CN106404484A - Method for displaying grain structure of invar alloy through high-temperature oxidation - Google Patents
Method for displaying grain structure of invar alloy through high-temperature oxidation Download PDFInfo
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- CN106404484A CN106404484A CN201610829124.XA CN201610829124A CN106404484A CN 106404484 A CN106404484 A CN 106404484A CN 201610829124 A CN201610829124 A CN 201610829124A CN 106404484 A CN106404484 A CN 106404484A
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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
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Abstract
A method for displaying the grain structure of invar alloy through high-temperature oxidation belongs to the field of metallographic structure analysis. The invar alloy is binary alloy and comprises 36 percent by weight of Ni and the balance of Fe; and the high-temperature oxidation conditions include oxidizing atmosphere and temperature being 600 to 1000 DEG C. A processed test sample is put into the high-temperature oxidation atmosphere to perform heat preservation for a certain time, the test sample is taken out, the oxide skin on the surface of the test sample is stripped and the test sample is lightly ground on abrasive paper, so that the clear grain structure can be observed. With the method, the defects that the corrosion time is difficult to control, the corrosive agent is toxic, dangerous and not suitable for corrosion of large test samples, and the like in the traditional chemical corrosion method are overcome. The method has the advantages that the method is simple in operation and good in display effect, time is easy to control, and the grain structure of the invar alloy can be displayed clearly.
Description
Technical field
The invention belongs to metallographic structure analysis field is and in particular to a kind of high-temperature oxydation shows invar alloy grain structure
Method.
Background technology
Fe-36Ni invar alloy is a kind of specific alloy, because its coefficient of expansion is minimum, also referred to as low-expansion alloy.By
In being 36% containing Ni content, alloy is corrosion-resistant preferably, general chemical mordant be difficult to quickly, clearly indicate its crystal grain group
Knit.
Traditional display packing of metal material grain structure is chemical corrosion method, and invar alloy caustic is rotten frequently with some
The stronger acids of corrosion.Patent CN105486567A discloses a kind of chemical erosion agent of display expansion alloy macroscopic view macrostructure
And its corrosion method, the chemical composition of this aggressive agent and proportioning are：Picric acid 3 ~ 4g, anhydrous alcohol 90 ~ 100ml, hydrochloric acid 2 ~
3ml, dodecylbenzene sodium sulfonate 2g（Surfactant）.The corrosion method of this aggressive agent：The aggressive agent having configured is heated to
Then the sample light grinding is faced down by fluidized state, and suspension is put in the etchant of boiling, and erosion time is 3 ~ 5min；
Erosion uses alcohol washes erosion surface after terminating, shows macroscopical macrostructure after carrying out clear water flushing.In this patent also
The method introducing other several display invar alloy grain structures, all adopts strong acid to prepare corrosion without exception.For example：Using
10g CuSO4+50ml HCl +50ml H2O solution wipes to sample；Using volume ratio HCl:HNO3=3:1 chloroazotic acid is molten
Liquid wipes to sample；Using volume ratio HCl:H2O=1:1 aqueous solution is in 70 ~ 80 DEG C of heat etching samples.
Several traditional chemical etch are all using the strong acid of organic or inorganic above, such as picric acid, HCl or HNO3, these
Strong acid configuration forms that caustic is poisonous, corrosivity strong, and sometimes also needs to be heated, and increases further to personal harm
Property.The corrosivity of strong acid are stronger, and the time of corrosion should not be grasped, and produce one layer of attachment in specimen surface after corrosion, unsuitable clear
Wash, the effect of impact structure observation.Chemical corrosion method due to configuring the volumetric constraint of solution, unsuitable for corroding larger block
Sample.
In sum, there is problem above in existing invar alloy traditional chemical etch, thus need to develop a kind of new,
Simply, the method for the grain structure of clear display invar alloy.
Content of the invention
The problem existing for traditional chemical etch, the present invention provides a kind of high-temperature oxydation to show invar alloy crystal grain group
The method knitted is it is therefore an objective to using the method is simple, the clear grain structure showing invar alloy.
The present invention is achieved by the following technical programs：
A kind of method that high-temperature oxydation shows invar alloy grain structure, it is characterized in that high temperature oxidizing conditions be oxidizing atmosphere and
Temperature is 600 ~ 1000 DEG C.
Described oxidizing atmosphere includes any one atmosphere following：
（1）Pure O2；
（2）Pure CO2；
（3）O2With N2Mixed gas；O2Based on volume percent content, 0 ＜ VO2＜ 100%.
（4）CO2With N2Mixed gas；CO2Based on volume percent content, 50 ＜ VCO2＜ 100%.
（5）O2Mixed gas with Ar；O2Based on volume percent content, 0 ＜ VO2＜ 100%.
