CN102443840A - 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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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
Material properties such as the internal organizational structure of metallic substance and hardness, intensity, ductility have direct and close getting in touch, and metallographicobservation then is the most directly effective means of research metallic substance internal organizational structure.Adopt the quantitative metallography principle, confirm the three-dimensional space pattern of the metallographic structure of sample by the measurements and calculations of the metallographic microstructure of two-dimentional metallographic specimen flour milling or film, thereby set up the quantitative relationship between moity, tissue and performance.Metallographic is meant that chemical ingredients and the various composition of metal or alloy are at metal or alloy internal physical state and chemical state.
Carry out metallographicobservation the crystal boundary structure of metal is shown, use the metallographic structure of metallography microscope sem observation metal then.Crystal boundary is identical and the interface of orientation between the different crystal, the just contact surface of crystal grain and intergranule of structure.On the crystal boundary face, atomic arrangement carries out the transition to another orientation from an orientation, and the atomic arrangement of Gu Jingjiechu is in an interim state.
To be example as the cobalt of target or the metallographicobservation of cobalt-base alloy, in the prior art, general method is: from cobalt or cobalt-base alloy target, cut a part as sample; Said sample is done to come to the surface processing, remove the oxide compound on surface; Place the etching solution that constitutes by hydrochloric acid and hydrofluoric acid to carry out corrosion treatment on said sample; Take out said sample; Clean and oven dry, utilize metaloscope that the metallographic structure of said sample is observed, in addition; The display packing of relevant metal or its alloy metallographic structure, the correlation technique content that can consult the one Chinese patent application file of publication number CN1167839A.
If what adopt is that a kind of etching solution of hydrochloric and hydrofluoric acid carries out corrosion treatment to the sample of said cobalt or cobalt-base alloy; Cobalt or cobalt-base alloy corrosion speed are too fast on the one hand, and etching time is difficult to control, and success ratio is lower; The Display of Grain Boundary effect is barely satisfactory; Can not satisfy the industrial production requirement far away, another aspect contains the hyperoxia voltinism, highly corrosive of the mixed solution of hydrochloric acid and hydrofluoric acid and when mixed solution and target sample react, can generate toxic gas such as chlorine there are very big potential safety hazard in the environment and the person; And hydrochloric acid is again the starting material of making methamphetamine, receives the nation's security management and control.
Therefore, how cobalt or cobalt-base alloy target are corroded, how to select suitable corrosive fluid, make that the corrosive effect of cobalt or cobalt-base alloy and Display of Grain Boundary are 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 provides the caustic solution of a kind of metallographic structure electrolytic solution, cobalt or cobalt-base alloy and the display packing of metallographic structure thereof; With Display of Grain Boundary effect that improves cobalt or cobalt-base alloy metallographic structure and the potential safety hazard that reduces metallographic structure electrolytic solution, starting material are not in the scope of national security management and control simultaneously.
For addressing the above problem, the embodiment of the invention provides a kind of metallographic structure electrolytic solution, and said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
Optional, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33 in the said metallographic structure electrolytic solution: (10～15): (10～15).
For addressing the above problem, the embodiment of the invention also provides the caustic solution of a kind of cobalt or cobalt-base alloy, comprising:
Cobalt or cobalt-base alloy target are provided;
Said cobalt or cobalt-base alloy target are carried out electropolishing in metallographic structure electrolytic solution, said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
Optional, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33 in the said metallographic structure electrolytic solution: (10～15): (10～15).
Optional, the time of said electropolishing is 10s～20s.
Optional, the voltage of said electropolishing is 28V～35V.
For addressing the above problem, the embodiment of the 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;
Said cobalt or cobalt-base alloy target are polished;
Cobalt or cobalt-base alloy target to after the polishing carry out mechanical polishing;
Cobalt after the mechanical polishing or cobalt-base alloy target are carried out electropolishing in metallographic structure electrolytic solution, said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
Optional, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33 in the said metallographic structure electrolytic solution: (10～15): (10～15).
Optional, the time of said electropolishing is 10s～20s.
Optional, the voltage of said electropolishing is 28V～35V.
Optional, use diamond paste that said cobalt or cobalt-base alloy target are carried out mechanical polishing in the said mechanical polishing process.
