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CN109211645A - The metallographic etching agent of chromium tantalum-titanium alloy and its display methods of metallographic structure - Google Patents

The metallographic etching agent of chromium tantalum-titanium alloy and its display methods of metallographic structure Download PDF

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Publication number
CN109211645A
CN109211645A CN201710546141.7A CN201710546141A CN109211645A CN 109211645 A CN109211645 A CN 109211645A CN 201710546141 A CN201710546141 A CN 201710546141A CN 109211645 A CN109211645 A CN 109211645A
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China
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titanium alloy
metallographic
chromium tantalum
alloy sample
etching agent
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姚力军
潘杰
相原俊夫
王学泽
罗明浩
胡淼锡
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching

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  • Life Sciences & Earth Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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Abstract

The present invention provides the display methods of metallographic etching agent and its metallographic structure of a kind of chromium tantalum-titanium alloy, and the display methods includes: to provide chromium tantalum-titanium alloy sample;The chromium tantalum-titanium alloy sample is surface-treated, an at least burnishing surface is formed;Corrosion treatment is carried out using burnishing surface of the metallographic etching agent to the chromium tantalum-titanium alloy sample, the metallographic etching agent is the mixed solution of hydrofluoric acid, sulfuric acid, nitric acid and hydrochloric acid.Using the mixed solution of hydrofluoric acid, sulfuric acid, nitric acid and hydrochloric acid as metallographic etching agent, corrosion treatment is carried out to the burnishing surface of chromium tantalum-titanium alloy sample, the technology stability of the corrosion treatment is higher, the metallographic etching agent is higher to the controllability of the corrosion rate of metallographic structure, with good corrosive effect, the crystal boundary pattern of the chromium tantalum-titanium alloy sample after making corrosion is clear, so that good metallographic structure Display of Grain Boundary effect is obtained, convenient for observing using metallographic microscope metallographic structure.

Description

The metallographic etching agent of chromium tantalum-titanium alloy and its display methods of metallographic structure
Technical field
The present invention relates to the metallographic etching agent of material corrosion technical field more particularly to a kind of chromium tantalum-titanium alloy and its metallographics The display methods of tissue.
Background technique
With the development of science and technology, industrial production wants the material properties such as the hardness, intensity, ductility of metal material Ask also higher and higher, and the material properties such as internal organizational structure and hardness, intensity, ductility of golden metal material have it is direct and Close connection, therefore the internal organizational structure of research material becomes particularly important.Metallographic observation is then in research metal material Portion's institutional framework effective method the most direct.
Metallographic observation to be carried out first has to show the metallographic of metal material, then uses metallography microscope sem observation institute State the metallographic structure of metal material.Crystal boundary in metallographic structure is that structure is identical and be orientated the interface between different crystal, in crystalline substance On interface, atomic arrangement is transitioned into another orientation from an orientation, therefore grain boundaries atomic arrangement is in an interim state.Crystal grain with Contact surface between crystal grain is just called crystal boundary.Metallic grain boundaries generally are allowed to display by using the method that etchant corrodes, It has particularly important meaning for the internal organizational structure of research material.
With the development of science and technology, industrial production increasingly increases the demand of alloying metal, for some novel Alloy material needs new Phase structure study method.Chromium tantalum-titanium alloy is a kind of novel conjunction for hard disk magnetic recording material Golden material then needs suitable metallographic etching agent and metallographic structure to sufficiently show the metallographic structure of chromium tantalum-titanium alloy Display methods.
Summary of the invention
Problems solved by the invention is to provide the display side of metallographic etching agent and its metallographic structure of a kind of chromium tantalum-titanium alloy Method makes the metallographic structure of chromium tantalum-titanium alloy have good display effect, convenient for metallographic observation and analyzes the chromium tantalum-titanium alloy Metallographic structure.
To solve the above problems, the present invention provides a kind of metallographic etching agent of chromium tantalum-titanium alloy, comprising: the metallographic etching Agent is the mixed solution of hydrofluoric acid, sulfuric acid, nitric acid and hydrochloric acid.
Optionally, the metallographic etching agent by mass percent concentration be 40% to 43% the hydrofluoric acid, quality hundred Divide the nitric acid and quality that the sulfuric acid, mass percent concentration that specific concentration is 95% to 98% are 65% to 68% The hydrochloric acid that percent concentration is 36% to 38% is that 5:2:2:2 is formulated according to volume ratio.
Correspondingly, the present invention also provides a kind of display methods of chromium tantalum-titanium alloy metallographic structure, comprising: provide chromium tantalum titanium and close Golden sample;The chromium tantalum-titanium alloy sample is surface-treated, an at least burnishing surface is formed;Using metallographic of the present invention Etchant carries out corrosion treatment to the burnishing surface of the chromium tantalum-titanium alloy sample.
Optionally, the metallographic etching agent by mass percent concentration be 40% to 43% the hydrofluoric acid, quality hundred Divide the nitric acid and quality that the sulfuric acid, mass percent concentration that specific concentration is 95% to 98% are 65% to 68% The hydrochloric acid that percent concentration is 36% to 38% is that 5:2:2:2 is formulated according to volume ratio.
