CN109708939B - Simple erosion method for three-dimensional shape of MnS precipitate in sulfur-containing steel - Google Patents
Simple erosion method for three-dimensional shape of MnS precipitate in sulfur-containing steel Download PDFInfo
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- CN109708939B CN109708939B CN201910070057.1A CN201910070057A CN109708939B CN 109708939 B CN109708939 B CN 109708939B CN 201910070057 A CN201910070057 A CN 201910070057A CN 109708939 B CN109708939 B CN 109708939B
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Abstract
The invention relates to a precipitate detection method, in particular to a special MnS display method for sulfur-containing microalloyed steel. The sulfur-containing microalloyed steel is common industrial non-quenched and tempered steel and is mainly used for manufacturing parts in the automobile industry. According to the method, a sample metallographic phase sample is prepared by adopting a traditional metallographic polishing method, deep erosion is carried out by adopting a special erosion method, and finally special wiping treatment is carried out to obtain a sample, and the three-dimensional morphology of MnS in the steel is observed under a scanning electron microscope. The method has very obvious three-dimensional display effect on the manganese sulfide precipitate in the sulfur-containing microalloyed steel, and has great significance on the accurate detection and analysis of the manganese sulfide precipitate in the sulfur-containing microalloyed steel.
Description
Technical Field
The invention relates to a precipitate detection method, in particular to a special MnS display method for sulfur-containing microalloyed steel.
Background
The sulfur-containing microalloyed steel is a common high-added-value steel product, is widely applied to important fields of automobile industry and the like, and is mainly used for manufacturing parts such as automobile crankshafts, connecting rods and the like. Metallographic analysis is a common analysis and detection means in the field of metal materials, and can display the microstructure of the metal materials so as to provide guidance for subsequent analysis.
At present, picric acid is mainly used for eroding microscopic dendritic structures, the erosion time is short, generally 10s, and if the erosion time is too long, the surface of a sample becomes black, and the dendritic structures cannot be seen. In addition, the three-dimensional morphology of the MnS precipitated phase in the sulfur-containing steel is detected by an electrolytic etching method, so that MnS falls off from a matrix or the residual part of MnS remains in the matrix, but the electrolytic etching method is complicated in process.
The patent numbers are: the patent of CN201610631231.1, a method for showing austenite grain boundary of microalloy steel under vacuum hot corrosion condition, can realize showing austenite grain boundary of microalloy steel under vacuum hot corrosion condition and compare with traditional technology, it combines the two experimental technologies of heating system simulation of the sample and austenite grain hot corrosion showing together to finish, has simplified the experimental process, helps to reduce energy consumption and emission, improves the experimental efficiency. But does not involve an effective display of manganese sulphide precipitates.
The patent numbers are: the invention discloses a method for extracting and separating nano-scale precipitates in steel by using an organic electrolyte, and particularly discloses a method for extracting and separating nano-scale precipitates in steel by using an organic electrolyte, which can completely and nondestructively extract and separate the nano-scale precipitates in the steel, and solves the problem that the nano-scale precipitates in the steel are easy to agglomerate in the traditional detection method, so that the components, the sizes and the three-dimensional morphological characteristics of the nano-scale precipitates in the steel can be accurately detected. But does not refer to the efficient display of MnS precipitates, the process designed by this patent is electrolytic and the precipitates extracted are of nanometric dimensions, while their characterization is matrix-free.
The patent numbers are: the patent of CN201310643630.6, multi-stage sampling and systematic analysis method for analyzing non-metallic inclusions in steel, mainly extracts various non-metallic inclusions in steel by electrolytic corrosion method, and weighs them. The patent is required to completely separate precipitates from the matrix in order to obtain useful information. Agglomeration is inevitable during the separation process, and the patent adopts a combined process of acid etching and electrolytic etching when acquiring three-dimensional information of inclusions, which may cause information distortion.
The method for displaying precipitates in sulfur-containing microalloyed steel has not been satisfactory, and particularly, the method for displaying precipitates is almost an electrolysis method, and the electrolysis method has complicated steps. The manganese sulfide precipitate is a key component for researching the quality of the sulfur-containing microalloyed steel product, so that a simple method capable of effectively displaying the manganese sulfide precipitate is urgently needed. Hitherto, the display of precipitates in sulfur-containing microalloyed steel has not been sound, and manganese sulfide precipitates are an important component in the study of sulfur-containing microalloyed steel, so that a method capable of easily and effectively displaying the three-dimensional morphology of manganese sulfide precipitates is urgently required.
Disclosure of Invention
Considering that the existing steel has tiny precipitated phases, the existing metallographic polishing method can only observe two-dimensional morphology, and no simple display method capable of effectively displaying the three-dimensional morphology of the manganese sulfide precipitated in the sulfur-containing microalloyed steel exists. The invention provides a special display method for precipitates in sulfur-containing microalloyed steel, which can effectively display the three-dimensional appearance of manganese sulfide precipitates in the sulfur-containing microalloyed steel, and has the advantages of good effect and simple operation.
