CN111721764A - Method for identifying equiaxed titanium alloy - Google Patents
Method for identifying equiaxed titanium alloy Download PDFInfo
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- CN111721764A CN111721764A CN201910219369.4A CN201910219369A CN111721764A CN 111721764 A CN111721764 A CN 111721764A CN 201910219369 A CN201910219369 A CN 201910219369A CN 111721764 A CN111721764 A CN 111721764A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/204—Structure thereof, e.g. crystal structure
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Abstract
The invention relates to a method for identifying an equiaxial titanium alloy, which comprises the following steps: polishing a sample to be identified to obtain a polished surface, wherein the roughness of the polished surface meets the preset roughness range; etching the polished face to obtain a viewing face; and judging that the sample to be identified is the equiaxial titanium alloy according to the first phase and the second phase which are regularly distributed on the observation surface. The identification method of the invention has low cost, short time and good accuracy.
Description
Technical Field
The invention relates to the technical field of titanium alloys, in particular to a method for identifying equiaxial titanium alloys.
Background
Titanium alloys have been widely used in various fields because of their high strength, good corrosion resistance, high heat resistance, and the like. Different phase compositions and structures of the titanium alloy can be obtained by adjusting the heat treatment process, and experiments show that the fine equiaxial structure (namely equiaxial titanium alloy) has better plasticity, thermal stability and fatigue strength.
At present, the equiaxial titanium alloy is identified mainly by adopting an XRD (X-ray Diffraction) detection mode, and the problems of high detection cost, long detection time, need of contrast mapping and the like exist.
Disclosure of Invention
In view of the above, there is a need to provide a method for identifying equiaxed titanium alloy with low detection cost, short time and good accuracy, so as to solve the above problems.
The invention provides a method for identifying an equiaxial titanium alloy, which comprises the following steps:
polishing a sample to be identified to obtain a polished surface, wherein the roughness of the polished surface meets the preset roughness range;
etching the polished face to obtain a viewing face;
and judging that the sample to be identified is the equiaxial titanium alloy according to the first phase and the second phase which are regularly distributed on the observation surface.
Further, the predetermined roughness range is less than 5 microns.
Further, the etching step includes a step of etching the polishing surface by an etching solution, and the etching solution is a hydrofluoric acid solution or a fluorine-containing salt solution.
Further, the mass fraction of the corrosive liquid is 0.1-40%.
Further, in the etching step, the polishing surface is etched for 5-30 seconds by the etching liquid. Further, the method includes a step of rinsing the etching solution on the polishing surface.
Further, the method may further comprise a step of drying the polished surface by blow-drying or baking with an air gun.
Further, the first phase is an alpha phase and the second phase is a beta phase.
The method for identifying the equiaxial titanium alloy provided by the invention identifies whether the sample to be identified is the equiaxial titanium alloy or not by observing the phase after polishing and etching processes meeting certain conditions, and can accurately identify the equiaxial titanium alloy when a first phase and a second phase which are regularly distributed appear on an observation surface. Compared with the traditional identification technology, the identification method provided by the invention is low in cost, short in time and good in accuracy, can be widely applied to the field of titanium and titanium alloy surface treatment, and plays a great help role in subsequently preparing the grain boundary type oxide film.
Drawings
FIG. 1 is a flow chart of a method of identifying an equiaxed titanium alloy according to an embodiment of the present invention.
Fig. 2 is an SEM image of an equiaxed titanium alloy observed using the method of identifying equiaxed titanium alloys shown in fig. 1.
Fig. 3 is an SEM image of an non-equiaxed titanium alloy observed using the method of identifying equiaxed titanium alloys shown in fig. 1.
Fig. 4 is an SEM image of another non-equiaxed titanium alloy observed using the method of identifying equiaxed titanium alloys shown in fig. 1.
Detailed Description
In order to make the objects, technical solutions and advantageous effects of the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and the detailed description. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Referring to fig. 1, an embodiment of the present invention provides a method for identifying an equiaxed titanium alloy, which mainly includes the following steps:
s1 cutting the titanium alloy to be identified to obtain a sample to be identified;
s2, polishing the sample to be identified to obtain a polished surface, wherein the roughness of the polished surface meets the preset roughness range;
s3 etching the polished surface;
s4, washing the polished surface;
s5, drying the polished surface to obtain an observation surface;
s6, according to the first phase and the second phase with regularly distributed observation surfaces, judging that the sample to be identified is the equiaxial titanium alloy.
