CN105695995A - Preparation method for H62 common brass metallographic etchant and metallographic etching method of H62 common brass metallographic etchant - Google Patents
Preparation method for H62 common brass metallographic etchant and metallographic etching method of H62 common brass metallographic etchant Download PDFInfo
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- CN105695995A CN105695995A CN201610215548.7A CN201610215548A CN105695995A CN 105695995 A CN105695995 A CN 105695995A CN 201610215548 A CN201610215548 A CN 201610215548A CN 105695995 A CN105695995 A CN 105695995A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/18—Acidic compositions for etching copper or alloys thereof
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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Abstract
The invention discloses a preparation method for an H62 common brass metallographic etchant and a metallographic etching method of the H62 common brass metallographic etchant. The metallographic etchant is prepared from water and concentrated nitric acid according to certain proportion. The metallographic etching method of the H62 common brass metallographic etchant mainly comprises the steps of cutting and obtaining of a sample, inlaying of the sample, grinding and polishing of the sample, washing of the sample, etching of the sample, washing of the etched sample and metallographic observation of the sample. The preparation method for the H62 common brass metallographic etchant and the metallographic etching method of the H62 common brass metallographic etchant have the advantages that the ratio of the metallographic etchant is more reasonable, and the content of the concentrated nitric acid is lowered, so that the metallographic etchant is suitable for metallographic detection of the H62 common brass, the over-etching phenomenon is avoided, and a metallographic structure can be obtained fast and efficiently through etching; enterprises can conveniently change and optimize technological parameters in the processing and production course, and the product quality is controlled and improved; the metallographic sample is subjected to sample inlaying before metallographic etching, so that the operation safety of the metallographic sample in the etching process is ensured, and potential safety hazards existing in the metallographic etching process are avoided.
Description
Technical field
The invention belongs to metal material technical field of metallographic detection, be specifically related to preparation method and the etching pit method thereof of a kind of H62 basis brass metallographic etchant。
Background technology
Metallographic detection is the important means that metal material research or manufacturing enterprise grasp product organizational structure and grain size in process of production in time, thus the quality problems occurred in production process are analyzed, change and Optimizing Process Parameters, control and improving product quality, etching pit is the link that metallographic detection is important, applicable caustic is only utilized to erode away metallographic structure clearly and crystal boundary, just can carry out the observation of metallographic structure and the analysis of grain size and each phase content, thus judging that whether Technology for Heating Processing is qualified, it is analyzed judging to the reasonable heat treatment process after adjusting。
H62 basis brass only has copper and two kinds of elements of zinc, its patience is poor, easily it is corroded, the more difficult control of etching pit, etching time is extremely difficult grasp also, very easily there is excessive erosion phenomenon, according to existing nitric acid and water or nitric acid, the corrosive liquid that hydrochloric acid and water configure according to a certain percentage carries out the corrosion of H62 basis brass metallographic specimen, there will be following problem, first is that metallographic etchant proportioning is unreasonable, metallographic etchant concentrated nitric acid content is higher, cause that the corrosive nature of metallographic etchant is stronger, it is unsuitable for the detection of H62 basis brass metallographic, second is that excessive erosion phenomenon takes place frequently, owing to the patience of H62 basis brass is poor, easily it is corroded, the concentration of metallographic etchant is higher, etching time is shorter, excessive erosion phenomenon often occurs, cause that black all occur in crystal boundary and crystal grain, do not observe metallurgical structure clearly, 3rd is that sample does not have sample to inlay step in the process that metallographic detects, have a strong impact on the production safety in metallographic detection process, once misoperation, easily there is the safety problem that staff's hand is scalded。
