CN104458374A - Preparation method of aluminum-silicon alloy testing sample with low-magnification grain size - Google Patents
Preparation method of aluminum-silicon alloy testing sample with low-magnification grain size Download PDFInfo
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- CN104458374A CN104458374A CN201410725527.0A CN201410725527A CN104458374A CN 104458374 A CN104458374 A CN 104458374A CN 201410725527 A CN201410725527 A CN 201410725527A CN 104458374 A CN104458374 A CN 104458374A
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Abstract
The invention provides a preparation method of an aluminum-silicon alloy testing sample with the low-magnification grain size. The preparation method comprises the following steps: complexing and corroding the surface of an aluminum-silicon alloy sample to be tested with a diluted hydrofluoric acid solution used as a complexing corroding agent, wherein the volume concentration of the diluted hydrofluoric acid solution is 30-70%; carrying out first oxidization on the surface of the aluminum-silicon alloy sample to be tested after complexing and corroding by taking hydrogen peroxide used as a first oxidizing agent; and carrying out second oxidization on the surface of the aluminum-silicon alloy sample to be tested after the first oxidization by taking a dilute nitric acid solution used as a second oxidizing agent to obtain the aluminum-silicon alloy testing sample with the low-magnification grain size, wherein the volume concentration of the dilute nitric acid solution is 5-25%. The low-magnification grain size of a cast eutectic aluminum-silicon alloy piston sample piece can be clearly displayed due to the method.
Description
Technical field
The present invention relates to field of metal alloy technology, particularly relate to the preparation method that a kind of Alpax low power grain size detects sample.
Background technology
Crystalline material, in growth course, owing to being subject to the restriction of free surrounding space, being failed to develop into the crystal with conformation of rules, and is just crystallized into graininess, become crystal grain.Grain size represents the yardstick of grain size, and average area or the mean diameter of useable die represent.The engineering properties such as pulling strengrth, toughness, plasticity of size on metal of crystal grain has conclusive impact.Therefore, the counting of crystal grain has considerable meaning in metallographic examination.
In prior art, cocrystallized Al-Si alloy overcomes the shortcoming that aluminium copper series alloy thermal expansivity is large, density is large, has been widely used in the production of automobile and motorcycle piston.Once used aluminium recovery material roughly has four classes so far: Al-Cu-Ni-Mg system, Al-Cu-Si system, cocrystallizing type Al-Si-Cu-Mg system and hypereutectic type Al-Si-Cu-Mg system, front two classes due to exist linear expansion coefficient large, be eliminated already than great, that volume is unstable shortcoming, the aluminium recovery material mainly cocrystallizing type aluminium alloy of current domestic use.The application of low power grain size on piston of aluminium-silicon alloy piston has important impact, mainly adopts the etch of NaOH aqueous solution to show or adopt HF+HCl+HNO in prior art for the detection of aluminium-silicon alloy piston low power grain size
3acid mixture etch shows, and visual inspection Alpax crystalline phase, obtains the grain size of aluminium-silicon alloy piston.
But this NaOH aqueous solution etch cocrystallized Al-Si alloy piston low power sample, is difficult to the black oxide film of the densification of scrubbing owing to producing one deck, so that the display of cocrystallized Al-Si alloy piston low power grain size is unintelligible; Adopt HF+HCl+HNO
3acid mixture etch cocrystallized Al-Si alloy piston low power sample, etch depth degree is inconsistent, has also had a strong impact on the sharpness of crystalline phase.Therefore, for the detection of aluminium-silicon alloy piston low power grain size in prior art, the low power sample crystalline phase display of preparation is unintelligible, makes the accuracy of testing result lower.
Summary of the invention
The object of the present invention is to provide a kind of Alpax low power grain size to detect the preparation method of sample, the detection sample that method provided by the invention prepares can demonstrate the low power grain size on Alpax surface clearly.
The invention provides the preparation method that a kind of Alpax low power grain size detects sample, comprise the following steps:
Take dilute hydrofluoric acid solution as complexing mordant, complexing corrosion Alpax testing sample surface, the volumetric concentration of described dilute hydrofluoric acid solution is 30% ~ 70%;
Be the first oxygenant with hydrogen peroxide, the first oxidation is carried out to the Alpax testing sample surface after described complexing corrosion;
Be the second oxygenant with dilute nitric acid solution, carry out the second oxidation to the Alpax testing sample surface after described first oxidation, obtain Alpax low power grain size and detect sample, the volumetric concentration of described dilute nitric acid solution is 5% ~ 25%.
