CN111220441A - Chromium-containing pig iron metallographic corrosive agent and metallographic structure display method - Google Patents
Chromium-containing pig iron metallographic corrosive agent and metallographic structure display method Download PDFInfo
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- CN111220441A CN111220441A CN202010212896.5A CN202010212896A CN111220441A CN 111220441 A CN111220441 A CN 111220441A CN 202010212896 A CN202010212896 A CN 202010212896A CN 111220441 A CN111220441 A CN 111220441A
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Abstract
The invention relates to a chromium-containing pig iron metallographic corrosive agent and a metallographic structure display method, belonging to the technical field of chromium alloy detection. The invention solves the technical problem that no effective method for preparing and displaying the metallographic phase of chromium-containing pig iron exists at present. The metallographic corrosive disclosed by the invention comprises 3-8% of nitric acid by volume percentage and the balance of absolute ethyl alcohol, and the metallographic structure display method comprises the steps of cutting, sample embedding and surface treatment of chromium-containing pig iron to obtain a bright and scratch-free surface to be corroded, then carrying out cleaning and air drying on the surface to be corroded by the metallographic corrosive to obtain a metallographic sample to be detected, and finally carrying out metallographic observation and analysis under a metallographic microscope. The method has the advantages of simple operation method and good repeatability, can efficiently display the metallographic structure of the chromium-containing pig iron, has clear boundary of a high chromium phase and a matrix phase, and provides a basis for guiding process parameter control of links such as smelting, cooling, crushing and the like of the chromium-containing pig iron and product segregation detection.
Description
Technical Field
The invention belongs to the technical field of chromium alloy detection, and particularly relates to a metallographic corrosion and display method of chromium-containing pig iron.
Background
Currently, the product for smelting ferrochrome from the carbon thermal reduction chromite is mainly high-carbon ferrochrome, and the chromite with high chromium content and high chromium-iron ratio is generally adopted as a main raw material for smelting. However, as the global chromite with high chromium content and high ferrochrome ratio is gradually consumed, the proportion of the chromite or chromium slag with low chromium content and low ferrochrome ratio in the chromium resource is gradually increased. In order to fully utilize chromium resources with low chromium content and low chromium-iron ratio, chromium-containing pig iron with 5-50% of Cr content can be produced by utilizing chromite or chromium slag with low chromium content and low chromium-iron ratio through reactors such as a blast furnace, a resistance furnace or an electric arc furnace, the chromium-containing pig iron can be used as a substitute of national standard-grade ferrochrome (Cr is more than or equal to 55%) to be added into molten steel or cast iron for alloying, has practical significance of cost reduction and efficiency improvement on smelting of chromium-containing steel and chromium-containing cast iron, and has great potential utilization value in the steel industry. Moreover, the high-chromium vanadium extraction tailings of the Panzhihua contain certain valuable elements such as chromium, iron and the like, and can be singly reduced or reduced together with other chromium-containing raw materials to prepare chromium-containing pig iron, so that the method is a good comprehensive utilization way. Moreover, the production of chromium-containing pig iron can well absorb and recycle the chromium-containing dust sludge obtained by the collection of the smoke processor from the ferrochrome or stainless steel smelting process.
According to the Fe-Cr-C ternary phase diagram, different material compositions, smelting processes and heat treatment methods can obtain different phases which have different influences on the alloy performance, although the content of chemical elements in chromium-containing pig iron is mainly concerned in the detection process, the distribution rule and segregation condition of different impurity elements in the alloy phase can be analyzed through microstructure observation, and the composition, cooling-crushing system and the like of the alloy can be adjusted in time to obtain satisfactory results by combining with smelting process data. The current patents and documents mainly focus on the smelting method of chromium-containing pig iron and related researches, including smelting chromium-containing pig iron by using chromium slag, producing chromium-containing pig iron by blast furnace ironmaking and the like, but the metallurgical phase preparation and display methods of the prepared chromium-containing pig iron are rarely reported. Currently, the detection of chromium-containing pig iron is mainly carried out by determining alloy components through chemical analysis, and the analysis is carried out by utilizing phase detection analysis as X-ray diffraction. Therefore, there is an urgent need to develop a metallographic detection method for chromium-containing pig iron.
Disclosure of Invention
The invention solves the technical problem that no effective metallographic phase preparation and display method aiming at chromium-containing pig iron exists at present.
The technical scheme for solving the problems is to provide the chromium-containing pig iron metallographic corrosive agent, and the effective components comprise inorganic acid and volatile organic compounds.
