CN109187152A - It is a kind of for showing the corrosive agent and display methods of heat resisting steel original austenite crystal boundary - Google Patents
It is a kind of for showing the corrosive agent and display methods of heat resisting steel original austenite crystal boundary Download PDFInfo
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- CN109187152A CN109187152A CN201811031640.3A CN201811031640A CN109187152A CN 109187152 A CN109187152 A CN 109187152A CN 201811031640 A CN201811031640 A CN 201811031640A CN 109187152 A CN109187152 A CN 109187152A
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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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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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
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- G01N2021/8477—Investigating crystals, e.g. liquid crystals
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Abstract
The present invention relates to a kind of for showing the corrosive agent and display methods of heat resisting steel original austenite crystal boundary, belongs to technical field of metallographic sample preparation, solves the problems, such as complicated to the unintelligible and display methods of display of heat resisting steel original austenite crystal boundary in the prior art.Corrosive agent in the application is made of potassium permanganate, the concentrated sulfuric acid and distilled water;Display methods includes: the preparation, grinding and polishing of S1. sample, the preparation and chemical attack of S2. corrosive agent, the observation of S3. original austenite crystal boundary.The present invention can be fast and simple the original austenite crystal boundary for showing heat resisting steel and then infer its performance by analyzing and determining the problem of wherein whether there is coarse grains, provide important evidence to formulate production technology.
Description
Technical field
The present invention relates to technical field of metallographic sample preparation, more particularly to one kind is for showing that heat resisting steel original austenite is brilliant
The corrosive agent and display methods on boundary.
Background technique
Heat resisting steel is widely used in supercritical turbine, boiler, cylinder body, because it is higher using temperature, to its performance
It is required that it is stringent, and original austenite grains and its uniformity directly affect the various performances of steel, intensity, toughness, antioxygen such as steel
Change the performance indicators such as performance, fatigue life, coarse austenite grain often leads to obtain coarse tissue after material is cooling, lead
It causes material that there is lower toughness and plasticity, substantially reduces the comprehensive mechanical property of material.Therefore Display of Grain Boundary technology is steel
Essential work during PRODUCTION TRAITS.And heat resisting steel has strict requirements, therefore ferritic heat-resistant steel to grain size
The display technology of original austenite crystal prevention is particularly important, it has weight to the microstructure evolution of judgement material, performance, heat treatment process etc.
The meaning wanted.
In view of ferritic heat-resistant steel original austenite grains to the larger impact of material property, original austenite crystal boundary
Display problem is always key points and difficulties.Heat resisting steel original austenite Display of Grain Boundary method has much at present, and common method is to adopt
Use the saturation bitter taste aqueous acid for containing neopelex as the chemical etching method of etchant, the method is to crystal grain group
Knitting uniform, the lower carbon steel of alloying element content and quenched and tempered steel has certain effect, but, crystal grain group higher to alloying element content
The original austenite crystal boundary for knitting non-uniform ferritic heat-resistant steel displays with being but difficult complete display, thus influences former Ovshinsky
The measurement precision of body grain size is unfavorable for the quality control of material.
For ferritic heat-resistant steel, when corroding crystal grain with conventional etching methodologies, it is easy to appear martensitic structure, is corroded out
The crystal boundary come is easily covered by intergranular structure, and crystal boundary is difficult to show, and display ferritic heat-resistant steel original austenite crystal boundary becomes industry
Interior generally acknowledged problem.Following methods exist in the prior art: (1) use heat treatment method make precipitate crystal boundary collect around with
Show crystal boundary, but its method need to be heat-treated sample, it is more troublesome time-consuming;(2) electrolytic etching method, the sample that will be corroded are used
It is gently polished to show crystal boundary, but electrolytic etching method the high requirements on the equipment;(3) method heated to corrosive agent is used,
Corrosion sample 2 hours in the case where corrosive agent boiling, but etching condition is harsh, and etching time is long.Although these caustic solutions can
To show original austenite crystal prevention, but it is complicated for operation, height is required to operator, is unfavorable for large-scale industrial application.
Summary of the invention
In view of above-mentioned analysis, the present invention is intended to provide a kind of corrosive agent for showing heat resisting steel original austenite crystal boundary and aobvious
Show method, existing display methods is complicated for operation, display crystal boundary is unintelligible solving, and requires operator high, is unfavorable for big
The problem of technical scale is applied.
