CN105951100A - Magnesium-aluminum-strontium-yttrium alloy etching agent and method for obtaining metallographic structure through magnesium-aluminum-strontium-yttrium alloy etching agent - Google Patents
Magnesium-aluminum-strontium-yttrium alloy etching agent and method for obtaining metallographic structure through magnesium-aluminum-strontium-yttrium alloy etching agent Download PDFInfo
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- CN105951100A CN105951100A CN201610284811.8A CN201610284811A CN105951100A CN 105951100 A CN105951100 A CN 105951100A CN 201610284811 A CN201610284811 A CN 201610284811A CN 105951100 A CN105951100 A CN 105951100A
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- Prior art keywords
- strontium
- magnalium
- metallographic structure
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- magnesium
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/22—Acidic compositions for etching magnesium or alloys thereof
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
Abstract
The invention relates to the field of metallographic structure obtaining, in particular to a method for obtaining a clear magnesium-aluminum-strontium-yttrium alloy metallographic structure through a magnesium-aluminum-strontium-yttrium alloy etching agent. According to the magnesium-aluminum-strontium-yttrium alloy etching agent, 2.1 g of picric acid, 5 ml of deionized water, 35 ml of anhydrous ethanol and 5 ml of acetic acid are added into a container and stirred with a glass rod, so that the picric acid is completely dissolved; and after the picric acid is completely dissolved, the container is placed in a shade and dark place to be stored. The invention further provides the specific method for obtaining the clear metallographic structure. The phenomenon that magnesium alloy corrosion is difficult is effectively overcome.
Description
Technical field
The present invention relates to obtain metallographic structure field, be specially one and obtain magnalium strontium by magnalium strontium yittrium alloy etchant
The method of yittrium alloy metallographic structure clearly.
Background technology
Magnalium is the lightest non-ferrous alloy, have that density is little, specific strength is high, good heat dissipation bigger than elastic modelling quantity,
The features such as shock absorbing is good, and the load-carrying ability that withstands shocks is bigger than aluminium alloy, and the corrosive nature of resistance to Organic substance and alkali is good, are described as 21 generation
The green structural material recorded.
The alloying element added in magnesium alloy mainly has Al, Zn, Mn, Zr, Ca, Li, Sr and multiple rare earth element, according to
Alloy constituent element quantitative classification, magnesium alloy can be divided into binary, ternary and multi-element alloy system, can be divided into change by moulding process magnesium alloy
Shape magnesium alloy and cast magnesium alloy.Along with magnesium alloy is in electronics industry, Aero-Space, auto industry and housed device field day
Benefit development and application widely, its alloy composition is more complicated, diversification, moulding process more multiformity, the tissue of magnesium alloy
Composition the most constantly changes.Current existing magnesium alloy etching agent common issue is that the etch time is too short or etch
Agent acidity is more weak, and crystal boundary cannot clearly corrode out, and overlong time or etchant acidity are relatively strong, often at metallographic specimen
Surface forms thin film shape oxide layer, causes surface blackening, and the second phase is difficult to recognize.As can be seen here, current existing etch
Agent can not meet the most far away the requirement of increasing novel magnesium alloy fabric study.
Summary of the invention
The technical problem to be solved is: how to provide a kind of magnalium strontium yittrium alloy etchant, utilizes this magnalium
Strontium yittrium alloy etchant obtains magnalium strontium yittrium alloy metallographic structure clearly.
The technical solution adopted in the present invention is: a kind of magnalium strontium yittrium alloy etchant, adds 2.1 unit of gram in a reservoir
Picric acid, the deionized water of 5 unit milliliters, the dehydrated alcohol of 35 unit milliliters, the acetic acid of 5 unit milliliters, stir with Glass rod
Mix, make picric acid be completely dissolved, after picric acid is completely dissolved, is placed at shady and cool lucifuge and preserves.
As a kind of optimal way: a kind of magnalium strontium yittrium alloy etchant, add the bitterness of 2.1 unit of gram in a reservoir
Acid, the deionized water of 5 unit milliliters, the dehydrated alcohol of 35 unit milliliters, the acetic acid of 5 unit milliliters, the sodium chloride of 1 unit of gram,
Stir with Glass rod, make picric acid be completely dissolved, after picric acid is completely dissolved, is heated to 80 degrees Celsius and distills, distillation
When product is the 50% of gross mass, stops distillation, product of distillation is cooled to room temperature, be placed at shady and cool lucifuge and preserve.
