CN104266890B - A kind of method of room temperature Rapid Extraction heat-resisting austenitic stainless steel miscible precipitate - Google Patents
A kind of method of room temperature Rapid Extraction heat-resisting austenitic stainless steel miscible precipitate Download PDFInfo
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- CN104266890B CN104266890B CN201410550934.2A CN201410550934A CN104266890B CN 104266890 B CN104266890 B CN 104266890B CN 201410550934 A CN201410550934 A CN 201410550934A CN 104266890 B CN104266890 B CN 104266890B
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Abstract
The method that the present invention relates to a kind of room temperature Rapid Extraction heat-resisting austenitic stainless steel miscible precipitate, it is for heat-resisting austenitic stainless steel precipitate extraction difficulty, slow-footed situation, use at normal temperatures, in electrolysis of hydrochloric acid liquid, electrolytic extraction is quickly carried out under magnetic field agitation effect, this extracting process technique is advanced, data are the fullest and the most accurate, at room temperature 25 DEG C, quickly carry out under the action of a magnetic field, rate of extraction can improve 90% than prior art, extracting substance is CrNbN, Cr23C6, NbN powder body, the method of the Rapid Extraction heat-resisting austenitic stainless steel miscible precipitate being very good.
Description
Technical field
The method that the present invention relates to a kind of room temperature Rapid Extraction heat-resisting austenitic stainless steel miscible precipitate, belongs to resistance to
Hot rustless steel trace precipitate extracting method and the technical field of application.
Background technology
The heat-resisting austenitic stainless steel of HR3C is to add Nb element and N element on the basis of TP310 is stainless
Heat-resisting austenitic stainless steel；In the heat-resisting austenitic stainless steel of HR3C, the content of Cr is higher, and therefore it has
Good high-temperature oxidation resistance and anti-steam corrosion performance, be often applied to high temperature resistant device；This heat-resisting Austria
Family name's body rustless steel is mainly characterized by the interpolation by multiple alloying element so that it is permissible under high-temperature and high-pressure conditions
Separate out CrNbN, Cr23C6, NbN composite carbon, nitrogen compound, thus obtain high creep strength, with
Meet the performance requirement of creep rupture strength.
Owing to the heat-resisting austenitic stainless steel of HR3C contains many kinds of Nb, Mo, W, Cu, Re, Ni, N conjunction
Alloying element, therefore the kind of HR3C in use precipitated phase, quantity, position complexity, different Ageing Treatment
After can separate out that chemical composition is different, structure different and is distributed different CrNbN, Cr23C6, NbN composite carbon,
Nitrogen compound.
At present, analyzing of heat-resisting austenitic stainless steel precipitate lacks qualitative and quantitative analysis means, thus
Cause the formation of precipitate in heat-resisting austenitic stainless steel, developing is short in understanding, the therefore extraction of precipitated phase
Just become the important subject of heat-resisting austenitic stainless steel.
Summary of the invention
Goal of the invention
It is an object of the invention to the situation for background technology, austenitic stainless steel heat-resisting to HR3C is electrolysed
Extraction, under the action of a magnetic field, the miscible precipitate of the heat-resisting austenitic stainless steel of rapid extraction, reach analysis
Go out quantitative analysis and the precise Identification of thing, to analyze the kind of precipitated phase during heat-resisting austenitic stainless steel uses
Class, composition, the heat-resisting austenitic stainless steel for design with high creep strength provides guidance.