Preferably, the volumetric concentration of described dilute hydrofluoric acid solution is 40% ~ 60%.
Preferably, the time of described complexing corrosion is 2min ~ 10min.
Preferably, described complexing corrosion is specially:
Described dilute hydrofluoric acid solution is coated on described Alpax testing sample surface, carries out complexing corrosion.
Preferably, the time of described first oxidation is 1min ~ 5min.
Preferably, described first oxidation is specially:
Described hydrogen peroxide is applied in the Alpax testing sample surface after described complexing corrosion, carries out the first oxidation.
Preferably, the volumetric concentration of described dilute nitric acid solution is 10% ~ 20%.
Preferably, described second oxidation time >=1min.
Preferably, described second oxidation is specially:
Alpax testing sample after described first oxidation is dipped in described dilute nitric acid solution, carries out the second oxidation.
Preferably, also washing is comprised after described second oxidation.
The invention provides the preparation method that a kind of Alpax low power grain size detects sample, comprise the following steps: take dilute hydrofluoric acid solution as complexing mordant, complexing corrosion Alpax testing sample surface, the volumetric concentration of described dilute hydrofluoric acid solution is 30% ~ 70%; Be the first oxygenant with hydrogen peroxide, the first oxidation is carried out to the Alpax testing sample surface after described complexing corrosion; Be the second oxygenant with dilute nitric acid solution, carry out the second oxidation to the Alpax testing sample surface after described first oxidation, obtain Alpax low power grain size and detect sample, the volumetric concentration of described dilute nitric acid solution is 5% ~ 25%.First method provided by the invention utilizes volumetric concentration to be that the appropriate complexing corrosivity of the diluted hydrofluoric acid (HF) of 30% ~ 70% obtains the very thin metal fluoride layer of one deck, then utilizes hydrogen peroxide (H successively
2o
2), volumetric concentration is 5% ~ 25% dust technology (HNO
3) carry out the first oxidation and the second oxidation, the oxidisability of appropriateness is guaranteed to be easy to scrub black fluorinated film thin layer, thus clearly demonstrates the low power grain size of casting cocrystallized Al-Si alloy piston exemplar.
Accompanying drawing explanation
Fig. 1 is the aluminium-silicon alloy piston low power grain size sample drawing that the embodiment of the present invention 1 obtains;
Fig. 2 is the aluminium-silicon alloy piston low power grain size sample drawing that comparative example 1 of the present invention obtains;
Fig. 3 is the aluminium-silicon alloy piston low power grain size sample drawing that comparative example 2 of the present invention obtains.
Embodiment
The invention provides the preparation method that a kind of Alpax low power grain size detects sample, comprise the following steps:
Take dilute hydrofluoric acid solution as complexing mordant, complexing corrosion Alpax testing sample surface, the volumetric concentration of described dilute hydrofluoric acid solution is 30% ~ 70%;
Be the first oxygenant with hydrogen peroxide, the first oxidation is carried out to the Alpax testing sample surface after described complexing corrosion;
Be the second oxygenant with dilute nitric acid solution, carry out the second oxidation to the Alpax testing sample surface after described first oxidation, obtain Alpax low power grain size and detect sample, the volumetric concentration of described dilute nitric acid solution is 5wt% ~ 25wt%.
First method provided by the invention utilizes volumetric concentration to be that the appropriate complexing corrosivity of the diluted hydrofluoric acid (HF) of 30% ~ 70% obtains the very thin metal fluoride layer of one deck, then utilize hydrogen peroxide (H2O2) successively, volumetric concentration be 5% ~ 25% dust technology (HNO3) carry out the first oxidation and second oxidation, the oxidisability of appropriateness is guaranteed to be easy to scrub black fluorinated film thin layer, thus clearly demonstrates the low power grain size of casting cocrystallized Al-Si alloy piston exemplar.
Method provided by the invention take dilute hydrofluoric acid solution as complexing mordant, and complexing corrosion Alpax testing sample surface, the volumetric concentration of described dilute hydrofluoric acid solution is 30% ~ 70%.The present invention does not have special restriction to the kind of described Alpax testing sample and source, adopt the Alpax testing sample needing to detect low power grain size well known to those skilled in the art, in an embodiment of the present invention, described testing sample is specially casting cocrystallized Al-Si alloy piston exemplar.