It is only intended to show by the corrosive agent that potassium permanganate, the concentrated sulfuric acid and distilled water form in the prior art
It is different to be applicable in the type of steel from the present invention for the original austenite crystal boundary of 40Cr15Mo2VN bearing steel;It is not adopted in heat resisting steel field
With the corrosive agent comprising said components, picric acid solution is typically chosen to the corrosion of heat resisting steel in the prior art, this corrosive agent
When corroding to heat resisting steel, etching condition is harsh, and corrosive effect is bad;The discovery of the invention by potassium permanganate,
When the corrosive agent of the concentrated sulfuric acid and distilled water composition is used to corrode the 13Cr9Mo2Co1NiVNbNB steel in the application, corrosion process letter
Just, corrosive effect is good for folk prescription, can clearly indicate out original austenite crystal boundary.And the proportion of corrosive agent in the prior art is
2g potassium permanganate, the concentrated sulfuric acid and 96ml distilled water that 4ml mass fraction is 98%, corrode the application with the corrosive agent of this proportion
In heat resisting steel can not clearly show that its original austenite crystal boundary.
The purpose of the present invention is mainly achieved through the following technical solutions:
It is a kind of for showing the corrosive agent of heat resisting steel original austenite crystal boundary, include: 8~12g Gao Meng in every 1L corrosive agent
Sour potassium, the concentrated sulfuric acid and 850~900ml distilled water that 100~150ml mass fraction is 98%;
The heat resisting steel is 13Cr9Mo2Co1NiVNbNB steel.
Corrosive agent is made by the simple proportion of sulfuric acid, potassium permanganate and distilled water in the present invention, and process for preparation is simple and convenient,
Compared to other corrosive agent, corrosive agent of the invention is good to the corrosive effect of 13Cr9Mo2Co1NiVNbNB heat resisting steel, same to phase
It, can be industrially extensive than the corrosive agent in electrolytic etching method in the prior art, the present invention to the of less demanding of equipment
With.
Further, include: in every 1L corrosive agent 8g potassium permanganate, 100ml mass fraction be 98% the concentrated sulfuric acid and
900ml distilled water.
Further, include: in every 1L corrosive agent 12g potassium permanganate, 100ml mass fraction be 98% the concentrated sulfuric acid and
900ml distilled water.
The present invention also provides a kind of methods for showing heat resisting steel original austenite crystal boundary, comprising the following steps:
S1. the preparation, grinding and polishing of sample;
S2. the preparation of corrosive agent and to sample carry out chemical attack;
S3. heat resisting steel original austenite crystal boundary is observed.
Further, the preparation of sample are as follows: cut one block of metallographic specimen with cutting machine;The grinding of sample are as follows: adopt sample
It is ground with the silicon carbide water-proof abrasive paper of 180-1200 mesh, speed of grinding plate 300-600rpm, when replacing sand paper every time, by sample edge
Abradant surface is rotated by 90 °, and does lubricant using distilled water in process of lapping;The polishing of sample are as follows: use diamond particles suspending agent
It is polished, is polished to smooth interface, no marking and inviolateness, then use clear water and alcohol rinse burnishing surface, and dry up.
Further, the granularity of the diamond particles suspending agent includes 2.5 μm and 1.0 μm.
Further, in the step S2, the preparation of corrosive agent are as follows: weigh 0.8~1.0g potassium permanganate, pour into and be equipped with
In the beaker of 85ml~90ml distilled water, add measurement 10~15ml mass fraction be 98% the concentrated sulfuric acid, uniform stirring,
Stand for standby use.
Further, in the step S2, carrying out chemical attack to sample includes: that the corrosive agent prepared 1) is put into water-bath
It is heated in pot, uniform stirring solution during heating;2) to be heated to 65~70 DEG C and temperature it is constant after, sample is polished
It is put into corrosive agent up;3) sample is taken out after 20~30 minutes, then embathes in oxalic acid solution 5~10 seconds, then takes
Sample and surface is gently wiped under distilled water using absorbent cotton out, with alcohol rinse surface, then dried up.
The present invention can completely show that 13Cr9Mo2Co1NiVNbNB is heat-resisting through heating water bath using above-mentioned corrosive agent
Steel original austenite crystal boundary, convenient for accurate measurement initial grain size and grain size, for the material producing process formulation with it is excellent
Change provides powerful support.
Further, in the step S3, sample is placed on metallographic microscope and is observed, shoot sample metallograph.
