CN106498484A - A kind of electrolytic polishing method of complex brass - Google Patents
A kind of electrolytic polishing method of complex brass Download PDFInfo
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- CN106498484A CN106498484A CN201610936750.9A CN201610936750A CN106498484A CN 106498484 A CN106498484 A CN 106498484A CN 201610936750 A CN201610936750 A CN 201610936750A CN 106498484 A CN106498484 A CN 106498484A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
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Abstract
The present invention is a kind of electrolytic polishing method of complex brass.The method is comprised the following steps：（1）, after complex brass is ground, then mechanically polished；（2）, by mechanical polishing after complex brass make anode, lead makees negative electrode, electrobrightening 1 ~ 4V of DC voltage, 0.1 ~ 4A of electric current, and electrobrightening temperature is room temperature, and the electrobrightening time is 5 ~ 30S；Wherein, electrolytic polishing liquid consists of H3PO4, gelatin and oxalic acid, wherein, material proportion is every 30 70mlH3PO4In Jia 2 ~ 4g gelatin and 2 ~ 4g oxalic acid；H3PO4Concentration >=85%；（3）, by electrobrightening after complex brass take out, rinse post-drying well with absolute ethyl alcohol, that is, obtain product.The electrolytic polishing method of the present invention, not high to mechanical polishing quality requirement before electrobrightening, electrobrightening room temperature is operated；Electrobrightening formula of liquid is simple, nontoxic nonirritant；Not volatile, can preserve for a long time and Reusability.
Description
Technical field
The present invention relates to a kind of electrolytic polishing liquid and the electrolytic polishing method using the polishing fluid, more particularly to a kind of complicated
Brass electrolytic polishing liquid and the electrolytic polishing method using the electrolytic polishing liquid.
Background technology
Complex brass is to add, on the basis of copper zinc bianry alloy, the multicomponent alloy that the elements such as iron, manganese, silicon, aluminium are formed, its
There is intensity height, low coefficient of friction, good wearability and the features such as good processing forming, therefore equipment manufacturing, mechanical fitting and
The aspects such as automobile synchronizer tooth ring preparation are widely used.In complex brass structure observation, polishing is for observed result
There is crucial effect.The purpose of polishing is burr, the cut for removing metallographic specimen surface, makes metallographic surfacing.At present
Complex brass polishing common method is mechanical polishing, but, due to the design feature of complex brass, its mechanical polishing efficiency
Low, working strength is big, and quality is unstable.
The characteristics of electrobrightening be process after metal surface there is no scratch, deformable metal bits or the embedded metal surface of abrasive material
The problems such as, and for mechanical polishing, electrobrightening can make metal surface that there is satisfactory flatness, sample preparation efficiency
Height, effect are good, easy to operate, have good development space and application prospect.At present, the electrobrightening technology of copper alloy is obtained
Certain develop, for example, the method that discloses a kind of simple brass of electrobrightening in prior art is characterized in that it is using following
The polishing fluid of component：50～100ml of phosphoric acid, 30～50ml of sulfuric acid, 20～50ml of water, 3～5g of gelatin.Although it is to simple brass
Have preferable polishing effect, but, with the electrolyte to complex brass polish, complex brass surface easily occur cut or/and
Excessive erosion phenomenon.
Content of the invention：
The technical problem to be solved in the present invention is to mechanically polish that quality is unstable, efficiency during complex brass metallographic sample preparation
Low and existing electrolytic polishing method can make complex brass produce excessive erosion, so as to provide a kind of complex brass electrolytic polishing method.
The method electrolytic polishing liquid does not contain chromium ion, environmentally friendly；Electropolishing liquid prepares simple, nontoxic nonirritant gas
Taste, safe operation；Electrolytic polishing liquid is not volatile, can preserve for a long time and Reusability；By complicated to completing mechanical polishing
Brass sample electrobrightening, can obtain preferable polishing effect, clearly manifest the metallographic structure of complex brass.