A kind of method obtaining magnalium strontium yittrium alloy metallographic structure, is carried out according to the steps
Step one, will according to mass percent Mg be 89-91%, Al be 8.0-8.5%, Sr be 0.4-0.8%, Y be 0.2-0.6%
The cuboid sample that is fabricated to of magnalium strontium yittrium alloy be mounted on bakelite powder mosaics；
Step 2, the one side of the metallographic structure to be observed appeared by sample grind, after having ground on metallic phase polisher milling
Mechanically polish, after sample washes of absolute alcohol polishing completed is clean, dry up with hair-dryer；
Step 3, tweezers clamp the rayon balls soaked with the magnalium strontium yittrium alloy etchant prepared, and are processing through step 2
Specimen surface wiping, wiping complete after with alcohol rinse, then dry up with hair-dryer, use metallurgical microscope to carry out taking pictures i.e.
The metallographic structure of sample can be obtained.
As a kind of optimal way: grinding in step 2 refers to, it is manual that to use granularity the most successively be 400#, 600#,
The sand paper of 1000#, 1600#, 2000# carries out grinding to specimen surface, when grinding process often changes a sand paper, and sample grinding side
To changing 90 °, becoming vertical direction with former polishing scratch, grind along same direction until polishing scratch is wholly absent, new polishing scratch is equal
Even consistent time till, change sand paper ultrasonic cleaner simultaneously every time and sample cleaned.
As a kind of optimal way: when step 2 mechanically polishes, with the aluminum oxide polishing powder that granularity is 0.5 micron
The mass percentage concentration being configured to is that the aqueous solution of 25% is as polishing fluid.
As a kind of optimal way: step 3 refers in specimen surface wiping, specimen surface in a clockwise direction and
Mode the most alternately rotates wiping, and wiping speed is 2 circles/second, direction of rotation of conversion in every 10 seconds, corrosion altogether
The 20-40 second.
The invention has the beneficial effects as follows: the present invention be directed to the situation of novel rare-earth magnesium alloy etching pit difficulty, use
By being used in conjunction with of oxidizing acid based on acetic acid, picric acid and acetic acid, make the metallographic of coupling magnalium strontium yittrium alloy characteristic
Etchant, efficiently solves the phenomenon of Corrosion Behaviors of Magnesium Alloys difficulty；Each component of the present invention is the commercially available chemical reagent of routine, and
Compound method is simple, applies this chemical etching agent can quickly, clearly show the metallographic structure of magnalium strontium yittrium alloy, particularly solid solution
Metallographic structure after process.
Detailed description of the invention
Fig. 1 is the metallographic structure figure of as cast condition magnalium strontium yittrium alloy；
Fig. 2 is that the metallographic structure figure of the magnalium strontium yittrium alloy after solution treatment is (at the warm after being incubated 12 hours under the conditions of 380 DEG C
Reason state magnalium strontium yittrium alloy)；
Fig. 3 is that the metallographic structure figure of the magnalium strontium yittrium alloy after solution treatment is (at the warm after being incubated 24 hours under the conditions of 380 DEG C
Reason state magnalium strontium yittrium alloy).
Detailed description of the invention
Embodiment 1
The picric acid taking appropriate water seal protection with medicine spoon is placed on filter paper, and is placed into shady and cool dry place standing 12 hours,
Within the most every 2 hours, change a filter paper to divide with dewatered and washed, finally give pale yellow crystals solid, weigh 2.1 grams and put into capacity and be
In the brown reagent bottle of 50ml.
Measure 5ml deionized water with the graduated cylinder that capacity is 10ml, pour in the brown reagent bottle that above-mentioned capacity is 50ml.
Measure 35ml dehydrated alcohol with the graduated cylinder that capacity is 50ml, pour in the brown reagent bottle that above-mentioned capacity is 50ml.
Measure 5ml acetic acid with the graduated cylinder that capacity is 10ml, pour in the brown reagent bottle that above-mentioned capacity is 50ml.
Above four kinds of materials are used in reagent bottle Glass rod uniform stirring 3min, promotes picric acid rapid solution, treat hardship
After sour in the mouth is completely dissolved, it is thus achieved that magnalium strontium yittrium alloy etchant, it is placed at shady and cool lucifuge and preserves.