Optionally, the step of providing chromium tantalum-titanium alloy sample includes: to provide chromium tantalum-titanium alloy target;It is closed from the chromium tantalum titanium A part is cut in gold target material as chromium tantalum-titanium alloy sample.
Optionally, the step of grinding technics includes: successively using the sand paper of grit progression to the chromium tantalum-titanium alloy Specimen surface is ground.
Optionally, the sand paper is respectively the aqueous sand paper of 400#, 800# and 1500#.
Optionally, in the grinding technics the step of, the sand paper is placed on grinder, using water as wetting agent It is ground.
Optionally, the revolving speed of the grinder is 300 revs/min to 400 revs/min, the total time of the grinding technics It is 5 minutes to 10 minutes.
Optionally, the step of polishing process includes: to use the flannelette for being moistened with diamond paste to the institute after grinding Chromium tantalum-titanium alloy specimen surface is stated to be mechanically polished.
Optionally, in the mechanical polishing the step of, the flannelette is set on grinder, and using water as wetting Agent is polished.
Optionally, the revolving speed of the grinder is 300 revs/min to 400 revs/min, and polishing time is 2 minutes to 3 points Clock.
Optionally, it after the surface treatment, before the corrosion treatment, further comprises the steps of: and institute is cleaned using clear water State chromium tantalum-titanium alloy sample.
Optionally, the processing time of the corrosion treatment is 60 seconds to 90 seconds.
Optionally, the step of corrosion treatment includes: to provide the metallographic etching agent;By the chromium tantalum-titanium alloy sample Burnishing surface immerse in the metallographic etching agent and corroded.
Optionally, so that the burnishing surface is parallel to horizontal plane direction, the burnishing surface is immersed in the metallographic etching agent; Alternatively, making the burnishing surface perpendicular to horizontal plane direction, the burnishing surface is immersed in the metallographic etching agent.
Optionally, it after carrying out corrosion treatment to the burnishing surface of the chromium tantalum-titanium alloy sample, further comprises the steps of: to the chromium Tantalum-titanium alloy sample carries out metallographic observation.
Optionally, after carrying out corrosion treatment to the burnishing surface of the chromium tantalum-titanium alloy sample, the chromium tantalum-titanium alloy is tried Before sample carries out metallographic observation, further comprises the steps of: and take out the chromium tantalum-titanium alloy sample from the metallographic etching agent;It takes out After the chromium tantalum-titanium alloy sample, the chromium tantalum-titanium alloy sample is started the cleaning processing;After the cleaning treatment, to described Chromium tantalum-titanium alloy sample carries out drying processing.
Optionally, the step of cleaning treatment includes: to clean the chromium tantalum-titanium alloy sample using alcohol or clear water;Or Person first uses chromium tantalum-titanium alloy sample described in alcohol washes again with clear water.
Compared with prior art, technical solution of the present invention has the advantage that
By forming an at least burnishing surface, the chromium tantalum-titanium alloy sample is set to obtain smooth bright surface, and be conducive to The scratch for removing the chromium tantalum-titanium alloy specimen surface is conducive to the effect for improving subsequent corrosion processing;In addition, using hydrogen fluorine Acid, sulfuric acid, nitric acid and hydrochloric acid mixed solution as metallographic etching agent, the burnishing surface of chromium tantalum-titanium alloy sample is carried out at corrosion Reason, the technology stability of the corrosion treatment is higher, the metallographic etching agent to the controllability of the corrosion rate of metallographic structure compared with Height has good corrosive effect, and the crystal boundary pattern of the chromium tantalum-titanium alloy sample after making corrosion is clear, to obtain good Metallographic structure Display of Grain Boundary effect, convenient for being observed metallographic structure using metallographic microscope.
Detailed description of the invention
Fig. 1 is the flow diagram of one embodiment of display methods of chromium tantalum-titanium alloy metallographic structure of the present invention;
Fig. 2 is the corresponding schematic diagram of step S1 in embodiment illustrated in fig. 1;
Fig. 3 is the corresponding schematic diagram of step S2 in embodiment illustrated in fig. 1;
Fig. 4 is the corresponding schematic diagram of step S3 in embodiment illustrated in fig. 1.
Specific embodiment
It is a kind of novel alloy material it can be seen from background technology that, chromium tantalum-titanium alloy, to by the metallographic of chromium tantalum-titanium alloy Tissue is sufficiently shown, then needs suitable metallographic etching agent and method for displaying metallographic structure.
To solve the above-mentioned problems, the present invention provides a kind of metallographic etching agent of chromium tantalum-titanium alloy.
In the present embodiment, the metallographic etching agent is the mixed solution of hydrofluoric acid, sulfuric acid, nitric acid and hydrochloric acid.
Chromium tantalum-titanium alloy is polycrystal, i.e., the described chromium tantalum-titanium alloy is made of crystal grain.Using metallographic etching agent to the chromium Tantalum-titanium alloy is corroded, and chemical etching is belonged to, and the Display of Grain Boundary of the chromium tantalum-titanium alloy can be made to come out.Wherein, chemistry leaching Erosion is the process of the dissolution of metallographic specimen surface chemistry or electrochemical dissolution.