The technical scheme is that：
A kind of electrolytic polishing method of complex brass, comprises the following steps：
(1), after, ground complex brass with 400#, 800#, 1500#, 2500# and 5000# sand paper successively, entered with antiscuffing paste
Row mechanical polishing；Described antiscuffing paste is≤Al of 1 μ2O3；
(2), by mechanical polishing after complex brass make anode, lead makees negative electrode, electrobrightening 1～4V of DC voltage, electricity
0.1～4A of stream, electrobrightening temperature are room temperature, and the electrobrightening time is 5～30S；
Wherein, electrolytic polishing liquid consists of H3PO4, gelatin and oxalic acid, wherein, material proportion is every 30-70mlH3PO4
In Jia 2～4g gelatin and 2～4g oxalic acid；H3PO4Concentration >=85%；
(3), by electrobrightening after complex brass take out, rinse post-drying well with absolute ethyl alcohol, that is, obtain product.
Described complex brass is complicated manganese brass or complex al-brass.
The content of described complicated manganese brass be 30～35%Zn, 0.1～0.5%Pb, 1.0～3.0%Mn, 0.1～
2.0%Si, 0.01～0.5%Sn, 0.1～1.0%Fe, 0.5～3.0%Al, 0.01～0.5%Ni, balance of Cu.
Described complex al-brass into being grouped into 20～25%Zn, 0.1～1.0%Pb, 1.0～4.0%Mn ,≤
0.2%Si, 0.1～0.5%Sn, 1.0～3.0%Fe, 3.0～9.0%Al, 0.1～1.0%Ni, balance of Cu.
The compound method of described electrolytic polishing liquid：According to adding 2～4g's of 2～4g of gelatin and oxalic acid per 30～70ml phosphoric acid
Proportioning, under room temperature is added to phosphoric acid, oxalic acid and gelatin in container, and stirs in 60 DEG C of constant temperature and all dissolve to gelatin, oxalic acid.
The present invention substantive distinguishing features be：
In prior art, complex brass polishing is more using mechanical polishing, and its polishing efficiency is low, and polishing effect is general, especially
It is that the cut and antiscuffing paste of mechanical polishing are embedded in phenomenon and have a strong impact on gold in AG observation by light microscope and electron microscopic observation
Phase photographic quality.And in existing electrolytic polishing process, it is not exclusively used in the electrobrightening side of complicated manganese brass and complex al-brass
Method.Therefore, the present invention proposes a kind of electrolytic polishing method, coordinates the polishing fluid provided in text, to complicated manganese brass and complex aluminium
Brass, by electrobrightening, can obtain the good complex brass metallographic specimen of polishing effect, and the sample is applied to complex brass
Fabric analysis, particularly AG light microscope and electron microscope observation.The step of this electrolytic polishing method most critical
Suddenly it is the preparation and the control of electrolytic parameter of electrolytic polishing liquid.Rational electrolytic polishing liquid and electrolytic parameter collocation, can make multiple
On ash metal metallographic specimen, at microcosmic hill, dissolution velocity, more than pocket dissolution velocity, as a result makes metallographic surfacing.In this
Between to also have a key link be exactly for the control of electrobrightening parameter, to be disappeared with reaching the mechanical mark of mechanical polishing residual
Remove and be unlikely to produce excessive erosion.
Beneficial effects of the present invention are using mechanical polishing+electrolytic polishing process, coordinate electrolytic polishing liquid, yellow to complicated manganese
Copper, complex al-brass have preferable polishing effect.General structure observation is applied to by metallographic specimen prepared by the present invention, special
Shi Yongyu not AG observation by light microscope and electron microscope observation.Simultaneously as clearly showing through the electrobrightening
Complex brass microscopic structure, facilitates statistics, the analysis of phase transition process disperse educt phase.Wherein, electrolytic polishing liquid of the invention is matched somebody with somebody
Side is simple, nontoxic nonirritant；Not volatile, can preserve for a long time and Reusability；The electrolytic polishing method of the present invention, to electrolysis
Before polishing, mechanical polishing quality requirement is not high, and electrobrightening room temperature is operated, and largely reduces experimental work intensity.
