CN109030338A - A kind of method of electro-catalysis chemical attack original austenite grain - Google Patents
A kind of method of electro-catalysis chemical attack original austenite grain Download PDFInfo
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Abstract
The invention discloses a kind of methods of electro-catalysis chemical attack original austenite grain, the following steps are included: preparing specific chemical corrosion liquid, using the electrochemical workstation of three electrode test systems, will sample be corroded as working electrode, platinum electrode is auxiliary electrode, and saturated calomel electrode is reference electrode.Catalyzed corrosion original austenite grain is carried out using the method for linear voltage scanning or constant current scanning.This method has the advantages that easy to operate, corrosion efficiency is high, and no toxic gas generates.
Description
Technical field
The invention belongs to steel material tissue corrosion technology fields, and in particular to a kind of electro-catalysis chemical attack original austenite
The method of crystal grain.
Background technique
Original austenite grain size has important influence to the mechanical performance of steel material, and the method shown to it is equally standby
It is concerned.The corrosion complexity of original austenite crystal prevention is by chemical component, institutional framework, condition of heat treatment of sample etc. itself spy
Matter limitation, and the control of the outside causes such as corrosive agent ingredient, caustic solution used.Existing original austenite corrosion side
Method has oxidizing process, ferrite net method, segregation of Mn method, network cementite method, heating slow cooling method and thermo-chemical erosion method etc..
But these methods are complicated for operation, not no being widely used property, and corrosive effect is unsatisfactory.Such as: thermo-chemical erosion method needs
It wants higher vacuum degree and process is complicated；Using chemical mordant CrO3, NaOH and picric aqueous solution be heated to 120 DEG C of energy
It is enough clearly to corrode original austenite grain out, but toxic gas can be released during being somebody's turn to do.As people are difficult to understand to original in recent years
The extensive research of family name's body chemical attack, it was found that a kind of chemical reagent that certain corrosion inhibiter is added based on saturation picric acid, it can
Corrode the original austenite grain of quenched and tempered steel out well.But if appropriate for the corrosion of other steel grades, it need further to study.
Therefore a kind of method for inventing convenient and efficient, environmental-friendly corrosion original austenite grain with universality is aobvious
It obtains particularly important.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of method of electro-catalysis chemical attack original austenite grain, bases
In picric acid solution, other corrosive agent and corrosion inhibiter of certain content are added, it is brilliant to be catalyzed original austenite by access electric current
The corrosion of grain.This method is suitable for low-carbon to the original austenite grain of high-carbon straight carbon steel and steel alloy and corrodes.
In order to achieve the above objectives, the method for a kind of electro-catalysis chemical attack original austenite grain of the present invention, matches first
Produce the etchant solution for resistant alloy steel or straight carbon steel；Then corroded out using three electrode test system of electrochemical workstation
The original austenite grain of steel alloy or straight carbon steel, wherein working electrode is steel alloy or straight carbon steel, and auxiliary electrode is conductive material
Manufactured electrode, reference electrode are saturated calomel electrode, three electrodes are submerged in etchant solution simultaneously, then using linear electricity
Pressure or constant current scan method make to maintain follow current between working electrode and auxiliary electrode, carry out to steel alloy or straight carbon steel rotten
Erosion, corrodes original austenite grain out.
Further, straight carbon steel linear voltage scan method, steel alloy use constant current scan method.
Further, straight carbon steel uses linear voltage scan method, detailed process are as follows: measurement working electrode and reference electricity
Open-circuit voltage is set as initial voltage by the open-circuit voltage between pole, and sweep speed is+0.01V/s, and scanning range 0.1V is swept
Retouching number is 3-8 times.
Further, steel alloy uses constant current scan method, sweep parameter are as follows: sweep current 15mA-20mA, when scanning
Between be set as 30s-80s.
Further, a kind of method of electro-catalysis chemical attack original austenite grain, comprising the following steps:
Step 1 prepares etchant solution, which is pure water, and bitter taste acid concentration is 0.3wt.%-
0.5wt.%, neopelex concentration is 1wt.%-2wt.%, sodium nitrate concentration 3wt.%-5wt.%, hydrochloric acid body
Fraction is 1vol.%-2vol.%；
Step 2 will prepare metallographic sample according to metallography sample preparation standard to resistant alloy steel or straight carbon steel, then will lead
Line is electrically connected with metallographic sample, then is wrapped up metallographic sample with insulating cement, only reserves a surface to be corroded；
The conducting wire for connecting metallographic sample is connected by step 3 with the working electrode of electrochemical workstation, platinum electrode and auxiliary electricity
Extremely it is connected, saturated calomel electrode is connected with reference electrode, and then metallographic sample and platinum electrode and saturated calomel electrode submerge corrosion
In solution；
Step 4 opens electrochemical workstation, makes working electrode and auxiliary electrode using linear voltage or constant current scan method
Between maintain follow current, until obtain original austenite grain, then etch-stop, and close electrochemical workstation.