The invention relates to a simple erosion method for the three-dimensional shape of MnS precipitates in sulfur-containing steel; the sulfur-containing steel is sulfur-containing and manganese-containing microalloyed steel; the simple erosion method comprises the following steps:
step one
Grinding and polishing the sample;
step two
Eroding the sample by adopting an electroless method; the etching agent is prepared by adding 3-5g picric acid and 0.5-1ml liquid detergent into 100ml water;
during erosion, the temperature is controlled to be 60-80 ℃ and the time is 10-20 min;
step three
And wiping the corroded sample to obtain the product.
As a preferred scheme, the invention relates to a simple erosion method for the three-dimensional shape of MnS precipitates in sulfur-containing steel; the non-quenched and tempered steel contains Fe, C, Si, Mn, P, S, Nb, V, Ti, Ni, Cr, and N.
As a further preferable scheme, the invention relates to a simple erosion method for the three-dimensional shape of MnS precipitates in sulfur-containing steel; the microalloyed steel comprises the following components in percentage by mass:
C 0.3-0.6％，
Si0.2-0.5％，
Mn0.6-0.9％，
P0.005-0.01％，
S0.04-0.07％，
Nb0.01-0.03％，
V0.08-0.12％，
Ti0.02-0.05％，
Ni0.1-0.3％，
Cr0.1-0.3％，
N0.1-0.2％,
the balance of Fe.
As a further preferable scheme, the invention relates to a simple erosion method for the three-dimensional shape of MnS precipitates in sulfur-containing steel; the microalloyed steel comprises the following components in percentage by mass:
C0.4-0.5％,
Si0.3-0.4％，
Mn0.7-0.8％，
P0.006-0.008％，
S0.05-0.06％，
Nb0.015-0.025％，
V0.09-0.11％，
Ti0.03-0.04％，
Ni0.15-0.25％，
Cr0.15-0.25％，
N0.12-0.18％,
fe: and (4) the balance.
As a preferred scheme, the invention relates to a simple erosion method for the three-dimensional shape of MnS precipitates in sulfur-containing steel; during flattening, metallographic abrasive paper is adopted for flattening; the sand paper is sequentially polished by 160#, 400#, 800#, 1200#, 1500# and 2000 #; during polishing, a metallographic turntable is adopted, and the rotation speed is 300-; the polishing cloth is flannelette for 3-6 min. When in use, the sample can be ground by hand or by a sample grinder.
As a preferred scheme, the invention relates to a simple erosion method for the three-dimensional shape of MnS precipitates in sulfur-containing steel; the wiping treatment in step three is as follows: the same kind of flannelette for polishing is adopted to wipe in the same direction under the condition of water flow until the corroded black surface becomes bright obviously and can not become brighter. Wiping includes manual.
As a preferred scheme, the invention relates to a simple erosion method for the three-dimensional shape of MnS precipitates in sulfur-containing steel; the obtained product is used for metallographic detection or scanning electron microscope detection. The method is particularly suitable for scanning electron microscope detection.
The invention relates to a simple erosion method for the three-dimensional morphology of MnS precipitates in sulfur-containing steel.
In the process of technical development, the invention has discovered unintentionally that, for a steel containing sulfur of a particular composition; the three-dimensional shape of MnS precipitates in the sulfur-containing steel can be well and completely displayed by adopting a non-electrolytic mode to carry out proper long-time erosion and then matching with a wiping process. So as to facilitate the characterization thereof, wherein the characterization comprises metallographic characterization, scanning electron microscope detection, electron probe detection and the like. The method is very effective for representing the three-dimensional appearance of the manganese sulfide precipitate in the sulfur-containing microalloyed steel. In particular, the mode developed by the present invention has natural advantages in terms of the distribution pattern of precipitates in the matrix and the size of the precipitates in the product when the mode is used for studying a blank having a large thickness.
The invention relates to a simple erosion method for the three-dimensional shape of MnS precipitates in sulfur-containing steel, wherein the precipitates are in a nano level or a micron level in the sulfur-containing steel; the processing of the invention can be objectively characterized by combining with the subsequent characterization process.
The invention mainly aims at the precipitate MnS in the sulfur-containing steel, does not relate to inclusions in the steel, and the precipitated MnS is three-dimensionally observed on a matrix, does not need electrolysis and is not extracted. For thick parts, the distribution of MnS precipitates in the matrix and the dimensional information can be substantially determined by surface and cross-sectional treatment. Compared with the existing method, the efficiency of the method is greatly improved. The time for removing subsequent characterization is only 1/3 in the prior art, and even not available.
Drawings
FIG. 1 is an SEM photograph of the product obtained in example 1;
FIG. 2 is a graph representing the product obtained in comparative example 1.