Description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the as cast condition complex al-brass metallographic structure obtained according to the embodiment of the present invention 1, amplifies 500 times；
Fig. 2 is the normalizing state complex al-brass metallographic structure obtained according to the embodiment of the present invention 2, amplifies 500 times；
Fig. 3 is the as cast condition complexity manganese brass metallographic structure obtained according to the embodiment of the present invention 3, amplifies 500 times；
Fig. 4 is the normalizing state complexity manganese brass metallographic structure obtained according to the embodiment of the present invention 4, amplifies 500 times；
Fig. 5 is the along with the furnace cooling complexity manganese brass metallographic structure obtained according to the embodiment of the present invention 5, amplifies 500 times；
Fig. 6 is the as cast condition complexity manganese brass metallographic structure obtained according to the embodiment of the present invention 6, amplifies 1000 times；
Fig. 7 is the normalizing state complexity manganese brass metallographic structure obtained according to the embodiment of the present invention 7, amplifies 500 times；
Fig. 8 is rapid cooling complexity manganese brass metallographic structure after the solid solution obtained according to the embodiment of the present invention 8, amplifies 200 times；
Fig. 9 is rapid cooling complexity manganese brass metallographic structure after the solid solution obtained according to the embodiment of the present invention 9, amplifies 500 times；
Figure 10 obtains as cast condition complex al-brass metallographic structure for comparative example 1, amplifies 500 times；
Figure 11 obtains as cast condition complexity manganese brass metallographic structure for comparative example 2, amplifies 500 times；
Figure 12 obtains as cast condition complexity manganese brass metallographic structure for comparative example 3, amplifies 500 times；
Figure 13 obtains as cast condition complexity manganese brass metallographic structure for comparative example 4, amplifies 500 times；
Figure 14 obtains as cast condition complex al-brass metallographic structure for comparative example 5, amplifies 500 times.
Specific embodiment
Hereinafter, the complex brass electrolytic polishing method that invention will be described in conjunction with exemplary embodiments.
The electrolytic polishing method of complex brass according to an exemplary embodiment of the present invention is comprised the following steps：
A, grind away
When preparing metallographic sample, it is necessary first to grind away process is carried out to sample, to reduce specimen surface roughness, mitigate examination
The polishing scratch on sample surface and Surface Machining deformation layer, are that further polishing is prepared.According to the present invention, the process of grind away can be by one
As grind away process carry out, such as according to 400#, 800#, 1500#, 2500#, 5000# from coarse to fine sand paper order carry out,
When changing sand paper, the cut direction strict conformance that ground in confirmation together, and without hiding after cut under surface scratch, the mill of sample
Pi/2 should be changed in direction processed, and constantly observe specimen surface grinding state；
B, polishing
The purpose of polishing is to remove trickle polishing scratch and the surface deformation later that abradant surface is stayed by fine grinding, makes abradant surface become nothing
The smooth mirror surface of cut.According to the present invention, the process of polishing is carried out according to general polishing process, for example, using short flannel
Woollen goods cloth and polishes lubricant for water as polishing cloth material using aluminum oxide antiscuffing paste, and polishing disk rotating speed is controlled to 260
～300r/min, directly uses most thin antiscuffing paste, and keeps sample direction constant in polishing, meanwhile, more arrive the polishing later stage
Firmly lighter, until polished surface is bright and clean, and till visually observing less than obvious cut；
C, electrobrightening
The present invention to mechanical polishing after sample adopt electrobrightening, and electrobrightening is carried out at room temperature.First
Mechanical polishing sample is cleaned up, electrolytic polishing liquid after being completely dried, is put into.Complex brass as anode and as negative electrode
Lead 10～30mm of distance, take out after the 5～30S that is powered, with washes of absolute alcohol and dry up.Wherein, electrolytic polishing liquid is
H3PO430～70ml, 2～4g of gelatin, 2～4g of oxalic acid, 1～5V of operating voltage, 0.1～5A of operating current.
Its metallographic structure is examined under a microscope by completing the sample after above-mentioned process.