Optional, the wetting agent of said mechanical polishing is an absolute ethyl alcohol.
Optional, the sharpening machine rotating speed of said mechanical polishing is 400r/min～600r/min.
Optional, the time of said mechanical polishing is 2min～3min.
Compared with prior art; It is metallographic structure electrolytic solution that the embodiment of the invention adopts the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid; And with cobalt or cobalt-base alloy electropolishing in this metallographic structure electrolytic solution; Method in the embodiment of the invention has good corrosive effect and display effect to cobalt or cobalt-base alloy, and the method that cobalt or cobalt-base alloy target carry out chemical corrosion is compared as etching reagent with existing hydrofluoric acid and nitric acid, and it is smaller to operating personnel's Health hazard and environmental pollution with above-mentioned metallographic structure electrolytic solution cobalt or cobalt-base alloy target to be carried out mechanical polishing; And starting material do not receive the nation's security management and control, and supply is more convenient.
Description of drawings
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
The present invention at first 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 the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33 in the said metallographic structure electrolytic solution: (10～15): (10～15).Said alcoholic acid mass percent concentration is 99.7%; The mass percent concentration of said propyl carbinol is 96%; The mass percent concentration of said hydrofluoric acid is 39%～41%; The mass percent concentration of said nitric acid is 63%～65%.Cobalt or cobalt-base alloy electropolishing in this metallographic structure electrolytic solution are had 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 all are polycrystal, that is to say, they all are made up of crystal grain.Use metallographic structure electrolytic solution that metal and alloy are corroded, the crystal boundary of metal and alloy grain is displayed.
The present invention also provides the embodiment of caustic solution of a cobalt or cobalt-base alloy as shown in Figure 1, comprising:
Step S11 provides cobalt or cobalt-base alloy target;
Step S12 carries out electropolishing with said cobalt or cobalt-base alloy target in metallographic structure electrolytic solution, said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
Said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid; The volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33 in the said metallographic structure electrolytic solution: (10～15): (10～15), and said alcoholic acid mass percent concentration is 99.7%; The mass percent concentration of said propyl carbinol is 96%; The mass percent concentration of said hydrofluoric acid is 39%～41%; The mass percent concentration of said nitric acid is 63%～65%, and the time of said electropolishing is 10s～20s, and the voltage of said electropolishing is 28V～35V.
Concrete operating process can be with reference to the corrosion step of the embodiment in the display packing of cobalt below the present invention or cobalt-base alloy metallographic structure.
Metal or alloy is carried out metallographicobservation be used for the microtexture of analyzing samples, it mainly is to study its weave construction through metallography microscope sem observation metal or alloy sample, for example the size of crystal grain, shape and orientation etc.
In practical application in industry, metal or alloy carried out metallographicobservation before, need earlier to the 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 invention or cobalt-base alloy metallographic structure is as shown in Figure 2, comprising:
Step S21 provides cobalt or cobalt-base alloy target;
Step S22 cuts a part as sample from said target;
Step S23 polishes to said cobalt or cobalt-base alloy sample;
Step S24 carries out mechanical polishing to cobalt or cobalt-base alloy sample after the polishing;
Step S25 carries out electropolishing with cobalt after the mechanical polishing or cobalt-base alloy sample in metallographic structure electrolytic solution, said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid;
Step S26 cleans said sample;
Step S27 utilizes metaloscope that said sample is observed.
Display packing with 6N cobalt or cobalt-base alloy metallographic structure is an example below, is elaborated in conjunction with the embodiment of 2 pairs of the invention described above of accompanying drawing.
At first performing step S21 provides cobalt or cobalt-base alloy target.
In the present embodiment, the material of said target can be that purity is 99.9% or above cobalt or cobalt-base alloy.For example be 3N5 (99.95%), 4N5 (99.995%) or 5N (99.999%).The shape of said target can be according to the actual requirement of applied environment, sputtering equipment, for example is in rectangle, circle, annular, taper shape or other analogous shapes (comprising regular shape and irregularly shaped) any.
Then performing step S22 cuts a part as sample from said target.
In the present embodiment, for example can adopt modes such as handsaw, sawing machine or cutting off machine cut a part as sample from target.The dimensioned area of said sample is 100mm
2, thickness is 10mm.In addition, which kind of no matter adopts cut method, all should note the temperature condition of said sample, use water cooling in case of necessity, to avoid said sample because of overheated its tissue that changes.