Further, auxiliary electrode is platinum electrode, graphite electrode or copper electrode.
Further, in step 1, picric acid, neopelex and content of hydrochloric acid are according to the carbon to corrosion material
Content is adjusted, and when carbon content is lower than 0.7wt.%, picric concentration is 0.4-0.5wt.%, 12 in etchant solution
The concentration of sodium alkyl benzene sulfonate is 2wt.%, and hydrochloric acid volume fraction is 1vol.%；When carbon content is higher than 0.7wt.%, corrosion
Picric concentration is 0.3-0.4wt.% in solution, and the concentration of neopelex is 1wt.%, hydrochloric acid volume fraction
For 2vol.%.
Further, in step 2, conducting wire is connect with metallographic sample soldering.
Further, in step 4, the linear voltage scan method of straight carbon steel use are as follows: sweep speed is+0.01V/s, is swept
Retouching range is 0.05V-0.5V, and when carbon content is less than 0.7wt.%, scanning times are 5-8 times；When carbon content is higher than 0.7wt.%,
Scanning times 3-5 times；Steel alloy uses constant current scan method, when carbon content is less than 0.7wt.%, sweep current 18mA-
20mA, sweep time are set as 50s-80s；When carbon content is higher than 0.7wt.%, sweep current 15-18mA, sweep time is set
It is set to 30s-50s.
Compared with prior art, the present invention at least has technical effect beneficial below, the more traditional caustic solution of this method
Required etchant solution is only needed to configure, is then electrified to corrode, it is only necessary to 30s-400s for etching time, are suitable for different carbon contents
Straight carbon steel and steel alloy, can clearly corrode the original austenite grain of various grain sizes out, compared with Conventional thermal corrode
It does not need vacuum environment, need to heat, no toxic gas generates, therefore has convenient and efficient, and environmental-friendly, universality etc. is excellent
Point.This method is with easy to operate, corrosion efficiency is high, corrosive effect is good and wider applicability.
Further, conducting wire and metallographic sample are electrically connected, are finally wrapped up metallographic sample with insulating cement,
Only reserve a surface to be corroded；Guarantee metallographic sample to be corroded in addition to corrosion surface, other surfaces are both needed to insulate
Processing, metallographic sample electrical connecting wire are that sample is connected with electrochemical workstation for convenience.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention 1 is that X80 pipe line steel passes through this method corrosion original austenite grain figure；
Fig. 2 is that the embodiment of the present invention 2 is that 45 steel of quenched and tempered state passes through this method corrosion original austenite grain figure；
Fig. 3 is that the embodiment of the present invention 3 is that the steel alloy typical die that carbon content is 0.65wt.% corrodes original by this method
Austenite grain figure；
Fig. 4 is that the embodiment of the present invention 4 is that the steel alloy Ultra-fine Grained that carbon content is 0.65wt.% corrodes former Austria by this method
Family name's body crystal grain figure；
Fig. 5 is that the steel alloy typical die that 5 carbon content of the embodiment of the present invention is 0.90wt.% corrodes former Austria by this method
Family name's body crystal grain figure；
Fig. 6 is that the steel alloy Ultra-fine Grained that 6 carbon content of the embodiment of the present invention is 0.90wt.% corrodes former Ovshinsky by this method
Body crystal grain figure；
Fig. 7 is that the embodiment of the present invention 7 is that the steel alloy typical die that carbon content is 1.4wt.% corrodes original by this method
Austenite grain figure.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments, and however, it is not limited to this.
Embodiment 1
A kind of method of electro-catalysis chemical attack original austenite grain, comprising the following steps:
Step 1 pours into 100ml aqueous solution in beaker, then weighs 0.5g picric acid, 2g dodecyl benzene sulfonic acid respectively
Sodium, 3g sodium nitrate pour into beaker, are then poured into beaker with graduated cylinder measurement 1ml hydrochloric acid and are stirred evenly with glass bar, obtained
Etchant solution；
Quenched and tempered state X80 pipe line steel is heated to 900 degree of heat preservation 20min Water Quenchings by step 2.Then by processed material
Metallographic phase sample is made according to metallography sample preparation standard in material, and then conducting wire and metallographic sample are electrically connected, then will with insulating cement
Metallographic sample wraps up, and only reserves a surface to be corroded；
The conducting wire for connecting metallographic sample is connected by step 3 with the working electrode of electrochemical workstation, platinum electrode and auxiliary electricity
Extremely it is connected, saturated calomel electrode is connected with reference electrode, then submerges metallographic sample and platinum electrode and saturated calomel electrode
In etchant solution.