As can be seen from figure 1, the three-dimensional shape display effect of MnS in the sulfur-containing microalloyed steel is very obvious, and the distribution and the shape of precipitates in the solidification process of the microalloyed steel are effectively displayed. The method is an effective simple display method for the three-dimensional shape of the MnS precipitate of the sulfur-containing microalloy steel.
As can be seen from fig. 2, short-time erosion fundamentally sees the three-dimensional morphology of the precipitates.
Detailed Description
Example 1
In the embodiment, the simple erosion method for the three-dimensional shape of the MnS precipitate in the sulfur-containing steel comprises the following steps:
step one
Grinding and polishing the sample; carrying out sample grinding treatment on sulfur-containing microalloyed steel with chemical components of Fe-0.46C-0.35Si-0.71Mn-0.0075P-0.055S-0.022Nb-0.094V-0034Ti-0.21Ni-0.19Cr-0.014N in wt%, wherein sand paper is adopted for carrying out sample grinding treatment on the sulfur-containing microalloyed steel sequentially according to the sequence of No. 160, No. 400, No. 800, No. 1200, No. 150, No. 0 and No. 2000; polishing the sample after sample grinding, wherein a metallographic turntable is adopted, the revolution is 800r/min, and the time is 5 min; the polishing cloth is flannelette.
Step two
Carrying out deep erosion on the sample by adopting a special erosion method; the erosion agent is picric acid water solution (3-5g picric acid, 100ml water); 1-2 drops of liquid detergent are also added; controlling the temperature to be 60-80 ℃; the erosion time is 10-20 min.
Step three
And wiping the corroded sample, and manually wiping the corroded sample in the same direction by using the same type of flannelette for polishing under the condition of water flow until the black surface becomes obviously bright and cannot be brighter.
The electron micrograph of the precipitated phase of the corroded manganese sulfide of the sample is shown in figure 1.
Comparative example 1
Picric acid attack, attack time 10s, sample surface showing microscopic dendrite structure, as shown in fig. 2, no three-dimensional morphology of precipitates can be seen at all.
Comparative example 2
If the film is etched for a long time, the surface is black without any special wiping treatment, and precipitates are not observed at all.
Comparative example 3
The other operations are identical to those of example 1, except that: the erosion time is 25 min; in the later wiping, it was found that it was difficult to wipe the surface brightly. Further, the three-dimensional morphology of the manganese sulfide precipitated phase cannot be clearly distinguished in the subsequent observation of a scanning electron microscope.
Claims (5)
1. A simple erosion method for the three-dimensional shape of MnS educt in sulfur-containing steel; the method is characterized in that: the sulfur-containing steel is sulfur-containing and manganese-containing microalloyed steel; the microalloyed steel comprises the following components in percentage by mass:
C0.3-0.6％，
Si0.2-0.5％，
Mn0.6-0.9％，
P0.005-0.01％，
S0.04-0.07％，
Nb0.01-0.03％，
V0.08-0.12％，
Ti0.02-0.05％，
Ni0.1-0.3％，
Cr0.1-0.3％，
N0.1-0.2％,
the balance of Fe;
the simple erosion method comprises the following steps:
step one
Grinding and polishing the sample;
step two
Eroding the sample by adopting an electroless method; the etching agent is prepared by adding 3-5g picric acid and 0.5-1ml liquid detergent into 100ml water;
during erosion, the temperature is controlled to be 60-80 ℃ and the time is 10-20 min;
step three
Wiping the corroded sample to obtain a product; the wiping treatment is that the same kind of flannelette for polishing is adopted to wipe towards the same direction under the condition of water flow until the corroded black surface becomes obviously bright and can not become brighter.
2. The simple erosion method for the three-dimensional morphology of MnS precipitates in the sulfur-containing steel according to claim 1; the method is characterized in that: the microalloyed steel comprises the following components in percentage by mass:
C0.4-0.5％,
Si0.3-0.4％，
Mn0.7-0.8％，
P0.006-0.008％，
S0.05-0.06％，
Nb0.015-0.025％，
V0.09-0.11％，
Ti0.03-0.04％，
Ni0.15-0.25％，
Cr0.15-0.25％，
N0.12-0.18％,
fe: and (4) the balance.
3. The simple erosion method for the three-dimensional morphology of MnS precipitates in the sulfur-containing steel according to claim 1; the method is characterized in that: during flattening, metallographic abrasive paper is adopted for flattening; the sand paper is sequentially polished by 160#, 400#, 800#, 1200#, 1500# and 2000 #; during polishing, a metallographic turntable is adopted, and the rotation speed is 300-; the polishing cloth is flannelette for 3-6 min.
4. The simple erosion method for the three-dimensional morphology of MnS precipitates in the sulfur-containing steel according to claim 1; the method is characterized in that: the obtained product is used for metallographic detection or scanning electron microscope detection.
5. The simple erosion method of the three-dimensional morphology of MnS precipitates in the sulfur-containing steel according to claim 4; the method is characterized in that: the obtained product is used for scanning electron microscope detection.
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