Then performing step S23 polishes to said cobalt or cobalt-base alloy sample.
The purpose 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 the cobalt or the cobalt-base alloy specimen surface smooth that need carry out metallographicobservation, to guarantee follow-up corrosive effect.
In the present embodiment, it mainly is successively said 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 makees wetting agent with water during polishing.
To the processing of polishing of said target.Said polishing is handled and specifically comprised: as wetting agent, at first use the surface (surface that needs observation) of flint paper (present embodiment is 400# water-based sand paper) polishing cobalt or cobalt-base alloy sample with water, the polishing time generally can be 5min～10min; Use the surface (surface that needs observation) of slightly thick sand paper (present embodiment is 800# water-based sand paper) polishing cobalt or cobalt-base alloy sample then, the polishing time generally can be 5min～10min; Use fine sandpaper (present embodiment is 1500# water-based sand paper) to continue the surface (surface that needs observation) of polishing cobalt or cobalt-base alloy sample at last, the polishing time generally can be 5min～10min, can obtain the flour milling of smooth like this.
In when polishing, water-based sand paper is driven by sharpening machine, and it is wetting that the sharpening machine top has water ceaselessly to flow to carry out on the sand paper, pins cobalt or cobalt-base alloy sample (surface of observing with needs is towards sand paper) and on sand paper, grinds.After changing sand paper said target is rotated 90 degree at every turn, grind off up to the cut last one procedure, new cut direction is consistent, and must said target be cleaned up water before changing sand paper at every turn, to remove sand grains.
In other embodiments, the wetting agent that also can use alcohol to handle as polishing.
Performing step S24 carries out mechanical polishing to cobalt or cobalt-base alloy sample after the polishing then.
The purpose that cobalt or cobalt-base alloy sample are carried out mechanical polishing is to remove the polishing scratch that polishing cobalt or cobalt-base alloy sample produce, and makes the cobalt or the cobalt-base alloy specimen surface that need carry out metallographicobservation more smooth, further guarantees follow-up corrosive effect.
In the present embodiment, it mainly is with diamond paste said cobalt or cobalt-base alloy target to be carried out mechanical polishing that cobalt or cobalt-base alloy target are polished, and makees wetting agent with absolute ethyl alcohol (alcohol) during mechanical polishing.
Specifically; Diamond paste is spread upon on the flannelette; Flannelette is driven by sharpening machine, and it is wetting that sharpening machine top has absolute ethyl alcohol ceaselessly to flow to carry out on the flannelette, pins cobalt or cobalt-base alloy sample (surface of observing with needs is towards flannelette) and on flannelette, polishes.In the present embodiment, the 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; Then the sample after the polishing is bright inadequately clear; Influence the display packing and the observations of metallographic structure, the time of mechanical polishing is long more, and the smooth finish of specimen surface is good more; But consider the working efficiency of mechanical polishing, present embodiment is no more than 3min to mechanical polishing time of said sample and is advisable.After the mechanical polishing, cobalt or cobalt-base alloy sample wash is clean with a large amount of water.
Need to prove; The common water of the mechanical polishing of traditional cobalt or cobalt-base alloy sample is cooked wetting agent; But the contriver finds; Then can reduce the surface tension of cobalt or cobalt-base alloy sample with absolute ethyl alcohol (alcohol), make absolute ethyl 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 preferred absolute ethyl alcohol (alcohol) as wetting agent.
Through the surface treatment of above-mentioned steps S23 and S24, remove the oxide compound of said specimen surface, form at least one polished surface.
Follow performing step S25; Cobalt after the mechanical polishing or cobalt-base alloy sample are carried out electropolishing in metallographic structure electrolytic solution; Said 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 promptly therefore the intersection of each crystal grain can make a distinction each crystal grain.In the above-mentioned metallographic structure electrolytic solution, nitric acid and hydrofluoric acid have intensive corrodibility to metals such as cobalt or cobalt-base alloys, can react with cobalt or cobalt-base alloy; The corrodibility and the oxidisability that contain ethanol, propyl carbinol in the metallographic structure electrolytic solution are low.