Dilute hydrofluoric acid solution is preferably coated on described Alpax testing sample surface by the present invention, carries out complexing corrosion.The method of the present invention to described coating does not have special restriction, adopts the technical scheme of coating well known to those skilled in the art.In an embodiment of the present invention, can be specially: dilute hydrofluoric acid solution is dripped in Alpax testing sample surface, and with the whole analysis face of degreasing dough wiping.
In the present invention, the volumetric concentration of described dilute hydrofluoric acid solution is 30% ~ 70%, is preferably 35% ~ 65%, is more preferably 40% ~ 60%; In an embodiment of the present invention, the volumetric concentration of described diluted hydrofluoric acid can be specially 40%, 45%, 50%, 55% or 60%.In the present invention, described dilute hydrofluoric acid solution is preferably the aqueous solution of hydrofluorite, is specially the mixed solution of hydrogen fluoride and distilled water.In the present invention, the time of described complexing corrosion is preferably 2min ~ 10min, is more preferably 4min ~ 8min; In an embodiment of the present invention, the time of described complexing corrosion can be specially 4min, 5min, 8min or 10min.
After completing described complexing corrosion, the present invention is the first oxygenant with hydrogen peroxide, carries out the first oxidation to the Alpax testing sample surface after described complexing corrosion.In the present invention, described first oxidation is preferably: described hydrogen peroxide is applied in the Alpax testing sample surface after described complexing corrosion, carries out the first oxidation.The present invention does not have special restriction to described method of smearing, and adopts technical scheme of smearing well known to those skilled in the art.In an embodiment of the present invention, can be specially: by the Alpax testing sample analysis face of described dioxygen water droplet after described complexing corrosion, and with the whole analysis face of degreasing dough wiping.
In the present invention, the volumetric concentration of described hydrogen peroxide is preferably 20% ~ 50%, is more preferably 30% ~ 45%, most preferably is 35% ~ 40%.The source of the present invention to described hydrogen peroxide does not have special restriction, adopts the commercial goods of hydrogen peroxide well known to those skilled in the art.In the present invention, the time of described first oxidation is preferably 1min ~ 5min, is more preferably 2min ~ 4min.
After completing described first oxidation, the present invention is the second oxygenant with dilute nitric acid solution, carry out the second oxidation to the Alpax testing sample surface after described first oxidation, obtain Alpax low power grain size and detect sample, the volumetric concentration of described dilute nitric acid solution is 5% ~ 25%.In the present invention, described second oxidation is preferably specially: be dipped in described dilute nitric acid solution by the Alpax testing sample after described first oxidation, carry out the second oxidation.In an embodiment of the present invention, by dilute nitric acid solution as in dust technology pond, the Alpax testing sample after described first oxidation can be dipped in described dilute nitric acid solution.
In the present invention, the volumetric concentration of described dilute nitric acid solution is preferably 10% ~ 20%, is more preferably 10% ~ 15%.In an embodiment of the present invention, the volumetric concentration of described dilute nitric acid solution can be specially 5%, 10%, 15% or 20%.In the present invention, time of described second oxidation preferably >=1min, be more preferably 1min ~ 5min, most preferably be 2min ~ 4min.
After completing described second oxidation, the Alpax testing sample after described second oxidation is preferably washed by the present invention, obtains Alpax low power grain size and detects sample.The method of the present invention to described washing does not have special restriction, adopts the technical scheme of washing well known to those skilled in the art; In an embodiment of the present invention, can be specially flowing water washing, the rule alloy testing sample after adopting hairbrush to wash away clean described second oxidation in flowing water analyzes face.
After completing described washing, the present invention preferably dries up the Alpax testing sample after described washing, obtains Alpax low power grain size and detects sample.The present invention does not have special restriction to the described method dried up, and adopts the technical scheme dried up well known to those skilled in the art.
