CN102486460A - Method for discriminating Laves phase and carbide phase in high Nb iron nickel base high temperature alloy - Google Patents
Method for discriminating Laves phase and carbide phase in high Nb iron nickel base high temperature alloy Download PDFInfo
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Abstract
The invention relates to a method for discriminating Laves phase and carbide phase in a high Nb iron nickel base high temperature alloy, which is characterized in that the method comprises the following steps: A) grinding and polishing the high Nb iron nickel base high temperature alloy sample, exposing a polished surface, then placing in a heat treatment furnace, keeping the furnace temperature at 350-600 DEG C, standing for 10-200 minutes, air cooling; B) using a metallographic microscope for observing the high Nb iron nickel base high temperature alloy sample treated in step A). According to the invention, the common metallographic microscope can be used for discriminating a precipitated phase, and the method of the invention is convenient for practical operation of factory, and has the advantages of simple and practical operation, and low cost.
Description
Technical field
The present invention relates to the qualitative checking method of phase in the high temperature alloy, provide in a kind of high Nb iron nickel base superalloy in the difference high temperature alloy Laves mutually and the analytical approach of carbonide especially.
Background technology
Nb is an intensified element common in the high temperature alloy.The addition (wt.%) of Nb is all at 3% ~ 6% in iron nickel base superalloys such as GH4169 (claiming IN718 abroad), GH907, Thermo-Span, and this makes alloy in middle low temperature range, have excellent comprehensive mechanical properties.In process of setting, in these alloys the Nb segregation strong, the block Laves that the interdendritic forms a large amount of rich Nb easily is mutually and carbonide such as NbC.The Laves of bulk is mutually hard, and its existence can cause the rapid reduction of the impact property and the plasticity of material and crisp, in alloy pig cogging process, is prone to cause cracking, and becomes other mechanical properties that formation of crack influences material.Aviation forging test stone has stipulated not allow in the GH4169 forging to exist the Laves phase, but not corresponding method for quickly detecting about the Laves phase.Work for inspection in the past, how from composition difference Laves and NbC mutually, this need arrive, and research institution with good conditionsi passes through ESEM or electron probe is distinguished, and this has influenced round of visits greatly.
Therefore invent a kind of practicality fast Laves just seem with NbC carbonide detection method mutually and be even more important.
Summary of the invention
Laves is mutually and carbonide detection method mutually fast to the object of the present invention is to provide a kind of practicality that is adapted at carrying out under factory's simple experiment condition.
The present invention provides Laves phase and carbonide detection method mutually in a kind of high Nb iron nickel base superalloy, and it is characterized in that: concrete step is following,
A) with high Nb iron nickel base superalloy sample through grinding, after the polishing, polished surface being exposed, place heat-treatment furnace then, Control for Kiln Temperature left standstill air cooling 10 ~ 200 minutes at 350 ~ 600 ℃.
B) utilize metallography microscope sem observation A) high Nb iron nickel base superalloy sample after handling, get final product.Wherein, what be more coarse brown or brown is the Laves phase, and the surface has metallic luster, and what one deck clad was arranged on every side is the carbonide phase.
When if described high Nb iron nickel base superalloy sample is the as cast condition or the sample in early stage homogenising stage, at A) processing stage in Control for Kiln Temperature at 450 ~ 550 ℃, time of repose is 20 ~ 90 minutes.
If described high Nb iron nickel base superalloy sample is when being the deformation states sample, at A) processing stage before, at 1020 ~ 1100 ℃ of insulation 0.5 ~ 2h, air cooling or water-cooled are so that the d phase of separating out in the solid solution deformation process with sample.
Laves phase and carbonide detection method mutually in the high Nb iron nickel base superalloy provided by the invention; According to Laves mutually and carbonide phase constituent content different; In oxidizing atmosphere, expose, form the different film of thickness, under the incident light irradiation; Produce different interference effects, thereby can under optical microscope, demonstrate different colors.According to the difference of alloy inoxidizability, treatment temperature and asynchronism(-nization) are to avoid the blocked up reflecting effect that influences of oxide film.When treatment temperature was high, the time can correspondingly reduce; When treatment temperature was hanged down, the time can correspondingly prolong, and is moderate with the oxide thickness that guarantees the precipitated phase surface.