Picric acid in this etchant is the etchant that etch magnesium alloy is conventional, but owing to its acidity is too strong, along with dense
The minimizing of degree or increase, can cause corrosion to kick the beam or overweight situation, can not get metallographic structure clear, preferable, therefore
Etchant of the present invention is especially added with oxidizing acid based on this weak acid of acetic acid, acetic acid and ethanol in picric catalytic action
Under there occurs that esterification generates ethyl acetate, corrosion process defines a kind of protecting film in metal surface, so can be big
Slow down greatly picric corrosion rate, and do not affect the metallographic structure observing metal.
Embodiment 2
The picric acid taking appropriate water seal protection with medicine spoon is placed on filter paper, and is placed into shady and cool dry place standing 12 hours,
Within the most every 2 hours, change a filter paper to divide with dewatered and washed, finally give pale yellow crystals solid, weigh 2.1 grams and put into capacity and be
In the brown reagent bottle of 50ml.
Weigh with scale the sodium chloride of 1 gram, pours in the brown reagent bottle that above-mentioned capacity is 50ml.
Measure 5ml deionized water with the graduated cylinder that capacity is 10ml, pour in the brown reagent bottle that above-mentioned capacity is 50ml.
Measure 35ml dehydrated alcohol with the graduated cylinder that capacity is 50ml, pour in the brown reagent bottle that above-mentioned capacity is 50ml.
Measure 5ml acetic acid with the graduated cylinder that capacity is 10ml, pour in the brown reagent bottle that above-mentioned capacity is 50ml.
Above five kinds of materials are used in reagent bottle Glass rod uniform stirring 3min, promotes picric acid rapid solution, treat hardship
After sour in the mouth is completely dissolved, puts in alembic and distill in the sea water bath of 80 degrees Celsius, when product of distillation is gross mass
When 50%, stop distillation, product of distillation is cooled to room temperature, be placed at shady and cool lucifuge and preserve.
Obtaining etchant by distillation, extent of corrosion is suitable, and corrosion rate is moderate, observes the magnalium strontium yttrium metallographic group of metal
When knitting, image is the most clear.
Embodiment 3
Will according to mass percent Mg be 89-91%, Al be 8.0-8.5%, Sr be 0.4-0.8%, Y be the as cast condition of 0.2-0.6%
The cuboid sample that is fabricated to of magnalium strontium yittrium alloy be mounted on bakelite powder mosaics, sample is cut on WEDM
Taking the block of a size of 10mm × 10mm × 5mm, use metallic phase sample inlaying machine to inlay this block afterwards, inlaying temperature is 1305 DEG C, temperature retention time is 8-10min；
Abrasive paper for metallograph is laid on the glass of surfacing, it is manual that to use granularity the most successively be 400#, 600#, 1000#, 1600#,
The sand paper of 2000# carries out grinding of magnalium strontium yittrium alloy metallographic specimen, when often changing a sand paper during grinding, and the sample side of grinding
To 90 ° must be changed, become vertical direction with former polishing scratch, grind along direction to polishing scratch and be wholly absent, new polishing scratch uniform
Till during cause, must be cleaned by sample with ultrasonic cleaner, scavenging period is 30s, and hands is cleaned the most simultaneously simultaneously every time.To grind
After magnalium strontium yittrium alloy sample mechanically polish on metallic phase polisher milling, with the aluminum oxide polishing powder that granularity is 0.5 micron
The mass percentage concentration being configured to be the aqueous solution of 25% as polishing fluid, sample flour milling is pressed in equably the polishing disk of rotation
On, and constantly diametrically reciprocate along the edge of dish to center, the time is 3-5min, till flour milling light is seamless, and will
Polished magnalium strontium yittrium alloy sample (as cast condition) with washes of absolute alcohol clean after, dry up with hair-dryer；
The etchant configured with glue head dropper extraction embodiment 1, soaks the rayon balls being of moderate size, and clamps with tweezers
Living, rotate wiping with mode the most alternately in a clockwise direction at sample surfaces, wiping speed is 2 circles/second, every 10
Direction of rotation of second conversion, corrosion used rapidly alcohol rinse after 20 seconds altogether, and hair-dryer dries up, and used metallurgical microscope to carry out
Take pictures the metallographic structure of the cleaning that can obtain sample, as shown in Figure 1.