The chromium tantalum-titanium alloy is the alloy with corrosion resistance, if the corrosivity of the metallographic etching agent is too low, It is difficult to show the metallographic structure of the chromium tantalum-titanium alloy completely;If the corrosivity of the metallographic etching agent is excessively high, The metallographic structure of the chromium tantalum-titanium alloy is corroded excessively, equally also will affect the display effect of the chromium tantalum-titanium alloy metallographic structure Fruit.
In the present embodiment, using the mixed solution of hydrofluoric acid, sulfuric acid, nitric acid and hydrochloric acid as metallographic etching agent, the gold Phase etchant stablizes the corrosion rate on chromium tantalum-titanium alloy surface, and it is rotten can to carry out appropriateness to chromium tantalum-titanium alloy surface The crystal boundary pattern of erosion, the chromium tantalum-titanium alloy after making corrosion is clear, so that good metallographic structure Display of Grain Boundary effect is obtained, Convenient for being observed using metallographic microscope the metallographic structure.
In order to make the metallographic etching agent carry out appropriate corrosion to chromium tantalum-titanium alloy surface, make the chromium tantalum-titanium alloy The display effect of metallurgical structure is preferable, and the mass percent that need to rationally control each solution when configuring the metallographic etching agent is dense Degree and volume ratio.
If the mass percent concentration of any solution or content are excessive in the hydrofluoric acid, sulfuric acid, nitric acid and hydrochloric acid, Then it is easy to cause the chromium tantalum-titanium alloy that excessive corrosion phenomenon occurs, to destroy the structure of the chromium tantalum-titanium alloy;Such as The mass percent concentration of any solution or content are too small in hydrofluoric acid, sulfuric acid described in fruit, nitric acid and hydrochloric acid, due to corroding not It is enough abundant, it is easy to cause the crystal boundary of the chromium tantalum-titanium alloy not obvious enough, so as to cause being difficult to be clearly observed the chromium tantalum The structure of titanium alloy.
For this purpose, in the present embodiment, the hydrogen fluorine that the metallographic etching agent is 40% to 43% by mass percent concentration Acid, mass percent concentration be 95% to 98% the sulfuric acid, mass percent concentration be 65% to 68% the nitric acid, And the hydrochloric acid that mass percent concentration is 36% to 38% according to volume ratio is that 5:2:2:2 is formulated.
Correspondingly, the present invention also provides a kind of display methods of chromium tantalum-titanium alloy metallographic structure.
To make the above purposes, features and advantages of the invention more obvious and understandable, with reference to the accompanying drawing to the present invention Specific embodiment be described in detail.
Referring to FIG. 1, showing the process signal of one embodiment of display methods of chromium tantalum-titanium alloy metallographic structure of the present invention Figure.The display methods of the present embodiment chromium tantalum-titanium alloy metallographic structure includes following basic step:
Step S1: chromium tantalum-titanium alloy sample is provided;
Step S2: being surface-treated the chromium tantalum-titanium alloy sample, forms an at least burnishing surface;
Step S3: corrosion treatment, the gold are carried out using burnishing surface of the metallographic etching agent to the chromium tantalum-titanium alloy sample Phase etchant is the mixed solution of hydrofluoric acid, sulfuric acid, nitric acid and hydrochloric acid.
Specific embodiments of the present invention are described further below in conjunction with attached drawing.
In conjunction with reference Fig. 1 and Fig. 2, Fig. 2 shows the corresponding schematic diagrames of step S1 in embodiment illustrated in fig. 1, execute step S1 provides chromium tantalum-titanium alloy sample 200 (as shown in Figure 2).
Subsequent handling is for realizing the display to 200 metallographic structure of chromium tantalum-titanium alloy sample.
Specifically, in the chromium tantalum-titanium alloy sample 200, the mass percentage content of chromium is 36% to 38%, The mass percentage content of tantalum element is 35% to 37%, and the mass percentage content of titanium elements is 14% to 16%.
In the present embodiment, the shape of the chromium tantalum-titanium alloy sample 200 is cuboid.In some other embodiment, institute It is annular or other shapes (including rule and not that the shape for stating chromium tantalum-titanium alloy sample, which can also be square, cylindrical body, section, Regular shape) in any column.
In the present embodiment, the chromium tantalum-titanium alloy sample 200 include first surface 210 (as shown in Figure 2) and with it is described The opposite second surface 220 (as shown in Figure 2) of first surface 210, subsequent step include using metallographic etching agent to described first Surface 210 and second surface 220 carry out corrosion treatment, thus to after corrosion the first surface 210 and second surface 220 into Row metallographic observation.
But it is not limited only to carry out corrosion treatment to the first surface 210 and second surface 220, the present embodiment treats corrosion Surface without limitation.
In further embodiments, subsequent step can also be only to any surface in the first surface and second surface Carry out corrosion treatment.
In some other embodiment, any other surface of the chromium tantalum-titanium alloy sample can also be carried out at corrosion Reason.
