CN105628480A - Corrosive for displaying grain boundary of original austenite of tempered martensite and corroding method - Google Patents
Corrosive for displaying grain boundary of original austenite of tempered martensite and corroding method Download PDFInfo
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- CN105628480A CN105628480A CN201510973402.4A CN201510973402A CN105628480A CN 105628480 A CN105628480 A CN 105628480A CN 201510973402 A CN201510973402 A CN 201510973402A CN 105628480 A CN105628480 A CN 105628480A
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Abstract
The invention discloses a corrosive for displaying a grain boundary of original austenite of tempered martensite and a corroding method. The corroding method comprises the following steps: preparation of a tempered martensite corroding test sample: obtaining the tempered martensite corroding test sample by a conventional method; preparation of the corrosive: putting 1 gram of picric acid into 100 ml of distilled water, adding b ml of a washing agent after the picric acid is completely dissolved, fully stirring, and stewing under normal temperature; corrosion: putting the tempered martensite corroding test sample into the corrosive, corroding the test sample for T time, taking out the test sample, washing with running water, and cleaning and drying the test sample with alcohol; grain judgment: observing under a microscope of 500 times to obtain a grain displaying picture, and performing grain judgment. According to the corroding method, the test sample is corroded under the normal temperature without heating, so that the method is economical; furthermore, the grain boundary of the corroded tempered martensite is clear and is not affected by tissues, so that respective grains can be observed clearly; the grain judgment can be performed by a comparison method, a grid method and a resection method according to an actual condition, so that the accuracy and the precision are higher.
Description
Technical field
The present invention relates to a kind of caustic and caustic solution, particularly to a kind of caustic showing tempered martensite original austenite grains border and caustic solution, belong to technical field of heat treatment.
Background technology
Grain size is an important indicator of pinion steel, and austenite grain size also directly influences the form of tempered martensite, substructure and toughness. The austenite crystal of fine uniform in pinion steel, obtains thin tempered martensite, hence it is evident that improve the fatigue behaviour of gear after quenched low-temperature tempering, reduce the deflection after gear heat treatment simultaneously. But, the original grain that how can clearly indicate tempered martensite is the problem always perplexing vast metallographic testing staff.
The mode that present most of testing staff detects grain size is that the size of the tempered martensite lath bundle relying on the presence of a phase with the nital of 4% after corroding is to pass judgment on austenite grain size; As shown in Figure 5, with the metallograph of 500 times of sample after the nitric acid ethanol caustic corrosion of 4%, examine and can indistinctly see crystal boundary, but more serious by tissue interference ratio, passing judgment on grain size only by tempered martensite phase place, above method can not show crystal grain intuitively.
Or, some heatings could show crystal grain; Also have and adopt oxidizing process display crystal grain, these methods or crystal grain can not be shown intuitively; Comparison between detecting methods is loaded down with trivial details, it is necessary to bigger energy resource consumption, and testing result is also not ideal.
Inventor have found that application number: 201310376654.X, subject name is " method on a kind of room temperature display tempering bainite tissue's original austenite grains border ", disclose a kind of caustic that can show tempering bainite tissue's crystal boundary at ambient temperature and method, caustic and method in this application can not effectively be suitable for tempered martensite, after tempered martensite's sample being corroded according to the method, sample burnishing surface is almost without reaction; Even if after prolongation etching time, crystal grain display photos as shown in Figure 6, is still difficult to find out clearly the crystal boundary of crystal grain from figure.
Therefore, demand provides a kind of caustic that can clearly indicate tempering tempered martensite crystal boundary and caustic solution so that can clearly indicate tempering tempered martensite grain size under an optical microscope.
Summary of the invention
The purpose of the present invention is contemplated to solve the above-mentioned problems in the prior art, it is provided that a kind of caustic showing tempered martensite original austenite grains border and caustic solution.
The purpose of the present invention will be achieved by the following technical programs:
A kind of caustic for showing tempered martensite original austenite grains border, it is characterized in that: include distilled water, picric acid, detergent, described picric mass percent is 1wt%, and the mass percent of described detergent is 7wt%-13wt%, and all the other are distilled water.
Preferably, described a kind of caustic for showing tempered martensite original austenite grains border, wherein: described detergent includes dodecylbenzene sodium sulfonate and alkylolamides; The mass percent of the dodecylbenzene sodium sulfonate in described caustic is 1wt%-2wt%, and the mass percent of described alkylolamides is 0.1wt%-0.2wt%.