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of H62 basis brass metallographic etchant and etching pit method thereof; unreasonable to solve metallographic etchant proportioning in prior art; excessive erosion phenomenon takes place frequently, and does not observe metallurgical structure clearly, the problem that metallographic specimen lacks safety precautions。
For reaching above-mentioned purpose, the preparation method that the technical scheme is that a kind of H62 basis brass metallographic etchant, beaker adds water, add concentrated nitric acid, the ratio of water and concentrated nitric acid is 8-12:1, utilizes the liquid in Glass rod stirring beaker, stands 10-15min after its mix homogeneously。
Preferably, water is 10:1 with the ratio of concentrated nitric acid。
A kind of H62 basis brass etching pit method, comprises the following steps:
(1) intercepting of sample: utilize wire cutting machine to intercept the sample of 10-20mm from H62 basis brass ingot casting；
(2) grinding and polishing of sample: a) utilize varigrained abrasive paper for metallograph that metallographic specimen is carried out grinding and polishing；B) utilizing abrasive pastes to carry out grinding and polishing on buffing machine, polishing time is 1.5-2min；C) specimen surface without any cut and bright sliding time, with distilled water as lubricant, utilize polishing cloth to carry out grinding and polishing, polishing time is 0.5-1.5min；
(3) flushing of sample: first rinse specimen surface with water, then use alcohol rinse specimen surface；
(4) corrosion of sample: sample is put in glass dish, utilizes plastic dropper to draw corrosive liquid as claimed in claim 1, corrosive liquid drops in specimen surface, and etching time is 1-2min；
(5) flushing of sample after corrosion: utilize ferrum to hold the sample after son holds corrosion under the arm under the arm, and put into be loaded with in the large beaker of water and be rinsed；Then distilled water is utilized to be rinsed, washing time 1-2min；Finally utilize absorbent cotton and alcohol rinse specimen surface, and utilize hair-dryer to dry up specimen surface；
(6) metallographic observation of sample: utilize the metallographic of metallography microscope sem observation sample。
Preferably, sample is inlayed after terminating by step (1), utilizes metallographic pointing machine that sample is inlayed, preset that to inlay temperature be 140 DEG C, sample is put in pointing machine, and powder is inlayed in addition, put into and inlay mould and itself and sample are fixed, power transmission, pressurization, when inlaying after temperature reaches 140 DEG C, being incubated 15-20min, sample is also taken out in power-off after natural cooling 10-15min。
Preferably, inlaying powder is resinox。
Preferably, the diameter of H62 basis brass ingot casting is 5mm。
Preferably, abrasive pastes buffing machine used are diamond paste。
Preferably, the etching time of step (4) is 1.5-2min。
Preferably, the etching time of step (4) is 1.8-2min。
It is an advantage of the current invention that: water and concentrated nitric acid are gone out metallographic etchant according to the proportions that volume ratio is 8-12:1, the proportioning making metallographic etchant is more reasonable, reduce the content of concentrated nitric acid, metallographic etchant is made to be applicable to the metallographic detection of H62 basis brass, avoid the generation of excessive erosion phenomenon, can be quick, erode away metallographic structure efficiently, the internal structure of H62 basis brass can be observed clearly, enterprise is facilitated to observe the metallographic structure of H62 basis brass, enterprise is facilitated to change and Optimizing Process Parameters in processing process, control the quality of also improving product, metallographic specimen carries out sample before carrying out etching pit and inlays, ensure that the processing safety in metallographic specimen corrosion process, avoid the potential safety hazard existed in etching pit process。
Accompanying drawing explanation
Fig. 1 is the metallurgical structure schematic diagram (× 100) of 1# sample。
Fig. 2 is the metallurgical structure schematic diagram (× 100) of 2# sample。
Fig. 3 is the metallurgical structure schematic diagram (× 100) of 3# sample。
Fig. 4 is the metallurgical structure schematic diagram (× 100) of 4# sample。
Detailed description of the invention
Illustrate that the invention will be further described with embodiment below in conjunction with accompanying drawing。