In the present embodiment, the step of providing chromium tantalum-titanium alloy sample 200 includes: to provide chromium tantalum-titanium alloy target 100 (as schemed Shown in 2);A part is cut from the chromium tantalum-titanium alloy target 100 as chromium tantalum-titanium alloy sample 200.
Specifically, as shown in Fig. 2, cutting leftover pieces 150 from the chromium tantalum-titanium alloy target 100 first with circumference saw, Then utilize crystal orientation cutting machine by the chromium tantalum-titanium alloy sample 200 of the 150 cut growth cube of leftover pieces.
It is subsequent that corrosion treatment, therefore the chromium tantalum titanium are carried out to the chromium tantalum-titanium alloy sample 200 using metallographic etching agent The size of alloy sample 200 is less than the subsequent container volume for holding the metallographic etching agent.
It should be noted that should be noted the chromium tantalum titanium during cutting acquisition chromium tantalum-titanium alloy sample 200 The temperature change of alloy sample 200 can be cooled down using clear water, to avoid the chromium tantalum-titanium alloy sample 200 because of temperature It is excessively high and occur metallographic structure change the problem of.
It continues to refer to figure 1, and combines and refer to Fig. 3, Fig. 3 is the corresponding schematic diagram of step S2 in embodiment illustrated in fig. 1, is executed Step S2 is surface-treated the chromium tantalum-titanium alloy sample 200 (as shown in Figure 3), forms an at least burnishing surface 250.
By forming burnishing surface 250, the chromium tantalum-titanium alloy sample 200 is made to obtain the surface of smooth light, surface texture Rule, and the scratch for being conducive to remove 200 surface of chromium tantalum-titanium alloy sample can be kept away in subsequent corrosion treatment process Exempt from etchant to accumulate at scratch, corrodes the etchant equably to the burnishing surface 250, to be conducive to The effect of subsequent corrosion processing is improved, and then the metallographic structure of the chromium tantalum-titanium alloy sample 200 is made to better emerge from out.
In the present embodiment, the step of surface treatment includes the grinding technics and polishing process successively carried out.
By the grinding technics, to remove the oxide layer on 200 surface of chromium tantalum-titanium alloy sample, make it is subsequent need into 200 smooth surface of chromium tantalum-titanium alloy sample of row metallographic observation is bright, to improve the effect of subsequent corrosion processing.
In the present embodiment, it is subsequent to the first surface 210 (as shown in Figure 2) and second surface 220 (as shown in Figure 2) into Therefore row metallographic observation carries out grinding technics to the first surface 210 and second surface 220.In some other embodiment In, grinding technics can also be carried out to all surface of the chromium tantalum-titanium alloy sample.
In the present embodiment, the step of grinding technics includes: successively using the sand paper of grit progression to the chromium tantalum titanium It is ground on 200 surface of alloy sample.Wherein, in the grinding technics the step of, the sand paper is placed on grinder, And it is ground using water as wetting agent.
Specifically, by replacing sand paper, successively using the sand paper of grit progression to 200 surface of chromium tantalum-titanium alloy sample It is ground, and is every time cleaned up the chromium tantalum-titanium alloy sample 200 with clear water before replacement sand paper at least once, with removal The sand grains on 200 surface of chromium tantalum-titanium alloy sample.
In the present embodiment, the sand paper is respectively the aqueous sand paper of 400#, 800# and 1500#.
It should be noted that being used when the revolving speed of the grinder is too low or the total time of the grinding technics is very few The aqueous sand paper of the granularity is easy to cause the finish on 200 surface of chromium tantalum-titanium alloy sample after grinding not meet subsequent Metallographic structure display requires, and the effect for causing subsequent corrosion to handle is deteriorated;When the revolving speed of the grinder is excessively high or the grinding When the total time of technique is excessive, it is easy to cause 200 surface of chromium tantalum-titanium alloy sample that overground phenomenon occurs, to cause described Chromium tantalum-titanium alloy sample 200 is scrapped.For this purpose, in the present embodiment, in order to ensure to 200 surface of chromium tantalum-titanium alloy sample Grinding stability and grinding effect, the revolving speed of the grinder are 300 revs/min to 400 revs/min, the grinding technics Total time be 5 minutes to 10 minutes.
Wherein, in the step of being ground using the aqueous sand paper of 400#, milling time is 1 minute to 2 minutes;Using In the step of aqueous sand paper of 800# is ground, milling time is 1 minute to 2 minutes, so as to preferably realize grinding Effect obtains the flour milling of substantially smooth light.
By the polishing process, polishing scratch generated during the grinding technics, scratch are removed, and make the chromium The smoother light in 200 surface of tantalum-titanium alloy sample to further increase the effect of subsequent corrosion processing, and then improves subsequent institute State the display of 200 metallographic structure of chromium tantalum-titanium alloy sample.
It is subsequent that metallographic observation is carried out to the first surface 210 and second surface 220 in the present embodiment, therefore, to grinding The first surface 210 and second surface 220 afterwards carries out polishing process.It in other embodiments, can also be by the chromium tantalum The all surface of titanium alloy sample carries out polishing process.
