CN102443840B - Metallographic structure electrolytic solution, corrosion method of cobalt and display method of cobalt metallographic structure - Google Patents
Metallographic structure electrolytic solution, corrosion method of cobalt and display method of cobalt metallographic structure Download PDFInfo
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- CN102443840B CN102443840B CN201110396245.7A CN201110396245A CN102443840B CN 102443840 B CN102443840 B CN 102443840B CN 201110396245 A CN201110396245 A CN 201110396245A CN 102443840 B CN102443840 B CN 102443840B
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Abstract
The invention discloses a metallographic structure electrolytic solution, a corrosion method of cobalt or cobalt alloy and a display method of the cobalt or cobalt alloy metallographic structure. The display method of the cobalt or cobalt alloy metallographic structure comprises the following steps of: providing a cobalt or cobalt alloy target; grinding the cobalt or cobalt alloy target; mechanically polishing the ground cobalt or cobalt alloy target; and performing electroplishing on the cobalt or cobalt alloy target subjected to mechanical polishing in the metallographic structure electrolytic solution, wherein the metallographic structure electrolytic solution is a mixed solution of ethanol, normal butanol, water, nitric acid and hydrofluoric acid. The metallographic structure electrolytic solution prepared from the ethanol, the normal butanol, the water, the nitric acid and the hydrofluoric acid has a favorable corrosion effect on the cobalt or cobalt alloy; the crystal boundary display effect of the cobalt or cobalt alloy metallographic structure is improved; the potential safe hazards of the metallographic structure electrolytic solution are reduced; and meanwhile, raw materials are not limited by safety control of China.
Description
Technical field
The present invention relates to the caustic solution of metallographic structure electrolytic solution, cobalt or cobalt-base alloy and the display packing of metallographic structure thereof.
Background technology
The material properties such as the internal organizational structure of metallic substance and hardness, intensity, ductility have direct and close contacting, and metallographicobservation is the most directly effective means of research metallic substance internal organizational structure.Adopt quantitative metallography principle, by the measurements and calculations of the metallographic microstructure of two-dimentional metallographic specimen flour milling or film, determine the three-dimensional space pattern of the metallographic structure of sample, thereby set up the quantitative relationship between moiety, tissue and performance.Metallographic refers to that the chemical composition of metal or alloy and various composition are at physical condition and the chemical state of metal or alloy inside.
Carry out metallographicobservation and first will make the crystal boundary structure of metal show, then use the metallographic structure of metallography microscope sem observation metal.Crystal boundary is identical and the interface of orientation between different crystal, the namely contact surface of crystal grain and intergranule of structure.On crystal boundary face, atomic arrangement is transitioned into another orientation from an orientation, therefore the atomic arrangement of grain boundaries is in an interim state.
Take as the cobalt of target or the metallographicobservation of cobalt-base alloy is example, and in the prior art, general method is: from cobalt or cobalt-base alloy target, cut a part as sample; To the processing that comes to the surface of described sample, remove surperficial oxide compound; Described sample is placed in to the etching solution consisting of hydrochloric acid and hydrofluoric acid and carries out corrosion treatment; Take out described sample, clean and dry, utilize metaloscope to observe the metallographic structure of described sample, in addition, the display packing of metal or its alloy microstructure, the correlation technique content that can consult the Chinese patent application file of publication number CN1167839A.
If adopt be hydrochloric and a kind of etching solution hydrofluoric acid carries out corrosion treatment to the sample of described cobalt or cobalt-base alloy, cobalt or cobalt-base alloy corrosion speed are too fast on the one hand, etching time is difficult to control, success ratio is lower, Display of Grain Boundary effect is barely satisfactory, can not meet demand of industrial production far away, another aspect, the hyperoxia voltinism of the mixed solution that contains hydrochloric acid and hydrofluoric acid, highly corrosive and can generate the toxic gases such as chlorine when mixed solution reacts with target sample environment and the person are existed to very large potential safety hazard, and hydrochloric acid is again the starting material of manufacturing methamphetamine, be subject to nation's security management and control.