When using Laves provided by the invention mutually with mutually detection method of carbonide; In the observed effect of metaloscope; As shown in Figure 1; Laves is pale brown look (low temperature in short-term) or bronzing (when high temperature is long) mutually, and similar oil film shape gloss appears in the carbonide phase surface, and should the normal on every side mutually characteristics that similar coating stratiform occurs.
Laves phase and carbonide detection method mutually in the high Nb iron nickel base superalloy provided by the invention, its advantage is: only can be convenient to factory's practical operation to the discriminating of precipitated phase through common metaloscope, simple and practical, with low cost.
Description of drawings
Fig. 1 is the dyeing situation synoptic diagram of GH4169G alloy behind 500 ℃ of heat tinting 40min;
Fig. 2 is the metallographic structure figure of GH4169 cast alloy behind 500 ℃ of exposure 60min;
Fig. 3 is the metallographic structure figure of the conventional corrosion of GH4169 cast alloy attitude;
Fig. 4 is the metallographic structure figure of GH4169G cast alloy behind 520 ℃ of exposure 60min;
Fig. 5 is the metallographic structure figure of the conventional corrosion of GH4169G cast alloy attitude;
Fig. 6 is the metallographic structure figure of Thermo-Span alloy casting state sample behind 450 ℃ of exposure 80min;
Fig. 7 is the metallographic structure figure of Thermo-Span alloy casting state test routine corrosion attitude;
Fig. 8 is the metallographic structure figure of GH4169G alloy behind 500 ℃ of heat tinting 20min;
Fig. 9 is the metallographic structure figure of the conventional corrosion of GH4169G alloy attitude.
Embodiment
Embodiment 1
After grinding, polishing, the chamber type electric resistance furnace that the specimen surface that polishes is exposed to 500 ℃ of furnace temperature is incubated 1h with GH4169 cast alloy sample, and air cooling guarantees that the specimen surface of polishing is not contaminated.After treating the sample cooling, directly under metaloscope, observe.Organizing behind 500 ℃ of processing of sample 1h is as shown in Figure 2.It is thus clear that behind 500 ℃ of heat tinting 1h, the Laves in the sample has become bronzing mutually, and carbonide presents certain gloss, and coating film is arranged on every side.
Comparative Examples 1
GH4169 cast alloy sample after grinding, polishing, is rinsed well specimen surface with alcohol, and dried up, adopt caustic solution common in the high temperature alloy directly to corrode then, it organizes as shown in Figure 3.
Embodiment 2
After grinding, polishing, the chamber type electric resistance furnace insulation 60min that the specimen surface of polishing is exposed to 520 ℃ of furnace temperature treats directly under metaloscope, to observe after the sample cooling with GH4169G alloy casting state sample.Organizing behind 520 ℃ of processing of sample 60min is as shown in Figure 4, visible, and behind 520 ℃ of heat tinting 60min, the Laves phase in the sample is overstrike, and carbonide presents certain gloss.
Comparative Examples 2
GH4169G alloy casting state sample after grinding, polishing, is rinsed well specimen surface with alcohol, and dried up.When common caustic solution directly corroded in selecting the employing high temperature alloy, it organized as shown in Figure 5.
Embodiment 3
With Thermo-Span cast alloy sample at the sample of 1120 ℃ of homogenising 20h through through grinding, after the polishing, the specimen surface of polishing being exposed to the chamber type electric resistance furnace insulation 80min of 450 ℃ of furnace temperature, treat directly observation under metaloscope after the sample cooling.Organizing behind 450 ℃ of processing of sample 80min is as shown in Figure 6, visible, and behind 450 ℃ of heat tinting 80min, the Laves in the sample has become bronzing mutually, and carbonide presents certain gloss.
Comparative Examples 3
The sample of Thermo-Span cast alloy sample at 1120 ℃ of homogenising 20h passed through after grinding, polishing, with alcohol specimen surface is rinsed well, and dried up.When common caustic solution directly corroded in selecting the employing high temperature alloy, it organized as shown in Figure 7.
Embodiment 4
Portion cuts sample from the GH4169G alloy bar material heart, and at 1030 ℃ of insulation 1h, air cooling is so that it separates out the d phase in the solid solution deformation process with sample.After grinding, polishing, polished surface is exposed on sample, place heat-treatment furnace, Control for Kiln Temperature left standstill 20 minutes at 500 ℃, directly existed after the sample cooling again
The tissue that metaloscope is observed down, as shown in Figure 8, visible, this moment, there were a large amount of glossiness carbide particles in alloy inside, but had the brown phase of gathering heap in indivedual positions, and these are undissolved Laves phase mutually; Be the carbonide phase and have mutually than light pool.