Embodiment 4
Will according to mass percent Mg be 89-91%, Al be 8.0-8.5%, Sr be 0.4-0.8%, Y be the solid solution of 0.2-0.6%
The cuboid sample that the magnalium strontium yittrium alloy (being incubated 12 hours under the conditions of 380 DEG C) after process is fabricated to is mounted to bakelite powder edge
On inlay, sample cuts the block of a size of 10mm × 10mm × 5mm on WEDM, uses metallographic specimen afterwards
This block inlayed by pointing machine, and inlaying temperature is 1305 DEG C, temperature retention time is 8-10min；
Abrasive paper for metallograph is laid on the glass of surfacing, it is manual that to use granularity the most successively be 400#, 600#, 1000#, 1600#,
The sand paper of 2000# carries out grinding of magnalium strontium yittrium alloy metallographic specimen, when often changing a sand paper during grinding, and the sample side of grinding
To 90 ° must be changed, become vertical direction with former polishing scratch, grind along direction to polishing scratch and be wholly absent, new polishing scratch uniform
Till during cause, must be cleaned by sample with ultrasonic cleaner, scavenging period is 30s, and hands is cleaned the most simultaneously simultaneously every time.To grind
After magnalium strontium yittrium alloy sample mechanically polish on metallic phase polisher milling, with the aluminum oxide polishing powder that granularity is 0.5 micron
The mass percentage concentration being configured to be the aqueous solution of 25% as polishing fluid, sample flour milling is pressed in equably the polishing disk of rotation
On, and constantly diametrically reciprocate along the edge of dish to center, the time is 3-5min, till flour milling light is seamless, and will
Polished magnalium strontium yittrium alloy sample (solid solution state) with washes of absolute alcohol clean after, dry up with hair-dryer；
The etchant configured with glue head dropper extraction embodiment 1, soaks the rayon balls being of moderate size, and clamps with tweezers
Living, rotate wiping with mode the most alternately in a clockwise direction at sample surfaces, wiping speed is 2 circles/second, every 10
Direction of rotation of second conversion, corrosion used rapidly alcohol rinse after 30 seconds altogether, and hair-dryer dries up, and used metallurgical microscope to carry out
Take pictures the metallographic structure of the cleaning that can obtain sample, as shown in Figure 2.
Embodiment 5
Will according to mass percent Mg be 89-91%, Al be 8.0-8.5%, Sr be 0.4-0.8%, Y be the solid solution of 0.2-0.6%
The cuboid sample that the magnalium strontium yittrium alloy (being incubated 24 hours under the conditions of 380 DEG C) after process is fabricated to is mounted to bakelite powder edge
On inlay, sample cuts the block of a size of 10mm × 10mm × 5mm on WEDM, uses metallographic specimen afterwards
This block inlayed by pointing machine, and inlaying temperature is 1305 DEG C, temperature retention time is 8-10min；
Abrasive paper for metallograph is laid on the glass of surfacing, it is manual that to use granularity the most successively be 400#, 600#, 1000#, 1600#,
The sand paper of 2000# carries out grinding of magnalium strontium yittrium alloy metallographic specimen, when often changing a sand paper during grinding, and the sample side of grinding
To 90 ° must be changed, become vertical direction with former polishing scratch, grind along direction to polishing scratch and be wholly absent, new polishing scratch uniform
Till during cause, must be cleaned by sample with ultrasonic cleaner, scavenging period is 30s, and hands is cleaned the most simultaneously simultaneously every time.To grind
After magnalium strontium yittrium alloy sample mechanically polish on metallic phase polisher milling, with the aluminum oxide polishing powder that granularity is 0.5 micron
The mass percentage concentration being configured to be the aqueous solution of 25% as polishing fluid, sample flour milling is pressed in equably the polishing disk of rotation
On, and constantly diametrically reciprocate along the edge of dish to center, the time is 3-5min, till flour milling light is seamless, and will
Polished magnalium strontium yittrium alloy sample (solid solution state) with washes of absolute alcohol clean after, dry up with hair-dryer；
The etchant configured with glue head dropper extraction embodiment 2, soaks the rayon balls being of moderate size, and clamps with tweezers
Living, rotate wiping with mode the most alternately in a clockwise direction at sample surfaces, wiping speed is 2 circles/second, every 10
Direction of rotation of second conversion, corrosion used rapidly alcohol rinse after 40 seconds altogether, and hair-dryer dries up, and used metallurgical microscope to carry out
Take pictures the metallographic structure of the cleaning that can obtain sample, as shown in Figure 3.