Technical scheme
The chemical substance material that the present invention uses is: heat-resisting austenite stainless steel disc, copper sheet, hydrochloric acid, Pyroxylin
Glue, dehydrated alcohol, deionized water, sand paper, it is as follows that a combination thereof prepares consumption: with milliliter, millimeter for metering
Unit
Heat-resisting austenite stainless steel disc: Fe53Cr25Ni20Mn1.44Nb0.3N0.2C0.06, 3mm × 30mm × 50mm
Copper sheet: Cu, 0.5mm × 80mm × 100mm
Hydrochloric acid: HCl, concentration 37%, 300mL ± 10mL
Collodion: C12H17(ONO2)3O7, concentration 5%, 30mL ± 1mL
Dehydrated alcohol: CH3CH2OH, 300mL ± 10mL
Deionized water: H2O, 3000mL ± 10mL
Sand paper: SiC, 3000 mesh, 300mm × 0.5mm × 200mm
Extracting process is as follows:
(1), preparation electrolysis of hydrochloric acid liquid
Measure hydrochloric acid 240mL ± 10mL, deionized water 760mL ± 10mL, add in beaker, stir 5min,
Become the aqueous hydrochloric acid solution of 3mol/L, i.e. electrolysis of hydrochloric acid liquid；
(2), pretreatment heat-resisting austenite stainless steel disc
Heat-resisting austenite stainless steel disc is placed on steel flat board, with each portion of sand papering periphery；
By the heat-resisting austenite stainless steel disc washes of absolute alcohol after polishing, then dry；
(3), pretreatment copper sheet
Copper sheet is placed on steel flat board, with each portion of sand papering periphery；
By the copper sheet after polishing, with washes of absolute alcohol, then dry；
(4), bag-shaped semipermeable membrane is prepared
1., collodion 30mL ± 1mL is placed in beaker, uniform rotation beaker, makes collodion uniformly adhere to
On beaker inwall, collodion is at beaker condensed on inner walls, until freezing film；
2., along beaker mouth mural margin strip off gap, admitting air into, air promotes thin film to divide with beaker inwall
From, instill deionized water, make thin film separately, become transparent membrane, the most bag-shaped semipermeable membrane；
(5), heat-resisting austenitic stainless steel miscible precipitate is extracted
Extract heat-resisting austenitic stainless steel miscible precipitate to carry out in pottery electrolysis bath, be at hydrochloric acid electricity
Solve in liquid, complete under the action of a magnetic field；
1., magneton agitator is placed in pottery electrolysis bath inner bottom part；
2., the electrolysis of hydrochloric acid liquid of configuration is added in pottery electrolysis bath；
3., heat-resisting austenite stainless steel disc is vertically arranged in right part in pottery electrolysis bath, for anode, and fixes；
Copper sheet is vertically arranged in left part in pottery electrolysis bath, for negative electrode, and fixes；
Heat-resisting austenitic stainless steel sheet is loaded in the U-shaped bag-shaped semipermeable membrane being disposed vertically, and by bag-shaped semi-transparent
Film is fixed；
Electrolysis of hydrochloric acid liquid to flood heat-resisting austenite stainless steel disc, copper sheet, bag-shaped semipermeable membrane；
4., opening anodization controller, cathodic control device, magneton agitator, electrolysis of hydrochloric acid liquid starts electrolysis；
Anode current 2A, cathode current 2A；
Magneton agitator revolution 60r/min；
Electrolysis temperature 25 DEG C；
Electrolysis time 600min；
Heat-resisting austenite stainless steel disc solid-state precipitate is attached on bag-shaped semipermeable membrane；
5., closing anodization controller, cathodic control device, electrolyte stands 60min in pottery electrolysis bath；
Heat-resisting austenite stainless steel disc separates out solid-state CrNbN, Cr in electrolytic process23C6, NbN, and adhere to
On semipermeable membrane；
6., heat-resisting austenite stainless steel disc will occur chemical reaction during electrolytic extraction miscible precipitate,
Reaction equation is as follows:
In formula: H2: hydrogen；
Cr23C6: six carbonization 23 chromium；
NbN: niobium nitride；
CrNbN: chromium niobium nitrogen；
NiCl2: Nickel dichloride.；
CrCl3: Chlorizate chromium；
FeCl2: ferrous chloride；
MnCl2: manganese chloride；
Wherein: chromium niobium nitrogen, niobium nitride, six carbonization 23 chromium are solid-state precipitate；
Nickel dichloride., Chlorizate chromium, manganese chloride, ferrous chloride are dissolving with hydrochloric acid thing；
(6), precipitate is extracted
1., the bag-shaped semipermeable membrane of attachment solid-state precipitate is placed in beaker, adds deionized water 200mL,
Agitator treating 2min；
Deionized water wash repeats three times, then precipitates, and retains precipitate；
2., precipitate is added in another beaker, add hydrochloric acid 50mL, mix and blend, dissolve in cleaning mixture
Ferrum simple substance, then precipitate, retain precipitate；
3., precipitate is added in another beaker, add deionized water 200mL, agitator treating 2min；
Deionized water wash repeats three times, washes out chloride ion, then precipitates, and retains precipitate；
4., sucking filtration, put the precipitate in the buchner funnel of bottle,suction, carry out with three layers of middling speed qualitative filter paper
Sucking filtration, remaining product filter cake, filtrate is evacuated in filter flask, discards；
(7), vacuum drying
Product cake is placed in quartz container, is subsequently placed in vacuum drying oven and is dried, baking temperature 50 DEG C,
Vacuum 10Pa, drying time 30min；
Dried material is heat-resisting austenitic stainless steel miscible precipitate powder；
(8), detect, analyze, characterize
The color and luster of heat-resisting austenitic stainless steel miscible precipitate, pattern, the chemical substance of extraction are detected,
Analyze, characterize；
Powder material phase analysis is carried out with X-ray diffractometer；
Conclusion: heat-resisting austenitic stainless steel miscible precipitate is CrNbN, Cr23C6, NbN, for black powder,
Particle diameters≤300nm.