Beneficial effects of the present invention are as follows:
(1) corrosive agent raw material used in the present invention is easy to get, and prepares simply, economical and practical, can industrially transport on a large scale
With;
(2) display methods of the invention is simple to operate, without in corrosion process to sample repeatedly gently throw, impregnate or
Wiping, can clearly show the original austenite crystal boundary of 13Cr9Mo2Co1NiVNbNB heat resisting cast steel;
(3) what display methods of the invention was fast and simple shows 13Cr9Mo2Co1NiVNbNB heat resisting steel in actual production
In the grain size of original austenite and then infer its performance by analyzing and determining the problem of wherein whether there is coarse grains,
Important evidence is provided to formulate production technology.
It in the present invention, can also be combined with each other between above-mentioned each technical solution, to realize more preferred assembled schemes.This
Other feature and advantage of invention will illustrate in the following description, also, certain advantages can become from specification it is aobvious and
It is clear to, or understand through the implementation of the invention.The objectives and other advantages of the invention can by specification, claims with
And it is achieved and obtained in specifically noted content in attached drawing.
Detailed description of the invention
Attached drawing is only used for showing the purpose of specific embodiment, and is not to be construed as limiting the invention, in entire attached drawing
In, identical reference symbol indicates identical component.
Fig. 1 is the original austenite crystal boundary figure for the 13Cr9Mo2Co1NiVNbNB heat resisting steel that embodiment 1 is shown;
Fig. 2 is the original austenite crystal boundary figure for the 13Cr9Mo2Co1NiVNbNB heat resisting steel that embodiment 2 is shown;
Fig. 3 is the original austenite crystal boundary figure for the 13Cr9Mo2Co1NiVNbNB heat resisting steel that comparative example 1 is shown;
Fig. 4 be using supersaturated bitter taste aqueous acid as corrosive agent when the 13Cr9Mo2Co1NiVNbNB that shows it is heat-resisting
The original austenite crystal boundary figure of steel;
The 13Cr9Mo2Co1NiVNbNB shown when Fig. 5 is using picric acid hydrochloride alcohol solution as corrosive agent is heat-resisting
The original austenite crystal boundary figure of steel.
Specific embodiment
Specifically describing the preferred embodiment of the present invention with reference to the accompanying drawing, wherein attached drawing constitutes the application a part, and
Together with embodiments of the present invention for illustrating the principle of the present invention, it is not intended to limit the scope of the present invention.
All raw materials of the present invention, are not particularly limited its source, buying on the market or according to those skilled in the art
The preparation of conventional method known to member.
All raw materials of the present invention, are not particularly limited its purity, pure present invention preferably employs analyzing.
Embodiment 1
The component of corrosive agent in the present embodiment are as follows: 1.2g potassium permanganate, 10ml mass fraction be 98% concentrated sulfuric acid and
90ml distilled water.
A kind of method showing heat resisting steel original austenite crystal boundary in the present embodiment, comprising the following steps:
S1. the preparation, grinding and polishing of sample;
The step specifically:
A. the preparation of sample: cutting a block size with electric spark wire cutting machine from 13Cr9Mo2Co1NiVNbNB steel is 10
The metallographic specimen of × 10 × 20mm;
B. sample successively the grinding of sample: is used to the carbonization of 180 mesh, 400 mesh, 600 mesh, 800 mesh, 1000 mesh, 1200 mesh
The grinding of silicon water-proof abrasive paper, the revolving speed of mill are set as 300-600rpm, and when replacing lower a time sand paper every time, sample edge is ground
Face is rotated by 90 °, and the polishing scratch of new passage is made vertically to go up the polishing scratch of a time until covering polishing scratch, successively replaces sand paper and be ground to
Until the silicon carbide water-proof abrasive paper of 1200 mesh, lubricant is done using distilled water in process of lapping;
C. the polishing of sample: the sample ground being placed on polishing machine and is polished, and successively uses polishing agent granularity
It is polished for 2.5 μm and 1.0 μm of diamond particles suspending agents, is polished to smooth interface, no marking and inviolateness, then uses
Clear water and alcohol rinse burnishing surface, and dried up with hair dryer.