Preferably, described a kind of caustic for showing tempered martensite original austenite grains border, wherein: described picric mass percent is 1wt%, in described caustic, the mass percent of dodecylbenzene sodium sulfonate is 1.5wt%, and the mass percent of described alkylolamides is 0.15wt%.
Preferably, described a kind of caustic for showing tempered martensite original austenite grains border, wherein: described picric acid is 1g, described detergent is 7g 13g, and described dodecylbenzene sodium sulfonate is 1g 2g, and described alkylol acyl is amine 0.1g 0.2g.
Preferably, described a kind of caustic for showing tempered martensite original austenite grains border, wherein: described bitter in the mouth acid is 1g, described detergent is 10g, and described dodecylbenzene sodium sulfonate is 1.5g, and described alkylol acyl is amine 0.15g.
A kind of caustic solution showing tempered martensite original austenite grains border, applies above-mentioned caustic and carries out etching pit, and it comprises the steps:
S1, tempered martensite corrosion sample preparation process: conventionally carry out pinion steel after carburizing and quenching, lonneal roughly grinding, fine grinding, polishing, clean, dry up after obtain tempered martensite corrosion sample;
S2, caustic preparation process: 1g picric acid is inserted in the distilled water of designated capabilities, after being completely dissolved, add volume to be the detergent of b and be sufficiently stirred for, described detergent includes dodecylbenzene sodium sulfonate and the alkylolamides of specifying mass percent, and room temperature obtains caustic after placing at least 10 minutes;
S3, corrosion step: be placed into upward in caustic by the burnishing surface of described tempered martensite corrosion sample, after the corrosion of T time, takes out tempered martensite corrosion sample, dries up with running water and with alcohol washes;
S4, crystal grain judges: observes and obtains crystal grain display photos under the microscope with 500 times, and adopt matching type or gridding method or resection to carry out crystal grain judgement.
Preferably, described a kind of caustic solution showing tempered martensite original austenite grains border, wherein: described pinion steel is 18CrNiMo7-6 carbonized Gear Steel or 20CrMnTi carbonized Gear Steel.
Preferably, described a kind of caustic solution showing tempered martensite original austenite grains border, wherein: described volume is b is 6-11ml.
Preferably, described a kind of caustic solution showing tempered martensite original austenite grains border, wherein: described volume is b is 8ml.
Preferably, described a kind of caustic solution showing tempered martensite original austenite grains border, wherein: described time T is 10-20min.
The advantage of technical solution of the present invention is mainly reflected in:
1. the present invention is corroded at normal temperatures, it is not necessary to heating, on the austenite crystal of sample without impact, economical and practical; And after corroding, only show crystal boundary, do not show intergranular structure, tempered martensite crystal boundary is not substantially completely by tissue effect, can clearly observe each crystal grain, matching type, gridding method, resection etc. can be adopted to carry out crystal grain judge according to practical situation, it is judged that accuracy, accuracy are higher.
2. the inventive method is simple to operate, and sample and caustic are easily prepared, and are absent from potential safety hazard, material consumption is few, and compared to prior art, the preparation of caustic is easier to, process simplifies more, and each material is more easy to acquisition, and their consumption, precision are easier to control.
Accompanying drawing explanation
Fig. 1 is the metallograph that the tempered martensite autstenitic grain size that in embodiment 1, the caustic of preparation corrodes 10 minutes amplifies 500 times;
Fig. 2 is the metallograph that the tempered martensite autstenitic grain size that in embodiment 1, the caustic of preparation corrodes 20 minutes amplifies 500 times;
Fig. 3 is the metallograph of the caustic corrosion tempered martensite autstenitic grain size amplification 500 times of preparation in embodiment 2;
Fig. 4 is the metallograph of the caustic corrosion tempered martensite autstenitic grain size amplification 500 times of preparation in embodiment 3;
Fig. 5 is the metallograph of the nitric acid ethanol caustic corrosion tempered martensite autstenitic grain size amplification 500 times of used in the prior art 4%;
Fig. 6 is the metallograph adopting the caustic corrosion tempered martensite autstenitic grain size in background technology to amplify 500 times.
Detailed description of the invention
The purpose of the present invention, advantage and feature, by for illustration and explanation by the non-limitative illustration of preferred embodiment below. These embodiments are only the prominent examples of application technical solution of the present invention, all technical schemes taking to be equal to replacement or equivalent transformation and formed, and all fall within the scope of protection of present invention.