Claims (5)
1. a magnalium strontium yittrium alloy etchant, it is characterised in that: add the picric acid of 2.1 unit of gram, 5 units in a reservoir
The deionized water of milliliter, the dehydrated alcohol of 35 unit milliliters, the acetic acid of 5 unit milliliters, stir with Glass rod, make picric acid complete
Dissolve, after picric acid is completely dissolved, is placed at shady and cool lucifuge and preserves.
2. the method obtaining magnalium strontium yittrium alloy metallographic structure, it is characterised in that: carry out according to the steps
Step one, will according to mass percent Mg be 89-91%, Al be 8.0-8.5%, Sr be 0.4-0.8%, Y be 0.2-0.6%
The cuboid sample that is fabricated to of magnalium strontium yittrium alloy be mounted on bakelite powder mosaics；
Step 2, the one side of the metallographic structure to be observed appeared by sample grind, after having ground on metallic phase polisher milling
Mechanically polish, after sample washes of absolute alcohol polishing completed is clean, dry up with hair-dryer；
The rayon balls that magnalium strontium yittrium alloy etchant described in step 3, tweezers clamping claim 1 soaks, through step
The two specimen surface wipings processed, wiping is used alcohol rinse after completing, is then dried up with hair-dryer, uses metallurgical microscope to carry out
Take pictures and can obtain the metallographic structure of sample.
A kind of method obtaining magnalium strontium yittrium alloy metallographic structure the most according to claim 2, it is characterised in that: step 2
In grind and refer to, specimen surface is entered by the manual sand paper using granularity to be 400#, 600#, 1000#, 1600#, 2000# the most successively
Row grinding, when often changing a sand paper in grinding process, sample grinding direction must change 90 °, becomes vertical direction, edge with former polishing scratch
The grinding of same direction until polishing scratch is wholly absent, during new polishing scratch uniformity till, change sand paper with ultrasonic simultaneously every time
Sample is cleaned by ripple washer.
A kind of method obtaining magnalium strontium yittrium alloy metallographic structure the most according to claim 2, it is characterised in that: step 2
In when mechanically polishing, the mass percentage concentration being configured to the aluminum oxide polishing powder that granularity is 0.5 micron be 25% water-soluble
Liquid is as polishing fluid.
A kind of method obtaining magnalium strontium yittrium alloy metallographic structure the most according to claim 2, it is characterised in that: step 3
In refer in specimen surface wiping, rotate wiping with mode counterclockwise alternately in a clockwise direction at specimen surface, wipe
Wiping speed is 2 circles/second, direction of rotation of conversion in every 10 seconds, the corrosion 20-40 second altogether.
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| CN201610284811.8A CN105951100A (en) | 2016-05-04 | 2016-05-04 | Magnesium-aluminum-strontium-yttrium alloy etching agent and method for obtaining metallographic structure through magnesium-aluminum-strontium-yttrium alloy etching agent |
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| CN201610284811.8A CN105951100A (en) | 2016-05-04 | 2016-05-04 | Magnesium-aluminum-strontium-yttrium alloy etching agent and method for obtaining metallographic structure through magnesium-aluminum-strontium-yttrium alloy etching agent |
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| CN113088972A (en) * | 2021-04-02 | 2021-07-09 | 河南科技大学 | Rare earth magnesium alloy metallographic corrosive agent and application thereof |
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| CN110468416A (en) * | 2019-08-08 | 2019-11-19 | 重庆科技学院 | Show the corrosive liquid and preparation method and application of super-high strength steel austenite grain boundary and transgranular bainite and martensite |
| CN110468416B (en) * | 2019-08-08 | 2021-08-03 | 重庆科技学院 | Corrosive liquid for displaying austenite grain boundary and intragranular bainite and martensite of ultrahigh-strength steel, and preparation method and application thereof |
| CN113088972A (en) * | 2021-04-02 | 2021-07-09 | 河南科技大学 | Rare earth magnesium alloy metallographic corrosive agent and application thereof |
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