Comparative Examples 4
Portion cuts sample from the GH4169G alloy bar material heart, and at 1030 ℃ of insulation 1h, air cooling is so that it separates out the d phase in the solid solution deformation process with sample.With sample through grind, after the polishing, clean and dry up with alcohol wash, when selecting to adopt when common caustic solution directly corrodes in the high temperature alloy, it organizes as shown in Figure 9.
Claims (3)
- In one kind high Nb iron nickel base superalloy Laves mutually and carbonide detection method mutually, it is characterized in that: concrete step is following,A) with high Nb iron nickel base superalloy sample through grinding, after the polishing, polished surface being exposed, place heat-treatment furnace then, Control for Kiln Temperature left standstill air cooling 10 ~ 200 minutes at 350 ~ 600 ℃;B) utilize metallography microscope sem observation A) high Nb iron nickel base superalloy sample after handling, get final product.
- 2. according to Laves phase and carbonide detection method mutually in the described high Nb iron nickel base superalloy of claim 1; It is characterized in that: when described high Nb iron nickel base superalloy sample is the as cast condition or the sample in early stage homogenising stage; At A) processing stage in Control for Kiln Temperature at 450 ~ 550 ℃, time of repose is 20 ~ 90 minutes.
- 3. according to Laves phase and carbonide detection method mutually in the described high Nb iron nickel base superalloy of claim 1; It is characterized in that: when described high Nb iron nickel base superalloy sample is the deformation states sample; At A) processing stage before; Sample is incubated 0.5 ~ 2h, air cooling or water-cooled at 1020 ~ 1100 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104133083A (en) * | 2014-07-09 | 2014-11-05 | 河冶科技股份有限公司 | Method for quantitative detection of MC carbide in high-V high-speed steel |
| CN110146532A (en) * | 2019-06-04 | 2019-08-20 | 中国科学院金属研究所 | A kind of differentiating method of MX phase and Laves phase for mutually counting |
| CN112525916A (en) * | 2020-11-03 | 2021-03-19 | 中国航发北京航空材料研究院 | Method for displaying harmful phase of isothermal forging die material for turbine disc |
| CN115753308A (en) * | 2023-02-13 | 2023-03-07 | 西北工业大学 | Preparation method of metallographic sample, and analysis method, device, medium and equipment thereof |
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| DE3333042A1 (en) * | 1982-11-22 | 1984-04-19 | Buehler Ltd., 60044 Lake Bluff, Ill. | Grinding compound supply device for preparing metallographic specimens |
| CN101699253A (en) * | 2009-10-29 | 2010-04-28 | 宁波江丰电子材料有限公司 | Method for displaying metallographic structure of target |
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| DE3333042A1 (en) * | 1982-11-22 | 1984-04-19 | Buehler Ltd., 60044 Lake Bluff, Ill. | Grinding compound supply device for preparing metallographic specimens |
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| 《Materials Science and Engineering: A》 20040825 A.J Ramirez, J.C Lippold High temperature behavior of Ni-base weld metal: Part II - Insight into the mechanism for ductility dip cracking 第245-258页 1-3 第380卷, 第1-2期 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104133083A (en) * | 2014-07-09 | 2014-11-05 | 河冶科技股份有限公司 | Method for quantitative detection of MC carbide in high-V high-speed steel |
| CN110146532A (en) * | 2019-06-04 | 2019-08-20 | 中国科学院金属研究所 | A kind of differentiating method of MX phase and Laves phase for mutually counting |
| CN110146532B (en) * | 2019-06-04 | 2021-08-03 | 中国科学院金属研究所 | Method for distinguishing MX phase and Laves phase for phase statistics |
| CN112525916A (en) * | 2020-11-03 | 2021-03-19 | 中国航发北京航空材料研究院 | Method for displaying harmful phase of isothermal forging die material for turbine disc |
| CN112525916B (en) * | 2020-11-03 | 2023-01-13 | 中国航发北京航空材料研究院 | Method for displaying harmful phase of isothermal forging die material for turbine disc |
| CN115753308A (en) * | 2023-02-13 | 2023-03-07 | 西北工业大学 | Preparation method of metallographic sample, and analysis method, device, medium and equipment thereof |
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