Step 4, using linear voltage scan method, sweep speed 0.01V/s, scanning range 0.1V, scanning times
It is 5 times, obtains original austenite grain.
Embodiment 2
A kind of method of electro-catalysis chemical attack original austenite grain, comprising the following steps:
Step 1 pours into 100ml aqueous solution in beaker, then weighs 0.4g picric acid, 2g dodecyl benzene sulfonic acid respectively
Sodium, 5g sodium nitrate pour into beaker, are then poured into beaker with graduated cylinder measurement 1ml hydrochloric acid and are stirred evenly with glass bar, obtained
Etchant solution；
45 steel of quenched and tempered state is heated to 850 degree and keeps the temperature to 30min Water Quenching by step 2.Then processed material is pressed
Metallographic phase sample is made according to metallography sample preparation standard, then conducting wire and metallographic sample are electrically connected, then with insulating cement by metallographic
Sample wraps up, and only reserves a surface to be corroded；
The conducting wire for connecting metallographic sample is connected by step 3 with the working electrode of electrochemical workstation, platinum electrode and auxiliary electricity
Extremely it is connected, saturated calomel electrode is connected with reference electrode, then submerges metallographic sample and platinum electrode and saturated calomel electrode
In etchant solution.
Step 4, using linear voltage scan method, sweep speed 0.01V/s, scanning range 0.15V, scanning times
It is 6 times, obtains original austenite grain.
Embodiment 3
A kind of method of electro-catalysis chemical attack original austenite grain, comprising the following steps:
Step 1 pours into 100ml aqueous solution in beaker, then weighs 0.4g picric acid, 2g dodecyl benzene sulfonic acid respectively
Sodium, 3g sodium nitrate pour into beaker, are then poured into beaker with graduated cylinder measurement 1ml hydrochloric acid and are stirred evenly with glass bar, obtained
Etchant solution；
The high-carbon steel that the carbon content of warm-rolling state is 0.65wt.% is heated to 850 degree of heat preservation 30min by step 2, immediately water
It quenches processing.To obtain coarse grain material, metallographic phase sample then is made according to metallography sample preparation standard in processed material, then will
Conducting wire is electrically connected with metallographic sample, then is wrapped up metallographic sample with insulating cement, only reserves a table to be corroded
Face；
The conducting wire for connecting metallographic sample is connected by step 3 with the working electrode of electrochemical workstation, platinum electrode and auxiliary electricity
Extremely it is connected, saturated calomel electrode is connected with reference electrode, then submerges metallographic sample and platinum electrode and saturated calomel electrode
In etchant solution.
Step 4, using linear voltage scan method, sweep speed 0.01V/s, scanning range 0.2V, scanning times
It is 4 times, obtains original austenite grain.
Fig. 3 is the original austenite grain figure that the present embodiment corrodes, as can be seen from the figure: original austenite grain size
It clearly displays, crystal boundary is clear and legible.
Embodiment 4
A kind of method of electro-catalysis chemical attack original austenite grain, comprising the following steps:
Step 1 pours into 100ml aqueous solution in beaker, then weighs 0.4g picric acid, 1.5g detergent alkylate sulphur respectively
Sour sodium, 4g sodium nitrate pour into beaker, are then poured into beaker with graduated cylinder measurement 1.5ml hydrochloric acid and are stirred evenly with glass bar,
Obtain etchant solution；
The high-carbon steel that the carbon content of warm-rolling state is 0.65wt.% is heated to 850 degree of heat preservation 5min, immediately water quenching by step 2
Processing.To obtain grained material, metallographic phase sample then is made according to metallography sample preparation standard in processed material, then will be led
Line is electrically connected with metallographic sample, then is wrapped up metallographic sample with insulating cement, only reserves a surface to be corroded；
The conducting wire for connecting metallographic sample is connected by step 3 with the working electrode of electrochemical workstation, platinum electrode and auxiliary electricity
Extremely it is connected, saturated calomel electrode is connected with reference electrode, then submerges metallographic sample and platinum electrode and saturated calomel electrode
In etchant solution.
Step 4, using linear voltage scan method, sweep speed 0.01V/s, scanning range 0.15V, scanning times
It is 4 times, obtains original austenite grain.