Therefore, how cobalt or cobalt-base alloy target are corroded, the corrosive fluid that How to choose is suitable, makes the corrosive effect of cobalt or cobalt-base alloy and Display of Grain Boundary respond well, and the potential safety hazard that can reduce metallographic structure electrolytic solution just seems very necessary.
Summary of the invention
The problem that the present invention solves is to provide a kind of metallographic structure electrolytic solution, cobalt or the caustic solution of cobalt-base alloy and the display packing of metallographic structure thereof, to improve the Display of Grain Boundary effect and the potential safety hazard that reduces metallographic structure electrolytic solution of cobalt or cobalt-base alloy metallographic structure, starting material are not in the scope of national security management and control simultaneously.
For addressing the above problem, the embodiment of the present invention provides a kind of metallographic structure electrolytic solution, and described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
Optionally, in described metallographic structure electrolytic solution, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33: (10～15): (10～15).
For addressing the above problem, the embodiment of the present invention also provides the caustic solution of a kind of cobalt or cobalt-base alloy, comprising:
Cobalt or cobalt-base alloy target are provided;
Described cobalt or cobalt-base alloy target are carried out to electropolishing in metallographic structure electrolytic solution, and described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
Optionally, in described metallographic structure electrolytic solution, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33: (10～15): (10～15).
Optionally, the time of described electropolishing is 10s～20s.
Optionally, the voltage of described electropolishing is 28V～35V.
For addressing the above problem, the embodiment of the present invention also provides the display packing of a kind of cobalt or cobalt-base alloy metallographic structure, comprising:
Cobalt or cobalt-base alloy target are provided;
Described cobalt or cobalt-base alloy target are polished;
Cobalt or cobalt-base alloy target after polishing are carried out to mechanical polishing;
Cobalt after mechanical polishing or cobalt-base alloy target are carried out to electropolishing in metallographic structure electrolytic solution, and described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
Optionally, in described metallographic structure electrolytic solution, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33: (10～15): (10～15).
Optionally, the time of described electropolishing is 10s～20s.
Optionally, the voltage of described electropolishing is 28V～35V.
Optionally, in described mechanical polishing process, use diamond paste to carry out mechanical polishing to described cobalt or cobalt-base alloy target.
Optionally, the wetting agent of described mechanical polishing is dehydrated alcohol.
Optionally, the sharpening machine rotating speed of described mechanical polishing is 400r/min～600r/min.
Optionally, the time of described mechanical polishing is 2min～3min.
Compared with prior art, the embodiment of the present invention adopts ethanol, propyl carbinol, water, the mixing solutions of nitric acid and hydrofluoric acid is metallographic structure electrolytic solution, and by cobalt or cobalt-base alloy electropolishing in this metallographic structure electrolytic solution, method in the embodiment of the present invention has good corrosive effect and display effect to cobalt or cobalt-base alloy, and compare with the method that existing hydrofluoric acid and nitric acid carry out chemical corrosion as etching reagent to cobalt or cobalt-base alloy target, with above-mentioned metallographic structure electrolytic solution, cobalt or cobalt-base alloy target are carried out to mechanical polishing smaller to operating personnel's Health hazard and environmental pollution, and starting material are not subject to nation's security management and control, it is more convenient to supply.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the caustic solution of one embodiment of the invention cobalt or cobalt-base alloy;
Fig. 2 is the schematic flow sheet of the display packing of one embodiment of the invention cobalt or cobalt-base alloy metallographic structure;
Fig. 3 is the schematic flow sheet of the display packing of another embodiment of the present invention cobalt or cobalt-base alloy metallographic structure.
