CN102364323A - Display method of tempered martensitic steel carbide colour metallography and electrothermal metallographic chromogenic device special for display method - Google Patents
Display method of tempered martensitic steel carbide colour metallography and electrothermal metallographic chromogenic device special for display method Download PDFInfo
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- CN102364323A CN102364323A CN2011103159266A CN201110315926A CN102364323A CN 102364323 A CN102364323 A CN 102364323A CN 2011103159266 A CN2011103159266 A CN 2011103159266A CN 201110315926 A CN201110315926 A CN 201110315926A CN 102364323 A CN102364323 A CN 102364323A
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Abstract
The invention discloses a display method of tempered martensitic steel carbide colour metallography, comprising the following steps of: (1) grinding and polishing the surface of a tempered martensitic steel sample to obtain a tempered martensitic steel metallographic sample; (2) heating the tempered martensitic steel metallographic sample in the oxidation atmosphere to 400-500 DEG C, keeping warm for 6-15 minutes, and forming an interference oxide-film, which makes the microstructure of metal and alloy to present different colors by the action of light, on the surface of the tempered martensitic steel sample, so as to display the tempered martensitic steel carbide color metallography. The method provided by the invention can be used to effectively display and raise the contrast between the T91 steel carbide and the matrix microstructure, so as to effectively observe the microstructure form of the martensitic steel.
Description
Technical field
The present invention relates to a kind of display packing of colour metallograpy of steel carbonide, belong to technical field of metallographic sample preparation, relate in particular to a kind of display packing of tempered martensite steel carbonide colour metallograpy.The invention still further relates to the special-purpose electric heating metallographic display device of this method.
Background technology
After the high-temperature metal parts high temperature long-time running of power station; The deterioration gradually of the constantly aging and macro property of microstructure all can take place in the metal material of these parts; Thereby promptly and accurately judge metal material microstructure Aging Damage degree under the effect when high temperature is long; To understanding and grasp the quality condition of high-temperature metal parts, reduce material aging in the operational process and all kinds of accidents that cause, and the reliability that improves the safe operation of high-temperature metal parts has important theory and is worth and practical significance.At present; To aging check of the tissue of the non-pearlitic steel of this type of tempered martensite steel and evaluation, mainly take all factors into consideration intracrystalline and grain boundary carbide and change and evaluate according to the tissue of the relevant non-pearlitic steel of power industry proposed standard DL/T 884-2004 " thermal power plant's metal inspection and assessment technology guide rule " assessment method and the non-pearlitic steel tissue signature that wears out that wears out.
T91 steel (Chinese trade mark 10Cr9Mo1VNbN, U.S. ASME SA-213 T91) with its excellent comprehensive performance, becomes the representative steel grade of the effective heat-resisting steel of high Cr station boiler.Nineteen ninety-five, this steel grade was just listed Chinese GB5310 " seamless steel tubes and pipes for high pressure boiler " standard in; Become the essential steel grade of China development supercritical generating unit, be used for subcritical, overcritical Utility Boiler Superheater (wall temperature≤625 ℃), reheater steel pipe and high temperature cabinet and main steam line (wall temperature≤600 ℃).The final thermal treatment of T91 steel is that normalizing increases temperature tempering; This type steel contains a large amount of alloying elements; In the high tempering after normalizing crystallization does not again take place and form ferrite matrix, but the deformation when discharging the martensite phase transformation with the formation of the lath fragmentation of high-temperature reply and metastable state dislocation network stores ability.The typical organization of T91 steel is a tempering lath martensitic stucture, is made up of the carbonitride that martensite lath, highdensity dislocation and disperse distribute.Separate out sediment in the T91 steel mainly by the M that is positioned at martensite lath circle and original austenite crystal prevention
23C
6(M mainly is Cr) type carbonide and disperse are distributed in the MX type Nb/V carbonitride of lath matrix and form.