The processing of sample, first, utilizes wire cutting machine to intercept three metallographic specimens of 15mm, sample respectively 1#, 2#, 3# and 4# from the H62 basis brass ingot casting that diameter is 5mm；Secondly, sample is inlayed, the XQ-2 type metallographic pointing machine that Shanghai Household Motor Factory produces is utilized respectively 1#, 2#, 3# and 4# sample to be carried out sample and inlayed, preset that to inlay temperature be 140 DEG C, sample is put in metallographic pointing machine, and add resinox and inlay powder, guarantee that sample and is in erectility in inlaying powder, put into and inlay mould and utilize screw to be fastened, power transmission, pressurization, when inlaying after temperature reaches 140 DEG C, being incubated 13-17 DEG C, sample is also taken out in power-off after natural cooling 10-15min；Again, respectively to 1#, 2# and 3# sample carries out grinding and polishing, first with 400 orders, the abrasive paper for metallograph of 800 orders and 1000 orders carries out the grinding and polishing of sample, eliminate the major part cutting cut of specimen surface, the abrasive paper for metallograph recycling 1500 order 2000 orders carries out the grinding and polishing of sample, make specimen surface more smooth, smooth, then the diamond paste utilizing 3 microns polishes on polished machine, polishing time is 1.5-2min, when observe specimen surface without any cut and bright sliding time, with distilled water as lubricant, polishing cloth is utilized to carry out grinding and polishing, polishing time is 0.5-1.5min, the grinding and polishing quality of metallographic specimen directly affects etching pit result and metallographic structure analysis；Again, the sample after grinding and polishing is rinsed, rinses specimen surface with water；Finally, use alcohol rinse specimen surface, wait the corrosion of sample。
Embodiment 1
In the preparation of metallographic etchant, the water first measuring 16ml the beaker adding 50ml range, then measure 2ml concentrated nitric acid again and add in beaker, the ratio of water and concentrated nitric acid is 8:1, utilize the liquid in Glass rod stirring beaker, after its mix homogeneously, stand 11min, stand-by。
Etching pit, take 1# sample and put in glass dish, plastic dropper is utilized to draw the metallographic etchant prepared, metallographic etchant is dropped in 1# specimen surface, etching time is 1.2min, after corrosion terminates, ferrum is utilized to hold the 1# sample after son holds corrosion under the arm under the arm, and put into be loaded with in the large beaker of water and be carried out, then utilize distilled water that 1# sample is rinsed, washing time is 1.2min, utilize absorbent cotton wiping 1# specimen surface, then alcohol rinse 1# specimen surface is utilized, the ethanol of 1# specimen surface is dried up again with hair-dryer, and guarantee that 1# specimen surface is without after residual acid and salt ion, utilize the metallographic of metallography microscope sem observation 1# sample。
1# metallurgical structure schematic diagram as shown in Figure 1, observes it can be seen that adopt the H62 basis brass ingot casting that rapid solidification method produces, forms fine grained region in ingot casting edge。
Embodiment 2
In the preparation of metallographic etchant, the water first measuring 18ml the beaker adding 50ml range, then measure 2ml concentrated nitric acid again and add in beaker, the ratio of water and concentrated nitric acid is 9:1, utilize the liquid in Glass rod stirring beaker, after its mix homogeneously, stand 12min, stand-by。
Etching pit, take 2# sample and put in glass dish, plastic dropper is utilized to draw the metallographic etchant prepared, metallographic etchant is dropped in 2# specimen surface, etching time is 1.5min, after corrosion terminates, ferrum is utilized to hold the 2# sample after son holds corrosion under the arm under the arm, and put into be loaded with in the large beaker of water and be carried out, then utilize distilled water that 2# sample is rinsed, washing time is 1.5min, utilize absorbent cotton wiping 2# specimen surface, then alcohol rinse 2# specimen surface is utilized, the ethanol of 2# specimen surface is dried up again with hair-dryer, and guarantee that 2# specimen surface is without after residual acid and salt ion, utilize the metallographic of metallography microscope sem observation 1# sample。
2# metallurgical structure schematic diagram as shown in Figure 2, observes it can be seen that metallurgical structure corrosive effect is obvious, and equiax crystal, corrosion crystal boundary is very clear, and contrast is clearly visible。
Embodiment 3
In the preparation of metallographic etchant, the water first measuring 20ml the beaker adding 50ml range, then measure 2ml concentrated nitric acid again and add in beaker, the ratio of water and concentrated nitric acid is 10:1, utilize the liquid in Glass rod stirring beaker, after its mix homogeneously, stand 13min, stand-by。
