipe after electrolytic etching in step 5 is placed in
The observation of austenite crystal is carried out under microscope.
The method of inspection of above-mentioned a kind of nuclear power Austenitic stainless steel pipe metallographic structure, it is characterised in that in step one
Described process of lapping is to grind step by step with the metallographic waterproof abrasive paper of 150# and 700# successively, when changing grit paper grinding each time
Grind direction and rotate 90 °, to guarantee last grinding marks is completely eliminated.
The method of inspection of above-mentioned a kind of nuclear power Austenitic stainless steel pipe metallographic structure, it is characterised in that in step 2
The polishing agent of described mechanical polishing is Cr2O3Solution and the Buddha's warrior attendant powder that granularity is 2.5 μm.
The method of inspection of above-mentioned a kind of nuclear power Austenitic stainless steel pipe metallographic structure, it is characterised in that in step 3
Described HCl and HNO3It is analytical reagent.
The present invention compared with prior art has the advantage that
1, the present invention uses by HNO3, HCL and H2The electrolytic solution that O mixes carries out electrolytic etching to stainless steel surfaces,
By rationally selecting electrolytic etching voltage, it is to avoid the Eroded of ferritic phase is affected, can clearly obtain Ovshinsky again simultaneously
The organizational structure level of body crystal grain and ferritic phase.
2, the inventive method is easily operated, is not required to any special installation, can clearly detect Austenitic stainless steel pipe γ
Crystal grain and α phase, efficiently solve the problem that existing Austenitic stainless steel pipe metallographic structure is difficult to obtain clear tissue.
Below in conjunction with the accompanying drawings and embodiment, technical scheme is described in further detail.
Accompanying drawing explanation
Fig. 1 is the α phase metallographic structure figure of the Austenitic stainless steel pipe of the embodiment of the present invention 1.
Fig. 2 is the γ phase metallographic structure figure of the Austenitic stainless steel pipe of the embodiment of the present invention 1.
Fig. 3 is the α phase metallographic structure figure of the Austenitic stainless steel pipe of the embodiment of the present invention 2.
Fig. 4 is the γ phase metallographic structure figure of the Austenitic stainless steel pipe of the embodiment of the present invention 2.
Fig. 5 is the α phase metallographic structure figure of the Austenitic stainless steel pipe of the embodiment of the present invention 3.
Fig. 6 is the γ phase metallographic structure figure of the Austenitic stainless steel pipe of the embodiment of the present invention 3.
Detailed description of the invention
Embodiment 1
The present embodiment is 10.5mm to external diameter, and wall thickness is that the stainless metallographic structure of 316L of 0.5mm is tested, specifically
Method comprises the following steps:
Step one, on nuclear power Austenitic stainless steel pipe, it is machined into metallographic observation plane, then by machining
The metallographic observation plane gone out is ground on metallographic grinder, grinds backlash and washes the sand grains in metallographic observation plane off；Described grinding
Process be to grind step by step with the metallographic waterproof abrasive paper of 150# and 700# successively, the grinding side when changing grit paper each time and grinding
To rotating 90 °, to guarantee last grinding marks is completely eliminated；
Step 2, the metallographic observation plane rinsing out the nuclear power Austenitic stainless steel pipe of sand grains in step one is placed in throwing
On ray machine, use Cr2O3Solution and the Buddha's warrior attendant powder that granularity is 2.5 μm mechanically polish, until metallographic observation plane surface is without drawing
Trace and pulling；
Step 3, will in step 2 mechanical polishing after nuclear power Austenitic stainless steel pipe be placed in electrolytic etching as anode
Carrying out electrolytic etching in device, the cathode material of electrolytic etching is corrosion resistant plate, and electrolyte is HNO3, HCL and H2O is according to 10:1:
The mixed solution of the volume ratio mixing of 5, the voltage of electrolytic etching is 3.5V, and electric current is 0.4A, and the time of electrolytic etching is 2s；Institute
State HCl and HNO3It is analytical reagent；
Step 4, the metallographic observation plane of nuclear power Austenitic stainless steel pipe after electrolytic etching in step 3 is placed in
Observation and the measurement of α phase metallographic structure is carried out under microscope；
Step 5, will in step 4 observation after nuclear power Austenitic stainless steel pipe be replaced in step 3 as anode
Described electrolyzing and corroding device continues electrolytic etching 5s；
Step 6, the metallographic observation plane of nuclear power Austenitic stainless steel pipe after electrolytic etching in step 5 is placed in
The observation of austenite crystal is carried out under microscope.
The α phase metallographic structure figure of the nuclear power Austenitic stainless steel pipe that the present embodiment observes is as it is shown in figure 1, observe α
The image of phase is clear, and recording α phase content with Quantitative metallography is 7%；The nuclear power austenitic stainless steel that the present embodiment observes
The γ crystal grain of pipe is as in figure 2 it is shown, crystal particle crystal boundary is the most clear.