With the T91 steel is that the tempered martensite heat-resisting steel original structure state of representative is a tempered martensite, and metallographic structure is more tiny and complicated than pearlite heatproof steel in the past, in the long term high temperature use; High temperature ageing can appear; Tempered martensite in the T91 steel is replied, and carbide particle is separated out the tendency that alligatoring is grown up and had the crystal boundary gathering to grow up is taken place, but carbonide is separated out in original austenite crystal prevention or lath circle; Carbide precipitate is tiny, wherein larger-size M
23C
6Carbonide is generally at 200～300nm, and the size of MX type carbonitride is littler, has only tens nanometers, grows up even the gathering of carbonide takes place, and tissue is aging, the precipitated phase after the alligatoring is still tiny.The aging evaluation of T91 structure of steel rank figure (Fig. 5 a ~ 5d) be not difficult to find out from DL/T 884 appendix B (standardization appendix); The method that " thermal power plant's metal inspection and assessment technology guide rule " adopted can not show tempered martensite steel microstructure effectively; Especially the details of carbide particle; Subject matter is that tempered martensite steel microstructure and carbide particle are more tiny than organizing of pearlitic steel; The demonstration of carbonide is to rely on the etch method to show the phase boundary between two phases in the tradition metallographic microstructure; The shallow demonstration phase border that then is difficult for is crossed in etch during etch method display organization, and etch is crossed deeply and caused coming off or the phase obscurity boundary of tiny phase again easily, therefore; Carbonide phase obscure boundary is clear in the microstructure of tempered martensite steel classic method preparation, between carbonide and matrix contrast too lowly make that the distinguishing ability of carbonide is limited.
The demonstration of tempered martensite steel tradition metallographic microstructure is to rely on the etch method; Its principle is to utilize various tissues to receive the difference of etch degree to be shown as different gray scales; This black and white contrast is a kind of univariate contrast, and is often obvious inadequately, for those reflecting powers have only nuance microstructure; On the metallographic of the faint variation of gray scale, be difficult to distinguish, even covered.And the color contrast is the contrast of the ternary of brightness, color harmony color saturation.Therefore through the color contrast, different objects had higher distinguishing ability.The heat tinting method is to be placed on the steel samples for preparing under the oxidizing atmosphere to heat, and makes the metal surface generate one deck and interferes oxide film.Wherein, oxidation rate to composition difference and crystal degree to very sensitive, thereby in the sample not homophase under the microscope illumination condition, can be observed many different form and aspect because oxidation rate difference and deposited the oxide film of different-thickness at specimen surface.Utilize the thin film interference effects of light, make the microstructure of metal and alloy demonstrate various colors, thereby the method for going to discern microstructure through color is called colour metallograpy.Mosaic gold is on good terms and is made in the black and white metallographic some phases that are difficult for showing and organize details fully to show, and colour metallograpy is not only bright-coloured, contrast and sharpness are high, and has remedied the deficiency of black and white metallographic.
The method of the film interference display organization of colour metallograpy technology preparation metal microstructure test sample has physics method and chemical method.Heat tinting is owned by France in chemical staining method, and major advantage is workable, can be used for each discriminating mutually in the alloy.Heat tinting method heating-up temperature (generally not being higher than 500 ℃) is lower than the normal serviceability temperature of heat-resisting steel (＞550 ℃), applicable to this tempered martensite heat-resisting steel of T91.When utilizing the ready-made interference oxide film of heat tinting method; The variation of heat tinting color generally demonstrates pale yellow-deep yellow-reddish brown-purplish red-blueness-light blue (green grass or young crops)-green-grey Changing Pattern; But the heat tinting color depends on the thickness of film, and interference thin film thickness is relevant with the alloying component and the institutional framework of heating-up temperature, temperature retention time and metal material again.This shows, select suitable heat tinting parameter, tempered martensite steel matrix and carbonide are demonstrated than big color contrast and sharpness becomes key of problem.
In addition, generally, the heating metallographic structure display device of heat tinting method adopts common heat treatment to use resistance furnace, but the heat tinting method uses resistance furnace to handle, and has following weak point:
(1)Resistance furnace is made up of heating, masonry, metal shell, fire door and electric control system etc., and for the metal lographic examination sample of reduced size, the resistance furnace volume is big, operation inconvenience;
(2)Resistance furnace is divided into by the serviceability temperature scope: working temperature is in the low temperature oven below 650 ℃; The moderate oven that working temperature is 650～1000 ℃; Working temperature is high temperature furnace more than 1000 ℃; Their working temperature is less than or equal to 500 ℃ heating-up temperature height than the heat tinting method, and conventional, electric-resistance furnace temperature control accuracy is low in the temperature range of heat tinting method, and error is bigger;
(3)Can't observe directly oxide film change in color situation in the heating process color with resistance furnace heating colour developing;
(4)The resistance furnace heating is not easy to move, can't be to on-the-spot metal lographic examination sample heating colour developing;
(5)The resistance furnace that uses at present needs manual control heat time heating time, is difficult to control experiment effect.
