CN110146532A - A kind of differentiating method of MX phase and Laves phase for mutually counting - Google Patents
A kind of differentiating method of MX phase and Laves phase for mutually counting Download PDFInfo
- Publication number
- CN110146532A CN110146532A CN201910479873.8A CN201910479873A CN110146532A CN 110146532 A CN110146532 A CN 110146532A CN 201910479873 A CN201910479873 A CN 201910479873A CN 110146532 A CN110146532 A CN 110146532A
- Authority
- CN
- China
- Prior art keywords
- phase
- laves
- electrolytic etching
- laves phase
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The differentiating method of the MX phase and Laves phase that the invention discloses a kind of for mutually counting, counted suitable for solidifying state high temperature alloy the area fraction of MX phase and Laves phase, the specific operation process of the differentiating method are as follows: step 1: by polished sample in NaOH aqueous solution electrolytic etching 2s (current density 0.2-0.3A/cm2), the sample after corrosion is cleaned by ultrasonic, heated-air drying is then used；Second step, by sample as being observed under the back-scattered electron mode of scanning electron microscope.Using differentiating method of the invention, MX phase and Laves phase can be distinguished with being apparent, and the statistics of the information such as the size subsequently with respect to phase, distribution, quantity and content can be carried out.This method is easy to operate, and the differentiation effect of phase is good, the differentiation of MX phase and Laves phase suitable for Ni based high-temperature alloy.
Description
Technical field
The present invention relates to the fabric analysis technical fields of alloy material, and in particular to a kind of MX phase for mutually counting and
The differentiating method of Laves phase.
Background technique
Ni based high-temperature alloy has excellent high temperature strength and antioxygenic property, be widely used in aerospace, the energy and
The critical equipment in the fields such as petrochemical industry manufactures, and Ni based high-temperature alloy weld metal or cast member are often analysed simultaneously in solidification
MX carbide (nitride) and Laves intermetallic compound out.In investigation of materials, it is often necessary to quantity, ruler to both phases
The information such as very little and distribution are counted.The size of MX phase and Laves phase is generally at 5 microns hereinafter, optical microscopy can not understand
Observation.Pass through corrosive agent oxalic acid or CuSO conventional in high temperature alloy4MX phase and Laves after solution corrosion, under scanning electron microscope
Phase color is close, can not distinguish well.Further, since MX phase and Laves phase all contain heavy element (such as Nb), even if the two exists
It can not still be distinguished under scanning electron microscope back scattering contrast mode.This causes to be stranded to the Information Statistics work of two kinds of phases in high temperature alloy
It disturbs.
Summary of the invention
In order to solve when MX phase coexists with Laves phase in Ni based high-temperature alloy, existing microcosmic imaging technique is not easy to
The two is carried out to distinguish this technical problem, the MX phase and Laves phase that the purpose of the present invention is to provide a kind of for mutually counting
Differentiating method, this is a kind of new corrosion observation method, and this method can make MX phase and laves in electron microscopic tissue
Mutually show apparent colouring discrimination, quite convenient for individually for statistical analysis to the quantity of both phases, distribution and size.
To achieve the above object, technical solution of the present invention is as follows:
A kind of differentiating method of MX phase and Laves phase for mutually counting, this method are for solidification state high temperature alloy material
Material carries out electrolytic etching as corrosive agent using NaOH aqueous solution, and realizes MX phase and Laves phase by scanning electron microscope
Significant differentiation.The differentiating method includes the following steps:
(1) polished nickel base superalloy sample electrolytic etching: is subjected to electrolytic etching, electric current in NaOH aqueous solution
Density 0.2-0.3A/cm2, electrolytic etching time 2-8s；The sample after corrosion is cleaned by ultrasonic with alcohol, hot wind after cleaning
Drying for standby；
(2) sample after step (1) electrolytic etching is placed in scanning electron microscope to observe, according to color difference
MX phase and Laves phase can obviously be distinguished.
During above-mentioned steps (1) electrolytic etching, the concentration of the NaOH aqueous solution is 0.1-0.2g/mL.
In above-mentioned steps (2), sample observation method is the back-scattered electron mode of scanning electron microscope.
The differentiating method suitable under electron scanning micrograph to solidification state Ni based high-temperature alloy MX phase and
Laves phase distinguishes.
Advantages of the present invention is as follows:
The method that the present invention is combined using particular etch liquid, caustic solution and scanning electron microscope back-scattered electron mode, simply
It is easy, MX can be mutually clearly distinguished with two kinds of Laves, be highly suitable for coexisting in Ni base height in MX with Laves phase
When in temperature alloy, applied when statisticalling analyze phase amount, distribution and size.
