CN106908460B - A kind of preparation method of the hot rolling nickel tungsten sample for the test of microcosmic texture - Google Patents
A kind of preparation method of the hot rolling nickel tungsten sample for the test of microcosmic texture Download PDFInfo
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- CN106908460B CN106908460B CN201710113118.9A CN201710113118A CN106908460B CN 106908460 B CN106908460 B CN 106908460B CN 201710113118 A CN201710113118 A CN 201710113118A CN 106908460 B CN106908460 B CN 106908460B
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- 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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/203—Measuring back scattering
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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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Abstract
The invention discloses a kind of preparation methods of hot rolling nickel tungsten sample for the test of microcosmic texture.Hot rolling nickel tungsten sample is immersed in aqueous citric acid solution first, then will be immersed in potassium hydroxide aqueous solution and pre-process again after the hot-rolled sample taking-up residual solution on alcohol rinse surface；Then using hot rolling texture nickel tungsten as anode, stainless steel is cathode, D.C. regulated power supply is connected with conducting wire, hot rolling nickel tungsten and stainless steel are immersed in configured polishing fluid in advance simultaneously and polished, then will after sample taking-up alcohol rinse immerse potassium hydroxide aqueous solution in, finally take out sample drying can be obtained surface stress is small, surface quality it is bright it is smooth, EBSD test in can obtain the diffraction pattern of high quality, the hot rolling nickel tungsten sample of good in oxidation resistance.
Description
Technical field
The present invention relates to textured metal base band microarrays techniques more particularly to a kind of hot rollings for the test of microcosmic texture
The preparation method of nickel tungsten sample.
Background technique
Nickel-tungsten alloy base-band with strong cubic texture is the key that acquisition second generation high temperature coating superconducting tape, and hot rolling
Technique is an essential process in base band preparation process, formation shadow of the texture that hot rolling generates to subsequent cold rolling texture
Sound is larger, therefore the microcosmic texture studied in hot-rolled sample is particularly important in the research of textured metal base band.
Electron backscatter diffraction (EBSD) technology is the conventional method of the microcosmic textile analysis of sample surfaces, the measuring technology pair
The surface quality of sample is higher, and it is as small as possible to require sample surfaces stress to answer.However it can be produced in the course of hot rolling of alloy
Raw stress, and a degree of stress can be also brought into during machinery removes oxide skin, it seriously affects EBSD test and obtains
Reliable micro orientation information.
In the research of textured metal base band, nickel-tungsten alloy base-band is the textured metal base band of most study, for hot rolling
Firstly the need of the oxide skin for removing surface for sample, the method removal of Mechanical polishing is generallyd use, but the effect is unsatisfactory,
How to pass through that suitable method eliminates stress present in hot-rolled sample and to obtain bright surface microcosmic in nickel tungsten hot-rolled sample
There is certain challenge in the characterization of texture.
Summary of the invention
Prepare that a kind of surface stress is small, surface quality is bright smooth for microcosmic it is an object of the present invention to provide a kind of method
The hot rolling nickel tungsten sample of texture test, to meet the application requirement of more areas.
A kind of preparation method of the hot rolling nickel tungsten sample for the test of microcosmic texture, comprising the following steps:
Step 1: nickel tungsten hot-rolled sample surface is pre-processed:
The nickel tungsten sample that hot rolling deformation amount is 50%~74% is immersed into the citric acid water that concentration is 50~120g/L
In solution impregnate 5~8min, then by the residual solution on hot rolling nickel tungsten sample taking-up its surface of alcohol rinse, then by its
It is immersed in 3~6min in the potassium hydroxide aqueous solution that concentration is 20~30g/L；
Step 2: configuration electrobrightening solution:
By distilled water, butoxy ethanol, nitric acid and sodium phosphate according to volume ratio be 3:0.3~0.6:2~7:0.1~1
Configure electrolytic polishing liquid；
Step 3: the hot rolling nickel tungsten sample finally obtained in step 1 is subjected to electrobrightening:
Using hot rolling nickel tungsten sample as anode, stainless steel is cathode, D.C. regulated power supply is connected with conducting wire, by hot rolling nickel
Tungsten alloy sample and stainless steel are immersed in polishing fluid are polished simultaneously, and wherein voltage is 80~90V, and electric current is 120~
180mA, temperature are 10~35 DEG C, and polishing time is 5~8min, then takes out the hot rolling nickel tungsten sample after polishing, are used
It is immersed in potassium hydroxide aqueous solution after alcohol rinse, soaking time is 1~3min, finally takes out sample drying.
It is preferred that tungsten atom content is 3%~7.5% in the nickel tungsten in step 1.