Embodiment 2
The present embodiment is 9.8mm to external diameter, and wall thickness is that the stainless metallographic structure of 304L of 0.4mm is tested, specifically
Method comprises the following steps:
Step one, on nuclear power Austenitic stainless steel pipe, it is machined into metallographic observation plane, then by machining
The metallographic observation plane gone out is ground on metallographic grinder, grinds backlash and washes the sand grains in metallographic observation plane off；Described grinding
Process be to grind step by step with the metallographic waterproof abrasive paper of 150# and 700# successively, the grinding side when changing grit paper each time and grinding
To rotating 90 °, to guarantee last grinding marks is completely eliminated；
Step 2, the metallographic observation plane rinsing out the nuclear power Austenitic stainless steel pipe of sand grains in step one is placed in throwing
On ray machine, use Cr2O3Solution and the Buddha's warrior attendant powder that granularity is 2.5 μm mechanically polish, until metallographic observation plane surface is without drawing
Trace and pulling；
Step 3, will in step 2 mechanical polishing after nuclear power Austenitic stainless steel pipe be placed in electrolytic etching as anode
Carrying out electrolytic etching in device, the cathode material of electrolytic etching is corrosion resistant plate, and electrolyte is HNO3, HCL and H2O is according to 10:1:
The mixed solution of the volume ratio mixing of 2, the voltage of electrolytic etching is 2.0V, and electric current is 0.3A, and the time of electrolytic etching is 2s；Institute
State HCl and HNO3It is analytical reagent；
Step 4, the metallographic observation plane of nuclear power Austenitic stainless steel pipe after electrolytic etching in step 3 is placed in
Observation and the measurement of α phase metallographic structure is carried out under microscope；
Step 5, will in step 4 observation after nuclear power Austenitic stainless steel pipe be replaced in step 3 as anode
Described electrolyzing and corroding device continues electrolytic etching 10s；
Step 6, the metallographic observation plane of nuclear power Austenitic stainless steel pipe after electrolytic etching in step 5 is placed in
The observation of austenite crystal is carried out under microscope.
The α phase metallographic structure figure of the nuclear power Austenitic stainless steel pipe that the present embodiment observes is as it is shown on figure 3, observe α
The image of phase is clear, and recording α phase content with Quantitative metallography is 3%；The nuclear power austenitic stainless steel that the present embodiment observes
As shown in Figure 4, crystal particle crystal boundary is the most clear for the γ crystal grain of pipe.
Embodiment 3
The present embodiment is 11mm to external diameter, and wall thickness is that the stainless metallographic structure of 308L of 0.7mm is tested, specifically side
Method comprises the following steps:
Step one, on nuclear power Austenitic stainless steel pipe, it is machined into metallographic observation plane, then by machining
The metallographic observation plane gone out is ground on metallographic grinder, grinds backlash and washes the sand grains in metallographic observation plane off；Described grinding
Process be to grind step by step with the metallographic waterproof abrasive paper of 150# and 700# successively, the grinding side when changing grit paper each time and grinding
To rotating 90 °, to guarantee last grinding marks is completely eliminated；
Step 2, the metallographic observation plane rinsing out the nuclear power Austenitic stainless steel pipe of sand grains in step one is placed in throwing
On ray machine, use Cr2O3Solution and the Buddha's warrior attendant powder that granularity is 2.5 μm mechanically polish, until metallographic observation plane surface is without drawing
Trace and pulling；
Step 3, will in step 2 mechanical polishing after nuclear power Austenitic stainless steel pipe be placed in electrolytic etching as anode
Carrying out electrolytic etching in device, the cathode material of electrolytic etching is corrosion resistant plate, and electrolyte is HNO3, HCL and H2O is according to 10:1:
The mixed solution of the volume ratio mixing of 3.5, the voltage of electrolytic etching is 5.0V, and electric current is 0.5A, and the time of electrolytic etching is 2s；
Described HCl and HNO3It is analytical reagent；
Step 4, the metallographic observation plane of nuclear power Austenitic stainless steel pipe after electrolytic etching in step 3 is placed in
Observation and the measurement of α phase metallographic structure is carried out under microscope；
Step 5, will in step 4 observation after nuclear power Austenitic stainless steel pipe be replaced in step 3 as anode
Described electrolyzing and corroding device continues electrolytic etching 7s；
Step 6, the metallographic observation plane of nuclear power Austenitic stainless steel pipe after electrolytic etching in step 5 is placed in
The observation of austenite crystal is carried out under microscope.
The α phase metallographic structure figure of the nuclear power Austenitic stainless steel pipe that the present embodiment observes is as it is shown in figure 5, observe α
The image of phase is clear, and recording α phase content with Quantitative metallography is 2%；The nuclear power austenitic stainless steel that the present embodiment observes
As shown in Figure 6, crystal particle crystal boundary is the most clear for the γ crystal grain of pipe.
