CN102809500A - Method for rapidly preparing Ni-based superalloy electron backscatter diffraction sample - Google Patents

Abstract

The invention discloses a method for rapidly preparing a Ni-based superalloy electron backscatter diffraction (EBSD) sample. The method is characterized in that the electrolytic polishing is not required; and the sample is rapidly prepared by a chemical etching method. The method comprises the following steps of: cutting the sample by a wire cutting machine, pre-grinding the sample by using abrasive paper for metallograph, performing mechanical polishing, and etching the sample by using a chemical etchant. Kikuchi patterns of the Ni-based superalloy EBSD sample prepared by the method are clear. By the method, the disadvantages that a commonly used method for preparing an EBSD sample is complicated in electrolytic polishing sample preparation and has an unstable effect are overcome.

Description

A kind of quick method for preparing Ni based high-temperature alloy EBSD sample

Technical field

The present invention is a kind of method of the quick Ni of preparation based high-temperature alloy EBSD sample, belongs to the metallographic technology of preparing of Ni based high-temperature alloy.

Background technology

EBSD; Hereinafter to be referred as EBSD; Be the most important development of material micro-analysis in recent years technology, its ultimate principle is through the analysis of the diffraction Kikuchi band that electron beam in the ESEM is inspired and forms at the inclination sample surfaces, confirms crystal structure and orientation.At present EBSD analyzes main application has: crystallite dimension analysis, textile analysis, crystal boundary specificity analysis, misorientation analysis, the identification of phases and distribute mutually etc.China EBSD analyzes and just is widely used in each research field at present.In recent years, the EBSD analytical technology also obtains widespread use in nickel base superalloy.

The accuracy that EBSD analyzes and the preparation quality of sample have much relations.At present, obtain high-quality EBSD sample, generally all pass through final electrolytic polishing method.Smooth, bright and clean, the no deformation layer of specimen surface through electropolishing still obtains relatively difficulty of suitable polishing fluid and technological parameter, need carry out lot of test and grope.Alloying component is different, and perhaps the variation of test condition all can cause the adjustment of polishing fluid and technological parameter.

The development of aeronautical technology is to the demands for higher performance of engine, and the technical merit of aeromotor is the important symbol of a national science and technology level and industrial might.The development of Aeroengines key is to improve thrust-weight ratio and fuel efficiency, and the performance of engine depends on turbine inlet temperature (TIT) to a great extent.The Ni based high-temperature alloy is owing to have high creep rupture strength and croop property; Enough toughness; Good thermal fatigue resistance and mechanical fatigue performance; Excellent high-temperature such as good oxidization resistance and hot corrosion resistance performance, thereby nickel base superalloy is the main material of making aeromotor and gas turbine blades at present, the nickel base superalloy turbo blade has been widely used on the advanced military and civil aviation engine.In research Ni based high-temperature alloy process, utilize the EBSD technology can carry out crystallite dimension analysis, crystal boundary specificity analysis, misorientation analysis, the identification of phases and phase distributional analysis.

Summary of the invention

The present invention is directed against the situation of above-mentioned prior art just and designs the method that a kind of quick Ni of preparation based high-temperature alloy EBSD sample is provided, and its objective is to simplify Ni based high-temperature alloy EBSD method of sample preparation.

Method of the present invention is without electropolishing, with the quick sample preparation of chemical corrosion method.The steps include:

⑴ cut sample with wire cutting machine, with sample with abrasive paper for metallograph pre-grinding after mechanical buffing;

⑵ prepare chemical mordant

The composition of chemical corrosion liquid and volume parts ratio are: HF: H ₂O ₂: HCl=1～3: 10～20: 30～50;

⑶ the flat pendulum of sample is poured the corrosive liquid that has just prepared into vessel internal corrosion sample in glassware, when seeing that specimen surface presents the dendrite style, take out sample immediately and rinse well with alcohol after with distilled water flushing, uses drier.

The sample of technical scheme preparation of the present invention has the following advantages:

⑴ can distinguish the zones of different on the sample owing to can see the dendrite style, when EBSD is tested in ESEM; Can analyze to zones of different, and the method for making sample of electropolishing commonly used can not macroscopic view show zones of different; Can not distinguish zones of different, specific aim is relatively poor.

