CN101556225B - Method adopting neutral salt electrolyte to electrolytically extract tiny impurities from steel - Google Patents
Method adopting neutral salt electrolyte to electrolytically extract tiny impurities from steel Download PDFInfo
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- CN101556225B CN101556225B CN2009100847411A CN200910084741A CN101556225B CN 101556225 B CN101556225 B CN 101556225B CN 2009100847411 A CN2009100847411 A CN 2009100847411A CN 200910084741 A CN200910084741 A CN 200910084741A CN 101556225 B CN101556225 B CN 101556225B
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Abstract
The invention relates to a method adopting neutral salt electrolyte to electrolytically extract tiny impurities from steel and belongs to the research approach field of physics of metals. The method comprises the detailed steps of: mixing sodium citrate, sodium chloride, ferrous sulfate and ammonium chloride according to a certain proportion so as to be taken as a neutral electrolyte; adopting ammonium chloride solution to react with non-solute in water bath after electrolysis; repeatedly dissolving precipitate till the precipitation mass is stable; and obtaining the final product, namely, therequired impurities. By adopting the neutral salt electrolyte for electrolysis, the method can obtain the micron-level and nanometer-level tiny impurities which have complete appearance and distinct components by observation with a scanning electron microscope.
Description
Technical field
The present invention relates to a kind of method that adopts fine foreign matter in the neutral salt electrolytic solution electroextraction steel, belong to metal physics research method field.
Background technology
Fine foreign matter is significant for the multiple important mechanical property that improves ferrous materials in the research steel, in order better to study the pattern and the composition characteristics of its snotter, thereby analyze its effect, it need be extracted from the steel sample intactly for steel sample matrix.Traditional method often is confined to use acidity or alkaline electrolyte, and mainly there is shortcoming in it: 1, the sample quality of electrolysis is big, electrolysis time is long, and cost is higher; 2, the snotter that is soluble in acidity or alkaline environment in the steel then disappears in electrolytic process; 3, the snotter size that obtains is bigger, can't satisfy the demand of present research work.Solved above difficulty though the technology of some electrolysis snotteres that newly advance also has, electrolytic environments is had relatively high expectations, and cost is generally higher.
Summary of the invention
The purpose of this invention is to provide a kind of method that adopts fine foreign matter in the neutral salt electrolytic solution electroextraction steel,, effect low at cost significantly, obtain under the prerequisite of fine foreign matter, for the formation mechanism of studying steel inclusion reaches the various Effect on Performance of steel are laid the foundation, solve various relevant therewith production practical problemss.
The method of fine foreign matter in the neutral salt solution electroextraction steel involved in the present invention is characterized in that having following step:
1, preparation has the neutral salt electrolytic solution of special formulation, and neutral electrolyte forms by the chemical raw material of following weight ratio is composite:
Sodium citrate: 0.05～0.5%
Sodium chloride: 0.1～5%
Ferrous sulphate: 1～5%
Ammonium chloride: 1～5%
All the other are deionized water;
2, with graphite electrode as electrolysis cathode, be anode with the steel sample that contains snotter.The steel sample is made the thin slice of the thick 1～2mm of being, and length and width are exceeded can put into electrolytic tank, with the watery hydrochloric acid clean surface of 3-5%, carries out ultrasonic cleaning with alcohol again before electrolysis.Adjusting electrolytic potential during the beginning electrolysis is 3～10V, and cathode-current density is 0.02～0.1A/cm
2Electrolysis is dissolved fully until the anode sample.
3, use hydro-extractor centrifugal electrolytic solution after, will precipitate and add in saturated ammonium salt (as the ammonium nitrate) solution, and in water-bath, react.Adopt moistening litmus paper detection reaction whether to emit ammonia.
4, repeating step 3, emit until no longer including ammonia, and it is blue that promptly moistening litmus paper no longer becomes.Deposit is added deionized water, and centrifugal repeatedly on hydro-extractor, clarification, at last the fine foreign matter precipitation that obtains is dried, deposited, for observing, characterizing.
Mainly include fine oxide, nitride, carbonide, sulphide inculsion thing in the snotter of the steel that relates among the present invention.
In the neutral electrolyte of the present invention, the effect of ammonium chloride is to produce in the environment of heat in electrolysis, the celadon ferric hydroxide that the expectation electrolysis obtains, ferrous hydroxide mixed precipitation and ammonium chloride reaction dissolving.Look varying in size of steel sample, if the steel sample is less, then in electrolytic process, unnecessary ferric hydroxide, ferrous hydroxide mixed precipitation are chlorinated ammonium salt solution fully and dissolve; If the steel sample is bigger, then ammonium chloride can't dissolve all precipitations fully in the process of electrolysis, and the deposit that obtains after the electrolysis needs to adopt saturated ammonium salt (as ammonium nitrate) solution water-bath to remove.