Etching pit, take 3# sample and put in glass dish, plastic dropper is utilized to draw the metallographic etchant prepared, metallographic etchant is dropped in 3# specimen surface, etching time is 1.8min, after corrosion terminates, ferrum is utilized to hold the 3# sample after son holds corrosion under the arm under the arm, and put into be loaded with in the large beaker of water and be carried out, then utilize distilled water that 3# sample is rinsed, washing time is 1.8min, utilize absorbent cotton wiping 3# specimen surface, then alcohol rinse 3# specimen surface is utilized, the ethanol of 3# specimen surface is dried up again with hair-dryer, and guarantee that 3# specimen surface is without after residual acid and salt ion, utilize the metallographic of metallography microscope sem observation 3# sample。
3# metallurgical structure schematic diagram as shown in Figure 3, observes it can be seen that corrosion crystal boundary is very clear, and contrast is it is apparent that metallurgical structure corrosive effect is obvious。
Embodiment 4
In the preparation of metallographic etchant, the water first measuring 24ml the beaker adding 50ml range, then measure 2ml concentrated nitric acid again and add in beaker, the ratio of water and concentrated nitric acid is 12:1, utilize the liquid in Glass rod stirring beaker, after its mix homogeneously, stand 15min, stand-by。
Etching pit, take 4# sample and put in glass dish, plastic dropper is utilized to draw the metallographic etchant prepared, metallographic etchant is dropped in 4# specimen surface, etching time is 2min, after corrosion terminates, ferrum is utilized to hold the 4# sample after son holds corrosion under the arm under the arm, and put into be loaded with in the large beaker of water and be carried out, then utilize distilled water that 4# sample is rinsed, washing time is 2min, utilize absorbent cotton wiping 4# specimen surface, then alcohol rinse 4# specimen surface is utilized, the ethanol of 4# specimen surface is dried up again with hair-dryer, and guarantee that 4# specimen surface is without after residual acid and salt ion, utilize the metallographic of metallography microscope sem observation 4# sample。
4# metallurgical structure schematic diagram as shown in Figure 4, observes it can be seen that intermediate structure is equiax crystal, and edge is column crystal, and metallurgical structure corrosive effect is obvious, and corrosion crystal boundary is very clear, and contrast is clearly visible。
Above-described is only the preferred embodiments of the present invention; technical scheme is not limited thereto; should be understood that to those skilled in the art; under technology provided by the present invention is enlightened; known general knowledge as this area; other equivalent modifications and improvement can also be made, also should be regarded as protection scope of the present invention。
Claims (9)
1. the preparation method of a H62 basis brass metallographic etchant, it is characterised in that: adding water in beaker, the ratio adding concentrated nitric acid, water and concentrated nitric acid is 8-12:1, utilizes the liquid in Glass rod stirring beaker, stands 10-15min after its mix homogeneously。
2. the preparation method of a kind of H62 basis brass metallographic etchant as claimed in claim 1, it is characterised in that: the ratio of water and concentrated nitric acid is 10:1。
3. a H62 basis brass etching pit method, it is characterised in that comprise the following steps:
(1) intercepting of sample: utilize wire cutting machine to intercept the sample of 10-20mm from H62 basis brass ingot casting；
(2) grinding and polishing of sample: a) utilize varigrained abrasive paper for metallograph that metallographic specimen is carried out grinding and polishing；B) utilizing abrasive pastes to carry out grinding and polishing on buffing machine, polishing time is 1.5-2min；C) specimen surface without any cut and bright sliding time, with distilled water as lubricant, utilize polishing cloth to carry out grinding and polishing, polishing time is 0.5-1.5min；
(3) flushing of sample: first rinse specimen surface with water, then use alcohol rinse specimen surface；
(4) corrosion of sample: sample is put in glass dish, utilizes plastic dropper to draw corrosive liquid as claimed in claim 1, corrosive liquid drops in specimen surface, and etching time is 1-2min；
(5) flushing of sample after corrosion: utilize ferrum to hold the sample after son holds corrosion under the arm under the arm, and put into be loaded with in the large beaker of water and be rinsed；Then distilled water is utilized to be rinsed, washing time 1-2min；Finally utilize absorbent cotton and alcohol rinse specimen surface, and utilize hair-dryer to dry up specimen surface；
(6) metallographic observation of sample: utilize the metallographic of metallography microscope sem observation sample。