Wherein the inorganic acid is at least one of hydrochloric acid, sulfuric acid and nitric acid, and the volatile organic compound is at least one of absolute ethyl alcohol, acetone and methanol.
Wherein, H is contained in the etchant+The molar concentration is 0.42-1.12 mol/L.
The inorganic acid is preferably nitric acid, and the volatile organic compound is preferably absolute ethyl alcohol.
Specifically, the metallographic corrosive agent contains 3-8% of nitric acid and the balance of absolute ethyl alcohol by volume percentage. Preferably, the concentration of nitric acid is 65% by mass.
Wherein the chromium-containing pig iron is prepared from at least one of chromite, high-chromium type vanadium extraction tailings and chromium-containing dust mud by carbothermic reduction.
The invention also discloses a method for displaying the metallographic structure of chromium-containing pig iron, which comprises the following steps:
a. preparing the metallographic corrosive;
b. preparing chromium-containing pig iron, and then cutting, inlaying and carrying out surface treatment to obtain a bright and scratch-free surface to be corroded;
c. corroding the surface to be corroded by using a metallographic corrosive agent, and then cleaning and air-drying to obtain a metallographic sample to be detected;
d. and carrying out metallographic observation and analysis on the prepared metallographic specimen under a metallographic microscope.
And b, adding the volatile organic matters into a beaker according to the proportion, slowly adding inorganic acid, and uniformly mixing the solution.
Wherein, the step b of surface treatment comprises coarse grinding, fine grinding and polishing.
And c, etching in the step c, wherein the etching mode is etching, the etching temperature is room temperature, and the etching time is 3-10 s.
The invention has the beneficial effects that:
the invention provides a metallographic corrosive agent and a metallographic structure display method for chromium-containing pig iron obtained by carbothermic reduction of chromium-containing raw materials (chromite, high-chromium type vanadium extraction tailings, chromium-containing dust mud and the like), and the metallographic corrosive method can obtain good corrosion effect, the carbide, the sulfide and the like in the metallographic structure are clearer, the phase composition and the proportion can be analyzed by further using image software, the metallographic analysis, the scanning electron microscope and the energy spectrum analysis are carried out after the metallographic corrosion of the chromium-containing pig iron, the method can assist component analysis and X-ray diffraction analysis, is beneficial to accurately and completely evaluating the basic physical and chemical properties of the chromium-containing pig iron, has the advantages of simple operation method and good repeatability, can efficiently display the metallographic structure of the chromium-containing pig iron, has clear boundary of a high chromium phase and a matrix phase, and provides a basis for guiding process parameter control and product segregation detection of links such as smelting, cooling, crushing and the like of the chromium-containing pig iron.
Drawings
FIG. 1 is a metallographic structure of a metallographic specimen of chromium-containing pig iron in example 2 before corrosion;
FIG. 2 is a metallographic structure of a metallographic specimen of chromium-containing pig iron in example 2 after the metallographic specimen had been corroded.
Detailed Description
The invention fully considers that S element and part C element in raw materials of the chromium-containing pig iron smelting process can be enriched into the alloy, the affinity of Cr element with C and S element is strong, part Cr element is still in α -Fe, so the corrosive agent and the display method for the chromium-containing pig iron can accurately evaluate the precipitation state and the precipitation distribution characteristics in the pig iron, and provide guidance for the metallurgical structure detection, the cooling process guidance and the like of the pig iron.
The effective components of the corrosive agent comprise inorganic acid and volatile organic compounds.
Wherein the inorganic acid can be at least one of hydrochloric acid, sulfuric acid and nitric acid, and the volatile organic compound can be at least one of absolute ethyl alcohol, acetone and methanol.
Preferably, the inorganic acid in the corrosive agent is nitric acid, and the volatile organic substance is absolute ethyl alcohol.
In addition, the proper acid type is selected, if the preparation proportion is too high, over corrosion is easy to form, crystal boundaries and crystal grains form a black sheet, clear crystal boundaries and crystal grain sizes cannot be observed, and the contrast between phases cannot be observed, otherwise, if the preparation proportion is too low, the crystal boundaries cannot be corroded, and the microstructure cannot be observed. Therefore, clear metallographic structures are observed, so that different phases have obvious boundary lines and color differences, and the preparation and the use of the corrosive liquid are extremely critical.
H of the invention to corrosive agent+The molar concentration is controlled, H+If the concentration is too low, the corrosion is slow, the waiting time is long, and H+If the concentration is too high, the corrosion is too fast and excessive corrosion is easy to occur, and experiments show that H is controlled to ensure that the corrosion effect is right+The molar concentration is preferably 0.42 to 1.12 mol/L.