Summary of the invention
First purpose of the present invention is intended to overcome the deficiency that the prior art method exists in tempered martensite steel carbonide colour metallograpy display packing; A kind of display packing of tempered martensite steel carbonide colour metallograpy is provided; This method can effectively show and improve contrast between T91 steel carbonide and matrix, so that observe the microstructure morphology of martensite steel effectively.
Second purpose of the present invention provides the dedicated electric-thermal metallographic display device of above-mentioned tempered martensite steel carbonide colour metallograpy display packing.
Goal of the invention of the present invention realizes through following technical scheme: a kind of display packing of tempered martensite steel carbonide colour metallograpy may further comprise the steps:
(1) surface of tempered martensite steel sample is ground and polishing, obtain tempered martensite steel metallographic sample;
(2) tempered martensite steel metallographic sample is heated to 400 ~ 500 ℃ under oxidizing atmosphere; Insulation 6 ~ 15min; Form the interference oxide film that demonstrates various colors under the effect of microstructure that makes metal and alloy on tempered martensite steel sample surface, to show tempered martensite steel carbonide colour metallograpy at light.
The heating-up temperature of heat tinting method is influenced by alloy element component and institutional framework; And alloy element component in the iron and steel and institutional framework can be different because of different classes of iron and steel; Thereby heat tinting temperature meeting invar iron material is different and different, when application heat tinting legal system is equipped with metallographic sample, need carry out groping of heating-up temperature according to concrete iron and steel kind so.Find through inventor's experimental study that in the present invention during 400 ~ 500 ℃ of scopes of heating-up temperature, heat tinting can make the matrix colour developing of tempered martensite steel.Too high temperature can make the metallographic structure of tempered martensite steel show unintelligible; Even can change the institutional framework of tempered martensite steel; That just can't check the actual metallurgical structure of tempered martensite steel sample exactly; And low excessively temperature can make interference oxide film formation speed slow excessively, and the working time is long, is unfavorable for the application of practical operation.After the heating-up temperature of heat tinting is selected; The heat tinting temperature retention time will be decided according to the variation of specimen surface oxidation tint; Usually for the ease of operating and controlling generally the heat tinting time to be controlled in 6 ~ 15min scope and be advisable, because find that through experimental study the tempered martensite steel is 400 ~ 500 ℃ of temperature range heat tintings; The control heat tinting time can make the surface form the suitable interference thin film of thickness in 6 ~ 15min scope; Under the effect of light, make matrix present bluish violet, carbonide presents yellow, and this moment, matrix and carbonide demonstrated big color contrast and sharpness (referring to Fig. 6).
Grinding in the step according to the invention (1) is meant fine lapping after the first rough lapping in surface of tempered martensite steel sample; Concrete operations are: the tempered martensite steel sample is gone out smooth flour milling with crushing; Carry out rough lapping with No. 120 and No. 240 flint glass papers successively, carry out fine lapping with No. 400, No. 600, No. 800, No. 1000, No. 1500 and No. 2000 abrasive paper for metallograph successively again, when grinding, whenever change one time sand paper; The grinding direction of tempered martensite steel sample is vertical with last polishing scratch direction; Be milled to one polishing scratch and grind off, fully remove deformation layer, and till the new polishing scratch uniformity.Pressure is unsuitable excessive when grinding, and particularly last one sand paper must gently grind when grinding.
Deformation layer described in the present invention is meant in the buck process that the tissue below tiny polishing scratch produces very thin layer tissue distortion layer because of ablation.
Mechanical polishing method is adopted in polishing in the step according to the invention (1); That is: will move in the polishing disk that the even velvet of woollen cloth, nylon taffeta, velvet or other fiber finer is housed the polishing scratch that is polished to grinding with diamond polishing cream through the tempered martensite steel sample of fine lapping removes fully; The surface during as minute surface till; The polishing afterwash dry up, make the surface not have the water mark or dirt residual.As a kind of optimal way, concrete operation of the present invention is: will move to through the tempered martensite steel sample of fine lapping in the polishing disk that the even velvet of woollen cloth, nylon taffeta, velvet or fiber finer is housed, elder generation polishes with 1.0 microns diamond polishing cream; Polished 3 ~ 5 minutes; Use 0.5 micron diamond polishing cream polishing after the cleaning instead, polished 3 ~ 5 minutes, again with clear water polishing 1 ~ 2 minute; This moment, the polishing scratch of tempered martensite steel sample surface grinding was removed fully; The surface resembles minute surface, after cleaning, uses the absolute ethyl alcohol wiping then, dries up the processing of carrying out next step again.
