CN104846426B - A kind of Nb Si based material microscopic structure corrosive agent and electrolytic etching method - Google Patents
A kind of Nb Si based material microscopic structure corrosive agent and electrolytic etching method Download PDFInfo
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- CN104846426B CN104846426B CN201510212745.9A CN201510212745A CN104846426B CN 104846426 B CN104846426 B CN 104846426B CN 201510212745 A CN201510212745 A CN 201510212745A CN 104846426 B CN104846426 B CN 104846426B
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Abstract
The present invention relates to a kind of corrosive agent prepared for Nb Si based material microscopic structures sample and electrolytic etching method, the Metallographic Analysis field belonged in Physical Metallurgy.The present invention is using volume content as 98%H3PO4：H2O=1：99 solution is as corrosive agent, using the Nb Si based materials after polishing as anode, stainless steel is as negative electrode, electrolytic etching is carried out by dc source, Nb Si based materials microstructure observation sample is prepared, so as to conveniently be analyzed by light microscope the composition phase in Nb Si based materials and displaing micro tissue topography.
Description
Technical field
The invention belongs to the Metallographic Analysis field in Physical Metallurgy, is related to a kind of Nb-Si based materials microscopic structure that is used for and tries
Corrosive agent and electrolytic etching method prepared by sample.
Background technology
The raising of gas-turbine unit thrust-weight ratio is strongly dependent on the raising of inlet temperature before high-pressure turbine.A new generation
Inlet temperature is up to 2100~2200K before the engine turbine of thrust-weight ratio 15~20, in view of the cold of blade itself air cooling structure
But under the premise of the effect of heat insulation of effect and thermal barrier coating, the temperature capability that high-pressure turbine is oriented to working-blade in itself must reach
More than 1150 DEG C, substantially exceed current nickel-base high-temperature metal material limit temperature capability (operating temperature be no more than 1120 DEG C,
Through meet or exceed fusing point 85%).Therefore, traditional Ni based high-temperature alloys can not meet the elder generation of higher performance of new generation
Enter the needs of aero-engine, it is necessary to study new high temperature structural materials system.
Nb-Si based materials possess high-melting-point, low-density, excellent elevated temperature strength, and its design concept is to utilize Nb-Si binary
Wide two-phase section in phasor, it is intended to which, using the plasticity and toughness of Nb solid solution and the high intensity of Nb base silicides, obtaining has well
The exotic material of combination property.The target temperature in use of Nb-Si based materials is 1200-1400 DEG C, strong in temperature in use, high temperature
Degree, fatigue behaviour etc. have obvious advantage, and it is most potential as high-temperature structural material of future generation to substitute Ni based high-temperature alloys
One of material.
GE companies of the U.S., French aerospace institute etc. put into a large amount of manpower and materials exploitation Nb-Si based materials, and on basis
Achieved in terms of research and new material, new technology compared with quantum jump.2003, GE companies, which pour, outpoured the accurate casting of Nb-Si based materials
Make simulating piece.Work(has been carried out in the first generation Nb-Si systems superhigh temperature structural material engine blade that GE companies develop at present
Can examination.In addition, under the support of Luo-sieve company etc., the unit such as French aerospace institute has prepared length 320mm by hot investment casting
Nb-Si alloy vanes.China also in Devoting Major Efforts To Developing Nb-Si based materials, have studied from binary to multicomponent system, alloy phase composition
Also Nb based solid solutions+silicide of multicomponent system is developed into from Nb based solid solutions+silicide Nb3Si of the alloy of binary
Nb5Si3, in addition alloy part also contain Cr2Nb phases, alloy comprehensive mechanical property is improved largely.
But Nb-Si based materials are a kind of new structural materials, its composition is mutually totally different from existing ripe system
Material, such as steel, aluminium alloy, titanium alloy, high temperature alloy, using existing corrosive agent, formed for Nb-Si based materials mutually equal
Corrosion can be produced, so as to produce more illusion, the composition phase of alloy can not be differentiated well by observation by light microscope,
Need to be observed using SEM backscattered electron imaging function, deposited in terms of large dimension specimen multizone observation
In a definite limitation, and waste a large amount of manpower and materials.