Detailed description of the invention
Fig. 1 is in comparative example 1 using Ni-Fe based high-temperature alloy weld metal after the electrolytic etching of 10wt.% oxalic acid aqueous solution
Secondary electron scanned photograph.
Fig. 2 is that 20g CuSO is used in comparative example 24·5H2O+5ml H2SO4+100ml HCl+100ml H2O solution corrosion
The secondary electron scanned photograph of Ni-Fe based high-temperature alloy (weld metal) afterwards.
Fig. 3 is in comparative example 3 using solidification state Ni-Fe based high-temperature alloy (weldering after the electrolytic etching of 10wt.% oxalic acid aqueous solution
Stitch metal) back scattering scanned photograph.
Fig. 4 is that 20g NaOH+100ml H is used in comparative example 42State Ni-Fe based high-temperature alloy is solidified after O electrolytic etching
The secondary electron scanned photograph of (weld metal).
Fig. 5 is that 20g NaOH+100ml H is used in embodiment 12State Ni-Fe based high-temperature alloy is solidified after O electrolytic etching
The back scattering scanned photograph of (weld metal).
Fig. 6 is that 20g NaOH+100ml H is used in embodiment 22State GH4169 high temperature alloy (half is solidified after O electrolytic etching
Solid molding) back scattering scanned photograph.
Specific embodiment
The present invention is described in detail below by attached drawing and specific embodiment.
Comparative example 1
Using conventional corrosion agent 10wt.% oxalic acid aqueous solution electrolytic etching 10s (decomposition voltage 5V), it is high to obtain Ni-Fe base
The secondary electron of temperature alloy weld metal scans macrograph.It is as shown in Figure 1 the secondary of Ni-Fe based high-temperature alloy weld metal
Electron scanning photo, precipitated phase indicated by white and black arrow is respectively Laves phase and MX phase in photo, it is seen that two kinds of phases
And it can not obviously distinguish, the subsequent statistics that can not carry out phase.
Comparative example 2
Use conventional Ni (Ni-Fe) based high-temperature alloy corrosive agent Cu2SO4(formula is 20gCuSO to solution4·5H2O+5ml
H2SO4+100ml HCl+100ml H2O) chemical attack 15s, the secondary electron for obtaining Ni-Fe based high-temperature alloy weld metal are swept
Retouch photo.It is illustrated in figure 2 the secondary electron scanned photograph of Ni-Fe based high-temperature alloy weld metal, can not be divided at all in photo
Clear laves phase and MX phase.
Comparative example 3
Using conventional corrosion agent 10wt.% oxalic acid aqueous solution electrolytic etching 10s (decomposition voltage 5V), it is high to obtain Ni-Fe base
The scanning macrograph of temperature alloy weld metal.The Ni-Fe based high-temperature alloy weld seam being illustrated in figure 3 under back-scattered electron mode
The scanned photograph of metal, it is seen that laves phase and MX phase cannot be distinguished almost without difference in the contrast of the precipitated phase in tissue.
Comparative example 4
Use NaOH aqueous solution (20g NaOH+100ml H2O) electrolytic etching about 2s (corrosion electric current density 0.2-
0.3A/cm2), the secondary electron for obtaining Ni-Fe base weld metal scans macrograph.It is illustrated in figure 4 the conjunction of Ni-Fe base high temperature
The secondary electron scanned photograph of golden weld metal, precipitated phase indicated by white and black arrow is respectively Laves phase in photo
With MX phase, black in tissue mutually as MX phase, but Laves phase and matrix color are close, it is virtually impossible to recognize.
Embodiment 1
100ml water is placed in beaker at room temperature by the first step, and 20g NaOH is added, is dissolved into utmostly to NaOH.It will throw
The good sample of light (the Ni-Fe based high-temperature alloy weld metal of argon tungsten-arc welding built-up welding) electrolytic etching 2s, corrosion electric current density are
0.2-0.3A/cm2, then sample is put into alcohol and is cleaned by ultrasonic, it is spare with hot-air seasoning after cleaning；
The sample of first step electrolytic etching is placed under scanning electron microscopy Electronic Speculum, and is adjusted to backscattered electron by second step
Mode carries out structure observation.
As shown in figure 5, observing Ni-Fe based high-temperature alloy weld seam gold using the present embodiment MX and Laves phase differentiating method
MX phase (shown in black arrow) is in black in category, and Laves phase (shown in white arrow) is in canescence, and matrix is in dark gray, can be with
It is fine to distinguish MX phase and Laves phase.