A kind of caustic for showing tempered martensite original austenite grains border that the present invention discloses, including distilled water, picric acid, detergent, described picric mass percent is 1wt%, and the mass percent of described detergent is 7wt%-13wt%, and all the other are distilled water.
Wherein, described detergent include mass percent be about 15% dodecylbenzene sodium sulfonate and mass percent be about 1.5% alkylolamides; So that the mass percent of dodecylbenzene sodium sulfonate is 1wt%-2wt% in described caustic, the mass percent of described alkylolamides is 0.1wt%-0.2wt%.
Further, it is preferable that in described caustic, the mass percent of bitter in the mouth acid is 1wt%, and the mass percent of dodecylbenzene sodium sulfonate is 1.5wt%, and the mass percent of described alkylolamides is 0.15wt%.
Further, present invention is disclosed a kind of caustic solution showing tempered martensite original austenite grains border, applying above-mentioned caustic and carry out etching pit, it is adaptable to 18CrNiMo7-6 carbonized Gear Steel or 20CrMnTi carbonized Gear Steel, it specifically includes following steps:
S1, tempered martensite corrosion sample preparation process: conventionally carry out carbonized Gear Steel after carburizing and quenching, lonneal roughly grinding, fine grinding, polishing, clean, dry up after obtain tempered martensite corrosion sample, make burnishing surface is formed certain cut, in order to corrode.
S2, caustic preparation process: 1g picric acid is inserted in the distilled water of designated capabilities, after described picric acid is completely dissolved, adds volume and be the detergent of b and be sufficiently stirred for, room temperature obtains caustic after placing at least 10 minutes; Wherein said volume b is 6-11ml, corresponding described detergent is 7g 13g, and the weight respectively 1g 2g and 0.1g 0.2g of dodecylbenzene sodium sulfonate in described detergent and alkylolamides, thus providing up the mass percent requirement of above-mentioned caustic.
Further, the volume b of described detergent is preferably 8ml, and correspondence, described detergent is 10g, and described dodecylbenzene sodium sulfonate is 1.5g, and described alkylol acyl is amine 0.15.
S3, corrosion step: the burnishing surface of described tempered martensite corrosion sample is placed in caustic upward, after the corrosion of T time, corrode when the erosional surface of described tempered martensite corrosion sample becomes silver gray completely and terminate, take out tempered martensite corrosion sample, dry up with running water and with alcohol washes; Described time T is 10-20min.
S4, crystal grain judges: observes with 500 times under the microscope and obtains crystal grain display photos, adopts matching type or gridding method or resection to carry out crystal grain judgement subsequently.
Due to the substantial amounts of alloying element of austenite grain boundary region clustering, improve the interface energy of crystal boundary, so that austenite grain boundary is easier to corrosion compared to intergranular structure, therefore common caustic solution adopts weakly acidic picric acid to corrode, to avoid corrosion structure; Utilize dodecylbenzene sodium sulfonate as corrosion inhibiter simultaneously, inhibitory action is played in tissue corrosion, thus reaching only to corrode crystal boundary, the not effect of corrosion structure.
But, inventors have discovered that tempered martensite is the heterogeneous structure that Dispersed precipitate ultrafine transition carbide thin slice (being coherent boundary with the interface of matrix) in solid solution matrix (crystal structure has turned into body-centered cubic), it is to be obtained after quenching and lonneal by the austenite crystal of fine uniform, owing to austenite crystal is comparatively fine, the tempered martensite obtained is also comparatively fine, therefore the also relative tempering bainite of the border between crystal grain is more tiny, so, when carrying out etching pit, the corrosion rate on the border between crystal grain is higher than the corrosion rate of other state undertissues, thus causing under identical etching condition, tempered martensite itself is also corroded, thus border and tissue cannot effectively be distinguished.
On the other hand, studying discovery, dodecylbenzene sodium sulfonate highly volatile through inventor, in experimentation, content can constantly reduce, therefore wayward, and experimental result impact is bigger.
Therefore, for the problems referred to above, inventor is found by long-term thinking and experiment, use the detergent better effects if than directly use dodecylbenzene sodium sulfonate, and further by contrasting the experiment effect of multiple detergent on the market, it has been found that it is best that Shanghai Whitecat Shareholding Co., Ltd. produces the white cat detergent effect that net content is 500g.