（6）CO2Mixed gas with Ar；CO2Based on volume percent content, 50 ＜ VCO2＜ 100%.
（7）O2+CO2+ N2Mixed gas；O2And CO2Based on volume content, percent by volume 0 ＜ VO2 + CO2＜
100%, and 0 ＜ VO2, 0 ＜ VCO2.
（8）O2+CO2The mixed gas of+Ar；Percent by volume 0 ＜ VO2 + CO2＜ 100%, and 0 ＜ VO2, 0 ＜ VCO2
It is necessarily present the gas containing O, crystal boundary is the privileged way of O transmission, and invar alloy is Fe-Ni alloy/C in oxidizing atmosphere,
Due to the difference of Ni and Fe and O affinity, the Fe on the crystal boundary in heating is preferentially oxidized, leads to crystal boundary to occur.Heating-up temperature
Select 600 ~ 1000 DEG C, temperature is too low, oxide etch overlong time, and Display of Grain Boundary is unclear；Temperature is too high, and heat temperature raising is stranded
Difficulty, increased risk.
A kind of high-temperature oxydation shows the method for invar alloy grain structure it is characterised in that carrying out according to the following steps：
（1）Prepared by sample：Ingot casting intercepts sample, after grinding by waterproof abrasive paper, uses alcohol rinse specimen surface, hair-dryer blows
Dry.
（2）Airtight heating furnace is warming up to preset temperature, is passed through oxidizing atmosphere, prepared sample put into 600 ~
In 1000 DEG C of oxidizing atmospheres, the length of temperature retention time depends on the height of oxidizing temperature and the power of oxidizing atmosphere, typically
Insulation 30 ~ 60min, takes out after held for some time, peel test specimen surface scale, gently grinds on sand paper, you can observe
To clearly grain structure.
Compared with existing traditional chemical etch, this method has following technique effect：
1st, specimen surface need not be polished, and reduce the requirement to surface smoothness, simplify preparation procedure.
2nd, temperature retention time wide scope is it is easy to control the degree of oxidation.
3rd, the convenient sample to agglomerate body carries out high-temperature oxydation to show its grain structure.
4th, grain structure shows clearly, can direct visual perception crystallite dimension size.
Brief description
Fig. 1 is for aoxidizing the crystalline substance of the specimen surface of 30min at the embodiment of the present invention 1 invar alloy strand in atmosphere 700 DEG C
Grain tissue topography.
Fig. 2 is the sample longitudinal section of oxidation 30min at the embodiment of the present invention 1 invar alloy strand in atmosphere 700 DEG C
Grain structure pattern.
Fig. 3 is the embodiment of the present invention 2 invar alloy strand in 5%O2+95%N2The examination of 60min is aoxidized at 1000 DEG C in atmosphere
Sample longitudinal section tissue topography.
Specific embodiment
Below in conjunction with specific embodiment in detail the present invention is described in detail, but the invention is not limited in following embodiments.
Embodiment 1
Cut the sample of 20mm × 20mm × 30mm size in strand edge, by specimen surface successively 150#, 400#,
Grind on 600#, 1000#, 1500#, 2000# waterproof abrasive paper, use alcohol rinse specimen surface, hair-dryer dries up.Muffle furnace is energized
It is heated to 700 DEG C, is air in stove, the sample having prepared is put into Muffle furnace insulation 30min, take out sample afterwards and exist
In the air natural cooling.Peel off specimen surface iron scale, specimen surface is gently ground on waterproof abrasive paper, naked eyes
See invar alloy grain structure pattern.
Embodiment 2
Cut the sample of 20mm × 20mm × 30mm size in strand edge, by specimen surface successively 150#, 400#,
Grind on 600#, 1000#, 1500#, 2000# waterproof abrasive paper, use alcohol rinse specimen surface, hair-dryer dries up.Muffle furnace is energized
It is heated to 1000 DEG C, being filled with percent by volume in stove is 5%O2+95%N2Mixed atmosphere, the sample having prepared is put into
Muffle furnace is incubated 60min, and taking out sample afterwards is 5%O in percent by volume2+95% N2Mixed atmosphere in natural cooling.Peel off
Specimen surface iron scale, specimen surface is gently ground on waterproof abrasive paper, naked eyes are visible invar alloy grain structure
Pattern.
Claims (9)
1. a kind of high-temperature oxydation shows the method for invar alloy grain structure it is characterised in that described invar alloy closes for binary
Gold, Ni content percentage by weight is 36%, and remaining is Fe；Described high temperature oxidizing conditions are：Oxidizing atmosphere and temperature be 600 ~
1000℃.