Embodiment
First the present invention provides an embodiment of a metallographic structure electrolytic solution, above-mentioned metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid, and in described metallographic structure electrolytic solution, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33: (10～15): (10～15).The mass percent concentration of described ethanol is 99.7%; The mass percent concentration of described propyl carbinol is 96%; The mass percent concentration of described hydrofluoric acid is 39%～41%; The mass percent concentration of described nitric acid is 63%～65%.By cobalt or cobalt-base alloy, electropolishing in this metallographic structure electrolytic solution has good corrosive effect, can make the Display of Grain Boundary of metallographic structure of cobalt or cobalt-base alloy respond well, and also less to operating personnel's Health hazard and environmental pollution.
Metal and alloy are all polycrystal, that is to say, they are all comprised of crystal grain.Use metallographic structure electrolytic solution to corrode metal and alloy, can make the crystal boundary of metal and alloy grain display.
The present invention also provide a cobalt or cobalt-base alloy caustic solution embodiment as shown in Figure 1, comprising:
Step S11, provides cobalt or cobalt-base alloy target;
Step S12 carries out electropolishing by described cobalt or cobalt-base alloy target in metallographic structure electrolytic solution, and described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
Described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid, in described metallographic structure electrolytic solution, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33: (10～15): (10～15), and the mass percent concentration of described ethanol is 99.7%; The mass percent concentration of described propyl carbinol is 96%; The mass percent concentration of described hydrofluoric acid is 39%～41%; The mass percent concentration of described nitric acid is 63%～65%, and the time of described electropolishing is 10s～20s, and the voltage of described electropolishing is 28V～35V.
Concrete operating process can be with reference to the corrosion step of the embodiment in the display packing of the cobalt below the present invention or cobalt-base alloy metallographic structure.
Metal or alloy is carried out to metallographicobservation and be used for the microtexture of analyzing samples, it is mainly to study its weave construction by metallography microscope sem observation metal or alloy sample, such as size, shape and the orientation etc. of crystal grain.
In practical application in industry, metal or alloy is carried out before metallographicobservation, need first to metal or alloy sample polish, polishing and corrosion treatment so that its metallographic structure clear showing that be crystal boundary energy.The display packing of the cobalt of the embodiment of the present invention or cobalt-base alloy metallographic structure as shown in Figure 2, comprising:
Step S21, provides cobalt or cobalt-base alloy target;
Step S22 cuts a part as sample from described target;
Step S23, polishes to described cobalt or cobalt-base alloy sample;
Step S24, carries out mechanical polishing to cobalt or cobalt-base alloy sample after polishing;
Step S25 carries out electropolishing by the cobalt after mechanical polishing or cobalt-base alloy sample in metallographic structure electrolytic solution, and described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid;
Step S26, cleans described sample;
Step S27, utilizes metaloscope to observe described sample.
The display packing of 6N cobalt or cobalt-base alloy metallographic structure of take is below example, and the embodiment of 2 pairs of the invention described above is elaborated by reference to the accompanying drawings.
First perform step S21, cobalt or cobalt-base alloy target are provided.
In the present embodiment, the material of described target can be that purity is 99.9% or above cobalt or cobalt-base alloy.Be for example 3N5 (99.95%), 4N5 (99.995%) or 5N (99.999%).The shape of described target can be according to the actual requirement of applied environment, sputtering equipment, for example, be any in rectangle, circle, annular, taper shape or other analogous shapes (comprising regular shape and irregularly shaped).
Then perform step S22, from described target, cut a part as sample.
In the present embodiment, can adopt modes such as handsaw, sawing machine or cutting off machine from target, to cut a part as sample.The dimensioned area of described sample is 100mm
2, thickness is 10mm.In addition, which kind of no matter adopts cut method, all should note the temperature condition of described sample, use if desired water cooling, to avoid described sample because of overheated its tissue that changes.
Then perform step S23, described cobalt or cobalt-base alloy sample are polished.
The object that cobalt or cobalt-base alloy sample are polished is to remove the zone of oxidation of cobalt or cobalt-base alloy specimen surface, makes to carry out cobalt or the cobalt-base alloy specimen surface smooth of metallographicobservation, to guarantee follow-up corrosive effect.