It is preferred that the hot rolling deformation amount of nickel tungsten sample is 50% in step 1；Aqueous citric acid solution it is dense
Degree is 70g/L, is 5min in the time wherein impregnated；Potassium hydroxide aqueous solution concentration is 30g/L, is in the time wherein impregnated
6min。
It is preferred that in step 2, distilled water, butoxy ethanol, nitric acid and phosphoric acid in the electrobrightening solution
The volume ratio of sodium is 3:0.3:7:0.1.
It is preferred that in step 3, the anode dimension is 30 × 20 × 3mm, and the cathode stainless steel is not 304 not
Become rusty steel, and cathode size is 40 × 30 × 2mm.
It is preferred that the voltage of polishing is 80V, electric current 120mA, temperature is 10~35 DEG C, and polishing time is
8min；The concentration of the potassium hydroxide aqueous solution is 8g/L, soaking time 1min.
The present invention avoids the method bring surface stress of mechanical descale with specific method.
Specifically, being pre-processed first using faintly acid citric acid to hot rolling nickel tungsten sample, in clean the surface
While sample will not be caused corrosion injure, and using potassium hydroxide solution to hot rolling nickel tungsten sample treatment, by it
The remaining acid substance on surface removes；Then suitable electrolytic polishing liquid is prepared to polish hot rolling nickel tungsten sample, and
And big voltage and high current are used during electrobrightening, it not only can effectively remove answering for hot rolling nickel tungsten surface in this way
Power layer, and obtained hot rolled alloy surface-brightening is smooth, and the diffraction pattern of high quality can be obtained in EBSD test.
It can after immersion appropriate time in addition, the hot rolling nickel tungsten sample after electrobrightening is placed in potassium hydroxide solution
To effectively prevent the surface after polishing to again be oxidized.
Detailed description of the invention
It will be briefly described attached drawing used in this application below, it should be apparent that, these attached drawings are for explaining only the invention
Design.
Fig. 1 is (100) face pole figure on the hot rolling nickel tungsten surface obtained using the preparation method of the embodiment of the present invention 1.
Fig. 2 is (100) face pole figure on the hot rolling nickel tungsten surface obtained using the preparation method of the embodiment of the present invention 2.
Specific embodiment
A kind of preparation method of hot rolling nickel tungsten sample for the test of microcosmic texture of the invention is described below
Embodiment.
The embodiment recorded herein is specific specific embodiment of the invention, for illustrating design of the invention,
Be it is explanatory and illustrative, should not be construed as the limitation to embodiment of the present invention and the scope of the invention.Except what is recorded herein
Outside embodiment, those skilled in the art can also based on the claim of this application book and specification disclosure of that using aobvious and
The other technical solutions being clear to, these technical solutions include the embodiment recorded herein is made it is any it is obvious replacement and
The technical solution of modification.
Embodiment 1
The step of preparation method of the embodiment of the present invention 1, is as follows:
The nickel tungsten sample that hot rolling deformation amount is 50% is immersed in aqueous citric acid solution, soaking time 5min,
The concentration of middle aqueous citric acid solution is 70g/L, and tungsten atom content is 3% in nickel tungsten, then by hot-rolled sample taking-up wine
Fine is immersed in potassium hydroxide aqueous solution again after washing the residual solution on surface, soaking time 6min, wherein potassium hydroxide
Concentration is 30g/L；
Distilled water, butoxy ethanol, nitric acid and sodium phosphate are configured into electrobrightening according to volume ratio for 3:0.3:7:0.1
Liquid；
Using hot rolling texture nickel tungsten as anode, having a size of 30 × 20 × 3mm, 304 stainless steels are cathode, having a size of 40 ×
30 × 2mm connects D.C. regulated power supply with conducting wire, and hot rolling nickel tungsten and stainless steel are immersed in polishing fluid simultaneously and thrown
Light, voltage 80V, electric current 120mA, temperature are 10~35 DEG C, polishing time 8min, then rush sample taking-up with alcohol
It is immersed in potassium hydroxide aqueous solution after washing, soaking time 1min, the concentration of potassium hydroxide is 8g/L, finally takes out sample and blows
It is dry.
Fig. 1 is (001) face pole figure of the hot rolling Ni5W alloy surface obtained using EBSD technical testing, diffraction pattern calibration
Rate is 97%, and the style quality on the hot-rolled sample surface after showing electrobrightening is higher, and data are reliable, is suitble to be used as EBSD test
Analysis.
