CN106404477A - Sample preparation method for electron back scattering diffraction analysis of powder superalloy - Google Patents
Sample preparation method for electron back scattering diffraction analysis of powder superalloy Download PDFInfo
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- CN106404477A CN106404477A CN201610709460.0A CN201610709460A CN106404477A CN 106404477 A CN106404477 A CN 106404477A CN 201610709460 A CN201610709460 A CN 201610709460A CN 106404477 A CN106404477 A CN 106404477A
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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
- 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
- G01N1/34—Purifying; Cleaning
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention belongs to the technical field of detection analysis sample preparation, and relates to a sample preparation method for electron back scattering diffraction analysis of a powder superalloy. The method is as follows: surface mechanical grinding and mechanical polishing are performed on a powder superalloy sample; after the mechanical polishing, alcohol is used for washing and drying a to-be-analyzed surface; an electrolytic polishing liquid and a polishing cleaning liquid are prepared; an electrolyte is contained in an electrolyte tank as a negative pole; the polished surface of the sample is parallel to the liquid level of the electrolyte, and the sample is ultrasonically treated in the polishing process; after electrolysis is completed, the sample is quickly put into a methanol solution for ultrasonic cleaning; the sample is washed with the alcohol and dried until the surface is free of liquid stains; and the sample is put into a drying basin for saving for analysis. The method is simple in operation, by use of an ultrasonic manner for the sample respectively in an electrolytic polishing process and a cleaning process after the polishing process, the prepared sample has the advantages of clear Kikuchi patterns, easy calibration, little surface pollution and large analysis area, the surface quality is stable in preparation of a large number of samples, and the method has good popularization and application prospects.
Description
Technical field
The invention belongs to detection and analysis sample making technology field, it is related to one kind and is used for powder metallurgy superalloy EBSD
The method for making sample of analysis.
Background technology
Powder metallurgy superalloy is the high temperature alloy with powder metallurgy (PM, powder metallurgy) technique productions, due to
Which solve high-alloying degree wrought superalloy segregation serious and the problems such as hot-working character is poor, become modern high performance
The essential material of the core hot-end component such as aero-engine turbine disk.With the development further of aircraft industry, new height is had an high regard for
Than, high power to weight ratio and high fuel efficiency aero-engine, the performance of the hot-end component powder metallurgy superalloy such as turbine disk is proposed higher
Requirement.Powder metallurgy superalloy turbine disc of new generation adopts gradient heat treatment technics to obtain gradient structure, to meet diskware with this
The serviceability of different piece requires.In addition, utilizing bounding engineering (GBE, grain boundary engineering), pass through
The deformation optimizing and Technology for Heating Processing, can improve powder metallurgy superalloy low Σ CSL crystal boundary ratio, thus improve powder metallurgy closing
Golden plasticity and low cycle fatigue property.As can be seen here, the hot-end components such as the turbine disk are met by adjustment alloy structure state higher
Use requirement, be one of the first-selected technical scheme of powder metallurgy superalloy and route.
Generally, powder metallurgy superalloy preparation production technology include powder by atomization, powder deaeration, high temperature insostatic pressing (HIP), isothermal forging,
The processing steps such as heat treatment.Each thermal process step all can produce certain impact, especially isothermal forging and heat treatment to tissue
Technique.Due to the hereditary capacity of technical process and different process step tissue, need powder metallurgy superalloy technical process is carried out
System and comprehensive tissue detection and analysis.
EBSD (EBSD, electron backscatter diffraction) technology is based on scanning electricity
In mirror electron beam tilt the analysis of diffraction Kikuchi band that sample surfaces inspire and formed so that it is determined that crystal structure, orientation and
The method of relevant information.Because it has the unexistent quantitative crystallite dimension of conventional organization detection technique and distributional analysis, texture
Statistical analysis, grain boundary features and orientation analysis, the identification of phases and distributional analysis advantage, in recent years in powder metallurgy superalloy tissue detection
And analysis field obtains a wide range of applications.
For the method for making sample of powder metallurgy superalloy EBSD analysis, sample preparation step is many, is wherein electrolysed
Polishing affects larger on sample surfaces quality.Common electrolytic polishing method is due to cannot sample surfaces and electrolyte contacts face again
Produce stable high concentration saline solution polished film, the current density of local is higher or low will to produce throwing or electricity in polished surface
Solution derivative, these electrobrightening defects will cause EBSD Kikuchi style to be difficult to demarcate it is impossible to carry out diffraction
Analysis scanning, needs again to prepare sample.
Content of the invention
Present invention aims to above-mentioned sample making course present in not enough, provide and a kind of be used for powder metallurgy
The method for making sample of alloy EBSD analysis.