Specifically, in the said 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).Said ethanol, propyl carbinol are analytical pure solution, and promptly said alcoholic acid mass percent concentration is 99.7%; The mass percent concentration of said propyl carbinol is 96%; The mass percent concentration of said nitric acid is 63%～65%, and the mass percent concentration of said hydrofluoric acid is 39%～41%, and the metallographic structure electrolytic solution for preparing is packed on the electropolisher,, then cobalt or cobalt-base alloy sample is carried out electropolishing at normal temperatures.
In the present embodiment, electropolishing is to be anode with cobalt or cobalt-base alloy sample, and the metal that is insoluble to metallographic structure electrolytic solution is a negative electrode, and the two poles of the earth are immersed in the electrolyzer simultaneously, passes to direct current and produces anode dissolution selectively.
When 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.The surface microscopic convex part is thinner, and current density is bigger, and dissolving metal is very fast; Recess is thicker under the surface microscopic, and current density is less, and dissolving metal is slower.Because the ununiformity of consistence mucous membrane and electric current distribution, the microscopic protrusions portion size reduces very fast, and the recess size reduces slowlyer under the microcosmic, makes the reduction of cobalt or cobalt-base alloy specimen surface roughness, thereby reaches the purpose of anode dissolution.
In the present embodiment, carry out the electropolishing operation at normal temperatures, the time of said electropolishing is that etching time is generally 10s～20s, is preferably 10s.If the time of electropolishing, then the corrosion of cobalt or cobalt-base alloy sample was not enough, just can't demonstrate crystal boundary less than 10s; If the time of electropolishing, then cobalt or cobalt-base alloy sample were understood excessive corrosion greater than 20s, the crystal boundary and the crystal grain of cobalt or cobalt-base alloy sample all can be destroyed, and target is oxidized easily.
The voltage of electropolishing described in the present embodiment is 28V～35V, is preferably 30V.If the voltage of electropolishing is less than 28V, then the electric current of electropolishing is too little, and the speed of electropolishing is too slow, causes the corrosion of cobalt or cobalt-base alloy sample not enough easily, can't demonstrate crystal boundary; If the voltage of electropolishing is greater than 35V; Then the electric current of electropolishing is too big, and the speed of electropolishing is too fast, causes the meeting of cobalt or cobalt-base alloy specimen surface uneven easily; And excessive corrosion, the crystal boundary and the crystal grain of corresponding cobalt or cobalt-base alloy sample all can be destroyed.
Then performing step S26 cleans said sample.
After the corrosion, in the present embodiment, take out cobalt or cobalt-base alloy sample use immediately clear water to erosional surface clean, scavenging period is 1min～2min.Need to prove that present embodiment can clean all faces of cobalt or cobalt-base alloy sample, also can clean the surface that cobalt or cobalt-base alloy sample need be observed.
Dry up the said sample after the cleaning then.
Step S27 utilizes metaloscope that said sample is observed.
In the present embodiment; Because through above-mentioned each step; Particularly the corrosion treatment among the step S25 can utilize metaloscope just can observe well so that the metallographic structure of said sample has good display effect again, helps correct analysis is carried out in the metallographic structure of said sample.
Describe in the face of an alternative embodiment of the invention down.A last embodiment cuts a part as sample with cobalt or cobalt-base alloy target, polishes, polishing, burn into cleans and observe and handle, and whole treating processes is that the sample of cobalt or cobalt-base alloy target is handled.The difference of an an alternative embodiment of the invention and a last example is that cobalt or cobalt-base alloy target full-page proof are handled, i.e. metallographic structure to large-scale cobalt or cobalt-base alloy target shows.Fig. 3 is the cobalt of another embodiment of the present invention or the method for displaying metallographic structure of cobalt-base alloy, and is specifically as shown in Figure 3, comprising:
Step S31 provides cobalt or cobalt-base alloy target;
Step S32 polishes to said cobalt or cobalt-base alloy target;
Step S33 carries out mechanical polishing to cobalt or cobalt-base alloy target after the polishing;
Step S34 carries out electropolishing with cobalt after the mechanical polishing or cobalt-base alloy target in metallographic structure electrolytic solution, said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid;
Step S35 cleans said target;
Step S36 utilizes metaloscope that said target is observed.