In the present embodiment, the step of polishing process include: using the flannelette of diamond paste is moistened with to grinding after 200 surface of chromium tantalum-titanium alloy sample mechanically polished.Wherein, in the mechanical polishing the step of, by the suede Cloth is set on grinder, and is polished using water as wetting agent.
It should be noted that the revolving speed of the grinder is too low or excessively high in the mechanical polishing the step of, when polishing Between it is too short or too long, be easy to cause the finish on 200 surface of chromium tantalum-titanium alloy sample after polishing not meet subsequent metallographic Tissue display requires, and the effect for handling subsequent corrosion is deteriorated;Moreover, if the revolving speed of the grinder is too low or polishing time It is too long, also result in the decline of polishing efficiency.For this purpose, the revolving speed of the grinder is 300 revs/min to 400 in the present embodiment Rev/min, polishing time is 2 minutes to 3 minutes.
In the present embodiment, after carrying out polishing process to the first surface 210 and second surface 220, make first table Face 210 and second surface 220 become burnishing surface 250.
It should also be noted that, further comprising the steps of: behind the surface and cleaning the chromium tantalum-titanium alloy sample using clear water 200, to remove the impurity on 200 surface of chromium tantalum-titanium alloy sample, to provide good surface for subsequent corrosion treatment Quality.
It continues to refer to figure 1, and combines and refer to Fig. 4, Fig. 4 is the corresponding schematic diagram of step S3 in embodiment illustrated in fig. 1, is executed Step S3, using metallographic etching agent 350 (as shown in Figure 4) to the burnishing surface of the chromium tantalum-titanium alloy sample 200 (as shown in Figure 4) 250 progress corrosion treatments (as shown in Figure 4), the metallographic etching agent 350 are that the mixing of hydrofluoric acid, sulfuric acid, nitric acid and hydrochloric acid is molten Liquid.
By corrosion treatment, the crystal boundary of the chromium tantalum-titanium alloy sample 200 can be made to display, then can pass through metallographic Microscope observes the metallographic structure of the chromium tantalum-titanium alloy sample 200.
In the present embodiment, the metallographic etching agent 350 is formed by hydrofluoric acid, sulfuric acid, nitric acid and mixed in hydrochloric acid.The metallographic 350 preparation method of etchant is simply rapid, stablizes to the corrosion rate of the chromium tantalum-titanium alloy sample 200, can be to the chromium 200 surface of tantalum-titanium alloy sample carries out appropriate corrosion, and corrosive effect is good, the chromium tantalum-titanium alloy sample 200 after making corrosion Crystal boundary pattern it is clear, to obtain good metallographic structure Display of Grain Boundary effect, convenient for using metallographic microscope to metallographic group It knits and is observed.
If the mass percent concentration of any solution or content are excessive in the hydrofluoric acid, sulfuric acid, nitric acid and hydrochloric acid, Then it is easy to cause the chromium tantalum-titanium alloy sample 200 that excessive corrosion phenomenon occurs, to destroy the chromium tantalum-titanium alloy sample 200 Structure;If the mass percent concentration of any solution or content mistake in the hydrofluoric acid, sulfuric acid, nitric acid and hydrochloric acid It is small, since corrosion is not enough, it is easy to cause the crystal boundary of the chromium tantalum-titanium alloy sample 200 not obvious enough, so as to cause being difficult to It is clearly observed the structure of the chromium tantalum-titanium alloy sample 200.
So in the present embodiment, the hydrogen fluorine that the metallographic etching agent is 40% to 43% by mass percent concentration Acid, mass percent concentration be 95% to 98% the sulfuric acid, mass percent concentration be 65% to 68% the nitric acid, And the hydrochloric acid that mass percent concentration is 36% to 38% according to volume ratio is that 5:2:2:2 is formulated.
As shown in figure 4, specifically, the step of corrosion treatment includes: to provide the metallographic etching agent 350;It will be described Metallographic etching agent 350 is poured into container 300;The chromium tantalum-titanium alloy sample 200 is clamped with tweezers (not shown), by the chromium tantalum The burnishing surface 250 of titanium alloy sample 200, which immerses in the metallographic etching agent 350, to be corroded.
In the present embodiment, the first surface 210 (as shown in Figure 2) and second surface 220 (as shown in Figure 2) polished work Become the burnishing surface 250 after skill, the first surface 210 and second surface 220 are two parallel faces, therefore are made described Burnishing surface 250 immerses the burnishing surface 250 in the metallographic etching agent 350 perpendicular to horizontal plane direction.Wherein, make described Burnishing surface 250 is referred to perpendicular to horizontal plane direction: making the burnishing surface 250 and the metallographic of the chromium tantalum-titanium alloy sample 200 The liquid level of etchant is perpendicular.
Make the burnishing surface 250 perpendicular to horizontal plane direction, the burnishing surface 250 is immersed into the metallographic etching agent 350 In method, on the one hand, two burnishing surfaces 250 of the chromium tantalum-titanium alloy sample 200 can be made while touching the metallographic Etchant 350 so that guarantee is identical to the corrosive effect of 250 each position of burnishing surface of the chromium tantalum-titanium alloy sample 200, and has Conducive to raising corrosion efficiency;It on the other hand, can be by partially polished face 250 according to subsequent 250 region of burnishing surface to metallographic observation It immerses in the metallographic etching agent 350, i.e., without being totally submerged the chromium tantalum-titanium alloy sample 200 in the metallographic etching agent It, being capable of save the cost so as to avoid the waste of the metallographic etching agent 350 in 350.