The above, be only presently preferred embodiments of the present invention, and the present invention not does any restriction, every according to invention skill
Any simple modification, change and the equivalent structure change that above example is made by art essence, all still falls within the technology of the present invention
In the protection domain of scheme.
Claims (4)
1. the nuclear power method of inspection of Austenitic stainless steel pipe metallographic structure, it is characterised in that comprise the following steps:
Step one, on nuclear power Austenitic stainless steel pipe, it is machined into metallographic observation plane, then will be machined into
Metallographic observation plane is ground on metallographic grinder, grinds backlash and washes the sand grains in metallographic observation plane off；
Step 2, the metallographic observation plane rinsing out the nuclear power Austenitic stainless steel pipe of sand grains in step one is placed in buffing machine
On mechanically polish, until metallographic observation plane surface no marking and pulling；
Step 3, will in step 2 mechanical polishing after nuclear power Austenitic stainless steel pipe be placed in electrolyzing and corroding device as anode
In carry out electrolytic etching, the cathode material of electrolytic etching is corrosion resistant plate, and electrolyte is HNO3, HCL and H2O according to 10:1:(2～
5) volume ratio mixing mixed solution, the voltage of electrolytic etching is 2V～5V, and electric current is 0.3A～0.5A, electrolytic etching time
Between be 2s；
Step 4, the metallographic observation plane of nuclear power Austenitic stainless steel pipe after electrolytic etching in step 3 is placed in micro-
Observation and the measurement of α phase metallographic structure is carried out under mirror；
Step 5, will in step 4 observation after nuclear power Austenitic stainless steel pipe be replaced in described in step 3 as anode
Electrolyzing and corroding device continues electrolytic etching 5s～10s；
Step 6, the metallographic observation plane of nuclear power Austenitic stainless steel pipe after electrolytic etching in step 5 is placed in micro-
The observation of austenite crystal is carried out under mirror.
The method of inspection of a kind of nuclear power Austenitic stainless steel pipe metallographic structure the most according to claim 1, its feature exists
In, process of lapping described in step one is to grind step by step with the metallographic waterproof abrasive paper of 150# and 700# successively, changes grain each time
Degree sand paper grinds direction when grinding and rotates 90 °, to guarantee last grinding marks is completely eliminated.
The method of inspection of a kind of nuclear power Austenitic stainless steel pipe metallographic structure the most according to claim 1, its feature exists
In, described in step 2, the polishing agent of mechanical polishing is Cr2O3Solution and the Buddha's warrior attendant powder that granularity is 2.5 μm.
The method of inspection of a kind of nuclear power Austenitic stainless steel pipe metallographic structure the most according to claim 1, its feature exists
In, HCl and HNO described in step 33It is analytical reagent.
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Cited By (4)
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| CN107748098A (en) * | 2017-10-19 | 2018-03-02 | 上海实达精密不锈钢有限公司 | A kind of grain size test caustic solution of the thin stainless steel of spy |
| CN108627514A (en) * | 2018-04-03 | 2018-10-09 | 江苏科泰检测技术服务有限公司 | The quantitative detecting method of ferrite content in silicon steel |
| CN109738263A (en) * | 2018-12-18 | 2019-05-10 | 海洋石油工程股份有限公司 | The detection method of corrosion resistant alloy welding point macroscopic view metallographic |
| CN112730171A (en) * | 2020-12-30 | 2021-04-30 | 成都市海瑞产品质量技术检测有限公司 | Grain size detection method for low-carbon high-alloy material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107748098A (en) * | 2017-10-19 | 2018-03-02 | 上海实达精密不锈钢有限公司 | A kind of grain size test caustic solution of the thin stainless steel of spy |
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| CN109738263B (en) * | 2018-12-18 | 2021-08-31 | 海洋石油工程股份有限公司 | Detection method for macroscopic metallographic phase of corrosion-resistant alloy welded joint |
| CN112730171A (en) * | 2020-12-30 | 2021-04-30 | 成都市海瑞产品质量技术检测有限公司 | Grain size detection method for low-carbon high-alloy material |
| CN112730171B (en) * | 2020-12-30 | 2022-12-09 | 成都市海瑞产品质量技术检测有限公司 | Grain size detection method for low-carbon high-alloy material |
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Effective date of registration: 20190515 Address after: 710201 No. 18, Middle Section of Jinggao North Road, Jingwei New City, Xi'an Economic and Technological Development Zone, Xi'an City, Shaanxi Province Patentee after: Xi'an Han-Tang Analytical Testing Co., Ltd. Address before: 710065 No. three, No. 56, hi tech Zone, Shaanxi, Xi'an Patentee before: Xibu Metal Material Co., Ltd. |
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