In the present embodiment, it is mainly successively described cobalt or cobalt-base alloy sample to be polished with water-based sand paper from coarse to fine that cobalt or cobalt-base alloy sample are polished, and during polishing, with water, makees wetting agent.
Described target is carried out to grinding process.Described grinding process specifically comprises: using water as wetting agent, first use the surface (surface that needs observation) of flint paper (the present embodiment is 400# water-based sand paper) polishing cobalt or cobalt-base alloy sample, the polishing time can be generally 5min～10min; The surface (surface that needs observation) of then using slightly thick sand paper (the present embodiment is 800# water-based sand paper) polishing cobalt or cobalt-base alloy sample, the polishing time can be generally 5min～10min; Finally use fine sandpaper (the present embodiment is 1500# water-based sand paper) to continue the surface (surface that needs observation) of polishing cobalt or cobalt-base alloy sample, the polishing time can be generally 5min～10min, can obtain like this flour milling of smooth.
When polishing, water-based sand paper is driven by sharpening machine, and sharpening machine top has water ceaselessly to flow on sand paper and soak, and pins cobalt or cobalt-base alloy sample (surface of observing with needs is towards sand paper) and grinds on sand paper.After changing sand paper, described target is rotated to 90 degree, until the cut of a upper procedure is ground off, new cut direction is consistent at every turn, and must described target be cleaned up water before changing sand paper at every turn, to remove sand grains.
In other embodiments, also can use alcohol as the wetting agent of grinding process.
Then perform step S24, cobalt or cobalt-base alloy sample after polishing are carried out to mechanical polishing.
The object that cobalt or cobalt-base alloy sample are carried out to mechanical polishing is to remove the polishing scratch that polishing cobalt or cobalt-base alloy sample produce, and the cobalt or the cobalt-base alloy specimen surface that make to carry out metallographicobservation are more smooth, further guarantee follow-up corrosive effect.
In the present embodiment, it is mainly, with diamond paste, described cobalt or cobalt-base alloy target are carried out to mechanical polishing that cobalt or cobalt-base alloy target are carried out to polishing, during mechanical polishing, with dehydrated alcohol (alcohol), makees wetting agent.
Specifically, diamond paste is spread upon on flannelette, flannelette is driven by sharpening machine, and sharpening machine top has dehydrated alcohol ceaselessly to flow on flannelette and soak, and pins cobalt or cobalt-base alloy sample (surface of observing with needs is towards flannelette) polishing on flannelette.In the present embodiment, sharpening machine rotating speed can be 400r/min～600r/min, and the time of mechanical polishing is generally 2min～3min.If the time of mechanical polishing is less than 2min, the sample after polishing is bright not clear, affect display packing and the observations of metallographic structure, the time of mechanical polishing is longer, the smooth finish of specimen surface is better, but consider the working efficiency of mechanical polishing, the present embodiment is no more than 3min to the mechanical polishing time of described sample and is advisable.After mechanical polishing, with a large amount of water, cobalt or cobalt-base alloy sample wash is clean.
It should be noted that, the common water of mechanical polishing of traditional cobalt or cobalt-base alloy sample is cooked wetting agent, but contriver finds, with dehydrated alcohol (alcohol), can reduce the surface tension of cobalt or cobalt-base alloy sample, make dehydrated alcohol (alcohol) can be evenly distributed on the surface of cobalt or cobalt-base alloy sample, thereby improved the polishing effect of cobalt or cobalt-base alloy specimen surface.Therefore, in the present embodiment preferably dehydrated alcohol (alcohol) as wetting agent.
By the surface treatment of above-mentioned steps S23 and S24, remove the oxide compound of described specimen surface, form at least one polished surface.
Then perform step S25, cobalt after mechanical polishing or cobalt-base alloy sample are carried out to electropolishing in metallographic structure electrolytic solution, described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid, and wherein the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33: (10～15): (10～15).