This is because, in white cat detergent except containing dodecylbenzene sodium sulfonate, also have the very favorable alkylolamides of experimental result, alkylolamides is nonionic surfactant, as thickening agent and solubilizing agent, very strong stability is had with dodecylbenzene sodium sulfonate, it is to avoid dodecylbenzene sodium sulfonate waving in lab process after merging; It addition, alkylolamides also has antirust ability, in an experiment with dodecylbenzene sodium sulfonate together as corrosion inhibiter, tissue is corroded inhibitory action; In addition, alkylolamides also has soft softening performance, it is possible to improve the quality of distilled water in formula.
Further, inventor studies discovery, if white ratio added by cat detergent does not just fall flat in above-mentioned preferred scope, when white cat detergent very little time, owing to the dodecylbenzene sodium sulfonate suppressing tissue corrosion is less, then tissue will be corroded; When white cat detergent is too many, will seriously suppress corrosion, so that crystal boundary can not be corroded completely.
Certainly, the numbering of above-mentioned steps does not cause the unique restriction to operating process of the present invention, for instance S1, tempered martensite corrosion sample preparation process, it is possible to S2, caustic preparation process carries out simultaneously, it is also possible to carry out after this step.
Embodiment 1:
A kind of caustic showing tempering tempered martensite original austenite crystal boundary, including distilled water, picric acid, the washing of white cat, concrete matching method is the white cat detergent adding 1 gram of picric acid and 8 milliliters (10g) in 89 ml distilled waters, corresponding, described picric mass percent is 1wt%, the mass percent of detergent is 10wt%, the mass percent of dodecylbenzene sodium sulfonate is 1.5wt%, the mass percent of described alkylolamides is 0.15wt%, stirs rear room temperature and places 10 minutes.
When using this caustic corrosion tempered martensite original austenite grains border, after after carburizing and quenching, lonneal, conventionally method of preparing sample prepares tempered martensite corrosion sample, the burnishing surface of tempered martensite corrosion sample is immersed in caustic fully up, after room temperature is placed 10 minutes and 20 minutes, take out sample, after circulating water rinses, spray dehydrated alcohol is air-dry, under the microscope with 500 times of observations, corrode the result of 10 minutes as shown in Figure 1, corrode the result of 20 minutes as shown in Figure 2.
Embodiment 2:
A kind of caustic showing tempering tempered martensite original austenite crystal boundary, including distilled water, picric acid, the washing of white cat, concrete matching method is the white cat detergent adding 1 gram of picric acid and 6 milliliters (7g) in 92 ml distilled waters, corresponding, in described caustic, picric mass percent is 1wt%, the mass percent of detergent is 7wt%, the mass percent of dodecylbenzene sodium sulfonate is 1wt%, the mass percent of described alkylolamides is 0.1wt%, stirs rear room temperature and places 10 minutes.
When using this caustic corrosion tempered martensite original austenite grains border, after conventionally method of preparing sample prepares corrosion sample preparation, tempered martensite corrosion sample burnishing surface is immersed in caustic fully up, after room temperature is placed 15 minutes, take out sample, after circulating water rinses, spray dehydrated alcohol is air-dry, and the lower 500 times of observed results of microscope are as shown in Figure 3.
Embodiment 3
A kind of caustic showing tempering tempered martensite original austenite crystal boundary, including distilled water, picric acid, the washing of white cat, concrete matching method is the white cat detergent adding 1 gram of picric acid and 11 milliliters (13g) in 86 ml distilled waters, corresponding, in described caustic, picric mass percent is 1wt%, the mass percent of detergent is 13wt%, the mass percent of dodecylbenzene sodium sulfonate is 2wt%, the mass percent of described alkylolamides is 0.2wt%, stirs rear room temperature and places 10 minutes. When using this caustic corrosion tempered martensite original austenite grains border, after conventionally method of preparing sample prepares corrosion sample preparation, tempered martensite corrosion sample burnishing surface is immersed in caustic fully up, after room temperature is placed 15 minutes, take out sample, after circulating water rinses, spray dehydrated alcohol is air-dry, and the lower 500 times of observed results of microscope are as shown in Figure 4.
By contrasting it is found that the tempered martensite original austenite crystal boundary of Fig. 1��Fig. 4 is obvious, completely not by tissue effect, it is possible to clear each crystal grain of observation, matching type, gridding method, resection etc. can be adopted to carry out crystal grain judge according to practical situation.