Beneficial effect
The present invention has obvious advance compared with background technology, is to be combined for heat-resisting austenitic stainless steel
Precipitate extracts situation difficult, slow-footed, use at normal temperatures, in electrolysis of hydrochloric acid liquid, magnetic field agitation effect
The most quickly carrying out electrolytic extraction, this extracting process technique is advanced, and data are the fullest and the most accurate, at room temperature 25 DEG C,
Quickly carry out under the acceleration of magnetic field, rate of extraction than prior art improve 90%, extracting substance be CrNbN,
Cr23C6, NbN powder body, the method for the Rapid Extraction heat-resisting austenitic stainless steel miscible precipitate being very good.
Accompanying drawing explanation
Fig. 1, heat-resisting austenitic stainless steel electrolytic extraction miscible precipitate state diagram；
Fig. 2, heat-resisting austenitic stainless steel miscible precipitate shape appearance figure；
Fig. 3, heat-resisting austenitic stainless steel miscible precipitate diffracted intensity collection of illustrative plates；
Shown in figure, list of numerals is as follows:
1, pottery electrolysis bath, 2, electrolysis control station, 3, groove lid, 4, magneton agitator, 5, negative electrode copper sheet,
6, anode heat-resisting austenite stainless steel disc, 7, negative electrode fixed mount, 8, anode fixed mount, 9, first is semi-transparent thin
Film fixed mount, the 10, second semipermeable membrane fixed mount, 11, bag-shaped semipermeable membrane, 12, electrolysis of hydrochloric acid liquid, 13,
Display screen, 14, display lamp, 15, electrolytic switch, 16, anodization controller, 17, cathodic control device, 18,
Magnetic agitation controller.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described:
Shown in Fig. 1, for heat-resisting austenitic stainless steel electrolytic extraction miscible precipitate state diagram, position, each portion will be just
Really, according to quantity proportioning, sequentially operate.
The value of the chemical substance that extraction uses is to determine by the scope pre-set, with millimeter, milliliter for counting
Amount unit.
Extract heat-resisting austenitic stainless steel miscible precipitate to carry out in pottery electrolysis bath, be at electrolysis of hydrochloric acid
In liquid, complete under magnetic field condition；
Pottery electrolysis bath is vertical, is groove lid 3 for electrolysis control station 2, top bottom pottery electrolysis bath 1；Pottery
Porcelain electrolysis bath 1 inner bottom part places magneton agitator 4；At the upper left quarter vertically negative electrode copper sheet 5 of groove lid 3,
And stretch in pottery electrolysis bath 1, and fixed by negative electrode fixed mount 7；Upper right quarter at groove lid 3 is disposed vertically sun
The most heat-resisting austenite stainless steel disc 6, and fixed by anode fixed mount 8, and in the most ceramic electrolysis bath 1；?
The top of groove lid 3, the bag-shaped semipermeable membrane 11 of both sides storing of anode heat-resisting austenite stainless steel disc 6, and by
First semipermeable membrane fixed mount the 9, second semipermeable membrane fixed mount 10 is fixed, and bag-shaped semipermeable membrane 11 stretches into pottery
In porcelain electrolysis bath 1, bag-shaped semipermeable membrane 11 is u-shaped, around anode heat-resisting austenite stainless steel disc 6；
Holding electrolysis of hydrochloric acid liquid 12 in pottery electrolysis bath 1, electrolysis of hydrochloric acid liquid 12 negative electrode to be flooded copper sheet 5, anode are resistance to
Hot austenite stainless steel disc 6, bag-shaped semipermeable membrane 11, magneton agitator 4；Electrolysis control station 2 is provided with
Display screen 13, display lamp 14, electrolytic switch 15, anodization controller 16, cathodic control device 17, magnetic agitation
Controller 18.