In further embodiments, the burnishing surface can also be made to be parallel to horizontal plane direction, the burnishing surface is immersed In the metallographic etching agent.Correspondingly, the chromium tantalum-titanium alloy sample is immersed in the metallographic etching agent, to make described The burnishing surface of chromium tantalum-titanium alloy sample can touch the metallographic etching agent.Wherein, the burnishing surface is made to be parallel to horizontal plane Direction refers to: keeping the burnishing surface of the chromium tantalum-titanium alloy sample parallel with the liquid level of the metallographic etching agent, to guarantee It is identical to the corrosive effect of each position in any one burnishing surface of the chromium tantalum-titanium alloy sample.
In some other embodiment, for example, only a surface of the chromium tantalum-titanium alloy sample be burnishing surface when, then make The burnishing surface is parallel to horizontal plane direction, and the burnishing surface is immersed the burnishing surface towards the metallographic etching agent In the metallographic etching agent.Correspondingly, without being totally submerged the chromium tantalum-titanium alloy sample in the metallographic etching agent, from And can be avoided the waste of the metallographic etching agent, it being capable of save the cost.
It should be noted that the processing time of the corrosion treatment is unsuitable very few, it is also unsuitable excessive.If when the processing Between it is very few, due to corrosion be not enough, be easy to cause the crystal boundary of the chromium tantalum-titanium alloy sample 200 not obvious enough, so as to cause It is difficult to be clearly observed the structure of the chromium tantalum-titanium alloy sample 200;If the processing time is excessive, it is easy to make institute It states chromium tantalum-titanium alloy sample 200 and excessive corrosion phenomenon occurs, to destroy the structure of the chromium tantalum-titanium alloy sample 200. For this purpose, the processing time of the corrosion treatment is 60 seconds to 90 seconds in the present embodiment.
It further include step after carrying out corrosion treatment to the burnishing surface 250 of the chromium tantalum-titanium alloy sample 200 in the present embodiment It is rapid: the chromium tantalum-titanium alloy sample 200 is taken out from the metallographic etching agent 350;Take out the chromium tantalum-titanium alloy sample 200 Afterwards, the chromium tantalum-titanium alloy sample 200 is started the cleaning processing;After the cleaning treatment, to the chromium tantalum-titanium alloy sample 200 carry out drying processing.
By being started the cleaning processing to the chromium tantalum-titanium alloy sample 200, to remove 200 table of chromium tantalum-titanium alloy sample The metallographic etching agent 350 in face and impurity;By carrying out drying processing to the chromium tantalum-titanium alloy sample 200, with the drying chromium Tantalum-titanium alloy sample 200, to provide Process ba- sis for subsequent progress metallographic observation.
In the present embodiment, by the chromium tantalum-titanium alloy sample 200 after being taken out in the metallographic etching agent 350, with a large amount of Clear water cleans up the erosional surface of the chromium tantalum-titanium alloy sample 200;The chromium tantalum titanium is dried up using air gun after cleaning up Alloy sample 200.
It in further embodiments, can also be using chromium tantalum-titanium alloy sample described in alcohol washes.
In some other embodiment, the metallographic etching of the chromium tantalum-titanium alloy specimen surface can also be first removed with clear water Agent, then the chromium tantalum-titanium alloy sample described in alcohol washes, to enhance cleaning effect.
In the present embodiment, after the corrosion treatment, metallographic observation is carried out to the chromium tantalum-titanium alloy sample 200.
Specifically, metallographic observation is carried out to the chromium tantalum-titanium alloy sample 200 using metallographic microscope.
By These steps, in particular by the metallographic etching agent as made of hydrofluoric acid, sulfuric acid, nitric acid and mixed in hydrochloric acid The burnishing surface 250 of 350 pairs of chromium tantalum-titanium alloy samples 200 carries out corrosion treatment, makes the crystalline substance of the chromium tantalum-titanium alloy sample 200 Boundary is apparent, and metallographic structure has better display effect, can preferably carry out metallographic observation using metallographic microscope, favorably Correct Analysis is carried out in the structure to the chromium tantalum-titanium alloy sample 200.
Although oneself is disclosed in the preferred embodiments as above the present invention, present invention is not limited to this.Any art technology Personnel can make various changes or modifications, therefore protection scope of the present invention is answered without departing from the spirit and scope of the present invention When being defined by the scope defined by the claims..

Claims (20)

1. a kind of metallographic etching agent of chromium tantalum-titanium alloy characterized by comprising the metallographic etching agent be hydrofluoric acid, sulfuric acid, The mixed solution of nitric acid and hydrochloric acid.