Technical scheme：Specifically carry out according to the following steps：
1) treat analysed for powder high temperature alloy and cut sample using wire cutting, specimen size is 10～15mm cubic block, profit
With gasoline washed samples surface and oil contaminant, after being dried, mark face to be analyzed；
2) using 200～600# waterproof abrasive paper, sample non-marked face is polished on pre-grinding test sample of gold phase machine, during grinding
Between metallic luster exposed by lapped face be defined, 200#, 400#, 600#, 800#, 1000#, 1500# are sequentially passed through to index face
Waterproof abrasive paper grinds, and observes lapped face every 30～60s in process of lapping, observes polishing scratch twice and no significantly reduces and no larger
Longer polishing scratch changes next number waterproof abrasive paper, grinds and is cleaned with water after finishing；
3) on metallographic-sample polisher, to sample, face to be analyzed mechanically polishes, and is sprayed with 3.5um diamond and polishes
Agent be sprayed onto on polishing flannelet to sample polish 5～8 minutes, after with 1.5um diamond spraying polishing agent be sprayed onto right on polishing flannelet
Sample polishes 3～5 minutes, changes water throwing polishing cloth and carries out water throwing 2～3 minutes, completes alcohol rinse post-drying after mechanical polishing；
4) electrolytic cell is placed on ultrasonic wave emission source, after opening ultrasonic wave emission source, clamps sample using metal tweezers,
Make sample face to be electrolysed level downwards, tweezers clip position is higher than face 5～6mm to be electrolysed, metal tweezers are steady by wire and voltage stabilizing
Stream dc source anode is connected, and negative electrode connects electrolytic cell, holds the methanol solution 100 that electrolyte is 18～20% hydrochloric acid in groove
～120mL, sample immersion electrolyte 2～4.5mm during electrobrightening, electrobrightening 15～20s, to electrolytic cell in polishing process
Middle electrolyte and sample carry out ultrasonic wave, and frequency is 30～45KHz；Electrolytic cell is pure nickel rounding post cup-like trough, diameter 75～
105mm, capacity is 200～250mL；Voltage stabilization and current stabilization direct current power source voltage 25～30V, electric current 3.5～5A, voltage stabilization and current stabilization direct current
The positive pole wire in source is connected with metal tweezers and fixes, and negative pole is connected and fixing with edge in cell wall；
5), after electrobrightening terminates, sample is put in methanol solution, carry out ultrasonic, taking-up alcohol after 50～60s immediately
It is rinsed, put into be analyzed in drying basin after drying.
Described step 2) in pre-grinding test sample of gold phase machine rotating speed be 500～600rpm.
Described step 2) grind when changing next number waterproof abrasive paper in sample, grind direction and turn 90 ° and grind.
Described step 3) in metallographic-sample polisher rotating speed be 300～400rpm.
In described step all be related to chemical solution agents useful for same be analysis pure.
It is an advantage of the current invention that introducing ultrasonic during electrobrightening, make to form thickness as the sample surfaces of anode
Degree direction uniform high concentration saline solution polished film, it is to avoid such as the surface local roughness that produced due to polishing non-uniform film thickness or go out
The surface quality problems such as existing pit.Traditional negative electrode nickel plate is replaced by one cathode electrolytic cell it is ensured that electrobrightening face is steady
Fixed uniform current density.In cleaning process, sample is carried out ultrasonic after a polish, effectively prevent secondary pollution.Therefore should
Method is made to take sample Kikuchi style clear it is easy to demarcate, and surface contamination is few, can analyze area big, when producing a large amount of sample
Surface quality is stable.
Brief description
Fig. 1 is electrobrightening schematic diagram；
Fig. 2 is that powder metallurgy superalloy FGH96 back scattering diffraction grain structure IPZ schemes.