At first performing step S31 provides cobalt or cobalt-base alloy target.In the present embodiment, specifically can be with reference to a last embodiment.
Then performing step S32 polishes to said cobalt or cobalt-base alloy target.
The purpose 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 the cobalt or the cobalt-base alloy target material surface smooth that need carry out metallographicobservation, to guarantee follow-up corrosive effect.
In the present embodiment, it mainly is successively said 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 makees wetting agent with water during polishing.
To the polishing of large-scale cobalt or cobalt-base alloy the time, adopt the method for hand sand, cobalt or cobalt-base alloy target (surface of observing with needs is towards sand paper) are polished with portable sharpening machine.Can water in the bruting process or the wetting agent handled as polishing of alcohol.Concrete operations can be with reference to a last embodiment.
Performing step S33 carries out mechanical polishing to cobalt or cobalt-base alloy target after the polishing then.
The purpose that cobalt or cobalt-base alloy target are carried out mechanical polishing is to remove the polishing scratch that polishing cobalt or cobalt-base alloy target produce, and makes the cobalt or the cobalt-base alloy target material surface that need carry out metallographicobservation more smooth, further guarantees follow-up corrosive effect.Specific operation process can be with reference to a last embodiment.
Through the surface treatment of above-mentioned steps S32 and S33, remove the oxide compound of said target material surface, form at least one polished surface.
Then performing step S34 carries out electropolishing with cobalt after the mechanical polishing or cobalt-base alloy target in metallographic structure electrolytic solution, and said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
, large-scale cobalt or cobalt-base alloy target adopt portable electropolisher, that cobalt or cobalt-base alloy target material surface (surface that need observe) are carried out electropolishing when being carried out electropolishing.Metallographic structure electrolytic solution and electropolishing specifically can be with reference to last embodiment.
Then performing step S35 cleans said target.
Behind the 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 last embodiment.
Need to prove that present embodiment can clean all faces of cobalt or cobalt-base alloy target, also can clean the surface that cobalt or cobalt-base alloy target need be observed.
Dry up the said target after the cleaning then.
Then performing step S36 utilizes metaloscope that said target is observed.
In the present embodiment; Because through above-mentioned each step; Particularly the processing of the electropolishing among the step S34 can be so that the metallographic structure of said target has good display effect; Utilize metaloscope just can observe well again, help correct analysis is carried out in the metallographic structure of said target.
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 said ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33: (10～15): (10～15), the mass percent concentration of said nitric acid are 63%～65%; The mass percent concentration of said hydrofluoric acid is 39%～41%; Described ethanol, propyl carbinol are analytical pure concentration, and promptly said alcoholic acid mass percent concentration is 99.7%; The mass percent concentration of said propyl carbinol is 96%, and it has good corrosive effect to cobalt or cobalt-base alloy, and also less to operating personnel's Health hazard and environmental pollution, simultaneously, starting material such as hydrofluoric acid and nitric acid are not in the scope of national security management and control.
In addition, technique scheme is done the polishing effect that wetting agent can improve target material surface with absolute ethyl alcohol when cobalt or cobalt-base alloy target are carried out mechanical polishing; When cobalt or cobalt-base alloy target are carried out 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 advantages such as excessive corrosion or deficiency.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction.Any those of ordinary skill in the art; Do not breaking away under the technical scheme scope situation of the present invention; All the method for above-mentioned announcement capable of using and technology contents are made many possible changes and modification to technical scheme of the present invention, or are revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not break away from technical scheme of the present invention, all still belongs in the scope of technical scheme protection of the present invention any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.
Claims (14)
1. a metallographic structure electrolytic solution is characterized in that, said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
2. metallographic structure electrolytic solution as claimed in claim 1 is characterized in that, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33 in the said metallographic structure electrolytic solution: (10～15): (10～15).
3. the caustic solution of cobalt or cobalt-base alloy is characterized in that, comprising: cobalt or cobalt-base alloy target are provided; Said cobalt or cobalt-base alloy target are carried out electropolishing in metallographic structure electrolytic solution, said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
4. the caustic solution of cobalt as claimed in claim 3 or cobalt-base alloy is characterized in that, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33 in the said metallographic structure electrolytic solution: (10～15): (10～15).