Describe the exemplary embodiment of the present invention below by way of instantiation in detail.
Embodiment 1：
1st, the sample that chooses is as cast condition complex al-brass, and chemical composition (mass percent) is：64.76%Cu, 22.27%
Zn, 1.92%Fe, 7.49%Al, 2.51%Mn, 0.22%Pb, 0.52%Ni；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Polishing
Cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：By 50ml phosphoric acid, (weight/mass percentage composition >=85%- following examples and comparative example are also this
Concentration), 2g gelatin and 2g oxalic acid is well mixed.Afterwards to complete the sample for mechanically polishing as anode, with lead as negative electrode, electric current
0.26A, voltage 2.0V, time 15S.After the completion of electrobrightening, sample is taken out, with washes of absolute alcohol, after being dried up with secondary blower fan
Observed；
5th, sample metallographic, metallographic structure such as Fig. 1 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Embodiment 2：
1st, the sample that chooses is normalizing state complex al-brass, and chemical composition (mass percent) is：64.76%Cu,
22.27%Zn, 1.92%Fe, 7.49%Al, 2.51%Mn, 0.22%Pb, 0.52%Ni；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：50ml phosphoric acid, 2g gelatin and 2g oxalic acid are well mixed.Afterwards with complete mechanically polish examination
Sample is anode, with lead as negative electrode, electric current 0.30A, voltage 2.0V, time 15S.After the completion of electrobrightening, sample is taken out, with nothing
Water-ethanol is cleaned, and is observed after being dried up with secondary blower fan；
5th, sample metallographic, metallographic structure such as Fig. 2 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Embodiment 3：
1st, the sample that chooses is that as cast condition complexity manganese brass, chemical composition (mass percent) are：60.28%Cu, 33.3%
Zn, 0.29%Fe, 2.09%Al, 1.96%Mn, 1.05%Si, 0.43%Pb；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：50ml phosphoric acid, 2g gelatin and 2g oxalic acid are well mixed.Afterwards with complete mechanically polish examination
Sample is anode, with lead as negative electrode, electric current 0.26A, voltage 2.5V, time 15S.After the completion of electrobrightening, sample is taken out, with nothing
Water-ethanol is cleaned, and is observed after being dried up with secondary blower fan.
5th, sample metallographic, metallographic structure such as Fig. 3 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Embodiment 4：
1st, the sample that chooses is that normalizing state complexity manganese brass, chemical composition (mass percent) are：60.28%Cu,
33.3%Zn, 0.29%Fe, 2.09%Al, 1.96%Mn, 1.05%Si, 0.43%Pb；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：50ml phosphoric acid, 2g gelatin and 2g oxalic acid are well mixed.Afterwards with complete mechanically polish examination
Sample is anode, with lead as negative electrode, electric current 0.26A, voltage 2.0V, time 20S.After the completion of electrobrightening, sample is taken out, with nothing
Water-ethanol is cleaned, and is observed after being dried up with secondary blower fan.
5th, sample metallographic, metallographic structure such as Fig. 4 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Embodiment 5：
1st, the sample that chooses is that along with the furnace cooling complexity manganese brass, chemical composition (mass percent) are：60.28%Cu,
33.3%Zn, 0.29%Fe, 2.09%Al, 1.96%Mn, 1.05%Si, 0.43%Pb；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：50ml phosphoric acid, 2g gelatin and 2g oxalic acid are well mixed.Afterwards with complete mechanically polish examination
Sample is anode, with lead as negative electrode, electric current 0.30A, voltage 2.5V, time 18S.After the completion of electrobrightening, sample is taken out, with nothing
Water-ethanol is cleaned, and is observed after being dried up with secondary blower fan.