2. metallographic etching agent as described in claim 1, which is characterized in that the metallographic etching agent is by mass percent concentration The sulfuric acid that 40% to 43% hydrofluoric acid, mass percent concentration are 95% to 98%, mass percent concentration are The hydrochloric acid that 65% to 68% nitric acid and mass percent concentration is 36% to 38% is 5:2 according to volume ratio: 2:2 is formulated.
3. a kind of display methods of chromium tantalum-titanium alloy metallographic structure characterized by comprising
Chromium tantalum-titanium alloy sample is provided;
The chromium tantalum-titanium alloy sample is surface-treated, an at least burnishing surface is formed;
Corrosion treatment is carried out using burnishing surface of the metallographic etching agent as described in claim 1 to the chromium tantalum-titanium alloy sample.
4. the display methods of metallographic structure as claimed in claim 3, which is characterized in that the metallographic etching agent is by quality percentage The sulfuric acid that the hydrofluoric acid that specific concentration is 40% to 43%, mass percent concentration are 95% to 98%, quality percentage The hydrochloric acid that the nitric acid and mass percent concentration that specific concentration is 65% to 68% are 36% to 38% is according to volume Than being formulated for 5:2:2:2.
5. the display methods of metallographic structure as claimed in claim 3, which is characterized in that the step of providing chromium tantalum-titanium alloy sample Include:
Chromium tantalum-titanium alloy target is provided;
A part is cut from the chromium tantalum-titanium alloy target as chromium tantalum-titanium alloy sample.
6. the display methods of metallographic structure as claimed in claim 3, which is characterized in that the step of surface treatment include according to The grinding technics and polishing process of secondary progress.
7. the display methods of metallographic structure as claimed in claim 6, which is characterized in that the step of grinding technics includes: Successively the chromium tantalum-titanium alloy specimen surface is ground using the sand paper of grit progression.
8. the display methods of metallographic structure as claimed in claim 7, which is characterized in that the sand paper is respectively 400#, 800# With the aqueous sand paper of 1500#.
9. the display methods of metallographic structure as claimed in claim 7, which is characterized in that in the grinding technics the step of, The sand paper is placed on grinder, is ground using water as wetting agent.
10. the display methods of metallographic structure as claimed in claim 9, which is characterized in that the revolving speed of the grinder is 300 Rev/min to 400 revs/min, the total time of the grinding technics is 5 minutes to 10 minutes.
11. the display methods of metallographic structure as claimed in claim 6, which is characterized in that the step of polishing process includes: The chromium tantalum-titanium alloy specimen surface after grinding is mechanically polished using the flannelette for being moistened with diamond paste.
12. the display methods of metallographic structure as claimed in claim 11, which is characterized in that the mechanical polishing the step of In, the flannelette is set on grinder, and is polished using water as wetting agent.
13. the display methods of metallographic structure as claimed in claim 12, which is characterized in that the revolving speed of the grinder is 300 Rev/min to 400 revs/min, polishing time is 2 minutes to 3 minutes.
14. the display methods of metallographic structure as claimed in claim 3, which is characterized in that after the surface treatment, described Before corrosion treatment, further comprises the steps of: and the chromium tantalum-titanium alloy sample is cleaned using clear water.
15. the display methods of metallographic structure as claimed in claim 3, which is characterized in that the processing time of the corrosion treatment It is 60 seconds to 90 seconds.
16. the display methods of metallographic structure as claimed in claim 3, which is characterized in that the step of corrosion treatment includes:
The metallographic etching agent is provided;
The burnishing surface of the chromium tantalum-titanium alloy sample is immersed in the metallographic etching agent and is corroded.
17. the display methods of metallographic structure as claimed in claim 16, which is characterized in that the burnishing surface is made to be parallel to level Face direction immerses the burnishing surface in the metallographic etching agent;
Alternatively, making the burnishing surface perpendicular to horizontal plane direction, the burnishing surface is immersed in the metallographic etching agent.
18. the display methods of metallographic structure as claimed in claim 3, which is characterized in that the chromium tantalum-titanium alloy sample After burnishing surface carries out corrosion treatment, further comprises the steps of: and metallographic observation is carried out to the chromium tantalum-titanium alloy sample.
19. the display methods of metallographic structure as claimed in claim 18, which is characterized in that the chromium tantalum-titanium alloy sample After burnishing surface carries out corrosion treatment, before carrying out metallographic observation to the chromium tantalum-titanium alloy sample, further comprise the steps of:
The chromium tantalum-titanium alloy sample is taken out from the metallographic etching agent;
After taking out the chromium tantalum-titanium alloy sample, the chromium tantalum-titanium alloy sample is started the cleaning processing;
After the cleaning treatment, drying processing is carried out to the chromium tantalum-titanium alloy sample.
20. the display methods of metallographic structure as claimed in claim 19, which is characterized in that the step of cleaning treatment wraps It includes: the chromium tantalum-titanium alloy sample is cleaned using alcohol or clear water;
Alternatively, first using chromium tantalum-titanium alloy sample described in alcohol washes again with clear water.