Embodiment 2
100ml water is placed in beaker at room temperature by the first step, and 20g NaOH is added, is dissolved into utmostly to NaOH.It will throw
The good sample of light (semi-solid-state shaping GH4169 high temperature alloy) electrolytic etching 2s, corrosion electric current density 0.2-0.3A/cm2, so
Sample is put into alcohol afterwards and is cleaned by ultrasonic, it is spare with hot-air seasoning after cleaning；
The sample of first step electrolytic etching is placed under scanning electron microscopy Electronic Speculum, and is adjusted to backscattered electron by second step
Mode carries out structure observation.
As shown in fig. 6, observing the GH4169 high temperature of semi-solid-state shaping using the present embodiment MX and Laves differentiating method
Alloy microstructure, MX phase (shown in black arrow) are in black, and Laves phase (shown in white arrow) is in canescence, and matrix is in dark
Grey can clearly be debated, and profile is obvious.
Claims (5)
1. a kind of differentiating method of MX phase and Laves phase for mutually counting, it is characterised in that: this method is high for solidification state
Temperature alloy material carries out electrolytic etching as corrosive agent using NaOH aqueous solution, and realizes MX phase by scanning electron microscope
With the significant differentiation of Laves phase.
2. the differentiating method of the MX phase and Laves phase according to claim 1 for mutually counting, it is characterised in that: the area
Point method includes the following steps:
(1) polished nickel base superalloy sample electrolytic etching: is subjected to electrolytic etching, current density in NaOH aqueous solution
0.2-0.3A/cm2, electrolytic etching time 2-10s；The sample after corrosion is cleaned by ultrasonic with alcohol, hot air drying after cleaning
It is dry spare；
(2) sample after step (1) electrolytic etching scanning electron microscope is placed in observe, it can according to color difference
Obviously distinguish MX phase and Laves phase.
3. the differentiating method of the MX phase and Laves phase according to claim 2 for mutually counting, it is characterised in that: step
(1) during electrolytic etching, the concentration of the NaOH aqueous solution is 0.1-0.2g/mL.
4. the differentiating method of the MX phase and Laves phase according to claim 2 for mutually counting, it is characterised in that: step
(2) in, sample observation method is the back-scattered electron mode of scanning electron microscope.
5. the differentiating method of the MX phase and Laves phase according to claim 1 for mutually counting, it is characterised in that: the area
Point method is suitable for carrying out area with Laves phase to MX phase solidification state Ni based high-temperature alloy under electron scanning micrograph
Point.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910479873.8A CN110146532B (en) | 2019-06-04 | 2019-06-04 | Method for distinguishing MX phase and Laves phase for phase statistics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910479873.8A CN110146532B (en) | 2019-06-04 | 2019-06-04 | Method for distinguishing MX phase and Laves phase for phase statistics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110146532A true CN110146532A (en) | 2019-08-20 |
| CN110146532B CN110146532B (en) | 2021-08-03 |
Family
ID=67590354
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910479873.8A Active CN110146532B (en) | 2019-06-04 | 2019-06-04 | Method for distinguishing MX phase and Laves phase for phase statistics |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110146532B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112649259A (en) * | 2020-11-26 | 2021-04-13 | 中国科学院金属研究所 | Display method of boride in gamma-TiAl-based alloy |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60185136A (en) * | 1984-03-02 | 1985-09-20 | Mitsubishi Heavy Ind Ltd | Etching method |
| CN102486460A (en) * | 2010-12-01 | 2012-06-06 | 中国科学院金属研究所 | Method for discriminating Laves phase and carbide phase in high Nb iron nickel base high temperature alloy |
| CN102866172A (en) * | 2012-08-31 | 2013-01-09 | 广东电网公司电力科学研究院 | Measuring method of Laves phase content of T/P 92 steel |
| CN103674664A (en) * | 2013-10-21 | 2014-03-26 | 广东电网公司电力科学研究院 | Quantitative metallographic analysis method for phase M23C6 of Super 304H steel |
| KR20160038274A (en) * | 2014-09-30 | 2016-04-07 | 한국전력공사 | Evaluation method of stress corrosion cracking susceptibility on nickel based alloys |
| CN106637212A (en) * | 2016-09-14 | 2017-05-10 | 珠海格力电器股份有限公司 | Metallographic corrosive and alloy macrostructure display method |
| CN109342254A (en) * | 2018-09-19 | 2019-02-15 | 中国航发北京航空材料研究院 | A kind of method of fast quantitative analysis high temperature alloy inclusion content |
-
2019