⑵ sample preparation is simple, effect stability, can be with the disposable corrosion treatment of many samples, and method is simple.And the method for making sample of electropolishing, electrolytic polishing liquid increased along with the sample preparation time, and concentration and temperature variation are very fast, and the sample preparation effect is unstable, and sample must carry out one by one successively, and complicated operation is time-consuming.

Description of drawings

Fig. 1 is the Kikuchi style of the DD6 alloy EBSD sample of employing the inventive method preparation

Fig. 2 is the Kikuchi style of the DD3 alloy EBSD sample of employing the inventive method preparation

Embodiment

Below will combine accompanying drawing and embodiment that technical scheme of the present invention is done to detail further:

The Ni based high-temperature alloy of preparation EBSD sample is DD3 alloy and DD6 alloy in following examples.

The composition of the chemical corrosion liquid that table one adopts when preparing the EBSD sample for employing technical scheme of the present invention and the tabulation of volume parts ratio.

The Kikuchi style is that electron beam is beaten the diffraction pattern that forms at specimen surface in the ESEM.

Table one: the composition and the volume parts ratio of preparation EBSD sample chemical corrosion liquid

Sequence number	Alloy	HF	H 2O 2	HCl
					1	DD6	1	10	30
2	DD6	1	20	30
					3	DD6	1	20	50
4	DD6	1	15	30
					5	DD6	1	15	50
6	DD6	1	20	25
					7	DD6	2	10	30
8	DD6	2	20	30
					9	DD6	2	20	50
10	DD3	2	15	30
					11	DD3	2	15	50
12	DD3	2	20	25
					13	DD3	3	10	30
14	DD3	3	20	30
					15	DD3	3	20	50
16	DD3	3	15	30
					17	DD3	3	15	50
18	DD3	3	20	25

In the foregoing description 1, the step that employing the inventive method prepares Ni based high-temperature alloy EBSD sample is following:

1. cut sample with wire cutting machine, with the abrasive paper for metallograph pre-grinding of sample with No. 200 to No. 1200, using granularity more respectively is the brilliant polish mechanical buffing of 2.5 μ m, 1.5 μ m, 0.5 μ m;

2. preparation chemical mordant

The composition of chemical corrosion liquid and volume parts ratio are: HF: H2O2: HCl=1: 10: 30; The flat pendulum of sample is in glassware; Pour the corrosive liquid that has just prepared into vessel internal corrosion sample, when seeing that specimen surface presents the dendrite style, take out sample immediately and use distilled water flushing; Sample is rinsed well with alcohol, uses drier.The Kikuchi style of this sample is clear, sees shown in Figure 1.

In the foregoing description 15, the step that employing the inventive method prepares Ni based high-temperature alloy EBSD sample is following:

1. cut sample with wire cutting machine, with the abrasive paper for metallograph pre-grinding of sample with No. 200 to No. 1200, using granularity more respectively is the brilliant polish mechanical buffing of 2.5 μ m, 1.5 μ m, 0.5 μ m;

2. preparation chemical mordant

The composition of chemical corrosion liquid and volume parts ratio are: HF: H2O2: HCl=3: 20: 50; The flat pendulum of sample is in glassware; Pour the corrosive liquid that has just prepared into vessel internal corrosion sample, when seeing that specimen surface presents the dendrite style, take out sample immediately and use distilled water flushing; Sample is rinsed well with alcohol, uses drier.The Kikuchi style of this sample is clear, sees shown in Figure 2.

Compared with prior art; The inventive method has overcome EBSD method for making sample electropolishing sample preparation complicacy commonly used, the unsettled shortcoming of effect; The Kikuchi style of the nickel base superalloy EBSD sample of preparation is very clear; Be applicable to the preparation of equiax crystal in the Ni based high-temperature alloy, directed high temperature alloy, single crystal super alloy EBSD analytical sample, can be with big Lot sample single treatment, method of operating is simple.

Claims (1)

1. method for preparing fast Ni based high-temperature alloy EBSD sample, it is characterized in that: the step of this method is:

⑴ cut sample with wire cutting machine, with sample with abrasive paper for metallograph pre-grinding after mechanical buffing;

⑵ prepare chemical mordant

The composition of chemical corrosion liquid and volume parts ratio are: HF: H ₂O ₂: HCl=1～3: 10～20: 30～50;

⑶ the flat pendulum of sample is poured the corrosive liquid that has just prepared into vessel internal corrosion sample in glassware, when seeing that specimen surface presents the dendrite style, take out sample immediately and rinse well with alcohol after with distilled water flushing, uses drier.

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