Wherein the first phase is an alpha phase and the second phase is a beta phase. It is to be noted that titanium is a homoisomer, has a melting point of 1668 ℃, and has a close-packed hexagonal lattice structure below 882 ℃, and is called alpha titanium; the titanium alloy has a body-centered cubic lattice structure above 882 ℃, and is called beta titanium. By utilizing the different characteristics of the two structures of titanium, proper alloy elements are added, so that the phase transition temperature and the phase composition content of the titanium are gradually changed to obtain the titanium alloy with different structures. At room temperature, titanium alloys have three matrix structures, and the titanium alloys are classified into the following three types: alpha alloys, (alpha + beta) alloys, and beta alloys.
Specifically, the observation phase may employ a microscope, but is not limited thereto. In step S1, since the sample to be observed with the microscope needs to satisfy a certain shape and size, a portion of an appropriate size needs to be cut on the titanium alloy to be identified as the sample to be identified.
The principle of polishing and etching a surface of the sample to be identified in steps S2 and S3 is: the surface of a sample to be identified is more uniform after being polished, and the corrosion rates of the alpha phase and the beta phase are different in the etching process, so that the heights of the alpha phase region and the beta phase region are different, and the distribution condition of the alpha phase and the beta phase can be obviously observed when the sample is observed under a microscope.
Preferably, the predetermined roughness range of the polished surface is less than 5 μm.
In some embodiments, the etching solution is a hydrofluoric acid solution or a fluorine-containing salt solution. The chemical formula of the hydrofluoric acid solution and the fluorine-containing salt solution during etching is as follows:
2Ti+6HF→2TiF3+3H2× (hydrofluoric acid solution);
2Ti+6H2O+6F-→2TiF3+3H2↑+6OH-(fluoride salt solution).
In some preferred embodiments, the mass fraction of the corrosive liquid is 0.1-40%. It should be noted that, too large or too small mass fraction of the corrosive liquid may adversely affect the corrosion effect, for example, if too small mass fraction of the corrosive liquid, the corrosion effect is insufficient, which easily causes the boundary (i.e. grain boundary) between the α -phase region and the β -phase region to be inconspicuous, so that the distribution of the α -phase and β -phase cannot be accurately observed, which affects the identification accuracy; if the mass fraction of the corrosive liquid is too large, the corrosion condition is too serious, the microstructure observation is also influenced, and the identification accuracy is not facilitated. In addition, the time for the corrosive liquid to stay on the polishing surface is 5-30 seconds, so that the corrosion effect is better controlled.
Specifically, a dropper is adopted to drop the corrosive liquid onto the polishing surface so as to control the dropping amount and the dropping position of the corrosive liquid.
In step S4, the etching solution on the polishing surface is washed with clean water, which not only can wash away the etching solution on the polishing surface, but also has the characteristics of low cost, no chemical pollution, and the like.
In step S5, the drying and polishing surface is dried by an air gun, and the drying method has little influence on the surface state of the sample to be identified.
In one particular embodiment, a method of identifying an equiaxed titanium alloy includes the steps of: cutting the titanium alloy to be identified to obtain a sample to be identified; polishing a sample to be identified to obtain a polished surface with the roughness less than 5 microns; etching the polished surface for 10s by adopting a hydrofluoric acid solution with the mass fraction of 20%; washing the etched polished surface with clear water; drying the polished surface by an air gun to obtain an observation surface; the observation surface was observed with a microscope.
Referring to fig. 2 to 4, fig. 2 is an SEM (scanning Electron microscope) image of an equiaxed titanium alloy obtained by the method for identifying equiaxed titanium alloys, and fig. 3 and 4 are SEM images of an non-equiaxed titanium alloy obtained by the method for identifying equiaxed titanium alloys. It can be seen that the microstructure of the equiaxed titanium alloy has a regular distribution of alpha phase and beta phase in bulk, which is clearly different from the microstructure of the non-equiaxed titanium alloy. Therefore, if the observation surface shows alpha phase and beta phase which are regularly distributed, the sample to be identified is equiaxial titanium alloy; if the viewing surface does not exhibit a regular distribution of alpha and beta phases, e.g., the phases are randomly or striped, then the sample to be identified is an equiaxed titanium alloy.
The method for identifying the equiaxial titanium alloy provided by the invention identifies whether the sample to be identified is the equiaxial titanium alloy or not by observing the phase after polishing and etching processes meeting certain conditions, and can accurately identify the equiaxial titanium alloy when a first phase and a second phase which are regularly distributed appear on an observation surface. Compared with the traditional identification technology, the identification method provided by the invention is low in cost, short in time and good in accuracy, can be widely applied to the field of titanium and titanium alloy surface treatment, and plays a great help role in subsequently preparing the grain boundary type oxide film.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. A method of identifying an equiaxed titanium alloy, comprising: the method comprises the following steps:
polishing a sample to be identified to obtain a polished surface, wherein the roughness of the polished surface meets the preset roughness range;
etching the polished face to obtain a viewing face;
and judging that the sample to be identified is the equiaxial titanium alloy according to the first phase and the second phase which are regularly distributed on the observation surface.