Shown in Fig. 2, for heat-resisting austenitic stainless steel miscible precipitate shape appearance figure, shown in figure, miscible precipitate
For black powder, in irregular stacking.
Shown in Fig. 3, for heat-resisting austenitic stainless steel miscible precipitate diffracted intensity collection of illustrative plates, shown in figure, vertical seat
Being designated as diffracted intensity, abscissa is the angle of diffraction, and main precipitate CrNbN is chromium niobium nitrogen, and NbN is niobium nitride,
Cr23C6Being six carbonization 23 chromium, non-precipitate is dissolved in hydrochloric acid.
Claims (2)
1. the method for a room temperature Rapid Extraction heat-resisting austenitic stainless steel miscible precipitate, it is characterised in that:
The chemical substance material used is: heat-resisting austenite stainless steel disc, copper sheet, hydrochloric acid, collodion, nothing
Water-ethanol, deionized water, sand paper, it is as follows that a combination thereof prepares consumption: with milliliter, millimeter as measurement unit
Heat-resisting austenite stainless steel disc: Fe53Cr25Ni20Mn1.44Nb0.3N0.2C0.06, 3mm × 30mm × 50mm
Copper sheet: Cu, 0.5mm × 80mm × 100mm
Hydrochloric acid: HCl, concentration 37%, 300mL ± 10mL
Collodion: C12H17(ONO2)3O7, concentration 5%, 30mL ± 1mL
Dehydrated alcohol: CH3CH2OH, 300mL ± 10mL
Deionized water: H2O, 3000mL ± 10mL
Sand paper: SiC, 3000 mesh, 300mm × 0.5mm × 200mm
Extracting process is as follows:
(1), preparation electrolysis of hydrochloric acid liquid
Measure hydrochloric acid 240mL ± 10mL, deionized water 760mL ± 10mL, add in beaker, stir 5min,
Become the aqueous hydrochloric acid solution of 3mol/L, i.e. electrolysis of hydrochloric acid liquid；
(2), pretreatment heat-resisting austenite stainless steel disc
Heat-resisting austenite stainless steel disc is placed on steel flat board, with each portion of sand papering periphery；
By the heat-resisting austenite stainless steel disc washes of absolute alcohol after polishing, then dry；
(3), pretreatment copper sheet
Copper sheet is placed on steel flat board, with each portion of sand papering periphery；
By the copper sheet after polishing, with washes of absolute alcohol, then dry；
(4), bag-shaped semipermeable membrane is prepared
1., collodion 30mL ± 1mL is placed in beaker, uniform rotation beaker, makes collodion uniformly adhere to
On beaker inwall, collodion is at beaker condensed on inner walls, until freezing film；
2., along beaker mouth mural margin strip off gap, admitting air into, air promotes thin film to divide with beaker inwall
From, instill deionized water, make thin film separately, become transparent membrane, the most bag-shaped semipermeable membrane；
(5), heat-resisting austenitic stainless steel miscible precipitate is extracted
Extract heat-resisting austenitic stainless steel miscible precipitate to carry out in pottery electrolysis bath, be at hydrochloric acid electricity
Solve in liquid, complete under the action of a magnetic field；
1., magneton agitator is placed in pottery electrolysis bath inner bottom part；
2., the electrolysis of hydrochloric acid liquid of configuration is added in pottery electrolysis bath；
3., heat-resisting austenite stainless steel disc is vertically arranged in right part in pottery electrolysis bath, for anode, and fixes；
Copper sheet is vertically arranged in left part in pottery electrolysis bath, for negative electrode, and fixes；
Heat-resisting austenitic stainless steel sheet is loaded in the U-shaped bag-shaped semipermeable membrane being disposed vertically, and by bag-shaped semi-transparent
Film is fixed；
Electrolysis of hydrochloric acid liquid to flood heat-resisting austenite stainless steel disc, copper sheet, bag-shaped semipermeable membrane；
4., opening anodization controller, cathodic control device, magneton agitator, electrolysis of hydrochloric acid liquid starts electrolysis；
Anode current 2A, cathode current 2A；
Magneton agitator revolution 60r/min；
Electrolysis temperature 25 DEG C；
Electrolysis time 600min；
Heat-resisting austenite stainless steel disc solid-state precipitate is attached on bag-shaped semipermeable membrane；
5., closing anodization controller, cathodic control device, electrolyte stands 60min in pottery electrolysis bath；