5. the caustic solution of cobalt as claimed in claim 3 or cobalt-base alloy is characterized in that, the time of said electropolishing is 10s～20s.
6. the caustic solution of cobalt as claimed in claim 3 or cobalt-base alloy is characterized in that, the voltage of said electropolishing is 28V～35V.
7. the display packing of cobalt or cobalt-base alloy metallographic structure is characterized in that, comprising:
Cobalt or cobalt-base alloy target are provided;
Said cobalt or cobalt-base alloy target are polished;
Cobalt or cobalt-base alloy target to after the polishing carry out mechanical polishing;
Cobalt after the mechanical polishing or cobalt-base alloy target are carried out electropolishing in metallographic structure electrolytic solution, said metallographic structure electrolytic solution is the mixing solutions of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid.
8. the display packing of cobalt as claimed in claim 7 or cobalt-base alloy metallographic structure is characterized in that, the volume ratio of ethanol, propyl carbinol, water, nitric acid and hydrofluoric acid is 66: 11: 33 in the said metallographic structure electrolytic solution: (10～15): (10～15).
9. the display packing of cobalt as claimed in claim 7 or cobalt-base alloy metallographic structure is characterized in that, the time of said electropolishing is 10s～20s.
10. the display packing of cobalt as claimed in claim 7 or cobalt-base alloy metallographic structure is characterized in that, the voltage of said electropolishing is 28V～35V.
11. the display packing of cobalt as claimed in claim 7 or cobalt-base alloy metallographic structure is characterized in that, said mechanical polishing process uses diamond paste that said cobalt or cobalt-base alloy target are carried out mechanical polishing.
12. the display packing of cobalt as claimed in claim 11 or cobalt-base alloy metallographic structure is characterized in that, the wetting agent of said mechanical polishing is an absolute ethyl alcohol.
13. the display packing of cobalt as claimed in claim 11 or cobalt-base alloy metallographic structure is characterized in that, the sharpening machine rotating speed of said mechanical polishing is 400r/min～600r/min.
14. the display packing of cobalt as claimed in claim 11 or cobalt-base alloy metallographic structure is characterized in that, the time of said mechanical polishing is 2min～3min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102879254A (en) * | 2012-09-29 | 2013-01-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Hot-dipping aluminum-zinc alloy coated steel plate coating structure display method |
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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 |
| CN106346344A (en) * | 2015-07-15 | 2017-01-25 | 宁波江丰电子材料股份有限公司 | Copper target material surface processing method |
| CN106370489A (en) * | 2016-08-24 | 2017-02-01 | 江西稀有稀土金属钨业集团有限公司 | Sample production method used for hard alloy metallographic detection |
| CN107870112A (en) * | 2016-09-27 | 2018-04-03 | 宁波江丰电子材料股份有限公司 | Metallographic structure detection method |
| CN109763165A (en) * | 2019-02-22 | 2019-05-17 | 江苏科技大学 | The electrolytic etching method of precipitation phase in a kind of cobalt-base alloys |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103454115A (en) * | 2012-05-29 | 2013-12-18 | 宁波江丰电子材料有限公司 | Sampling method and detecting method for circular target |
| CN102879254A (en) * | 2012-09-29 | 2013-01-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Hot-dipping aluminum-zinc alloy coated steel plate coating structure display method |
| CN103913416A (en) * | 2012-12-31 | 2014-07-09 | 宁波江丰电子材料有限公司 | Target material detection method |
| CN106346344A (en) * | 2015-07-15 | 2017-01-25 | 宁波江丰电子材料股份有限公司 | Copper target material surface processing method |
| CN106370489A (en) * | 2016-08-24 | 2017-02-01 | 江西稀有稀土金属钨业集团有限公司 | Sample production method used for hard alloy metallographic detection |
| CN106370489B (en) * | 2016-08-24 | 2019-04-12 | 江西江钨硬质合金有限公司 | The method for making sample of hard alloy metallographic detection |
| CN107870112A (en) * | 2016-09-27 | 2018-04-03 | 宁波江丰电子材料股份有限公司 | Metallographic structure detection method |
| CN109763165A (en) * | 2019-02-22 | 2019-05-17 | 江苏科技大学 | The electrolytic etching method of precipitation phase in a kind of cobalt-base alloys |
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