The present invention still has numerous embodiments, all employing equivalents or equivalent transformation and all technical schemes of being formed, all falls within protection scope of the present invention.
Claims (10)
1. the caustic being used for showing tempered martensite original austenite grains border, it is characterized in that: include distilled water, picric acid, detergent, described picric mass percent is 1wt%, and the mass percent of described detergent is 7wt%-13wt%, and all the other are distilled water.
2. a kind of caustic for showing tempered martensite original austenite grains border according to claim 1, it is characterised in that: described detergent includes dodecylbenzene sodium sulfonate and alkylolamides; The mass percent of the dodecylbenzene sodium sulfonate in described caustic is 1wt%-2wt%, and the mass percent of described alkylolamides is 0.1wt%-0.2wt%.
3. a kind of caustic for showing tempered martensite original austenite grains border according to claim 2, it is characterized in that: described picric mass percent is 1wt%, in described caustic, the mass percent of dodecylbenzene sodium sulfonate is 1.5wt%, and the mass percent of described alkylolamides is 0.15wt%.
4. a kind of caustic for showing tempered martensite original austenite grains border according to claim 2, it is characterized in that: described picric acid is 1g, described detergent is 7g 13g, and described dodecylbenzene sodium sulfonate is 1g 2g, and described alkylol acyl is amine 0.1g 0.2g.
5. a kind of caustic for showing tempered martensite original austenite grains border according to claim 2, it is characterized in that: described bitter in the mouth acid is 1g, described detergent is 10g, and described DBSA is 1.5g, and described alkylol acyl is amine 0.15g.
6. the caustic solution showing tempered martensite original austenite grains border, it is characterised in that: the arbitrary described caustic of application claim 1-5 carries out etching pit, and it comprises the steps:
S1, tempered martensite corrosion sample preparation process: conventionally carry out pinion steel after carburizing and quenching, lonneal roughly grinding, fine grinding, polishing, clean, dry up after obtain tempered martensite corrosion sample;
S2, caustic preparation process: 1g picric acid is inserted in the distilled water of designated capabilities, after being completely dissolved, add volume to be the detergent of b and be sufficiently stirred for, described detergent includes dodecylbenzene sodium sulfonate and the alkylolamides of specifying mass percent, and room temperature obtains caustic after placing at least 10 minutes;
S3, corrosion step: be placed into upward in caustic by the burnishing surface of described tempered martensite corrosion sample, after the corrosion of T time, takes out tempered martensite corrosion sample, dries up with running water and with alcohol washes;
S4, crystal grain judges: observes and obtains crystal grain display photos under the microscope with 500 times, and adopt matching type or gridding method or resection to carry out crystal grain judgement.
7. a kind of caustic solution showing tempered martensite original austenite grains border according to claim 6, it is characterised in that: described pinion steel is 18CrNiMo7-6 carbonized Gear Steel or 20CrMnTi carbonized Gear Steel.
8. a kind of caustic solution showing tempered martensite original austenite grains border according to claim 6, it is characterised in that: described volume b is 6-11ml.
9. a kind of caustic solution showing tempered martensite original austenite grains border according to claim 6, it is characterised in that: described volume is b is 8ml.
10. according to the arbitrary described a kind of caustic solution showing tempered martensite original austenite grains border of claim 6-9, it is characterised in that: described time T is 10-20min.
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| CN110132962A (en) * | 2019-04-24 | 2019-08-16 | 东方电气集团东方锅炉股份有限公司 | A kind of original austenite crystal prevention display methods of boiler and pressure vessel tempering bainite steel |
| CN111811912A (en) * | 2020-07-17 | 2020-10-23 | 什邡新工金属材料有限公司 | Metallographic corrosion method for high-carbon martensitic stainless steel grain boundary |
| CN112082912A (en) * | 2020-09-10 | 2020-12-15 | 中车戚墅堰机车车辆工艺研究所有限公司 | Steel grain size etching agent and application thereof |
| CN113063707A (en) * | 2021-03-12 | 2021-07-02 | 浙江美力科技股份有限公司 | Corrosion method for prior austenite grain size of tempered troostite and martensite structure |
| CN113740131A (en) * | 2021-09-07 | 2021-12-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Crystal boundary display method of bainite steel |
| CN113740131B (en) * | 2021-09-07 | 2023-05-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Grain boundary display method of bainitic steel |
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