Mechanism of the present invention is: the matrix of steel sample has different electrode decomposition electric potentials with snotter in the steel sample, and electrolytic potential is controlled between the two, and steel matrix is constantly by electrolysis under the effect of electric current, and snotter then is retained in the electrolytic solution.
Principal feature of the present invention is: 1, adopt neutral salt electrolytic solution, can not produce the effect of corrosion and damage to the fine foreign matter that is soluble in acid or alkali; 2, adopt ammonium salt that electrolysis residue precipitation is dissolved, snotter is separated fully with electrolysis hydrogen oxidation iron, ferrous hydroxide mixed precipitation, reaction product is water-soluble, remains the neutral environment of solution, has guaranteed that the composition of snotter and pattern are all excellent; 3, adopt conventional electrochemical electrolysis device, simple, cost is lower, and is simple and convenient under laboratory environment.
Description of drawings
Fig. 1 is traditional conventional electrolysis device synoptic diagram of the present invention.
The Fe that Fig. 2 obtains for electrolysis X70 steel
3The C snotter.
The AlN snotter that Fig. 3 obtains for the electrolysis semi-technological electrical steel.
MoC snotter in the X80 steel that Fig. 4 obtains for electrolysis.
Embodiment
Embodiment one: at first configure electrolytic solution, it is as follows to fill a prescription: (wt%)
Sodium citrate: sodium chloride 0.2%: ferrous sulphate 1%: ammonium chloride 3%: 2%,
Deionized water: 93.8%
Above-mentioned electrolytic solution is put into electrolytic tank, as electrolysis cathode, is anode with the pipe line steel X70 steel sample that contains snotter with graphite electrode.Adjusting electrolytic potential during the beginning electrolysis is 3～10V, and cathode-current density is 0.02～0.1A/cm
2Electrolysis is dissolved fully until the anode sample.
After the solution that electrolysis is obtained uses hydro-extractor centrifugal, will precipitate and add in saturated ammonium salt (as the ammonium nitrate) solution, and reaction is dissolved in water-bath, repeated centrifugation, dissolving are emitted until no longer including ammonia.Deposit is added deionized water, and centrifugal repeatedly on hydro-extractor, clarification, at last the fine foreign matter precipitation that obtains is dried, deposited.And use scanning electron microscopic observation, analysis composition, find to obtain tiny size at nano level Fe
3C is mingled with, and three-dimensional appearance is good.As shown in Figure 2.
Embodiment two: at first configure electrolytic solution, it is as follows to fill a prescription: (wt%)
Sodium citrate: sodium chloride 0.1%: ferrous sulphate 4%: ammonium chloride 1%: 2%,
Deionized water; 92.9%
In the present embodiment, above-mentioned electrolytic solution being put into electrolytic tank, as electrolysis cathode, is anode with the semi-technological electrical steel steel sample that contains snotter with graphite electrode.Adjusting electrolytic potential during the beginning electrolysis is 3～10V, and cathode-current density is 0.02～0.1A/cm
2Electrolysis is dissolved fully until the anode sample.
After the solution that electrolysis is obtained uses hydro-extractor centrifugal, will precipitate and add in saturated ammonium salt (as the ammonium nitrate) solution, and reaction is dissolved in water-bath, repeated centrifugation, dissolving are emitted until no longer including ammonia.Deposit is added deionized water, and centrifugal repeatedly on hydro-extractor, clarification, at last the fine foreign matter precipitation that obtains is dried, deposited, for observing, characterizing.
Also analyze composition through scanning electron microscopic observation, find to obtain tiny size at several microns AlN snotter, three-dimensional appearance is good.As shown in Figure 3.
Embodiment three: at first configure electrolytic solution, it is as follows to fill a prescription: (wt%)
Sodium citrate: sodium chloride 0.4%: ferrous sulphate 1%: ammonium chloride 4%: 5%,
Deionized water: 89.6%;
In the present embodiment, above-mentioned electrolytic solution being put into electrolytic tank, as electrolysis cathode, is anode with the pipe line steel X80 steel sample that contains snotter with graphite electrode.Adjusting electrolytic potential during the beginning electrolysis is 3～10V, and cathode-current density is 0.02～0.1A/cm
2Electrolysis is dissolved fully until the anode sample.
After the solution that electrolysis is obtained uses hydro-extractor centrifugal, will precipitate and add in saturated ammonium salt (as the ammonium nitrate) solution, and reaction is dissolved in water-bath, repeated centrifugation, dissolving are emitted until no longer including ammonia.Deposit is added deionized water, and centrifugal repeatedly on hydro-extractor, clarification, at last the fine foreign matter precipitation that obtains is dried, deposited, for observing, characterizing.
Also analyze composition through scanning electron microscopic observation, find to obtain tiny size at several microns MoC snotter, three-dimensional appearance is good.As shown in Figure 4.