CN201710546141.7A 2017-07-06 2017-07-06 The metallographic etching agent of chromium tantalum-titanium alloy and its display methods of metallographic structure Pending CN109211645A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109738444A (en) * 2019-03-01 2019-05-10 株洲硬质合金集团有限公司 A kind of method of quick detection tantalum, niobium and its alloy microstructure
CN110118778A (en) * 2019-05-13 2019-08-13 中天钢铁集团有限公司 A kind of medium carbon steel ferrite metallographic etching agent and ferritic structure metallographic phase display method
CN111751184A (en) * 2020-07-03 2020-10-09 合肥工业大学 A kind of preparation method of tantalum and tantalum-tungsten alloy metallographic sample
CN111879845A (en) * 2020-07-24 2020-11-03 宁波江丰电子材料股份有限公司 Mixed acid for dissolving chromium-tantalum-titanium alloy and preparation method and application thereof
CN112665953A (en) * 2020-10-29 2021-04-16 北京星航机电装备有限公司 Metallographic structure corrosive agent and corrosion method for Ti60 titanium alloy oxide layer
CN112782168A (en) * 2020-12-24 2021-05-11 南京海通电子材料科技有限公司 Method for continuous cutting of metal and in-situ display of metallographic phase
CN114526978A (en) * 2022-02-25 2022-05-24 中国工程物理研究院材料研究所 Metallographic corrosive liquid of vanadium alloy and preparation method of metallographic sample of vanadium alloy

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1083096A1 (en) * 1982-01-05 1984-03-30 Северо-Западный Заочный Политехнический Институт Electrolyte for colored electrochemical etching of titanium alloys
JPS60114739A (en) * 1983-11-28 1985-06-21 Daido Steel Co Ltd Ti polishing and corrosion method
CN101519779A (en) * 2008-02-27 2009-09-02 株式会社神户制钢所 Surface treatment method of titanium material for electrode
CN101576454A (en) * 2008-05-08 2009-11-11 比亚迪股份有限公司 Amorphous alloy metallic phase corrosive agent and metallic phase display method
CN102331363A (en) * 2011-08-12 2012-01-25 西部金属材料股份有限公司 Method for observing metallographic structure of niobium-titanium alloy
CN102866047A (en) * 2012-09-28 2013-01-09 昆明理工大学 Method for preparing metallographic display sample made of Ti-Al laminated composite material
CN106415919A (en) * 2014-03-31 2017-02-15 泰克年研究发展基金会公司 Passive metal activation method and use thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1083096A1 (en) * 1982-01-05 1984-03-30 Северо-Западный Заочный Политехнический Институт Electrolyte for colored electrochemical etching of titanium alloys
JPS60114739A (en) * 1983-11-28 1985-06-21 Daido Steel Co Ltd Ti polishing and corrosion method
CN101519779A (en) * 2008-02-27 2009-09-02 株式会社神户制钢所 Surface treatment method of titanium material for electrode
CN101576454A (en) * 2008-05-08 2009-11-11 比亚迪股份有限公司 Amorphous alloy metallic phase corrosive agent and metallic phase display method
CN102331363A (en) * 2011-08-12 2012-01-25 西部金属材料股份有限公司 Method for observing metallographic structure of niobium-titanium alloy
CN102866047A (en) * 2012-09-28 2013-01-09 昆明理工大学 Method for preparing metallographic display sample made of Ti-Al laminated composite material
CN106415919A (en) * 2014-03-31 2017-02-15 泰克年研究发展基金会公司 Passive metal activation method and use thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
潘光华等: "显示钛合金组织中α相三维形貌的恒电位电解深蚀法", 《稀有金属》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109738444A (en) * 2019-03-01 2019-05-10 株洲硬质合金集团有限公司 A kind of method of quick detection tantalum, niobium and its alloy microstructure
CN110118778A (en) * 2019-05-13 2019-08-13 中天钢铁集团有限公司 A kind of medium carbon steel ferrite metallographic etching agent and ferritic structure metallographic phase display method
CN111751184A (en) * 2020-07-03 2020-10-09 合肥工业大学 A kind of preparation method of tantalum and tantalum-tungsten alloy metallographic sample
CN111879845A (en) * 2020-07-24 2020-11-03 宁波江丰电子材料股份有限公司 Mixed acid for dissolving chromium-tantalum-titanium alloy and preparation method and application thereof
CN112665953A (en) * 2020-10-29 2021-04-16 北京星航机电装备有限公司 Metallographic structure corrosive agent and corrosion method for Ti60 titanium alloy oxide layer
CN112782168A (en) * 2020-12-24 2021-05-11 南京海通电子材料科技有限公司 Method for continuous cutting of metal and in-situ display of metallographic phase
CN112782168B (en) * 2020-12-24 2022-08-09 南京海通电子材料科技有限公司 Method for continuous cutting of metal and in-situ display of metallographic phase
CN114526978A (en) * 2022-02-25 2022-05-24 中国工程物理研究院材料研究所 Metallographic corrosive liquid of vanadium alloy and preparation method of metallographic sample of vanadium alloy
CN114526978B (en) * 2022-02-25 2024-01-02 中国工程物理研究院材料研究所 Metallographic corrosive liquid of vanadium alloy and preparation method of metallographic sample of vanadium alloy

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