2. The method of identifying an equiaxed titanium alloy of claim 1, wherein: the predetermined roughness range is less than 5 microns.
3. The method of identifying an equiaxed titanium alloy of claim 1, wherein: the etching step comprises a step of etching the polishing surface by corrosive liquid, wherein the corrosive liquid is hydrofluoric acid solution or fluorine-containing salt solution.
4. A method of identifying an equiaxed titanium alloy according to claim 3, wherein: the mass fraction of the corrosive liquid is 0.1-40%.
5. A method of identifying an equiaxed titanium alloy according to claim 3, wherein: and in the etching step, the polished surface is etched for 5-30 seconds by the etching solution.
6. The method of identifying an equiaxed titanium alloy of claim 1, wherein: the method also includes a step of rinsing the etching solution on the polishing surface.
7. The method of identifying an equiaxed titanium alloy of claim 6, wherein: the method further comprises a step of drying the polished surface by blow-drying or baking with an air gun.
8. The method of identifying an equiaxed titanium alloy of claim 1, wherein: the first phase is an alpha phase and the second phase is a beta phase.
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| CN201910219369.4A CN111721764A (en) | 2019-03-21 | 2019-03-21 | Method for identifying equiaxed titanium alloy |
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Citations (7)
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| CN102808179A (en) * | 2011-05-31 | 2012-12-05 | 西安赛特金属材料开发有限公司 | Metallographic etchant and metallographic etching method for pure titanium and beta titanium alloy |
| CN103323310A (en) * | 2013-06-26 | 2013-09-25 | 西安赛特思迈钛业有限公司 | Preparation methods of large-size titanium and titanium alloy metallographic specimens |
| CN103484863A (en) * | 2012-06-07 | 2014-01-01 | 宁波江丰电子材料有限公司 | Metallographic corrosive, corrosion method for metallographic sample and display method for metallographic structure |
| CN104032303A (en) * | 2014-06-26 | 2014-09-10 | 北京石油化工学院 | Metallographic phase corrosive of pure titanium TA1 and TC4 titanium alloy |
| CN106702383A (en) * | 2016-07-05 | 2017-05-24 | 中国航空工业集团公司北京航空材料研究院 | Metallographic-phase corrosion liquid of beta titanium alloy and corrosion method |
| CN107723710A (en) * | 2017-11-15 | 2018-02-23 | 北京石油化工学院 | A kind of metallographic etching agent and its application method of the pure titanium or titanium alloy of annealed state |
| CN107988599A (en) * | 2017-12-06 | 2018-05-04 | 航天精工股份有限公司 | A kind of metallographic etching agent for distinguishing titanium alloy condition of heat treatment |
-
2019
- 2019-03-21 CN CN201910219369.4A patent/CN111721764A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102808179A (en) * | 2011-05-31 | 2012-12-05 | 西安赛特金属材料开发有限公司 | Metallographic etchant and metallographic etching method for pure titanium and beta titanium alloy |
| CN103484863A (en) * | 2012-06-07 | 2014-01-01 | 宁波江丰电子材料有限公司 | Metallographic corrosive, corrosion method for metallographic sample and display method for metallographic structure |
| CN103323310A (en) * | 2013-06-26 | 2013-09-25 | 西安赛特思迈钛业有限公司 | Preparation methods of large-size titanium and titanium alloy metallographic specimens |
| CN104032303A (en) * | 2014-06-26 | 2014-09-10 | 北京石油化工学院 | Metallographic phase corrosive of pure titanium TA1 and TC4 titanium alloy |
| CN106702383A (en) * | 2016-07-05 | 2017-05-24 | 中国航空工业集团公司北京航空材料研究院 | Metallographic-phase corrosion liquid of beta titanium alloy and corrosion method |
| CN107723710A (en) * | 2017-11-15 | 2018-02-23 | 北京石油化工学院 | A kind of metallographic etching agent and its application method of the pure titanium or titanium alloy of annealed state |
| CN107988599A (en) * | 2017-12-06 | 2018-05-04 | 航天精工股份有限公司 | A kind of metallographic etching agent for distinguishing titanium alloy condition of heat treatment |
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Application publication date: 20200929 |