Metallographic structure electrolytic solution usually occurs in crystal boundary to corrosion of metal, and the intersection of each crystal grain, therefore can separate each die region.In above-mentioned metallographic structure electrolytic solution, nitric acid and hydrofluoric acid have strong corrodibility to metals such as cobalt or cobalt-base alloys, can react with cobalt or cobalt-base alloy; The corrodibility and the oxidisability that in metallographic structure electrolytic solution, contain ethanol, propyl carbinol are low.
Specifically, in described metallographic structure electrolytic solution, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33: (10～15): (10～15).Described ethanol, propyl carbinol are analytical pure solution, and the mass percent concentration of described ethanol is 99.7%; The mass percent concentration of described propyl carbinol is 96%; The mass percent concentration of described nitric acid is 63%～65%, and the mass percent concentration of described hydrofluoric acid is 39%～41%, and the metallographic structure electrolytic solution preparing is packed on electropolisher,, then cobalt or cobalt-base alloy sample is carried out to electropolishing at normal temperatures.
In the present embodiment, electropolishing is that to take cobalt or cobalt-base alloy sample be anode, and the metal that is insoluble to metallographic structure electrolytic solution is negative electrode, and the two poles of the earth are immersed in electrolyzer simultaneously, pass to direct current and produce selectively anode dissolution.
While being specially electropolishing, cobalt or the cobalt-base alloy specimen surface high consistence mucous membrane of rate that can have a resistance during energising, its thickness is inhomogeneous at cobalt or cobalt-base alloy specimen surface.Surface microscopic convex part is thinner, and current density is larger, and dissolving metal is very fast; Under surface microscopic, recess is thicker, and current density is less, and dissolving metal is slower.Due to the ununiformity of consistence mucous membrane and electric current distribution, microscopic protrusions portion size reduces very fast, and under microcosmic, recess size reduces slowlyer, cobalt or cobalt-base alloy specimen surface roughness is reduced, thereby reach the object of anode dissolution.
In the present embodiment, carry out at normal temperatures electropolishing operation, the time of described electropolishing is that etching time is generally 10s～20s, is preferably 10s.If the time of electropolishing is less than 10s, cobalt or the corrosion of cobalt-base alloy sample are not enough, just cannot demonstrate crystal boundary; If the time of electropolishing is greater than 20s, cobalt or cobalt-base alloy sample are understood excessive corrosion, and the crystal boundary of cobalt or cobalt-base alloy sample and crystal grain all can be destroyed, and target is easily oxidized.
The voltage of electropolishing described in the present embodiment is 28V～35V, is preferably 30V.If the voltage of electropolishing is less than 28V, the electric current of electropolishing is too little, and the speed of electropolishing is too slow, easily causes cobalt or the corrosion of cobalt-base alloy sample not enough, cannot demonstrate crystal boundary; If the voltage of electropolishing is greater than 35V, the electric current of electropolishing is too large, and the speed of electropolishing is too fast, easily causes cobalt or the meeting of cobalt-base alloy specimen surface uneven, and excessive corrosion, crystal boundary and the crystal grain of corresponding cobalt or cobalt-base alloy sample all can be destroyed.
Then perform step S26, clean described sample.
After corrosion, in the present embodiment, take out cobalt or cobalt-base alloy sample immediately with clear water to erosional surface clean, scavenging period is 1min～2min.It should be noted that, the present embodiment can clean all faces of cobalt or cobalt-base alloy sample, and the surface that also can need to observe cobalt or cobalt-base alloy sample is cleaned.
Then dry up the described sample after cleaning.
Step S27, utilizes metaloscope to observe described sample.
In the present embodiment, owing to passing through above steps, particularly the corrosion treatment in step S25 can be so that the metallographic structure of described sample has good display effect, and recycling metaloscope just can be observed well, is conducive to the metallographic structure of described sample to carry out correct analysis.