The invention provides the preparation method that a kind of Alpax low power grain size detects sample, comprise the following steps: take dilute hydrofluoric acid solution as complexing mordant, complexing corrosion Alpax testing sample surface, the volumetric concentration of described dilute hydrofluoric acid solution is 30% ~ 70%; Be the first oxygenant with hydrogen peroxide, the first oxidation is carried out to the Alpax testing sample surface after described complexing corrosion; Be the second oxygenant with dilute nitric acid solution, carry out the second oxidation to the Alpax testing sample surface after described first oxidation, obtain Alpax low power grain size and detect sample, the volumetric concentration of described dilute nitric acid solution is 5% ~ 25%.First method provided by the invention utilizes volumetric concentration to be that the appropriate complexing corrosivity of the diluted hydrofluoric acid (HF) of 30% ~ 70% obtains the very thin metal fluoride layer of one deck, then utilizes hydrogen peroxide (H successively
2o
2), volumetric concentration is 5% ~ 25% dust technology (HNO
3) carry out the first oxidation and the second oxidation, the oxidisability of appropriateness is guaranteed to be easy to scrub black fluorinated film thin layer, thus clearly demonstrates the low power grain size of casting cocrystallized Al-Si alloy piston exemplar.
In order to further illustrate the present invention, below in conjunction with embodiment, the preparation method that Alpax low power grain size provided by the invention detects sample being described in detail, but they can not being interpreted as limiting the scope of the present invention.
Embodiment 1
In vent cabinet, be the dilute hydrofluoric acid solution of 50% by plastics drip nozzle volume aspirated concentration, drip on casting cocrystallized Al-Si alloy piston exemplar analysis face, and continuous plastic tweezer clamp degreasing cotton-wool evenly wipe erosion whole analysis face, after about 5 minutes, commercially available dioxygen water droplet is drawn on cocrystallized Al-Si alloy piston exemplar analysis face again with drip nozzle, and again clamp the whole analysis face of degreasing cotton-wool wiping erosion with tweezers, after about 1 minute, the casting cocrystallized Al-Si alloy piston exemplar obtained being positioned over volumetric concentration is dip about 1 minute in the dust technology pond of 10%, take out exemplar, in flowing water, wash away clean cocrystallized Al-Si alloy piston exemplar with hairbrush and analyze face, the testing sample of Alpax low power grain size is obtained after drying up.
Result as shown in Figure 1, Fig. 1 is the aluminium-silicon alloy piston low power grain size sample drawing that the embodiment of the present invention 1 obtains, can clearly be found out by Fig. 1, the testing sample that method provided by the invention obtains clearly can demonstrate the low power grain size of aluminium-silicon alloy piston sample surface.Result shows: crystal grain average area 1.2 square millimeters, belongs to three grades of grain sizes.
Embodiment 2
The low power grain size adopting the technical scheme of embodiment 1 to prepare casting cocrystallized Al-Si alloy piston exemplar detects sample, and the detection of low power grain size is carried out to the sample obtained, unlike, in the present embodiment, the volumetric concentration of dilute hydrofluoric acid solution is 40%, and after a hydrofluoric acid solution, the time of degreasing cotton-wool wiping is 2min, and after a hydrogen peroxide, the wiping time is 3min, the volumetric concentration of dust technology is 5%, and the time of soaking in dust technology pond is about 3min.
Result shows, and the testing sample that the present embodiment obtains can demonstrate the low power grain size of aluminium-silicon alloy piston exemplar clearly, and grain size testing result is: crystal grain average area 1.2 square millimeters, belongs to three grades of grain sizes.
Embodiment 3
The low power grain size adopting the technical scheme of embodiment 1 to prepare casting cocrystallized Al-Si alloy piston exemplar detects sample, and the detection of low power grain size is carried out to the sample obtained, unlike, in the present embodiment, the volumetric concentration of dilute hydrofluoric acid solution is 60%, and after a hydrofluoric acid solution, the time of degreasing cotton-wool wiping is 10min, and after a hydrogen peroxide, the wiping time is 2min, the volumetric concentration of dust technology is 15%, and the time of soaking in dust technology pond is about 5min.
Result shows, and the testing sample that the present embodiment obtains can demonstrate the low power grain size of aluminium-silicon alloy piston exemplar clearly, and grain size testing result is: crystal grain average area 1.2 square millimeters, belongs to three grades of grain sizes.