S2. the preparation of corrosive agent and to sample carry out chemical attack;
The step specifically:
A. the preparation of corrosive agent: weighing 1.2g potassium permanganate in the balance, pours into the beaker equipped with 90ml distilled water, then plus
Entering with the 10ml mass fraction that graduated cylinder measures is 98% concentrated sulfuric acid, uniform stirring, stand for standby use;
B. chemical attack: the corrosive agent prepared being put into water-bath and is heated, equal using glass bar during heating
Sample polishing is put into corrosive agent with tweezers clamping up after temperature is heated to 70 DEG C and temperature is constant by even agitating solution
In, corrode in constant temperature solution and take out sample after twenty minutes, is then placed in oxalic acid solution and embathes 5 seconds, remove the miscellaneous of erosional surface
Matter then takes out sample using absorbent cotton and gently wipes surface under distilled water, and with alcohol rinse surface, then using blowing
Machine drying, it is to be seen.
S3. heat resisting steel original austenite crystal prevention is observed;
The step specifically: sample is placed on metallographic microscope and is observed, 50 times of sample metallographs is shot, shows
The original austenite crystal boundary of 13Cr9Mo2Co1NiVNbNB heat resisting steel is as shown in Figure 1.
Crystal boundary is clear in the 13Cr9Mo2Co1NiVNbNB heat resisting steel original austenite crystal boundary figure shown in the embodiment 1
It is clear complete, it is in mesh approximation shape.
Embodiment 2
The component of the present embodiment corrosive agent unlike the first embodiment is different, specifically: 0.8g potassium permanganate, 10ml matter
Measuring score is 98% concentrated sulfuric acid and 90ml distilled water.
Other display methods steps are same as Example 1 in embodiment 2.
The original austenite crystal boundary for the 13Cr9Mo2Co1NiVNbNB heat resisting steel that embodiment 2 is shown is as shown in Fig. 2, in figure
Crystal boundary complete display is in mesh approximation shape.
Comparative example 1
The component of this comparative example corrosive agent unlike the first embodiment is different, specifically: 2g potassium permanganate, 4ml mass point
Number is 98% concentrated sulfuric acid and 96ml distilled water.
Other display methods steps are same as Example 1 in comparative example 1.
The original austenite crystal boundary for the 13Cr9Mo2Co1NiVNbNB heat resisting steel that comparative example 1 is shown is as shown in figure 3, in figure
Crystal boundary can not be clearly indicated out.
The present invention is also prepared for comparative example 2 and comparative example 3 for embodiment 1, and comparative example 2 and 3 is to use different corruption
The original austenite crystal boundary figure of the 13Cr9Mo2Co1NiVNbNB heat resisting steel shown in the case where erosion agent.
Comparative example 2
Corrosive agent in comparative example 2 are as follows: supersaturated bitter taste aqueous acid.
The step of 2 display methods of comparative example specifically:
S1. identical as S1 step in embodiment 1;
S2. polished sample is placed in supersaturated bitter taste aqueous acid, is placed in water-bath and heats, in the mistake of heating
Sample polishing is put into corrosive liquid, in constant temperature solution by uniform stirring in journey up after its temperature reaches 70 DEG C of constant temperature
After twenty minutes, sample is taken out with tweezers for corrosion, dries up surface with alcohol rinse surface, and using hair dryer.
S3. sample is placed on metallographic microscope and is observed, shot 50 times of sample metallographs, show
The original austenite crystal boundary of 13Cr9Mo2Co1NiVNbNB heat resisting steel is as shown in Figure 4.
Comparative example 3
Corrosive agent is picric acid hydrochloride alcohol solution in comparative example 3;Specifically: 1g picric acid, 5ml mass fraction are 38%
Hydrochloric acid and 60ml mass fraction be 75% alcohol.
The step of 3 display methods of comparative example specifically:
S1. identical as S1 step in embodiment 1;
S2. polished sample is put into the corrosive agent of picric acid hydrochloride alcohol solution, the corrosive agent prepared is put into
It is heated in water-bath, uniform stirring solution during heating, after when temperature is heated to 70 DEG C and after temperature is constant, by sample
Polishing is put into corrosive liquid with tweezers clamping up, is corroded after twenty minutes in constant temperature solution, is taken out sample, use alcohol rinse
Surface, and surface is dried up using hair dryer.
S3. sample is placed on metallographic microscope and is observed, shot 50 times of sample metallographs, show
The original austenite crystal boundary of 13Cr9Mo2Co1NiVNbNB steel is as shown in Figure 5.