The content of the invention
The present invention is directed to the above situation, and invention provides a kind of corrosive agent and electricity prepared for Nb-Si systems microscopic structure
Solve caustic solution.Microstructure observation of the Nb-Si systems sample prepared using the corrosive agent and caustic solution, in optics metallography microscope
The composition phase and pattern of Nb-Si based materials can be clearly told under mirror.
The technical solution of the present invention is that the composition and liquid volume proportion of the corrosive agent are：98%H3PO4：H2O=
1：99.
Corrosion step is as follows：
(1) in glass or ceramics or metalware, according to 98%H3PO4：H2O=1：99 ratio is by 98%H3PO4Add
Enter to H2In O, and it is uniformly mixing to obtain corrosive agent；
(2) the Nb-Si based materials by polishing are connected to the positive pole of dc source, stainless steel plate is connected to direct current
The negative pole in source；Nb-Si based materials after polishing and stainless steel plate are then immersed to corrosive agent that step (1) configure simultaneously ought
In, corrosive agent temperature range is 23-30 DEG C, and makes Nb-Si based materials burnishing surface and stainless steel plate relative, but can not be contacted；Beat
Dc source is driven, by voltage Tiao Jiedao 70-80V, observes curent change situation；When electric current is stablized it is constant when, close dc source,
Nb-Si based materials are taken out among solution, and with being dried up after alcohol washes.
The composition of Nb-Si based materials mutually includes Nb based solid solutions and Nb base silicides, can also include Cr2Nb phases.
The present invention has the advantage that and beneficial effect
The present invention is using volume content as 98%H3PO4：H2O=1：99 solution enters as corrosive agent to Nb-Si based materials
Row electrolytic etching can be adapted to the microscopic structure sample of observation by light microscope to prepare.The corrosive agent is to Nb-Si based materials
In contained Nb based solid solutions, Nb bases silicide and corrosive effect caused by Cr2Nb phases it is different, can be upper in corrosion process
State three kinds of different composition phase surfaces and adhere to different corrosion products films, absorption and reflectivity of these corrosion products films to light are not
Together, different color or gray scale will be presented in observation by light microscope, realizes effective differentiation of three kinds of composition phases, effectively improve
The convenient, fast degree of the tissue topography of Nb-Si based materials.Corrosion temperature, corrosion in used electrolytic etching method
The control of voltage and by " electric current is stablized constant " as corrosion three main technological parameters of finish time be specific to
Corrosive agent and the setting of Nb-Si based materials are stated, ensure that can be attached in the different composition phase surface of Nb-Si based materials in corrosion process
Corrosion products film；And it is to be different from other electrolytic etching methods using " electric current is stablized constant " as corrosion finish time.
Brief description of the drawings
Fig. 1 is the vacuum non-consumable electric arc melting Nb-22Ti-16Si-3Cr-3Al-2Hf sample lath silicon in embodiment 1
Compound microscopic structure
Fig. 2 is that the vacuum non-consumable electric arc melting Nb-22Ti-16Si-3Cr-3Al-2Hf sample Nb bases in embodiment 1 are consolidated
The eutectic structure of solution and silicide
Fig. 3 is that the orientation of electromagnetic cold crucible directional solidification Nb-22Ti-16Si-3Cr-3Al-2Hf samples in embodiment 2 is coagulated
Gu tissue
Embodiment
The present invention is furture elucidated in a manner of specific embodiment below, rather than is limited only to embodiment.
The present invention is using volume content as 98%H3PO4：H2O=1：99 solution is tried Nb-Si based materials as corrosive agent
Sample carries out electrolytic etching, and caustic solution is made up of following steps：
(1) in glass or ceramics or metalware, according to volume ratio by H3PO4(98%) it is added to H2In O, and stir
Uniformly；
(2) the Nb-Si based materials pole by polishing is connected to the anode of dc source, stainless steel plate (block) is connected to
The negative pole of dc source；Nb-Si based materials after polishing and stainless steel plate are then immersed to the corrosive agent that step 1 has configured simultaneously
It is central, and make Nb-Si based materials burnishing surface and stainless steel plate (block) relatively, but can not contact；Dc source is opened, voltage is fast
Velocity modulation section observes curent change situation to 70-80V；When electric current is stablized it is constant when, close dc source, taken out among solution
Nb-Si based materials, and with being dried up after alcohol washes.