4. a kind of H62 basis brass etching pit method as claimed in claim 3, it is characterized in that: sample is inlayed after terminating by step (1), utilize metallographic pointing machine that sample is inlayed, preset that to inlay temperature be 140 DEG C, sample is put in pointing machine, and powder is inlayed in addition, put into and inlay mould and itself and sample are fixed, power transmission, pressurization, when inlaying after temperature reaches 140 DEG C, being incubated 15-20min, sample is also taken out in power-off after natural cooling 10-15min。
5. as claimed in claim 4 a kind of H62 basis brass etching pit method, it is characterised in that: described in inlay powder be resinox。
6. a kind of H62 basis brass etching pit method as claimed in claim 5, it is characterised in that: the diameter of described H62 basis brass ingot casting is 5mm。
7. a kind of H62 basis brass etching pit method as claimed in claim 6, it is characterised in that: the abrasive pastes used on described buffing machine are diamond paste。
8. a kind of H62 basis brass etching pit method as described in claim as any in claim 3-7, it is characterised in that: the etching time of described step (4) is 1.5-2min。
9. a kind of H62 basis brass etching pit method as described in claim as any in claim 3-7, it is characterised in that: the etching time of described step (4) is 1.8-2min。
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107740102A (en) * | 2017-10-16 | 2018-02-27 | 国网吉林省电力有限公司电力科学研究院 | A kind of etching pit method of power transmission and transforming equipment copper conductor |
| CN109518186A (en) * | 2018-11-09 | 2019-03-26 | 宁波金田铜业(集团)股份有限公司 | A kind of α, β two-phase brass metallographic etching agent and its display methods of metallographic structure |
| CN109580315A (en) * | 2017-09-29 | 2019-04-05 | 富士康(昆山)电脑接插件有限公司 | The method for displaying metallographic structure of metallographic etching agent, copper and copper alloy |
| CN109580614A (en) * | 2017-09-29 | 2019-04-05 | 富士康(昆山)电脑接插件有限公司 | Metallographic etching agent, the method for displaying metallographic structure for crimping core wire |
| CN110618009A (en) * | 2019-10-30 | 2019-12-27 | 无锡隆达金属材料有限公司 | Method for microcosmic metallographic corrosion of cupronickel alloy |
| CN111662717A (en) * | 2020-07-14 | 2020-09-15 | 北京航空航天大学宁波创新研究院 | Metallographic corrosive liquid of bismuth selenide material and metallographic display method |
| CN113008650A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Metallographic corrosive agent and metallographic corrosive method for UN fuel pellets |
| CN113702379A (en) * | 2021-08-27 | 2021-11-26 | 华能国际电力股份有限公司 | Metallographic corrosion method for displaying homogenized structure of high-alloying nickel-based alloy |
| CN114457335A (en) * | 2022-02-15 | 2022-05-10 | 江西省科学院应用物理研究所 | Copper-iron-carbon alloy metallographic etchant and application method thereof |
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| CN109580315A (en) * | 2017-09-29 | 2019-04-05 | 富士康(昆山)电脑接插件有限公司 | The method for displaying metallographic structure of metallographic etching agent, copper and copper alloy |
| CN109580614A (en) * | 2017-09-29 | 2019-04-05 | 富士康(昆山)电脑接插件有限公司 | Metallographic etching agent, the method for displaying metallographic structure for crimping core wire |
| CN107740102A (en) * | 2017-10-16 | 2018-02-27 | 国网吉林省电力有限公司电力科学研究院 | A kind of etching pit method of power transmission and transforming equipment copper conductor |
| CN109518186A (en) * | 2018-11-09 | 2019-03-26 | 宁波金田铜业(集团)股份有限公司 | A kind of α, β two-phase brass metallographic etching agent and its display methods of metallographic structure |
| CN110618009A (en) * | 2019-10-30 | 2019-12-27 | 无锡隆达金属材料有限公司 | Method for microcosmic metallographic corrosion of cupronickel alloy |
| CN113008650A (en) * | 2019-12-20 | 2021-06-22 | 中核北方核燃料元件有限公司 | Metallographic corrosive agent and metallographic corrosive method for UN fuel pellets |
| CN111662717A (en) * | 2020-07-14 | 2020-09-15 | 北京航空航天大学宁波创新研究院 | Metallographic corrosive liquid of bismuth selenide material and metallographic display method |
| CN111662717B (en) * | 2020-07-14 | 2021-08-31 | 北京航空航天大学宁波创新研究院 | Metallographic corrosive liquid of bismuth selenide material and metallographic display method |
| CN113702379A (en) * | 2021-08-27 | 2021-11-26 | 华能国际电力股份有限公司 | Metallographic corrosion method for displaying homogenized structure of high-alloying nickel-based alloy |
| CN113702379B (en) * | 2021-08-27 | 2023-09-01 | 华能国际电力股份有限公司 | Metallographic corrosion method for displaying homogenized structure of high-alloyed nickel-based alloy |
| CN114457335A (en) * | 2022-02-15 | 2022-05-10 | 江西省科学院应用物理研究所 | Copper-iron-carbon alloy metallographic etchant and application method thereof |
| CN114457335B (en) * | 2022-02-15 | 2023-10-27 | 江西省科学院应用物理研究所 | Metallographic etchant for copper-iron-carbon alloy and use method thereof |
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Application publication date: 20160622 |