2. a kind of high-temperature oxydation shows the method for invar alloy grain structure it is characterised in that described as claimed in claim 1
Oxidizing atmosphere includes any one atmosphere following：
（1）Pure O2；
（2）Pure CO2；
（3）O2With N2Mixed gas；
（4）CO2With N2Mixed gas；
（5）O2Mixed gas with Ar；
（6）CO2Mixed gas with Ar；
（7）O2+CO2+ N2Mixed gas；
（8）O2+CO2The mixed gas of+Ar.
3. a kind of high-temperature oxydation shows the method for invar alloy grain structure it is characterised in that O as claimed in claim 22With N2
In mixed gas, O2Based on volume percent content, 0 ＜ VO2＜ 100%.
4. a kind of high-temperature oxydation shows the method for invar alloy grain structure it is characterised in that CO as claimed in claim 22With
N2In mixed gas, CO2Based on volume percent content, 50 ＜ VCO2＜ 100%.
5. a kind of high-temperature oxydation shows the method for invar alloy grain structure it is characterised in that O as claimed in claim 22With Ar
In mixed gas, O2Based on volume percent content, 0 ＜ VO2＜ 100%.
6. a kind of high-temperature oxydation shows the method for invar alloy grain structure it is characterised in that CO as claimed in claim 22With
In Ar mixed gas, CO2Based on volume percent content, 50 ＜ VCO2＜ 100%.
7. a kind of high-temperature oxydation shows the method for invar alloy grain structure it is characterised in that O as claimed in claim 22+
CO2+ N2Mixed gas in, O2And CO2Based on volume content, percent by volume 0 ＜ VO2 + CO2＜ 100%, and 0 ＜ VO2, 0 ＜
VCO2.
8. a kind of high-temperature oxydation shows the method for invar alloy grain structure it is characterised in that O as claimed in claim 22+
CO2In the mixed gas of+Ar, O2And CO2Based on volume content, percent by volume 0 ＜ VO2 + CO2＜ 100%, and 0 ＜ VO2, 0 ＜
VCO2.
9. a kind of high-temperature oxydation shows the method for invar alloy grain structure it is characterised in that showing as claimed in claim 1
Method comprises the steps：
（1）Prepared by sample：Ingot casting intercepts sample, after grinding by waterproof abrasive paper, uses alcohol rinse specimen surface, hair-dryer blows
Dry；
（2）Tissue display：Airtight heating furnace is warming up to preset temperature, is passed through oxidizing atmosphere, sample is put into 600 ~
In 1000 DEG C of oxidizing atmosphere, insulation 30 ~ 60min takes out, and peel test specimen surface scale grinds on sand paper, you can
Observe clearly grain structure.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535394A (en) * | 2015-01-19 | 2015-04-22 | 湖南大学 | Preparation method of metallographic samples of zirconium and zirconium alloy |
| CN105420554A (en) * | 2015-12-29 | 2016-03-23 | 钢铁研究总院 | Heat corrosion resistant directionally-solidified nickel-based high temperature alloy and preparation method thereof |
| CN105628474A (en) * | 2016-03-01 | 2016-06-01 | 银邦金属复合材料股份有限公司 | Preparation method of aluminum steel composite grain structure, sample, reagent and preparation method |
| CN106053471A (en) * | 2016-08-04 | 2016-10-26 | 南京钢铁股份有限公司 | Method for showing austenite crystal boundary of micro-alloyed steel in vacuum hot-corrosion condition |
-
2016
- 2016-09-19 CN CN201610829124.XA patent/CN106404484A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535394A (en) * | 2015-01-19 | 2015-04-22 | 湖南大学 | Preparation method of metallographic samples of zirconium and zirconium alloy |
| CN105420554A (en) * | 2015-12-29 | 2016-03-23 | 钢铁研究总院 | Heat corrosion resistant directionally-solidified nickel-based high temperature alloy and preparation method thereof |
| CN105628474A (en) * | 2016-03-01 | 2016-06-01 | 银邦金属复合材料股份有限公司 | Preparation method of aluminum steel composite grain structure, sample, reagent and preparation method |
| CN106053471A (en) * | 2016-08-04 | 2016-10-26 | 南京钢铁股份有限公司 | Method for showing austenite crystal boundary of micro-alloyed steel in vacuum hot-corrosion condition |
Non-Patent Citations (3)
| Title |
|---|
| 机械工业部科技与质量监督司，中国机械工程学会理化检验分会: "《机械工程材料测试手册，第一版 》", 30 November 1999 * |
| 胡美些: "《金属材料检测技术,第一版》", 31 May 2011 * |
| 那边是猎户座 上传: ""8-第八讲-高温金相技术"", 《百度文库：HPPTS:WENKU.BAIDU.COM/VIEW/A2CF671755270722192EF7CE.HTML》 * |
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Application publication date: 20170215 |