Embodiment 2
The step of preparation method of the embodiment of the present invention 1, is as follows:
The nickel tungsten sample that hot rolling deformation amount is 74% is immersed in aqueous citric acid solution, soaking time 5min,
The concentration of middle aqueous citric acid solution is 120g/L, and tungsten atom content is 7.5% in nickel tungsten, then takes out hot-rolled sample and uses
It is immersed in potassium hydroxide aqueous solution again after the residual solution on alcohol rinse surface, soaking time 3min, wherein potassium hydroxide
Concentration be 20g/L；
Distilled water, butoxy ethanol, nitric acid and sodium phosphate are configured into electrobrightening according to volume ratio for 3:0.6:7:1
Liquid；
Using hot rolling texture nickel tungsten as anode, having a size of 30 × 20 × 3mm, 304 stainless steels are cathode, having a size of 40 ×
30 × 2mm connects D.C. regulated power supply with conducting wire, and hot rolling nickel tungsten and stainless steel are immersed in polishing fluid simultaneously and thrown
Light, voltage 90V, electric current 180mA, temperature are 10~35 DEG C, polishing time 7min, then rush sample taking-up with alcohol
It is immersed in potassium hydroxide aqueous solution after washing, soaking time 1min, the concentration of potassium hydroxide is 8g/L, finally takes out sample and blows
It is dry.
Fig. 2 is (001) face pole figure of the hot rolling Ni5W alloy surface obtained using EBSD technical testing, diffraction pattern calibration
Rate is 99%, and the style quality on the hot-rolled sample surface after showing electrobrightening is higher, and data are reliable, is suitble to be used as EBSD test
Analysis.
Both examples above is merely to the specific specific embodiment for illustrating design of the invention and selecting, at this
In a little embodiments, specific technological parameter might not be configured to limitation of the scope of the invention.Illustrate of the invention one below
The preferred scope of a little technological parameters.
The stainless steel of cathode not necessarily 304 stainless steels, or the stainless steel of other models.
Step 1: nickel tungsten hot-rolled sample surface is pre-processed:
The nickel tungsten sample that hot rolling deformation amount is 50%~74% is immersed into the citric acid water that concentration is 50~120g/L
In solution impregnate 5~8min, then by the residual solution on hot rolling nickel tungsten sample taking-up its surface of alcohol rinse, then by its
It is immersed in 3~6min in the potassium hydroxide aqueous solution that concentration is 20~30g/L；
Step 2: configuration electrobrightening solution:
By distilled water, butoxy ethanol, nitric acid and sodium phosphate according to volume ratio be 3:0.3~0.6:2~7:0.1~1
Configure electrolytic polishing liquid；
Step 3: the hot rolling nickel tungsten sample finally obtained in step 1 is subjected to electrobrightening:
Using hot rolling nickel tungsten sample as anode, stainless steel is cathode, D.C. regulated power supply is connected with conducting wire, by hot rolling nickel
Tungsten alloy sample and stainless steel are immersed in polishing fluid are polished simultaneously, and wherein voltage is 80~90V, and electric current is 120~
180mA, temperature are 10~35 DEG C, and polishing time is 5~8min, then takes out the hot rolling nickel tungsten sample after polishing, are used
It is immersed in potassium hydroxide aqueous solution after alcohol rinse, soaking time is 1~3min, finally takes out sample drying.
The surface oxide layer for removing hot rolling nickel tungsten using mechanical means in the prior art, can not only bring new table
Face stress, and obtained sample surfaces quality is low, is not suitable for being used to do EBSD test.
The present invention avoids the method bring surface stress of mechanical descale with specific method.
Specifically, being pre-processed using citric acid and potassium hydroxide solution to hot rolling nickel tungsten sample, prepares and close
Suitable electrolytic polishing liquid polishes hot rolling nickel tungsten sample, and using big voltage and big electricity during electrobrightening
Stream.Not only it can effectively remove the stressor layers on hot rolling nickel tungsten surface in this way, and obtained hot rolled alloy surface-brightening is flat
It is whole, the diffraction pattern of high quality can be obtained in EBSD test.
It can after immersion appropriate time in addition, the hot rolling nickel tungsten sample after electrobrightening is placed in potassium hydroxide solution
To effectively prevent the surface after polishing to again be oxidized.
Above to a kind of implementation of the preparation method of hot rolling nickel tungsten sample for the test of microcosmic texture of the invention
Mode is illustrated.For the specific of the preparation method for being used for the hot rolling nickel tungsten sample that microcosmic texture is tested of the invention
Feature can specifically be designed such as specific technological parameter according to the effect of the feature disclosed in above-mentioned, these designs are abilities
Field technique personnel can be realized.Moreover, each technical characteristic of above-mentioned disclosure is not limited to disclosed and other feature group
It closes, those skilled in the art can also carry out other combinations between each technical characteristic according to the purpose of invention, to realize the present invention
Purpose subject to.
Claims (6)
1. a kind of preparation method of the hot rolling nickel tungsten sample for the test of microcosmic texture, comprising the following steps:
Step 1: nickel tungsten hot-rolled sample surface is pre-processed:
The nickel tungsten sample that hot rolling deformation amount is 50%~74% is immersed into the aqueous citric acid solution that concentration is 50~120g/L
5~8min of middle immersion, then by the residual solution on hot rolling nickel tungsten sample taking-up its surface of alcohol rinse, then is impregnated
3~6min in the potassium hydroxide aqueous solution that concentration is 20~30g/L；
Step 2: configuration electrobrightening solution:
By distilled water, butoxy ethanol, nitric acid and sodium phosphate according to volume ratio be 3:0.3~0.6:2~7:0.1~1 configure
Electrolytic polishing liquid；
Step 3: the hot rolling nickel tungsten sample finally obtained in step 1 is subjected to electrobrightening:
Using hot rolling nickel tungsten sample as anode, stainless steel is cathode, connects D.C. regulated power supply with conducting wire, hot rolling nickel tungsten is closed
Golden sample and stainless steel are immersed in polishing fluid simultaneously to be polished, and wherein voltage is 80~90V, and electric current is 120~180mA,
Temperature is 10~35 DEG C, and polishing time is 5~8min, then takes out the hot rolling nickel tungsten sample after polishing, is rushed with alcohol
It is immersed in potassium hydroxide aqueous solution after washing, soaking time is 1~3min, finally takes out sample drying.
2. preparation method as described in claim 1, wherein in step 1, in the nickel tungsten tungsten atom content be 3%~
7.5%.
3. preparation method as described in claim 1, wherein in step 1, the hot rolling deformation amount of nickel tungsten sample is 50%；
The concentration of aqueous citric acid solution is 70g/L, is 5min in the time wherein impregnated；
Potassium hydroxide aqueous solution concentration is 30g/L, is 6min in the time wherein impregnated.
4. preparation method as described in claim 1, wherein in step 2, distilled water, 2- fourth oxygen in the electrobrightening solution
The volume ratio of base ethyl alcohol, nitric acid and sodium phosphate is 3:0.3:7:0.1.
5. preparation method as described in claim 1, wherein in step 3, the anode dimension is 30 × 20 × 3mm, the yin
Pole stainless steel is 304 stainless steels, and cathode size is 40 × 30 × 2mm.
6. preparation method as described in claim 1, wherein in step 3, the voltage of polishing is 80V, electric current 120mA, temperature
It is 10~35 DEG C, polishing time 8min；
The concentration of the potassium hydroxide aqueous solution is 8g/L, soaking time 1min.
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| CN201710113118.9A CN106908460B (en) | 2017-02-28 | 2017-02-28 | A kind of preparation method of the hot rolling nickel tungsten sample for the test of microcosmic texture |
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| CN201710113118.9A CN106908460B (en) | 2017-02-28 | 2017-02-28 | A kind of preparation method of the hot rolling nickel tungsten sample for the test of microcosmic texture |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539216A (en) * | 2010-12-07 | 2012-07-04 | 北京有色金属研究总院 | Method for preparing nickel alloy EBSD (Electron Back Scattering Diffraction) sample |
| CN101985772B (en) * | 2010-12-01 | 2012-10-03 | 重庆大学 | Electrolytic polishing solution and electrolytic polishing process for detection pretreatment of magnesium alloy texture |
| CN103226074A (en) * | 2013-03-15 | 2013-07-31 | 北京工业大学 | Cu-Ni alloy electro-polishing method used for EBSD test |
| CN103808542A (en) * | 2012-11-10 | 2014-05-21 | 有研亿金新材料股份有限公司 | Method for preparing nickel-platinum alloy metallographic phase sample and displaying sample tissue |
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2017
- 2017-02-28 CN CN201710113118.9A patent/CN106908460B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101985772B (en) * | 2010-12-01 | 2012-10-03 | 重庆大学 | Electrolytic polishing solution and electrolytic polishing process for detection pretreatment of magnesium alloy texture |
| CN102539216A (en) * | 2010-12-07 | 2012-07-04 | 北京有色金属研究总院 | Method for preparing nickel alloy EBSD (Electron Back Scattering Diffraction) sample |
| CN103808542A (en) * | 2012-11-10 | 2014-05-21 | 有研亿金新材料股份有限公司 | Method for preparing nickel-platinum alloy metallographic phase sample and displaying sample tissue |
| CN103226074A (en) * | 2013-03-15 | 2013-07-31 | 北京工业大学 | Cu-Ni alloy electro-polishing method used for EBSD test |
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