Heat-resisting austenite stainless steel disc separates out solid-state CrNbN, Cr in electrolytic process23C6, NbN, and adhere to
On semipermeable membrane；
6., heat-resisting austenite stainless steel disc will occur chemical reaction during electrolytic extraction miscible precipitate,
Reaction equation is as follows:
In formula: H2: hydrogen；
Cr23C6: six carbonization 23 chromium；
NbN: niobium nitride；
CrNbN: chromium niobium nitrogen；
NiCl2: Nickel dichloride.；
CrCl3: Chlorizate chromium；
FeCl2: ferrous chloride；
MnCl2: manganese chloride；
Wherein: chromium niobium nitrogen, niobium nitride, six carbonization 23 chromium are solid-state precipitate；
Nickel dichloride., Chlorizate chromium, manganese chloride, ferrous chloride are dissolving with hydrochloric acid thing；
(6), precipitate is extracted
1., the bag-shaped semipermeable membrane of attachment precipitate is placed in beaker, adds deionized water 200mL, stir
Mix washing 2min；
Deionized water wash repeats three times, then precipitates, and retains precipitate；
2., precipitate is added in another beaker, add hydrochloric acid 50mL, mix and blend, dissolve in cleaning mixture
Ferrum simple substance, then precipitate, retain precipitate；
3., precipitate is added in another beaker, add deionized water 200mL, agitator treating 2min；
Deionized water wash repeats three times, washes out chloride ion, then precipitates, and retains precipitate；
4., sucking filtration, put the precipitate in the buchner funnel of bottle,suction, carry out with three layers of middling speed qualitative filter paper
Sucking filtration, remaining product filter cake, filtrate is evacuated in filter flask, discards；
(7), vacuum drying
Product cake is placed in quartz container, is subsequently placed in vacuum drying oven and is dried, baking temperature 50 DEG C,
Vacuum 10Pa, drying time 30min；
Dried material is heat-resisting austenitic stainless steel miscible precipitate powder；
(8), detect, analyze, characterize
The color and luster of heat-resisting austenitic stainless steel miscible precipitate, pattern, the chemical substance of extraction are detected,
Analyze, characterize；
Powder material phase analysis is carried out with X-ray diffractometer；
Conclusion: heat-resisting austenitic stainless steel miscible precipitate is CrNbN, Cr23C6, NbN, for black powder,
Particle diameters≤300nm.
A kind of room temperature Rapid Extraction heat-resisting austenitic stainless steel miscible precipitate the most according to claim 1
Method, it is characterised in that:
Extract heat-resisting austenitic stainless steel miscible precipitate to carry out in pottery electrolysis bath, be at hydrochloric acid electricity
Solve in liquid, complete under magnetic field condition；
Pottery electrolysis bath is vertical, and pottery electrolysis bath (1) bottom is groove for electrolysis control station (2), top
Lid (3)；Pottery electrolysis bath (1) inner bottom part places magneton agitator (4)；Upper left in groove lid (3)
Vertically negative electrode copper sheet (5), portion, and stretch in pottery electrolysis bath (1), and by negative electrode fixed mount (7)
Fixing；Upper right quarter at groove lid (3) is disposed vertically anode heat-resisting austenite stainless steel disc (6), and by sun
Pole fixed mount (8) is fixed, and deeply pottery electrolysis bath (1) is interior；Top, anode in groove lid (3) are resistance to
Bag-shaped semipermeable membrane (11) is put in the both sides of hot austenite stainless steel disc (6), and by the first semipermeable membrane
Fixed mount (9), the second semipermeable membrane fixed mount (10) are fixing, and bag-shaped semipermeable membrane (11) stretches into pottery
In electrolysis bath (1), bag-shaped semipermeable membrane (11) is u-shaped, around anode heat-resisting austenite stainless steel disc
(6)；Holding electrolysis of hydrochloric acid liquid (12) in pottery electrolysis bath (1), electrolysis of hydrochloric acid liquid (12) to flood
Negative electrode copper sheet (5), anode heat-resisting austenite stainless steel disc (6), bag-shaped semipermeable membrane (11), magneton
Agitator (4)；Electrolysis control station (2) is provided with display screen (13), display lamp (14), electrolysis
Switch (15), anodization controller (16), cathodic control device (17), magnetic agitation controller (18).
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