- 2019-06-04 CN CN201910479873.8A patent/CN110146532B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60185136A (en) * | 1984-03-02 | 1985-09-20 | Mitsubishi Heavy Ind Ltd | Etching method |
| CN102486460A (en) * | 2010-12-01 | 2012-06-06 | 中国科学院金属研究所 | Method for discriminating Laves phase and carbide phase in high Nb iron nickel base high temperature alloy |
| CN102866172A (en) * | 2012-08-31 | 2013-01-09 | 广东电网公司电力科学研究院 | Measuring method of Laves phase content of T/P 92 steel |
| CN103674664A (en) * | 2013-10-21 | 2014-03-26 | 广东电网公司电力科学研究院 | Quantitative metallographic analysis method for phase M23C6 of Super 304H steel |
| KR20160038274A (en) * | 2014-09-30 | 2016-04-07 | 한국전력공사 | Evaluation method of stress corrosion cracking susceptibility on nickel based alloys |
| CN106637212A (en) * | 2016-09-14 | 2017-05-10 | 珠海格力电器股份有限公司 | Metallographic corrosive and alloy macrostructure display method |
| CN109342254A (en) * | 2018-09-19 | 2019-02-15 | 中国航发北京航空材料研究院 | A kind of method of fast quantitative analysis high temperature alloy inclusion content |
Non-Patent Citations (2)
| Title |
|---|
| L. GARCIA-FRESNILLO ET AL.: "Oxidation behaviour and phase transformations of an interconnect material in simulated anode environment of intermediate temperature solid oxide fuel cells", 《MATERIALS AT HIGH TEMPERATURES》 * |
| 机械系统理化检验协作网 等: "《金相检验》", 30 November 1983, 《理化检验》编辑部 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112649259A (en) * | 2020-11-26 | 2021-04-13 | 中国科学院金属研究所 | Display method of boride in gamma-TiAl-based alloy |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110146532B (en) | 2021-08-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Hurley et al. | Volta potentials measured by scanning Kelvin probe force microscopy as relevant to corrosion of magnesium alloys | |
| CN101806684B (en) | Specimen preparation and organization exposure method of metallic phase of zinc and alloy thereof | |
| CN102507619B (en) | Method for displaying EQZ (Equiaxed Grain Zone) textures of welded joints and fusion zones of 5A90 aluminum-lithium alloy laser welding | |
| Kumar et al. | Facile synthesis of gallium oxide hydroxide by ultrasonic irradiation of molten gallium in water | |
| CN110146532A (en) | A kind of differentiating method of MX phase and Laves phase for mutually counting | |
| CN106501052B (en) | A kind of preparation method for copper aluminum composite material electron backscatter diffraction analysis test sample | |
| Singh et al. | An overview on the preparation, characterization and properties of electrodeposited-metal matrix nanocomposites | |
| CN105617871B (en) | The preparation and its application in emulsion separation of a kind of super infiltration cobaltosic oxide nano pin perforated membrane | |
| Adabi et al. | Electrodeposition mechanism of Ni–Al composite coating | |
| CN110219031A (en) | Anodic oxidation electrolyte and method, the aluminum or aluminum alloy with anode oxide film | |
| CN108687339A (en) | Titanium or titanium alloy spherical powder of low oxygen content and its preparation method and application | |
| CN107761160B (en) | A kind of electrolytic etching agent of high-strength invar microscopic structure and caustic solution | |
| CN101608985A (en) | Coating shows a display packing of etchant and multi-coated coating institutional framework | |
| Atalay et al. | Influences of deposition time and pH on magnetic NiFe nanowires fabrication | |
| CN109211648A (en) | A kind of preparation method of alumina dispersion-strenghtened copper microstructure of the alloy sample | |
| CN113668035A (en) | One-step in-situ generation Zn-MOF coating on surface of micro-arc magnesium oxide alloy and preparation method thereof | |
| CN103913475A (en) | Method for determining structure of cobalt phase in WC-Co cemented carbide | |
| Rostami et al. | Improvements in microstructure and mechanical properties of Al–Si–Cu alloy–Al2O3 nanocomposite modified by ZrO2 | |
| CN110441119A (en) | The application of saturated oxalic acid solution, the electrolytic etching method of GH4169 alloy and microstructure observation's method | |
| Gianoncelli et al. | An in situ electrochemical soft X-ray spectromicroscopy investigation of Fe galvanically coupled to Au | |
| CN207742004U (en) | Non-metallic inclusion device in a kind of anodic dissolution process extraction metal material | |
| García-Antón et al. | Online visualization of corrosion processes of zinc and a Cu/Zn galvanic pair in lithium bromide solutions | |
| KR20190086274A (en) | Particle analysis method for composite, particle dispersion analysis method for composite and particle dispersion analysis system for composite | |
| Yermolenko et al. | AFM surface analysis of Fe-Co-Mo electrolytic coatings | |
| CN104846426B (en) | A kind of Nb Si based material microscopic structure corrosive agent and electrolytic etching method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |