CN101545887B - Quantitative analysis method for boride - Google Patents
Quantitative analysis method for boride Download PDFInfo
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- CN101545887B CN101545887B CN 200810010793 CN200810010793A CN101545887B CN 101545887 B CN101545887 B CN 101545887B CN 200810010793 CN200810010793 CN 200810010793 CN 200810010793 A CN200810010793 A CN 200810010793A CN 101545887 B CN101545887 B CN 101545887B
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Abstract
The invention relates to a quantitative measurement technique for phases in high-temperature alloy, and in particular provides a quantitative analysis method for measuring boride in high-temperature alloy, which solves the problem that the prior method is high in workload, possible to have large deviations, and the like. The method comprises the following steps that: firstly, carbide and boride are quantitatively extracted by an electrochemical method; secondly, extracted powder is evenly got onto conductive adhesive and pressed flat, and the carbide and the boride are differentiated by use of the surface scanning of a Mo element under an electron probe; and thirdly, the volume fraction of the boride in the powder is obtained through the electron probe, and the total volume fraction of the boride is the volume fraction of the powder in the alloy, which is multiplied by the volume fraction of the boride in the powder. The method can obtain precise volume fractions through electrolytic extraction and can use the electron probe to prevent component fluctuation from causing errors which are difficult to avoid by a multiple composition method or a simultaneous equation method. The method can be used for quantitatively measuring the boride content of most high-temperature alloy.
Description
Technical field
The present invention relates to the quantitative measurment technology of phase in the high temperature alloy, a kind of quantitative analysis method of measuring modal boride in the high temperature alloy is provided especially.
Background technology
High temperature alloy refers to that with iron, nickel, cobalt be base, a metalloid material that can long-term work under the high temperature more than 600 ℃ and certain stress effect.Boron is micro-intensified element the most frequently used in the high temperature alloy.Since finding the beneficial effect of boron in high temperature alloy mid-term in last century, boron is added widely advances most the grade in axle cast superalloy and the directionally solidified superalloy, DS superalloy partly.In high temperature alloy, add an amount of boron, can increase substantially the croop property of high temperature alloy and improve plasticity.Boron mainly exists with two kinds of forms in high temperature alloy.The firstth, form boride, boron in most of high temperature alloy all with M
3B
2Form exist, have other borides to exist at indivedual alloys.The secondth, be present in matrix and in the crystal boundary enrichment, this enrichment will change the performance of crystal boundary with the form of solid solution, thereby improve the usability of alloy.This existence form is the fundamental purpose that adds boron in alloy.
A lot of high temperature alloys all will be heat-treated.In heat treatment process, solid solution and higher temperature timeliness will produce a very large impact quantity, the form of boride.Separate out a fairly large number of boride, the boride of particularly separating out bulk, thin slice dress in the high-temperature aging process can produce adverse influence to enduring quality.Separate out boride simultaneously and also can reduce the boron atom of solid solution, thereby reduced its invigoration effect to crystal boundary.Therefore, the boride quantity of measuring in the alloy is necessary.
The method of existing measurement boride is cumbersome, and its degree of accuracy is difficult to guarantee.A kind of method can be with determining one by one under the scanning electron microscope whether alloy phase is boride, and its volume fraction is added up, and divided by total volume number, obtains the volume fraction of boride.Another kind method is earlier quantitatively to extract MC and M in the alloy with electrochemical method
3B
2Etc. micro-phase, obtain M with forming method of multiplicity or equation solving approach then
3B
2Quantity.First method at first workload is huge, and because the relation that field of view is selected may produce bigger deviation.Second method is because MC and M
3B
2Composition is fluctuation within the specific limits all, is difficult to guarantee a certain characteristic element content in mutually.Therefore, second method also is difficult to realize satisfactory results.So need to seek a kind of convenient, fast and the boride measuring method of certain degree of accuracy arranged.
Summary of the invention
The object of the present invention is to provide a kind of measurement boride (M
3B
2Phase) quantitative analysis method of volume fraction, it is big to solve the workload that exists in the classic method, may produce than problems such as large deviations.
Technical scheme of the present invention is:
A kind of quantitative analysis method of boride comprises the steps:
The first step adopts electrochemical method, and quantified extract goes out carbonide and boride;
(1) make negative electrode with corrosion resistant plate, nickel plate or copper coin, make anode with sample, constant-current supply 0～10A as electrolysis power, carries out electrolysis; Consisting of of electrolytic solution: 48～52ml hydrochloric acid; 80～120ml glycerine; 1000ml～1050ml methyl alcohol; Faradaic current is 0.05～0.1A/cm
2, temperature is-5～10 ℃, takes out, and cleans in alcohol in 50～70 minutes;
(2) prepare a clean beaker, with analytical balance claim bare weight; Pour alcohol again in beaker, beaker is placed ultrasonic cleaner, put into sample and cleaned 3～5 minutes, take out;
(3) repeating step (1) and (2) again, 10～40 times so repeatedly, up to extracting enough extracts, extract reaches 0.01g～0.05g;
(4) electrolytic solution and cleaning fluid are filtered with filter paper, again the residue on the filter paper is flushed to anhydrous alcohol in the beaker of having collected extract, with this beaker oven dry, connect beaker and take by weighing weight; Simultaneously, sample after electrolysis is dried up, and measure the weight of sample after electrolysis, obtain the massfraction of extract;
Second step, with the powder that extracts, evenly be stained with conducting resinl, flatten, under electron probe, sweep with the face of Mo element, distinguish carbonide and boride;
The 3rd step obtained the volume fraction that boride accounts for powder by electron probe, and the total volume fraction of boride is that powder accounts for the alloy volume fraction and multiply by boride and account for the powder volume mark.
Before the described first step, the specimen surface of needs analysis is handled, remove oxide skin and other impurity on surface, with lathe or with emery wheel with surperficial polishing, specimen shape is bar-shaped or the square shape, coupon diameter 1～1.5cm, long 2.5～6cm, or the wide 1～3cm of square sample, thick 0.5～2cm, long 2.5～6cm, sample is polished to there not being obvious cut with 150～No. 400 coated abrasive surface.
Before the described first step, sample is put in the electrolytic tank by predefined electrolytic condition elder generation electrolysis 10～30 minutes, make negative electrode with corrosion resistant plate, nickel plate or copper coin, make anode with sample, constant-current supply 0～10A as electrolysis power, carries out electrolysis; Consisting of of electrolytic solution: 48～52ml hydrochloric acid; 80～120ml glycerine; 1000ml～1050ml methyl alcohol; Faradaic current is 0.05～0.1A/cm
2, temperature is-5～10 ℃, takes out in 10～30 minutes, and dries up, and weighs with analytical balance, and is stand-by.
Principle of the present invention is as follows:
The present invention uses electrochemical method earlier, and quantified extract goes out carbonide and boride; With the powder that extracts, evenly be stained with conducting resinl again, owing to the composition difference very big (listing in table 1 respectively) of boride and carbonide, under electron probe, sweep with the face of Mo element, to distinguish carbonide and boride.The oeverall quality mark of carbonide and boride can be obtained by quantified extract.Because its density of carbonide (NbC) is 7.8g/cm
3, boride (M
3B
2) its density is also at 7g/cm
3, and the density of most of high temperature alloy is also at 7.5～8.8cm
3, so massfraction directly can be considered as volume fraction, this processing accuracy can satisfy the accuracy requirement of metallographic.Can obtain the volume fraction that boride accounts for powder by electron probe, account for the alloy volume fraction and multiply by boride and account for the powder volume mark so the total volume fraction of boride is powder.
Table 1 be MC and M
3B
2Atomic percent
| W | C | Al | Y | Nb | Mo | Cr | Co | Ni | B | |
| M 3B 2 | 3.16 | 4 | 0.02 | 0.02 | 6.43 | 23.62 | 21.85 | 1.21 | 4.43 | 35.20 |
| MC | 0.83 | 45.30 | 0.06 | 0 | 45.80 | 1.94 | 1.08 | 1.09 | 3.91 | 0 |
Advantage of the present invention is:
1, convenient.The present invention not be used in the carbonide of discriminating one by one or the boride that microscopically carries out a lot of visuals field.
2, comprehensive.The present invention can obtain more comprehensive information because the sample of electrolysis is bigger, can not cause experimental error owing to the cause of local field of view;
3, precision is higher.Electrolytic extraction of the present invention can obtain accurate massfraction, the error that can avoid composition fluctuation to cause with the method for electron probe, and be difficult to avoid with composition method of multiplicity or equation solving approach.
Description of drawings
Fig. 1 (a)-(b) is example 1; Wherein, Fig. 1 (a) is the XRD diffraction spectra of anode extract,
Fig. 1 (b) sweeps for the electron probe face of the Mo element of its powder.
Fig. 2 (a)-(b) is example 2; Wherein, Fig. 2 (a) is the XRD diffraction spectra of anode extract,
Fig. 2 (b) sweeps for the electron probe face of the Mo element of its powder.
Fig. 3 (a)-(b) is example 3; Wherein, Fig. 3 (a) is the XRD diffraction spectra of anode extract,
Fig. 3 (b) sweeps for the electron probe face of the Mo element of its powder.
Embodiment
The quantitative analysis method of boride of the present invention comprises the steps:
(1) adopt electrochemical method, quantified extract goes out carbonide and boride;
Consisting of of electrolytic solution: 48～52ml hydrochloric acid; 80～120ml glycerine; 1000ml～1050ml methyl alcohol;
Detailed process is as follows:
At first, the specimen surface of needs analysis is handled, removed oxide skin and other impurity on surface.Generally with lathe or with emery wheel with surperficial polishing.General shape should be bar-shaped or square shape, coupon diameter 1～1.5cm, and long 2.5～6cm, or the wide 1～3cm of square sample, thick 0.5～2cm, long 2.5～6cm, sample is polished to there not being obvious cut with 150～No. 400 coated abrasive surface.
Then, sample is put in the electrolytic tank (electrolytic solution was formed the same, electrolytic condition and as follows in 10～30 minutes by the electrolysis of predefined electrolytic condition elder generation, be mainly used in getting rid of under the situations such as sample is coarse interference to measurement result), take out, and dry up, weigh with analytical balance, stand-by.Preparation electrolytic solution is prepared a glass beaker, pours 1000ml～1050ml methyl alcohol into, pours 80～120ml glycerine and 48～52ml hydrochloric acid into, fully stirs with glass bar, and is stand-by.Get clean corrosion resistant plate (or nickel plate), make negative electrode.Constant-current supply 0～10A is as electrolysis power.Make anode with sample, Faradaic current is 0.05～0.1A/cm
2, temperature is-5～10 ℃, the electronic refrigerator of available low temperature or refrigerator and constant temperature water bath control temperature.Took out, and in alcohol, cleaned in 10～30 minutes.Prepare a clean beaker, with analytical balance claim bare weight.Pour a small amount of alcohol again in beaker, beaker is placed ultrasonic cleaner, put into sample and cleaned 3～5 minutes, take out, electrolysis again, 10～40 times so repeatedly, up to extracting enough extracts (0.01g～0.05g).Electrolytic solution and cleaning fluid are filtered with filter paper, the residue on the filter paper is flushed to alcohol in the beaker of having collected extract again, this beaker is put in infrared ray bulb or the vacuum drying chamber, oven dry connects beaker and takes by weighing weight.Simultaneously, sample after electrolysis is dried up, and measure the weight of sample after electrolysis.Can obtain the massfraction of extract like this.
(2) with the powder that extracts, evenly be stained with conducting resinl, flatten, under electron probe, sweep with the face of Mo element, distinguish carbonide and boride.
(3) obtain the volume fraction that boride accounts for powder by electron probe, the total volume fraction of boride is that powder accounts for the alloy volume fraction and multiply by boride and account for the powder volume mark.
Further describe below by embodiment and accompanying drawing.
Embodiment 1
Select for use a Ni-based axle cast superalloy K495 that waits as technic metal.The one-tenth of this alloy is respectively in table 3.Getting an alloy test block plate tensile sample to be detected is wide 2cm, long 5cm, thick 0.5cm.Its surface is removed oxide and the impurity on surface with No. 400 sand paperings.Alloy is placed on electrolysis in the electrolytic solution (50ml hydrochloric acid+100ml glycerine+1050ml methyl alcohol).Faradaic current is determined according to electrolytic surface is long-pending, is 0.07A/cm substantially
2, temperature is 0 ± 5 ℃.Sample is anode, gets the nickel plate as negative electrode.
Coupon is cleaned then by the first electrolysis of above-mentioned condition 15 minutes, dries up, with the accurate weighing of analytical balance.Get a beaker, also dry up weighing behind the wash clean, stand-by.Again sample is formally put into the electrolytic solution electrolysis, each hour taken out sample, puts into alcohol and gently is stained with, and puts into the beaker that absolute ethyl alcohol is housed again, and with vibration of ultrasonic wave about three minutes, electrolysis again.Present embodiment 16 times so repeatedly is up to the micro-phase that extracts q.s.The coupon that has extracted is cleaned, dried up, accurately measure with analytical balance.Filter electrolytic solution and cleaning alcohol with the closeest filter paper (the filter paper aperture is 1～3 μ m), its anode extract that drops is filled on the filter paper, wash with absolute ethyl alcohol with filter paper again, whole anode extracts is poured in the beaker, again drying box is put in the beaker oven dry, oven dry is weighed with analytical balance.
Like this, just obtained the massfraction of extract:
The massfraction %=beaker weightening finish/electrolysis coupon loss of weight of anode extract;
Choose powder again and make XRD, shown in Fig. 1 (a), confirm that this powder is by MC (NbC) and M
3B
2Form, powder is stained with in the conducting resinl, flatten, the face that carries out the Mo element with electron probe instrument is swept again, because the rich Mo of boride, and carbonide contains Mo hardly.So, sweep the volume fraction that figure can obtain boride according to face.
In the present embodiment, samples weighed 40.02026g before the electrolysis, heavy 28.13372g after the electrolysis.The heavy 92.05169g of clean beaker, middle 92.07482g behind the adding powder.Like this,
(NbC+M
3B
2) massfraction %=(92.07482-92.05169)/(40.02026-28.13372)=0.193%;
By the electron probe result of Fig. 1 (b) as can be known, the boride volume is about 5% of powder, and obtaining the percent by volume that boride accounts in the alloy like this is 0.193% * 5%=0.01%.As can be known, the boride content of this alloy is about 0.01%.
Table 2 is the alloying component (mass percent) of embodiment 1 sample
| C | B | Y | Cr | Co | Mo | Nb | W | Al | Ni | |
| Embodiment 1 | 0.05 | 0.023 | 0.013 | 9 | 5 | 3 | 2.2 | 3.5 | 6 | Surplus |
Embodiment 2
The K495 alloy, its one-tenth is respectively in table 3, and different with precedent is Y content difference.Get a cylinder sample, with its surperficial car light, remove oxide and the impurity on surface with lathe with No. 400 sand paperings.Specimen finish is 1.5cm, long 2.5cm.Alloy is placed on electrolysis in the electrolytic solution (48ml hydrochloric acid+110ml glycerine+1000ml methyl alcohol).Electric current is 0.05A/cm
2, the temperature temperature is 0 ± 5 ℃.Sample is anode, gets corrosion resistant plate as negative electrode.As above example extracts 24 times repeatedly, and the face that carries out the Mo element under electron probe instrument is swept.Its XRD of the powder that extracts does the XRD diffraction, and its result is shown in Fig. 2 (a).
The preceding extraction sample mass of electrolysis is 36.82609g, extraction back 22.62545g, the heavy 92.05170g of clean beaker, heavy 92.073649g behind the adding powder.Like this,
(NbC+M
3B
2) massfraction %=(92.07364-92.05170)/(36.82609-22.62545)
＝0.02194/14.20064＝0.1545％；
And show that as the result of the EPMA of Fig. 2 (b) the boride volume fraction is about 3% of powder, like this, the volume fraction of boride in whole alloy is 0.1545% * 3%=0.005%.
Table 3 is the alloying component (mass percent) of embodiment 2 samples
| C | B | Y | Cr | Co | Mo | Nb | W | Al | Ni | |
| Embodiment 2 | 0.05 | 0.023 | 0.002 | 9 | 5 | 3 | 2.2 | 3.5 | 6 | Surplus |
Embodiment 3
Test material is the DZ951 alloy of directional solidification, and its one-tenth is respectively in table 4.Get cylinder sample, with its surperficial car light, remove oxide and the impurity on surface with lathe with No. 400 sand paperings.Specimen finish 1.2cm, long 5cm.Alloy is placed on electrolysis in the electrolytic solution (52ml hydrochloric acid+80ml glycerine+1020ml methyl alcohol).Electric current is 0.08A/cm
2, temperature is 0 ± 5 ℃.Sample is anode, gets the nickel plate as negative electrode.As above example extracts 20 times repeatedly, and the face that carries out the Mo element under electron probe instrument is swept.The powder that extracts is made XRD.As seen the XRD diffraction spectra mainly is MC and M shown in Fig. 3 (a)
23C
6, cannot see M basically
3B
2, M
23C
6Composition see Table 5.Can estimate M
3B
2Few or do not have.
Extraction sample before the electrolysis is 46.27412g, the heavy 37.50494g of sample after electrolysis.Clean beaker is the same, and is heavy by 92.08256 behind the adding powder.Then,
(NbC+M
3B
2)wt％＝(92.08256-92.05169)/(46.27412-37.50494)＝0.35％；
Extraction powder face is swept shown in Fig. 3 (b), and visible boride is few, can ignore;
Like this, the volume fraction of boride in whole alloy is that the result of 0%, XRD and the result of electron probe can verify mutually.
Table 4 is the alloying component (mass percent) of embodiment 3 samples
| C | B | Y | Cr | Co | Mo | Nb | W | Al | Ni | |
| Embodiment 3 | 0.05 | 0.005 | 0.017 | 9 | 5 | 3 | 2.2 | 3 | 6 | Surplus |
Table 5 is M among the embodiment 3
23C
6The composition of phase (atomic percent)
| C | B | Y | Cr | Co | Mo | Nb | W | Al | Ni | |
| Embodiment 3 | 17.03 | 2.96 | 0.011 | 41.40 | 1.78 | 4.96 | 0.86 | 1.13 | 4.05 | 25.8 |
Embodiment result shows that the present invention can be used for the quantitative measurment boride content of most high-temperature alloy, especially during as cast condition.Because M
6C type carbonide also is rich in the Mo element, so the alloy that is suitable for requires not separate out M
6C type carbonide.The powder that extracts is made XRD, can know whether this powder contains M
6C type carbonide.As contain M
6C type carbonide, then this method can not be suitable for.
Claims (3)
1. a quantitative analysis method of measuring boride in the high temperature alloy is characterized in that, described high temperature alloy is Ni-based axle cast superalloy K495 or the high temperature alloy DZ951 of waiting, and this method comprises the steps:
The first step adopts electrochemical method, and quantified extract goes out carbonide and boride;
(1) make negative electrode with corrosion resistant plate, nickel plate or copper coin, make anode with sample, constant-current supply 0～10A as electrolysis power, carries out electrolysis; Consisting of of electrolytic solution: 48～52ml hydrochloric acid; 80～120ml glycerine; 1000ml～1050ml methyl alcohol; Faradaic current is 0.05～0.1A/cm
2, temperature is-5～10 ℃, takes out, and cleans in alcohol in 50～70 minutes;
(2) prepare a clean beaker, with analytical balance claim bare weight; Pour alcohol again in beaker, beaker is placed ultrasonic cleaner, put into sample and cleaned 3～5 minutes, take out;
(3) repeating step (1) and (2) again, 10～40 times so repeatedly, up to extracting enough extracts, extract reaches 0.01g～0.05g;
(4) electrolytic solution and cleaning fluid are filtered with filter paper, again the residue on the filter paper is flushed to anhydrous alcohol in the beaker of having collected extract, with this beaker oven dry, connect beaker and take by weighing weight; Simultaneously, sample after electrolysis is dried up, and measure the weight of sample after electrolysis, obtain the massfraction of extract;
(5) powder that extracts is made XRD, as not containing M6C type carbonide in the powder, extract is swept with the face of Mo element under electron probe;
Second step, with the powder that extracts, evenly be stained with conducting resinl, flatten, under electron probe, sweep with the face of Mo element, distinguish carbonide and boride;
The 3rd step obtained the volume fraction that boride accounts for powder by electron probe, and the total volume fraction of boride is that powder accounts for the alloy volume fraction and multiply by boride and account for the powder volume mark.