Embodiment 1
Carry out preparing Nb-Si based material microscopic structure samples in accordance with the following steps：
1) corrosive agent configures：1ml H are measured using graduated cylinder amount respectively3PO4 and 99ml H2O, the H that will be measured first2O is inserted
In glass beaker, the H that will then measure3PO4 is poured into beaker, and stirs 30s or so with glass bar；
2) the Nb-22Ti-16Si-3Cr-3Al-2Hf material samples prepared using vacuum non-consumable electric arc melting are carried out
Polishing, and by wire be connected to rated operational voltage 120V, rated operational current 3A dc source XD173A-120 sun
Pole, stainless steel plate is connected to the negative electrode of the power supply by wire, keeps the throwing of Nb-22Ti-16Si-3Cr-3Al-2Hf samples
Smooth surface and stainless steel plate keep relative, but can not contact；
3) switch of dc source is opened, voltage is adjusted into rapidly 80V, observes the situation of change of electric current, when electric current is steady
Regularly, DC power supply switch is closed；
4) Nb-22Ti-16Si-3Cr-3Al-2Hf material samples are taken out from corrosive liquid, be rinsed with alcohol, and
Dried up with hair-dryer.
The Nb-22Ti-16Si-3Cr-3Al-2Hf samples obtained are observed using DM6000 light microscopes, seen
Examine result and show obvious lath silicide tissue (Fig. 1) in Nb-22Ti-16Si-3Cr-3Al-2Hf samples be present, and
The eutectic structure (Fig. 2) of Nb based solid solutions and silicide be present in subregion.
Embodiment 2
Carry out preparing Nb-Si based material microscopic structure samples in accordance with the following steps：
1) corrosive agent configures：1ml H are measured using graduated cylinder amount respectively3PO4 and 99ml H2O, the H that will be measured first2O is inserted
In glass beaker, the H that will then measure3PO4 is poured into beaker, and stirs 30s or so with glass bar；
2) by using the Nb-20Ti-16Si-3Cr-3Al-2Hf material crystallines forward position sample of electromagnetic cold crucible directional solidification
It is polished, and rated operational voltage 120V, rated operational current 3A dc source XD173A-120 is connected to by wire
Anode, stainless steel plate is connected to the negative electrode of the power supply by wire, keeps Nb-22Ti-16Si-3Cr-3Al-2Hf samples
Burnishing surface and stainless steel plate keep relative, but can not contact；
3) switch of dc source is opened, voltage is adjusted into rapidly 70V, observes the situation of change of electric current, when electric current is steady
Regularly, DC power supply switch is closed；
4) by electromagnetic cold crucible directional solidification Nb-22Ti-16Si-3Cr-3Al-2Hf material crystalline samples from corrosive liquid
Take out, be rinsed with alcohol, and dried up with hair-dryer.
Using DM6000 light microscopes to the electromagnetic cold crucible directional solidification Nb-22Ti-16Si-3Cr-3Al- that is obtained
2Hf samples are observed, observation indicate that in electromagnetic cold crucible directional solidification Nb-22Ti-16Si-3Cr-3Al-2Hf samples
In the presence of obvious oriented growth trend (Fig. 3).
Claims (1)
- A kind of 1. caustic solution of Nb-Si based materials microscopic structure corrosive agent, it is characterised in that：Using the composition and liquid of corrosive agent State volume proportion is：98%H3PO4：H2O=1：99, corrosion step is as follows：(1) in glass or ceramics or metalware, according to 98%H3PO4：H2O=1：99 by 98%H3PO4It is added to H2In O, And it is uniformly mixing to obtain corrosive agent；(2) the Nb-Si based materials by polishing are connected to the positive pole of dc source, stainless steel plate is connected to dc source Negative pole；Then the Nb-Si based materials after polishing and stainless steel plate are immersed among the corrosive agent that step (1) configure simultaneously, corruption It is 23-30 DEG C to lose agent temperature range, and makes Nb-Si based materials burnishing surface and stainless steel plate relative, but can not be contacted；Open direct current Power supply, by voltage Tiao Jiedao 70-80V, observe curent change situation；When electric current is stablized it is constant when, close dc source, from solution Central taking-up Nb-Si based materials, and with being dried up after alcohol washes.
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