The original austenite for the 13Cr9Mo2Co1NiVNbNB heat resisting steel that Examples 1 and 2 and comparative example 2 and 3 are shown
Crystal boundary figure is compared, and the display figure energy complete display in Examples 1 and 2 shows that crystal boundary, crystal boundary are in mesh approximation shape, and
The display figure of comparative example 2 and 3 cannot clearly indicate out crystal boundary;It can be seen that corrosive agent pair of the invention
The corrosive effect of 13Cr9Mo2Co1NiVNbNB heat resisting steel is more preferable.
In conclusion the corrosive agent that the present invention provides a kind of for showing heat resisting steel original austenite crystal boundary and display side
Method uses chemical attack to 13Cr9Mo2Co1NiVNbNB heat resisting steel to show crystal boundary, and wherein corrosive agent raw material is easy to get, and prepares letter
It is single, it is low for equipment requirements compared to electrochemical erosion method;It is simple to operate using the display methods of above-mentioned corrosive agent simultaneously, energy
The original austenite crystal boundary for crossing clear display 13Cr9Mo2Co1NiVNbNB heat resisting cast steel, to analyze the crystal grain of original austenite
The problem of degree, judgement wherein whether there is coarse grains, and then infer its performance, for formulate production technology provide it is important according to
According to.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of for showing the corrosive agent of heat resisting steel original austenite crystal boundary, which is characterized in that include: 8 in every 1L corrosive agent
~12g potassium permanganate, 100~150ml concentrated sulfuric acid and 850~900ml distilled water;
The heat resisting steel is 13Cr9Mo2Co1NiVNbNB steel.
2. according to claim 1 a kind of for showing the corrosive agent of heat resisting steel original austenite crystal boundary, which is characterized in that
It include: 8g potassium permanganate, the 100ml concentrated sulfuric acid and 900ml distilled water in every 1L corrosive agent.
3. according to claim 1 a kind of for showing the corrosive agent of heat resisting steel original austenite crystal boundary, which is characterized in that
It include: 12g potassium permanganate, the 100ml concentrated sulfuric acid and 900ml distilled water in every 1L corrosive agent.
4. a kind of method for showing heat resisting steel original austenite crystal boundary, which is characterized in that using described in any one of claim 1-3
Corrosive agent, the described method comprises the following steps:
S1. the preparation, grinding and polishing of sample;
S2. the preparation of corrosive agent and to sample carry out chemical attack;
S3. heat resisting steel original austenite crystal boundary is observed.
5. a kind of method for showing heat resisting steel original austenite crystal boundary according to claim 4, which is characterized in that the step
In rapid S1, the preparation of sample are as follows: cut one block of metallographic specimen with cutting machine.
6. a kind of method for showing heat resisting steel original austenite crystal boundary according to claim 4, which is characterized in that the step
In rapid S1, the grinding of sample are as follows: grind sample using the silicon carbide water-proof abrasive paper of 180-1200 mesh, speed of grinding plate 300-
Sample is rotated by 90 ° along abradant surface when replacing sand paper every time, does lubricant using distilled water in process of lapping by 600rpm.
7. a kind of method for showing heat resisting steel original austenite crystal boundary according to claim 4, which is characterized in that the step
In rapid S1, the polishing of sample are as follows: polished using diamond particles suspending agent, be polished to smooth interface, no marking and without dirt
Then point is used clear water and alcohol rinse burnishing surface, and is dried up.
8. a kind of method for showing heat resisting steel original austenite crystal boundary according to claim 7, which is characterized in that the gold
The granularity of hard rock particle suspension includes 2.5 μm and 1.0 μm.
9. a kind of method for showing heat resisting steel original austenite crystal boundary according to claim 4, which is characterized in that the step
In rapid S2, carrying out chemical attack to sample includes: that 1) corrosive agent prepared is put into water-bath to heat, during heating
Uniform stirring solution;2) to be heated to 65~70 DEG C and temperature it is constant after, by sample polishing be put into corrosive agent up;3)20
Sample is taken out after~30 minutes, is then embathed in oxalic acid solution 5~10 seconds, and sample is then taken out and is being distilled using absorbent cotton
Surface is gently wiped under water, with alcohol rinse surface, is then dried up.
10. a kind of method for showing heat resisting steel original austenite crystal boundary according to claim 4, which is characterized in that described
In step S3, sample is placed on metallographic microscope and is observed, shoots sample metallograph.
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CN110132697A (en) * | 2019-06-20 | 2019-08-16 | 洛阳Lyc轴承有限公司 | A kind of caustic solution of bearing steel grain size |
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