Claims (3)
1. method that adopts fine foreign matter in the neutral salt electrolytic solution electroextraction steel is characterized in that having following step:
A. preparation has the neutral salt electrolytic solution of special formulation, and neutral salt electrolytic solution forms by the chemical raw material of following weight ratio is composite:
Sodium citrate: 0.05～0.5%
Sodium chloride: 0.1～5%
Ferrous sulphate: 1～5%
Ammonium chloride: 1～5%
All the other are deionized water;
B. with graphite electrode as electrolysis cathode, be anode with the steel sample that contains snotter; The steel sample is made the thin slice of the thick 1～2mm of being, and length and width are exceeded can put into electrolytic tank, with the watery hydrochloric acid clean surface of 3-5%, carries out ultrasonic cleaning with alcohol again before electrolysis; Adjusting electrolytic potential during the beginning electrolysis is 3～10V, and cathode-current density is 0.02～0.1A/cm
2Electrolysis is dissolved fully until the anode sample;
C. after using hydro-extractor centrifugal electrolytic solution, will precipitate in the adding ammonium nitrate solution, and in water-bath, react; Adopt moistening litmus paper detection reaction whether to emit ammonia;
D. repeat the c step, emit until no longer including ammonia, it is blue that promptly moistening litmus paper no longer becomes; Deposit is added deionized water, and centrifugal repeatedly on hydro-extractor, clarification, at last the fine foreign matter precipitation that obtains is dried, deposited, for observing, characterizing.
2. according to the described a kind of method that adopts fine foreign matter in the neutral salt electrolytic solution electroextraction steel of claim 1, it is characterized in that: include fine oxide, nitride, carbonide, sulphide inculsion in the snotter of described steel.
3. according to the described a kind of method that adopts fine foreign matter in the neutral salt electrolytic solution electroextraction steel of claim 1, it is characterized in that: the deposit that obtains after the electrolysis, adopt the ammonium nitrate solution water-bath to remove electrolysis remaining celadon ferric hydroxide, ferrous hydroxide mixed precipitation.
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| CN103884550B (en) * | 2014-02-27 | 2017-03-29 | 江苏省沙钢钢铁研究院有限公司 | A kind of method that oxide in steel is analyzed by electroextraction |
| CN104807684A (en) * | 2015-05-12 | 2015-07-29 | 首钢总公司 | Method for extracting and analyzing high-carbon steel inclusions |
| CN108048914B (en) * | 2017-12-08 | 2023-11-07 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Method for electrolytic purification of large diamond monocrystal synthetic block |
| CN108827991B (en) * | 2018-07-27 | 2021-04-30 | 中南大学 | Reinforced phase characterization method of ferromagnetic alloy block and/or film |
| CN110579501A (en) * | 2019-09-27 | 2019-12-17 | 苏州大学 | Method for extracting three-dimensional shape of aluminum alloy phase |
| CN111596094B (en) * | 2020-05-12 | 2023-04-18 | 上海大学 | Three-dimensional etching device and method for nonmetallic inclusions in steel |
| CN113447509B (en) * | 2021-07-30 | 2022-09-16 | 钢铁研究总院 | Sample preparation method of scanning electron microscope sample for inclusions in rare earth weathering steel |
| CN114166603B (en) * | 2021-12-08 | 2024-05-03 | 安徽工业大学 | Method for extracting trace second phase in C-HRA-5 austenitic heat-resistant steel |
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| JP2004301605A (en) * | 2003-03-31 | 2004-10-28 | Jfe Steel Kk | Electrolyte for extraction analysis of deposit and/or inclusion in steel, and electrolytic extraction method of deposit and/or inclusion in steel using the same |
| JP2004317203A (en) * | 2003-04-14 | 2004-11-11 | Nippon Steel Corp | Method of evaluating inclusion and precipitate in metal and evaluation tool therefor |
| CN101074907A (en) * | 2007-03-29 | 2007-11-21 | 上海大学 | Method for extracting steel superfine varia by electrolysis method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2004301605A (en) * | 2003-03-31 | 2004-10-28 | Jfe Steel Kk | Electrolyte for extraction analysis of deposit and/or inclusion in steel, and electrolytic extraction method of deposit and/or inclusion in steel using the same |
| JP2004317203A (en) * | 2003-04-14 | 2004-11-11 | Nippon Steel Corp | Method of evaluating inclusion and precipitate in metal and evaluation tool therefor |
| CN101074907A (en) * | 2007-03-29 | 2007-11-21 | 上海大学 | Method for extracting steel superfine varia by electrolysis method |
Non-Patent Citations (2)
| Title |
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| 张毅等.钢中非金属夹杂物的分析研究进展.《宝钢技术》.2008,(第02期), * |
| 鞍钢钢铁研究所等.钢中气体、夹杂物及析出相分析.《实用冶金分析——方法与基础》.辽宁科学技术出版社,1990, * |
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