Specific embodiment
The present invention is specifically carried out according to the following steps：
Step 1), treat analysed for powder high temperature alloy and cut sample using wire cutting, specimen size is 10～15mm cube
Block.Using gasoline washed samples surface and oil contaminant, after being dried, mark face to be analyzed；
Step 2), pre-grinding test sample of gold phase machine is polished to sample non-marked face using 200～600# waterproof abrasive paper, in advance
Mill speed is 500～600rpm, and milling time is exposed metallic luster by lapped face and is defined, index face is sequentially passed through
200#, 400#, 600#, 800#, 1000#, 1500# waterproof abrasive paper grinds, and observes lapped face every 30～60s in process of lapping,
Observe that polishing scratch no significantly reduces and no larger longer polishing scratch is changed next number waterproof abrasive paper and ground direction and turn 90 ° of mills twice
System, grinds and is cleaned with water after finishing；
Step 3), on metallographic-sample polisher, to sample, face to be analyzed mechanically polishes, polishing machine rotating speed be 300～
400rpm, is sprayed onto on polishing flannelet with 3.5um diamond spraying polishing agent and sample is polished 5～8 minutes, use 1.5um Buddha's warrior attendant afterwards
Stone spraying polishing agent is sprayed onto and on polishing flannelet, sample is polished 3～5 minutes, changes water throwing polishing cloth and carries out water throwing 2～3 minutes,
Complete alcohol rinse post-drying after mechanical polishing；
Step 4), electrolytic cell 3 is placed on ultrasonic wave emission source 2, opens ultrasonic wave emission source, pressed from both sides using metal tweezers 5
Hold sample 6, make sample liquid to be electrolysed 4 liquid level downwards, tweezers clip position is higher than face 5～6mm to be electrolysed, metal tweezers by
Wire is connected with voltage stabilization and current stabilization dc source 1 anode, and negative electrode connects electrolytic cell, and electrolytic cell is pure nickel rounding post cup-like trough, directly
Footpath 75～105mm, capacity is 200～250mL, hold in groove methanol solution that electrolyte is 18～20% hydrochloric acid 100～
120mL, voltage stabilization and current stabilization direct current power source voltage 25～30V, electric current 3.5～5A, sample immersion electrolyte 2 during electrobrightening～
4.5mm, electrobrightening 15～20s, carry out ultrasonic wave to electrolyte in electrolytic cell and sample in polishing process, frequency be 30～
45KHz；
Step 5), after electrobrightening terminates, sample is put in methanol solution, carry out ultrasonic, taking-up after 50～60s immediately
It is rinsed with alcohol, put into be analyzed in drying basin after drying.
In described step all be related to chemical solution agents useful for same be analysis pure.
Embodiment 1
Treat analysed for powder high temperature alloy FGH96 and cut sample using wire cutting, specimen size is 10mm cubic block.Using
Gasoline washed samples surface and oil contaminant, marks face to be analyzed after being dried；
Pre-grinding test sample of gold phase machine is polished to sample non-marked face using 200～600# waterproof abrasive paper, pre-mill turns
Speed is 600rpm, and milling time exposes metallic luster by lapped face and be defined, index face is sequentially passed through 200#, 400#, 600#,
800#, 1000#, 1500# waterproof abrasive paper grinds, and observes lapped face every 60s in process of lapping, observes polishing scratch twice and no substantially subtracts
Less and no larger longer polishing scratch is changed next number waterproof abrasive paper and ground direction and turn 90 ° and grind, grind and cleaned with water after finishing；
On metallographic-sample polisher, to sample, face to be analyzed mechanically polishes, and polishing machine rotating speed is 400rpm, uses
3.5um diamond spraying polishing agent is sprayed onto and sample is polished 8 minutes on polishing flannelet, uses 1.5um diamond spraying polishing agent afterwards
It is sprayed onto and on polishing flannelet, sample is polished 5 minutes, change water throwing polishing cloth and carry out water throwing 3 minutes, complete alcohol after mechanical polishing
Rinse post-drying；
Clamp sample using metal tweezers, make sample face to be electrolysed level downwards, tweezers clip position is higher than face to be electrolysed
5mm, metal tweezers are connected with voltage stabilization and current stabilization dc source anode by wire, and negative electrode connects electrolytic cell, and electrolytic cell is pure nickel system
Cylinder cup-like trough, diameter 100mm, capacity is 250mL, holds the methanol solution 120mL that electrolyte is 20% hydrochloric acid, voltage stabilizing in groove
Current stabilization direct current power source voltage 25V, electric current 4A, sample immersion electrolyte 4mm during electrobrightening, electrobrightening 15s, in polishing process
Ultrasonic wave is carried out to electrolyte in electrolytic cell and sample, frequency is 40KHz；
After electrobrightening terminates, immediately sample is put into and carry out ultrasonic in methanol solution, taking-up after 60s is rushed with alcohol
Wash, put into be analyzed in drying basin after drying.