Specifically, when nitric acid and absolute ethyl alcohol are used as effective components, the nitric acid accounts for 3-8% by volume, and the balance is the absolute ethyl alcohol.
Preferably, the nitric acid is used in a concentration of 65% by mass.
The metallographic corrosive agent and the display method can be suitable for chromium-containing pig iron produced by various raw materials, and can be prepared by one or a combination of more of chromium-containing raw materials such as chromite, high-chromium type vanadium extraction tailings, chromium-containing dust mud and the like through carbothermic reduction. The high-chromium vanadium extraction tailings are obtained by extracting vanadium elements from high-chromium vanadium slag through vanadium-chromium separation, wherein the content of the Cr elements is 5-30% by mass, the content of the Fe elements is 5-50% by mass, and the chromium-containing dust mud is obtained by collecting chromium iron or stainless steel through a flue gas processor in a smelting process, the content of the Cr elements is 5-20% by mass, and the content of the Fe elements is 80-95% by mass.
The metallographic corrosive agent and the display method of the invention are suitable for chromium-containing pig iron with 5-50% of Cr content.
The sample usually needs to carry out certain surface treatment before the corruption to can be so that wait to examine the surface of examining and examine the surface property that has, and then the metallographical corrosive can be evenly effectively to waiting to examine the surface of examining and examine and corrode, the metallographic structure of the observation alloy sample that obtains is more clear. Preferably, the surface of the sample to be detected is subjected to coarse grinding, fine grinding and polishing through a multi-pass sand paper or polishing machine, and the ground surface of the sample to be detected is bright and flat without obvious scratches.
The corrosion mode of the invention can adopt etching, and the preferable mode is that a small cotton bunch is clamped by tweezers to dip corrosive liquid and lightly wipe the surface to be corroded of the metallographic sample, the brightness degree of the color of the corroded surface is observed, the wiping is stopped when the color of the corroded surface changes from bright to dark, and then the metallographic sample to be detected is obtained by cleaning and air drying.
The invention is further illustrated and described by the following examples.
Example 1
The test object is chromium-containing pig iron obtained by blast furnace carbothermic reduction of chromium-containing raw materials (chromite, high-chromium type vanadium extraction tailings, chromium-containing dedusting ash and the like), a smooth chromium-containing pig iron (the Cr content is 5%) metallographic sample is cut and embedded by wire-electrode cutting of electric sparks, and the surface to be ground is subjected to coarse grinding, fine grinding and polishing to obtain bright and scratch-free surfaceThe surface to be corroded; prepared corrosive agent H+The molar concentration is 0.42mol/L, wherein the volume percentage of the nitric acid is 3 percent, and the balance is absolute ethyl alcohol; clamping a small cotton bunch by using tweezers to dip corrosive liquid, slightly wiping the corrosive liquid on the surface to be corroded of the metallographic sample, wherein the etching time is 10s, repeatedly washing the surface of the sample to be detected by using absolute ethyl alcohol, and drying by using a blower; and carrying out metallographic observation and analysis on the prepared metallographic sample under a metallographic microscope.
Example 2
The test object is chromium-containing pig iron obtained by electrically heating a resistance furnace and carrying out carbothermic reduction on chromium-containing raw materials (chromite, high-chromium vanadium extraction tailings, chromium-containing dedusting ash and the like), a smooth chromium-containing pig iron (with the Cr content of 27.5%) metallographic samples are cut by wire cut electrical discharge machining and embedded, and the surface to be ground is subjected to coarse grinding, fine grinding and polishing to obtain a bright and scratch-free surface to be corroded; prepared corrosive agent H+The molar concentration is 1.12mol/L, wherein the volume percentage of the nitric acid is 8 percent, and the balance is absolute ethyl alcohol; clamping a small cotton bunch by using tweezers to dip corrosive liquid, slightly wiping the corrosive liquid on the surface to be corroded of the metallographic sample, wherein the etching time is 3s, repeatedly washing the surface of the sample to be detected by using absolute ethyl alcohol, and drying by using a blower; and carrying out metallographic observation and analysis on the prepared metallographic sample under a metallographic microscope.
The hexagonal precipitated phases and the dot-shaped cluster-shaped precipitates are evident from fig. 2.
Example 3
The test object is chromium-containing pig iron obtained by electrically heating and carbothermally reducing chromium-containing raw materials (chromite, high-chromium vanadium extraction tailings, chromium-containing dedusting ash and the like) through an electric arc furnace, cutting a smooth metallographic sample (the content of Cr is 50%) of the chromium-containing pig iron by wire cut electrical discharge machining, inlaying the metallographic sample, and performing coarse grinding, fine grinding and polishing on the surface to be ground to obtain a bright and scratch-free surface to be corroded; prepared corrosive agent H+The molar concentration is 1.12mol/L, wherein the volume percentage of the nitric acid is 8 percent, and the balance is absolute ethyl alcohol; clamping a small cotton bunch with tweezers, dipping in corrosive liquid, slightly wiping the surface of the metallographic sample to be corroded for 10s, and repeatedly flushing the surface of the sample to be detected with absolute ethyl alcoholCleaning, and drying by a blower; and carrying out metallographic observation and analysis on the prepared metallographic sample under a metallographic microscope.
In conclusion, the metallographic corrosive agent for the chromium-containing pig iron alloy comprises the effective components of inorganic acid and volatile organic matters, is prepared according to a specific proportion based on nitric acid and absolute ethyl alcohol, can be specially used for displaying the structure of various chromium-containing pig irons, and obtains an excellent metallographic structure display effect. The method for preparing the chromium-containing pig iron alloy sample is simple to operate and good in repeatability, can efficiently display the metallographic structure of the chromium-containing pig iron alloy, and provides a basis for the generation process control and the product inspection of the chromium-containing pig iron alloy.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The chromium-containing pig iron metallographic corrosive agent is characterized in that: the effective components of the corrosive comprise inorganic acid and volatile organic compounds.
2. The corrosive agent for chromium-containing pig iron metallography according to claim 1, wherein: the inorganic acid is at least one of hydrochloric acid, sulfuric acid and nitric acid, and the volatile organic matter is at least one of absolute ethyl alcohol, acetone and methanol.
3. The corrosive agent for chromium-containing pig iron metallography according to claim 1, wherein: in the etchant, H+The molar concentration is 0.42-1.12 mol/L.
4. The corrosive agent for chromium-containing pig iron metallography according to claim 1, wherein: the inorganic acid is nitric acid, and the volatile organic matter is absolute ethyl alcohol.
5. The corrosive agent for chromium-containing pig iron metallographic phases as claimed in claim 4, wherein: the nitric acid accounts for 3-8% by volume percentage, and the balance is absolute ethyl alcohol; the mass percentage concentration of the nitric acid is 65 percent.
6. The corrosive agent for chromium-containing pig iron metallography according to claim 1, wherein: the chromium-containing pig iron is prepared from at least one of chromite, high-chromium type vanadium extraction tailings and chromium-containing dust mud through carbothermic reduction.
7. The method for displaying the metallographic structure of chromium-containing pig iron is characterized by comprising the following steps of:
a. preparing the metallographic corrosive agent as defined in any one of claims 1 to 6;
b. preparing chromium-containing pig iron according to claim 6, and then cutting, inlaying and carrying out surface treatment to obtain a bright and scratch-free surface to be corroded;
c. corroding the surface to be corroded by using a metallographic corrosive agent, and then cleaning and air-drying to obtain a metallographic sample to be detected;
d. and carrying out metallographic observation and analysis on the prepared metallographic specimen under a metallographic microscope.
8. The method for displaying a metallographic structure of chromium-containing pig iron according to claim 7, wherein: the preparation method of the step a comprises the steps of adding the volatile organic matters into a beaker according to the proportion, then slowly adding the inorganic acid, and uniformly mixing the solution.
9. The method for displaying a metallographic structure of chromium-containing pig iron according to claim 7, wherein: the step b of surface treatment comprises coarse grinding, fine grinding and polishing.
10. The method for displaying a metallographic structure of chromium-containing pig iron according to claim 7, wherein: and c, etching the substrate in the etching mode, wherein the etching temperature is room temperature, and the etching time is 3-10 s.
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Cited By (3)
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| CN109884069A (en) * | 2019-03-04 | 2019-06-14 | 涟源康麓生物科技有限公司 | For detecting the solution and its preparation method and application of smooth surface defect |
| CN113822857A (en) * | 2021-08-20 | 2021-12-21 | 南京钢铁股份有限公司 | Method for counting carbide content of high-nickel-chromium cast iron roller, storage medium and system |
| CN114836758A (en) * | 2022-05-11 | 2022-08-02 | 云南大学 | Metallographic corrosive agent suitable for multi-component aluminum alloy and corrosion method thereof |
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