Fig. 4 is the original austenite grain figure that the present embodiment corrodes, as can be seen from the figure: original austenite grain size
It clearly displays, crystal boundary is clear and legible.
Embodiment 5
A kind of method of electro-catalysis chemical attack original austenite grain, comprising the following steps:
Step 1 pours into 100ml aqueous solution in beaker, then weighs 0.3g picric acid, 1.5g detergent alkylate sulphur respectively
Sour sodium, 4g sodium nitrate pour into beaker, are then poured into beaker with graduated cylinder measurement 2ml hydrochloric acid and are stirred evenly with glass bar, obtained
To etchant solution；
The high-carbon alloy steel that the carbon content of warm-rolling state is 0.9wt.% is heated to 850 degree of heat preservation 30min by step 2, immediately
Water Quenching.To obtain coarse grain material, metallographic phase sample then is made according to metallography sample preparation standard in processed material, then
Conducting wire and metallographic sample are electrically connected, then wrapped up metallographic sample with insulating cement, only reserve one it is to be corroded
Surface；
The conducting wire for connecting metallographic sample is connected by step 3 with the working electrode of electrochemical workstation, platinum electrode and auxiliary electricity
Extremely it is connected, saturated calomel electrode is connected with reference electrode, then submerges metallographic sample and platinum electrode and saturated calomel electrode
In etchant solution.
Step 4, using constant current method, sweep current 18mA, sweep time 10s, scanning times are 5 times, obtain original
Austenite grain.
Fig. 5 is the original austenite grain figure that the present embodiment corrodes, as can be seen from the figure: original austenite grain size
It clearly displays, crystal boundary is clear and legible.
Embodiment 6
A kind of method of electro-catalysis chemical attack original austenite grain, comprising the following steps:
Step 1 pours into 100ml aqueous solution in beaker, then weighs 0.3g picric acid, 1g dodecyl benzene sulfonic acid respectively
Sodium, 4g sodium nitrate pour into beaker, are then poured into beaker with graduated cylinder measurement 2ml hydrochloric acid and are stirred evenly with glass bar, obtained
Etchant solution；
The high-carbon alloy steel that the carbon content of warm-rolling state is 0.9wt.% is heated to 850 degree of heat preservation 5min by step 2, immediately
Water Quenching.To obtain grained material, metallographic phase sample then is made according to metallography sample preparation standard in processed material, then
Conducting wire and metallographic sample are electrically connected, then wrapped up metallographic sample with insulating cement, only reserve one it is to be corroded
Surface；
The conducting wire for connecting metallographic sample is connected by step 3 with the working electrode of electrochemical workstation, platinum electrode and auxiliary electricity
Extremely it is connected, saturated calomel electrode is connected with reference electrode, then submerges metallographic sample and platinum electrode and saturated calomel electrode
In etchant solution.
Step 4, using constant current method, sweep current 15mA, sweep time 10s, scanning times are 6 times, obtain original
Austenite grain.
Fig. 6 is the original austenite grain figure that the present embodiment corrodes, as can be seen from the figure: original austenite grain size
It clearly displays, crystal boundary is clear and legible.
Embodiment 7
A kind of method of electro-catalysis chemical attack original austenite grain, comprising the following steps:
Step 1 pours into 100ml aqueous solution in beaker, then weighs 0.3g picric acid, 1g dodecyl benzene sulfonic acid respectively
Sodium, 3g sodium nitrate pour into beaker, are then poured into beaker with graduated cylinder measurement 2ml hydrochloric acid and are stirred evenly with glass bar, obtained
Etchant solution；
The high-carbon alloy steel that the carbon content of warm-rolling state is 1.4wt.% is heated to 850 degree of heat preservation 20min by step 2, immediately
Water Quenching.Then metallographic phase sample is made according to metallography sample preparation standard in processed material, then by conducting wire and metallographic sample
It is electrically connected, then is wrapped up metallographic sample with insulating cement, only reserve a surface to be corroded；
The conducting wire for connecting metallographic sample is connected by step 3 with the working electrode of electrochemical workstation, platinum electrode and auxiliary electricity
Extremely it is connected, saturated calomel electrode is connected with reference electrode, then submerges metallographic sample and platinum electrode and saturated calomel electrode
In etchant solution.
Step 4, using constant current method, sweep current 10mA, sweep time 10s, scanning times are 4 times, obtain original
Austenite grain.
Fig. 7 is the original austenite grain figure that the present embodiment corrodes, as can be seen from the figure: original austenite grain size
It clearly displays, crystal boundary is clear and legible.