Claims (5)
1. a kind of method for making sample for the analysis of powder metallurgy superalloy EBSD is it is characterised in that specifically press following
Step is carried out：
1) treat analysed for powder high temperature alloy and cut sample using wire cutting, specimen size is 10～15mm cubic block, using vapour
Oily washed samples surface and oil contaminant, marks face to be analyzed after being dried；
2) using 200～600# waterproof abrasive paper, sample non-marked face is polished on pre-grinding test sample of gold phase machine, milling time with
Lapped face exposes metallic luster and is defined, and index face is sequentially passed through with 200#, 400#, 600#, 800#, 1000#, 1500# water sand
Paper grinds, and observes lapped face every 30～60s in process of lapping, observes polishing scratch twice and no significantly reduces and no larger longer
Polishing scratch changes next number waterproof abrasive paper, grinds and is cleaned with water after finishing；
3) on metallographic-sample polisher, to sample, face to be analyzed mechanically polishes, with the spraying polishing agent spray of 3.5um diamond
To polishing flannelet to sample polish 5～8 minutes, after with 1.5um diamond spraying polishing agent be sprayed onto on polishing flannelet to sample
Polishing 3～5 minutes, changes water throwing polishing cloth and carries out water throwing 2～3 minutes, complete alcohol rinse post-drying after mechanical polishing；
4) electrolytic cell is placed on ultrasonic wave emission source, after opening ultrasonic wave emission source, clamps sample using metal tweezers, make examination
Downwards, tweezers clip position is higher than face 5～6mm to be electrolysed to sample face to be electrolysed level, and metal tweezers are straight by wire and voltage stabilization and current stabilization
Stream power anode is connected, and negative electrode connects electrolytic cell, hold in groove methanol solution that electrolyte is 18～20% hydrochloric acid 100～
120mL, sample immersion electrolyte 2～4.5mm, electrobrightening 15～20s during electrobrightening, in electrolytic cell in polishing process
Electrolyte and sample carry out ultrasonic wave, and frequency is 30～45KHz；Electrolytic cell is pure nickel rounding post cup-like trough, diameter 75～
105mm, capacity is 200～250mL；Voltage stabilization and current stabilization direct current power source voltage 25～30V, electric current 3.5～5A, voltage stabilization and current stabilization direct current
The positive pole wire in source is connected with metal tweezers and fixes, and negative pole is connected and fixing with edge in cell wall；
5), after electrobrightening terminates, immediately sample is put into and carry out ultrasonic in methanol solution, taking-up after 50～60s is carried out with alcohol
Rinse, put into be analyzed in drying basin after drying.
2. a kind of method for making sample for the analysis of powder metallurgy superalloy EBSD according to claim 1, its
It is characterised by：Described step 2) in pre-grinding test sample of gold phase machine rotating speed be 500～600rpm.
3. a kind of method for making sample for the analysis of powder metallurgy superalloy EBSD according to claim 1, its
It is characterised by：Described step 2) grind when changing next number waterproof abrasive paper in sample, grind direction and turn 90 ° and grind.
4. a kind of method for making sample for the analysis of powder metallurgy superalloy EBSD according to claim 1, its
It is characterised by：Described step 3) in metallographic-sample polisher rotating speed be 300～400rpm.
5. a kind of method for making sample for the analysis of powder metallurgy superalloy EBSD according to claim 1, its
It is characterised by：In described step all be related to chemical solution agents useful for same be analysis pure.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108918561A (en) * | 2018-06-05 | 2018-11-30 | 哈尔滨工业大学深圳研究生院 | A kind of three-dimensional rebuilding method of pair of Ni based high-temperature alloy |
| CN109001128A (en) * | 2018-06-29 | 2018-12-14 | 国网河南省电力公司电力科学研究院 | A kind of method of analysis of metallic materials matrix and precipitated phase Elemental partition |
| CN109537041A (en) * | 2018-10-18 | 2019-03-29 | 昆明理工大学 | A kind of polishing method of making Nano surface Cu and the Cu alloy for electron backscatter diffraction test |
| CN111455446A (en) * | 2020-03-25 | 2020-07-28 | 贵州大学 | Method and system for electropolishing surface of metal cylindrical sample |
| CN113188861A (en) * | 2021-03-30 | 2021-07-30 | 酒泉钢铁(集团)有限责任公司 | Preparation method of granular primary ore polished section |
| CN114088497A (en) * | 2021-12-02 | 2022-02-25 | 北京星航机电装备有限公司 | Preparation device and method of titanium alloy EBSD sample |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108918561A (en) * | 2018-06-05 | 2018-11-30 | 哈尔滨工业大学深圳研究生院 | A kind of three-dimensional rebuilding method of pair of Ni based high-temperature alloy |
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| CN111455446A (en) * | 2020-03-25 | 2020-07-28 | 贵州大学 | Method and system for electropolishing surface of metal cylindrical sample |
| CN111455446B (en) * | 2020-03-25 | 2022-07-01 | 贵州大学 | Method and system for electropolishing surface of metal cylindrical sample |
| CN113188861A (en) * | 2021-03-30 | 2021-07-30 | 酒泉钢铁(集团)有限责任公司 | Preparation method of granular primary ore polished section |
| CN114088497A (en) * | 2021-12-02 | 2022-02-25 | 北京星航机电装备有限公司 | Preparation device and method of titanium alloy EBSD sample |
| CN114088497B (en) * | 2021-12-02 | 2023-09-19 | 北京星航机电装备有限公司 | Preparation device and method of titanium alloy EBSD sample |
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Application publication date: 20170215 |