Below an alternative embodiment of the invention is described.A upper embodiment cuts a part as sample using cobalt or cobalt-base alloy target, polishes, polishing, burn into cleans and observe and process, and whole treating processes is that the sample of cobalt or cobalt-base alloy target is processed.An alternative embodiment of the invention and a upper routine difference are that cobalt or cobalt-base alloy target full-page proof are processed, and the metallographic structure of large-scale cobalt or cobalt-base alloy target are shown.Fig. 3 is the cobalt of another embodiment of the present invention or the method for displaying metallographic structure of cobalt-base alloy, specifically as shown in Figure 3, comprising:
Step S31, provides cobalt or cobalt-base alloy target;
Step S32, polishes to described cobalt or cobalt-base alloy target;
Step S33, carries out mechanical polishing to cobalt or cobalt-base alloy target after polishing;
Step S34 carries out electropolishing by the cobalt after mechanical polishing or cobalt-base alloy target in metallographic structure electrolytic solution, and described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid;
Step S35, cleans described target;
Step S36, utilizes metaloscope to observe described target.
First perform step S31, cobalt or cobalt-base alloy target are provided.In the present embodiment, specifically can be with reference to a upper embodiment.
Then perform step S32, described cobalt or cobalt-base alloy target are polished.
The object that cobalt or cobalt-base alloy target are polished is to remove the zone of oxidation of cobalt or cobalt-base alloy target material surface, makes to carry out cobalt or the cobalt-base alloy target material surface smooth of metallographicobservation, to guarantee follow-up corrosive effect.
In the present embodiment, it is mainly successively described cobalt or cobalt-base alloy target to be polished with water-based sand paper from coarse to fine that cobalt or cobalt-base alloy target are polished, and during polishing, with water, makees wetting agent.
When to large-scale cobalt or cobalt-base alloy polishing, adopt the method for hand sand, with Portable grinder, cobalt or cobalt-base alloy target (surface of observing with needs is towards sand paper) are polished.Can water in bruting process or alcohol as the wetting agent of grinding process.Concrete operations can be with reference to a upper embodiment.
Then perform step S33, cobalt or cobalt-base alloy target after polishing are carried out to mechanical polishing.
The object that cobalt or cobalt-base alloy target are carried out to mechanical polishing is to remove the polishing scratch that polishing cobalt or cobalt-base alloy target produce, and the cobalt or the cobalt-base alloy target material surface that make to carry out metallographicobservation are more smooth, further guarantee follow-up corrosive effect.Specific operation process can be with reference to a upper embodiment.
By the surface treatment of above-mentioned steps S32 and S33, remove the oxide compound of described target material surface, form at least one polished surface.
Then perform step S34, the cobalt after mechanical polishing or cobalt-base alloy target are carried out to electropolishing in metallographic structure electrolytic solution, described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
When being carried out to electropolishing, large-scale cobalt or cobalt-base alloy target adopt portable electrolysis polishing machine to carry out electropolishing to cobalt or cobalt-base alloy target material surface (surface that need to observe).Metallographic structure electrolytic solution and electropolishing specifically can be with reference to upper embodiment.
Then perform step S35, clean described target.
After electropolishing, in the present embodiment, take out cobalt or cobalt-base alloy target and with clear water, erosional surface is cleaned immediately, concrete operations can be with reference to a upper embodiment.
It should be noted that, the present embodiment can clean all faces of cobalt or cobalt-base alloy target, and the surface that also can need to observe cobalt or cobalt-base alloy target is cleaned.
Then dry up the described target after cleaning.
Then perform step S36, utilize metaloscope to observe described target.
In the present embodiment, owing to passing through above steps, particularly the processing of the electropolishing in step S34 can be so that the metallographic structure of described target has good display effect, recycling metaloscope just can be observed well, is conducive to the metallographic structure of described target to carry out correct analysis.
In sum, technique scheme adopts ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid to be mixed with metallographic structure electrolytic solution, the volume ratio of described ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33: (10～15): (10～15), and the mass percent concentration of described nitric acid is 63%～65%; The mass percent concentration of described hydrofluoric acid is 39%～41%; Described ethanol, propyl carbinol are analytical pure concentration, and the mass percent concentration of described ethanol is 99.7%; The mass percent concentration of described propyl carbinol is 96%, and it has good corrosive effect to cobalt or cobalt-base alloy, also less to operating personnel's Health hazard and environmental pollution, and meanwhile, the starting material such as hydrofluoric acid and nitric acid are not in the scope of national security management and control.
In addition, technique scheme, when cobalt or cobalt-base alloy target are carried out to mechanical polishing, does with dehydrated alcohol the polishing effect that wetting agent can improve target material surface; When cobalt or cobalt-base alloy target are carried out to etching pit, adopt the method for electropolishing, the time of electropolishing and the voltage of electropolishing are moderate, can improve the corrosive effect of target material surface.Therefore, technique scheme has process stabilizing, and controllability is strong, is difficult for the advantages such as excessive corrosion or deficiency.
The above, be only preferred embodiment of the present invention, not the present invention done to any pro forma restriction.Any those of ordinary skill in the art, do not departing from technical solution of the present invention scope situation, all can utilize method and the technology contents of above-mentioned announcement to make many possible changes and modification to technical solution of the present invention, or be revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not depart from technical scheme of the present invention,, all still belongs in the scope of technical solution of the present invention protection any simple modification made for any of the above embodiments, equivalent variations and modification according to technical spirit of the present invention.
Claims (9)
1. a caustic solution for cobalt or cobalt-base alloy, is characterized in that, comprising: cobalt or cobalt-base alloy target are provided; Described cobalt or cobalt-base alloy target are carried out to electropolishing in metallographic structure electrolytic solution, and described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
2. the caustic solution of cobalt as claimed in claim 1 or cobalt-base alloy, is characterized in that, in described metallographic structure electrolytic solution, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66:11:33:(10～15): (10～15).
3. the caustic solution of cobalt as claimed in claim 1 or cobalt-base alloy, is characterized in that, the time of described electropolishing is 10s～20s.
4. the caustic solution of cobalt as claimed in claim 1 or cobalt-base alloy, is characterized in that, the voltage of described electropolishing is 28V～35V.
5. a display packing for cobalt or cobalt-base alloy metallographic structure, is characterized in that, comprising:
Cobalt or cobalt-base alloy target are provided;
Described cobalt or cobalt-base alloy target are polished;
Cobalt or cobalt-base alloy target after polishing are carried out to mechanical polishing;
Cobalt after mechanical polishing or cobalt-base alloy target are carried out to electropolishing in metallographic structure electrolytic solution, described metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid, in described metallographic structure electrolytic solution, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66:11:33:(10～15): (10～15), the time of described electropolishing is 10s～20s, and the voltage of described electropolishing is 28V～35V.
6. the display packing of cobalt as claimed in claim 5 or cobalt-base alloy metallographic structure, is characterized in that, described mechanical polishing process is used diamond paste to carry out mechanical polishing to described cobalt or cobalt-base alloy target.
7. the display packing of cobalt as claimed in claim 6 or cobalt-base alloy metallographic structure, is characterized in that, the wetting agent of described mechanical polishing is dehydrated alcohol.
8. the display packing of cobalt as claimed in claim 6 or cobalt-base alloy metallographic structure, is characterized in that, the sharpening machine rotating speed of described mechanical polishing is 400r/min～600r/min.
9. the display packing of cobalt as claimed in claim 6 or cobalt-base alloy metallographic structure, is characterized in that, the time of described mechanical polishing is 2min～3min.
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| CN103913416A (en) * | 2012-12-31 | 2014-07-09 | 宁波江丰电子材料有限公司 | Target material detection method |
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