2. according to the quantitative analysis method of the described boride of claim 1, it is characterized in that, before the described first step, the specimen surface of needs analysis is handled, remove oxide skin and other impurity on surface, with lathe or with emery wheel with surperficial polishing, specimen shape is bar-shaped or the square shape, coupon diameter 1～1.5cm, long 2.5～6cm, or the wide 1～3cm of square sample, thick 0.5～2cm, long 2.5～6cm, sample is polished to there not being obvious cut with 150～No. 400 coated abrasive surface.
3. according to the quantitative analysis method of the described boride of claim 1, it is characterized in that, before the described first step, sample is put in the electrolytic tank by the first electrolysis of predefined electrolytic condition 10～30 minutes, make negative electrode with corrosion resistant plate, nickel plate or copper coin, make anode with sample, constant-current supply 0～10A, as electrolysis power, carry out electrolysis; Consisting of of electrolytic solution: 48～52ml hydrochloric acid; 80～120ml glycerine; 1000ml～1050ml methyl alcohol; Faradaic current is 0.05～0.1A/cm
2, temperature is-5～10 ℃, takes out in 10～30 minutes, and dries up, and weighs with analytical balance, and is stand-by.
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| CN108918221A (en) * | 2018-07-12 | 2018-11-30 | 中国航发哈尔滨轴承有限公司 | Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel |
| CN112553679B (en) * | 2020-11-03 | 2024-02-09 | 中国航发北京航空材料研究院 | Method for separating harmful phase monomer from isothermal forging die material for turbine disk |
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| CN1278063A (en) * | 1999-05-28 | 2000-12-27 | 株式会社明电舍 | Electrochemical analysis using electrode coated with conductive diamond, and electrochemical analysis system therewith |
| WO2003041835A1 (en) * | 2001-11-13 | 2003-05-22 | Metanomics Gmbh & Co. Kgaa | Method for the extraction and analysis of contents made from organic material |
| CN1912570A (en) * | 2006-09-14 | 2007-02-14 | 中国铝业股份有限公司 | Method for analysing metallographic structure in aluminium alloy |
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|---|---|---|---|---|
| CN1278063A (en) * | 1999-05-28 | 2000-12-27 | 株式会社明电舍 | Electrochemical analysis using electrode coated with conductive diamond, and electrochemical analysis system therewith |
| WO2003041835A1 (en) * | 2001-11-13 | 2003-05-22 | Metanomics Gmbh & Co. Kgaa | Method for the extraction and analysis of contents made from organic material |
| CN1912570A (en) * | 2006-09-14 | 2007-02-14 | 中国铝业股份有限公司 | Method for analysing metallographic structure in aluminium alloy |
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| 《Boron solubility and boride compostions in a2+r titanium aluminides》;D.J.Larson et al;《Intermetallics》;19971231(第5期);411-414 * |
| 《Quantification of the minor precipitates in UDIMET ALLOY(LI) using electrolytic extraction and X-ray diffraction》;S.E. KiM el al;《MATERIALS SCIENCE &ENGINEERING A》;19981231(第245期);225-232 * |
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