Comparative example 1
With the casting cocrystallized Al-Si alloy piston exemplar adopted in embodiment 1 for detected object, employing concentration is the sodium hydrate aqueous solution etch casting cocrystallized Al-Si alloy piston sample surface of 200g/L, and the etch time is 20min, obtains piston exemplar low power sample.
Result as shown in Figure 2, Fig. 2 is the aluminium-silicon alloy piston low power grain size sample drawing that comparative example 1 of the present invention obtains, as seen from Figure 2, the low power sample low power grain size display that this comparative example obtains is unintelligible, this is because sodium hydroxide solution is when carrying out etch to aluminium-silicon alloy piston sample surface, create the black oxide film of the densification that one deck is difficult to scrub, have impact on the display of low power grain size.
Comparative example 2
With the casting cocrystallized Al-Si alloy piston exemplar adopted in embodiment 1 for detected object, adopt the acid mixture etch casting cocrystallized Al-Si alloy piston sample surface that volumetric concentration is the hydrofluorite 5mL of 42% (V/V), the nitric acid 25mL of the hydrochloric acid 175mL and 68% (V/V) of 37% (V/V) forms, the etch time is 3min, obtains piston exemplar low power sample.
Result as shown in Figure 3, Fig. 3 is the aluminium-silicon alloy piston low power grain size sample drawing that comparative example 2 of the present invention obtains, as seen from Figure 3, the low power sample low power grain size display that this comparative example obtains is unintelligible, this is because dense hydrofluorite can react with the Alpax on surface, forms the metal fluoride layer that one deck is thicker and hard to tolerate; Although due to hydrochloric acid and the stronger complexing oxidisability of nitric acid, the difficulty of scrubbing of metal fluoride is made moderate progress, but due to its larger oxidisability, to the more difficult control of the etch of cocrystallized Al-Si alloy, etch depth degree is uneven, makes the display of low power grain size unintelligible.
As seen from the above embodiment, first method provided by the invention utilizes volumetric concentration to be that the appropriate complexing corrosivity of the diluted hydrofluoric acid (HF) of 30% ~ 70% obtains the very thin metal fluoride layer of one deck, then utilizes hydrogen peroxide (H successively
2o
2), volumetric concentration is 5% ~ 25% dust technology (HNO
3) carry out the first oxidation and the second oxidation, the oxidisability of appropriateness is guaranteed to be easy to scrub black fluorinated film thin layer, thus clearly demonstrates the low power grain size of casting cocrystallized Al-Si alloy piston exemplar.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. Alpax low power grain size detects a preparation method for sample, comprises the following steps:
Take dilute hydrofluoric acid solution as complexing mordant, complexing corrosion Alpax testing sample surface, the volumetric concentration of described dilute hydrofluoric acid solution is 30% ~ 70%;
Be the first oxygenant with hydrogen peroxide, the first oxidation is carried out to the Alpax testing sample surface after described complexing corrosion;
Be the second oxygenant with dilute nitric acid solution, carry out the second oxidation to the Alpax testing sample surface after described first oxidation, obtain Alpax low power grain size and detect sample, the volumetric concentration of described dilute nitric acid solution is 5% ~ 25%.
2. preparation method according to claim 1, is characterized in that, the volumetric concentration of described dilute hydrofluoric acid solution is 40% ~ 60%.
3. preparation method according to claim 1, is characterized in that, the time of described complexing corrosion is 2min ~ 10min.
4. the preparation method according to claims 1 to 3 any one, is characterized in that, described complexing corrosion is specially:
Described dilute hydrofluoric acid solution is coated on described Alpax testing sample surface, carries out complexing corrosion.
5. preparation method according to claim 1, is characterized in that, the time of described first oxidation is 1min ~ 5min.
6. preparation method according to claim 1 or 5, is characterized in that, described first oxidation is specially:
Described hydrogen peroxide is applied in the Alpax testing sample surface after described complexing corrosion, carries out the first oxidation.
7. preparation method according to claim 1, is characterized in that, the volumetric concentration of described dilute nitric acid solution is 10% ~ 20%.
8. preparation method according to claim 1, is characterized in that, described second oxidation time >=1min.
9. the preparation method according to claim 1,7 or 8, is characterized in that, described second oxidation is specially:
Alpax testing sample after described first oxidation is dipped in described dilute nitric acid solution, carries out the second oxidation.
10. preparation method according to claim 1, is characterized in that, also comprises washing after described second oxidation.
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