5th, sample metallographic, metallographic structure such as Fig. 5 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Embodiment 6：
1st, the sample that chooses is that as cast condition complexity manganese brass, chemical composition (mass percent) are：61.27%Cu, 34.43%
Zn, 0.34%Fe, 1.09%Al, 1.5%Mn, 0.62%Si, 0.32%Pb, 0.2%Ni；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：50ml phosphoric acid, 2g gelatin and 2g oxalic acid are well mixed.Afterwards with complete mechanically polish examination
Sample is anode, with lead as negative electrode, electric current 0.18A, voltage 2.0V, time 15S.After the completion of electrobrightening, sample is taken out, with nothing
Water-ethanol is cleaned, and is observed after being dried up with secondary blower fan；
5th, sample metallographic, metallographic structure such as Fig. 6 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Embodiment 7：
1st, the sample that chooses is that normalizing state complexity manganese brass, chemical composition (mass percent) are：61.27%Cu,
34.43%Zn, 0.34%Fe, 1.09%Al, 1.5%Mn, 0.62%Si, 0.32%Pb, 0.2%Ni；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：60ml phosphoric acid, 2g gelatin and 2g oxalic acid are well mixed.Afterwards with complete mechanically polish examination
Sample is anode, with lead as negative electrode, electric current 0.26A, voltage 2.0V, time 15S.After the completion of electrobrightening, sample is taken out, with nothing
Water-ethanol is cleaned, and is observed after being dried up with secondary blower fan；
5th, sample metallographic, metallographic structure such as Fig. 7 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Embodiment 8：
1st, the sample that chooses is that solution treatment complexity manganese brass, chemical composition (mass percent) are：61.27%Cu,
34.43%Zn, 0.34%Fe, 1.09%Al, 1.5%Mn, 0.62%Si, 0.32%Pb, 0.2%Ni；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：50ml phosphoric acid, 3g gelatin and 2g oxalic acid are well mixed.Afterwards with complete mechanically polish examination
Sample is anode, with lead as negative electrode, electric current 0.26A, voltage 2.0V, time 15S.After the completion of electrobrightening, sample is taken out, with nothing
Water-ethanol is cleaned, and is observed after being dried up with secondary blower fan；
5th, sample metallographic, metallographic structure such as Fig. 8 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Embodiment 9：
1st, the sample that chooses is that solution treatment complexity manganese brass, chemical composition (mass percent) are：61.27%Cu,
34.43%Zn, 0.34%Fe, 1.09%Al, 1.5%Mn, 0.62%Si, 0.32%Pb, 0.2%Ni；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：50ml phosphoric acid, 2g gelatin and 3g oxalic acid are well mixed.Afterwards with complete mechanically polish examination
Sample is anode, with lead as negative electrode, electric current 0.26A, voltage 2.0V, time 15S.After the completion of electrobrightening, sample is taken out, with nothing
Water-ethanol is cleaned, and is observed after being dried up with secondary blower fan；
5th, sample metallographic, metallographic structure such as Fig. 9 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Comparative example 1：
1st, the sample that chooses is as cast condition complex al-brass, and chemical composition (mass percent) is：64.76%Cu, 22.27%
Zn, 1.92%Fe, 7.49%Al, 2.51%Mn, 0.22%Pb, 0.52%Ni；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, antiscuffing paste is carried out according to order from coarse to fine, and when antiscuffing paste is changed, pi/2 should be changed in the polishing direction of sample, and ensure to polish
The cut of supreme one antiscuffing paste on face.Meanwhile, more arrive the polishing later stage and exert oneself lighter, in polishing process, keep sample direction not
Become, prevent excessively to intersect cut；
4th, chemical corrosion liquid：FeCl3, HCl and absolute ethyl alcohol are pressed 1：4:20 ratios are well mixed.Rotten using the corrosive agent
Erosion is not into the complex brass sample of mechanical polishing.Washes of absolute alcohol metallographic specimen is used, is observed after being dried up with secondary blower fan；
5th, sample metallographic, metallographic structure such as Figure 10 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Comparative example 2：
1st, the sample that chooses is that as cast condition complexity manganese brass, chemical composition (mass percent) are：60.28%Cu, 33.3%
Zn, 0.29%Fe, 2.09%Al, 1.96%Mn, 1.05%Si, 0.43%Pb；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, antiscuffing paste is carried out according to order from coarse to fine, and when antiscuffing paste is changed, pi/2 should be changed in the polishing direction of sample, and ensure to polish
The cut of supreme one antiscuffing paste on face.Meanwhile, more arrive the polishing later stage and exert oneself lighter, in polishing process, keep sample direction not
Become, prevent excessively to intersect cut；
4th, sample metallographic, metallographic structure such as Figure 11 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Comparative example 3：
1st, the sample that chooses is that as cast condition complexity manganese brass, chemical composition (mass percent) are：61.27%Cu, 34.43%
Zn, 0.34%Fe, 1.09%Al, 1.5%Mn, 0.62%Si, 0.32%Pb, 0.2%Ni；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, antiscuffing paste is carried out according to order from coarse to fine, and when antiscuffing paste is changed, pi/2 should be changed in the polishing direction of sample, and ensure to polish
The cut of supreme one antiscuffing paste on face.Meanwhile, more arrive the polishing later stage and exert oneself lighter, in polishing process, keep sample direction not
Become, prevent excessively to intersect cut；
4th, sample metallographic, metallographic structure such as Figure 12 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Comparative example 4：
1st, the sample that chooses is that as cast condition complexity manganese brass, chemical composition (mass percent) are：61.27%Cu, 34.43%
Zn, 0.34%Fe, 1.09%Al, 1.5%Mn, 0.62%Si, 0.32%Pb, 0.2%Ni；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：Phosphoric acid 50ml, sulfuric acid 30ml, water 20ml, gelatin 2g.Afterwards with complete mechanically polish sample
For anode, with lead as negative electrode, electric current 0.6A, voltage 18V, time 15S.After the completion of electrobrightening, sample is taken out, anhydrous second is used
Alcohol is cleaned, and is observed after being dried up with secondary blower fan；
5th, sample metallographic, metallographic structure such as Figure 13 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
Comparative example 5：
1st, the sample that chooses is as cast condition complex al-brass, and chemical composition (mass percent) is：64.76%Cu, 22.27%
Zn, 1.92%Fe, 7.49%Al, 2.51%Mn, 0.22%Pb, 0.52%Ni；
2nd, metallographic specimen is ground according to the order of 400#, 800#, 1500#, 2500#, 5000# sand paper, is changed sand paper
When, sample grinds the polishing scratch that supreme one sand paper on pi/2, inspection face should be changed in direction, and lubricant is water；
3rd, mechanically polish according to general metallographic specimen polishing process, using short flannel woollen goods cloth, 0.3 μm of Al2O3Throw
Light cream and lubricant are water, and polishing disk rotating speed is 300r/min, is polished to the cut that surface is visible by naked eyes.Polishing process will be noted
Meaning, more arrive the polishing later stage and exerts oneself lighter, and in polishing process, holding sample direction is constant, prevents excessively to intersect cut；
4th, electrolytic polishing liquid：Phosphoric acid 50ml, sulfuric acid 30ml, water 20ml, gelatin 2g are well mixed.Afterwards completing mechanical throwing
The sample of light is anode, with lead as negative electrode, electric current 0.26A, voltage 2.0V, time 15S.After the completion of electrobrightening, examination is taken out
Sample, with washes of absolute alcohol, is observed after being dried up with secondary blower fan；
5th, sample metallographic, metallographic structure such as Figure 14 are observed using ZEISS AG metallographic microscope Axio Vert.A1.
As can be seen from the above embodiments, after the present invention, the good metallographic specimen of polishing effect can be obtained, convenient
The structure observation of complex brass and analysis, particularly AG light microscope and electron microscope observation.Meanwhile, higher gold
Phase quality meets disperse phase statistics in phase transition process analysis, analyzes for the requirement of metallograph quality.
In metallographic preparation process, sample is ground with compared with fine sandpaper such as 3000# or/and 5000# sand paper, it is possible to increase sample
Surface smoothness；During mechanical polishing, directly using small grain size (<1 μ) aluminum oxide/diamond polishing cream, the very short time just can be with
Reach the step to require, largely reduce the working strength of operating personnel in metallographic specimen preparation process, improve metallographic
Sample sample preparation efficiency；During electrobrightening, rational parameter is set, electric current, voltage, sample and cathode spacing quickly can be prepared
High-quality metallographic specimen.Comparative example 1 is that complex al-brass mechanical polishing+(corrosive liquid proportioning is for corrosion：FeCl3:HCl:Alcohol
=1：4：20) metallographic specimen after, it can be seen which is having obvious cut, that is, the corrosion after mechanically polishing compared with high magnification (500)
Link does not remove the tiny cut in mechanical polishing process completely.Comparative example 2,3 is the gold after complicated manganese brass mechanical polishing
Phase photo, its have obvious cut.Relative to above-mentioned comparative example, example 1-9 then can eliminate mechanical polishing institute by electrobrightening
The deformation layer and cut of cause, improves metallographic sample preparation quality.Comparative example 4,5 is the metallograph using existing electrolytic polishing liquid, by
Although figure is as can be seen that matrix flatness preferably, has obvious excessive erosion (comparative example 4), appearance " twin boundary " around the second phase
(comparative example 5, mark of the twin boundary for excessive erosion).Basic without cut on embodiment of the present invention matrix, without mistake around the second phase
Corrosion phenomenon, meanwhile, each tissue and phase structure is clearly shown, is the tissue point of applied statistics complicated software analysis brass
Analysis, particularly phase amount mutation analysis, the research of phase Precipitation Behavior provide greatly cheap.
Unaccomplished matter of the present invention is known technology.
Claims (4)
1. a kind of electrolytic polishing method of complex brass, it is characterized by the method is comprised the following steps：
（1）, after complex brass is ground with 400#, 800#, 1500#, 2500# and 5000# sand paper successively, machine is carried out with antiscuffing paste
Tool is polished；Described antiscuffing paste is≤Al of 1 μ2O3；
（2）, by mechanical polishing after complex brass make anode, lead makees negative electrode, electrobrightening 1 ~ 4V of DC voltage, electric current 0.1 ~
4A, electrobrightening temperature are room temperature, and the electrobrightening time is 5 ~ 30S；
Wherein, electrolytic polishing liquid consists of H3PO4, gelatin and oxalic acid, wherein, material proportion is every 30-70mlH3PO4In Jia 2 ~
4g gelatin and 2 ~ 4g oxalic acid；H3PO4Concentration >=85%；
（3）, by electrobrightening after complex brass take out, rinse post-drying well with absolute ethyl alcohol, that is, obtain product；
Described complex brass is complicated manganese brass or complex al-brass.
2. the electrolytic polishing method of complex brass as claimed in claim 1, it is characterized by the content of described complicated manganese brass
For 30 ~ 35%Zn, 0.1 ~ 0.5%Pb, 1.0 ~ 3.0%Mn, 0.1 ~ 2.0%Si, 0.01 ~ 0.5%Sn, 0.1 ~ 1.0%Fe, 0.5 ~ 3.0%
Al, 0.01 ~ 0.5%Ni, balance of Cu.
3. the electrolytic polishing method of complex brass as claimed in claim 1, it is characterized by the composition of described complex al-brass
20 ~ 25%Zn is consisted of, 0.1 ~ 1.0%Pb, 1.0 ~ 4.0%Mn ,≤0.2%Si, 0.1 ~ 0.5%Sn, 1.0 ~ 3.0%Fe, 3.0 ~ 9.0%
Al, 0.1 ~ 1.0%Ni, balance of Cu.
4. the electrolytic polishing method of complex brass as claimed in claim 1, it is characterized by the preparation of described electrolytic polishing liquid
Method：According to the proportioning for adding 2 ~ 4g of 2 ~ 4g of gelatin and oxalic acid per 30 ~ 70ml phosphoric acid, phosphoric acid, oxalic acid and gelatin are added under room temperature
To in container, and stir in 60 DEG C of constant temperature and all dissolve to gelatin, oxalic acid.
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