Claims (9)
1. a kind of method of electro-catalysis chemical attack original austenite grain, which is characterized in that made first for resistant alloy
The etchant solution of steel or straight carbon steel；Then steel alloy out or straight carbon steel are corroded using three electrode test system of electrochemical workstation
Original austenite grain, wherein working electrode is steel alloy or straight carbon steel, and auxiliary electrode is electrode made of conductive material, reference electricity
Three electrodes are submerged in etchant solution simultaneously, then use linear voltage or constant current scan method by extremely saturated calomel electrode
Make to maintain follow current between working electrode and auxiliary electrode, steel alloy or straight carbon steel are corroded, corrodes original austenite out
Crystal grain.
2. a kind of method of electro-catalysis chemical attack original austenite grain according to claim 2, which is characterized in that general carbon
Steel linear voltage scan method, steel alloy use constant current scan method.
3. a kind of method of electro-catalysis chemical attack original austenite grain according to claim 2, which is characterized in that general carbon
Steel uses linear voltage scan method, detailed process are as follows: the open-circuit voltage between measurement working electrode and reference electrode will be opened
Road voltage is set as initial voltage, and sweep speed is+0.01V/s, and scanning range 0.1V, scanning times are 3-8 times.
4. a kind of method of electro-catalysis chemical attack original austenite grain according to claim 1, steel alloy uses constant current
Scan method, sweep parameter are as follows: sweep current 15mA-20mA, sweep time are set as 30s-80s.
5. a kind of method of electro-catalysis chemical attack original austenite grain according to claim 1, which is characterized in that including
Following steps:
Step 1 prepares etchant solution, which is pure water, and bitter taste acid concentration is 0.3wt.%-0.5wt.%, ten
Dialkyl benzene sulfonic acids na concn is 1wt.%-2wt.%, sodium nitrate concentration 3wt.%-5wt.%, and hydrochloric acid volume fraction is
1vol.%-2vol.%；
Step 2 will prepare metallographic sample according to metallography sample preparation standard to resistant alloy steel or straight carbon steel, then by conducting wire with
Metallographic sample is electrically connected, then is wrapped up metallographic sample with insulating cement, only reserves a surface to be corroded；
The conducting wire for connecting metallographic sample is connected by step 3 with the working electrode of electrochemical workstation, platinum electrode and auxiliary electrode phase
Even, saturated calomel electrode is connected with reference electrode, and then metallographic sample and platinum electrode and saturated calomel electrode submerge etchant solution
In；
Step 4 opens electrochemical workstation, is made between working electrode and auxiliary electrode using linear voltage or constant current scan method
Follow current is maintained, until obtain original austenite grain, then etch-stop, and close electrochemical workstation.
6. a kind of method of electro-catalysis chemical attack original austenite grain according to claim 5, auxiliary electrode is platinum electricity
Pole, graphite electrode or copper electrode.
7. a kind of method of electro-catalysis chemical attack original austenite grain according to claim 5, which is characterized in that step
In 1, picric acid, neopelex and content of hydrochloric acid are adjusted according to the carbon content to corrosion material, work as carbon content
When lower than 0.7wt.%, picric concentration is 0.4-0.5wt.% in etchant solution, the concentration of neopelex is
2wt.%, hydrochloric acid volume fraction are 1vol.%；When carbon content is higher than 0.7wt.%, picric concentration is in etchant solution
0.3-0.4wt.%, the concentration of neopelex are 1wt.%, and hydrochloric acid volume fraction is 2vol.%.
8. a kind of method of electro-catalysis chemical attack original austenite grain according to claim 5, which is characterized in that step
In 2, conducting wire is connect with metallographic sample soldering.
9. a kind of method of electro-catalysis chemical attack original austenite grain according to claim 5, which is characterized in that step
In 4, the linear voltage scan method of straight carbon steel use are as follows: sweep speed is+0.01V/s, scanning range 0.05V-0.5V, carbon
When content is less than 0.7wt.%, scanning times are 5-8 times；When carbon content is higher than 0.7wt.%, scanning times 3-5 times；Steel alloy
Using constant current scan method, when carbon content is less than 0.7wt.%, sweep current 18mA-20mA, sweep time is set as 50s-
80s；When carbon content is higher than 0.7wt.%, sweep current 15mA-18mA, sweep time is set as 30s-50s.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110344060A (en) * | 2019-07-10 | 2019-10-18 | 马鞍山钢铁股份有限公司 | It is a kind of for showing the corrosive agent and its preparation and application of zinc-iron alloy hot-dip galvanized steel sheet coating structure |
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