Described tempered martensite steel sample is used absolute ethyl alcohol before in moving to polishing disk and is carried out wiping, and it is residual to make the surface not have a dirt.
Described tempered martensite steel sample is the T91 steel, the T91 steel behind the hot operation 85000h, the T91 steel behind the hot operation booster after original supply of material attitude T91 steel, the 700 ℃ of high temperature ageing timeliness.
Second purpose of the present invention is to realize through following technical measures: the electric heating metallographic display device of the special use of the display packing of tempered martensite steel carbonide colour metallograpy; Comprise well heater, be used for the temperature control unit of control heater temperature and be used to control the time control unit of heat time heating time; Described temperature control unit and time control unit are electrically connected, and the output control terminal of described temperature control unit is connected with the input control end of well heater.Temperature control unit starts the temperature that well heater is heated to setting by the temperature parameter control of setting; The time control unit startup picks up counting; The predetermined value that arrives the heat tracing time of setting is to cut off the electricity supply, and stops detecting the heat tracing of metal metallographic specimen.
As one of them embodiment of the present invention; Described well heater is made up of the heating element of heating with the metal metallographic sample that is used to heat different size; Described heating has hollow chamber; Described heating element has working end and installation portion, and hollow chamber's size of the size of the installation portion of heating element and heating is suitable, and is set in the hollow chamber of heating; The working end of described heating element then extend out to outside the heating, is used for the heating of metal metallographic sample.
The installation portion of described heating element has the passage that is used for detected temperatures, and that end that this passage is positioned at the working end is in communication with the outside, and can inject different atmosphere gas from this passage, reserves controlled atmospher electric heating coloring function; Be provided with temperature measuring equipment in the passage of described heating element; The signal output part of this temperature measuring equipment is connected with the signal input part of temperature control unit; The temperature that this temperature measuring equipment detects heating element feeds back to temperature control unit then, if temperature is lower than predetermined value, then temperature control unit startup well heater heats; If temperature is higher than predetermined value, then temperature control unit is closed well heater and is stopped heating.
The working end of described heating element is a tabular, is used for preparation or the preparation of on-the-spot color metal metallographic of the color metal metallographic sample of flour milling diameter phi＞15mm.
The working end of described heating element is a tubular; Its hollow chamber is used to place metal sample; The color metal metallographic sample that is used for flour milling diameter phi≤15mm, its hollow chamber's opening part can cover a quartz glass plate than its somewhat larger in diameter, is used for insulation and observation.
This present invention also comprises a heat insulation handle, and this heat insulation handle comprises the grip part, and described connecting portion is connected with well heater, and described temperature control unit and time control unit are installed on the grip part.
Between the grip part of described heat insulation handle and well heater, the heat radiation overcoat is set,, accelerates to reduce the temperature of the link of heat insulation handle, avoid high temperature to damage temperature control unit and time control unit to promote heat radiation.
As an embodiment of the invention: described heat insulation handle comprises connecting pipe and heat-barrier material; One end of described connecting pipe is connected with well heater; Described heat-barrier material is coated on the outside surface of connecting pipe part body and forms the grip part, and described heat radiation overcoat then is arranged on the outside surface of connecting pipe body exposed between grip part and the well heater.
Said heating element removably is sleeved in the chamber of heating, conveniently changes corresponding heating element according to actual specimen size.
At the outside suit one heat-insulation and heat-preservation housing of well heater, with quickening heating head programming rate, and the temperature of maintenance well heater, reduce the loss of heat.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention is simple, and easy to operate, the microstructure of tempered martensite steel and carbonide clear display, and resolution is high.
Tempered martensite steel metallographic sample through grinding and polishing is heated to 400 ~ 500 ℃ under oxidizing atmosphere; Insulation 6 ~ 15min; Form the interference oxide film on tempered martensite steel sample surface, under the effect of light, make carbonide and matrix present various colors, utilize heterochromia to improve the contrast of carbonide largely; Can differentiate carbonide and matrix preferably, improve the resolution of microstructure.
(2) grinding of the present invention and polishing method; Can remove the deformation layer that occurs in the process of lapping preferably; Avoid responsive especially to deformation layer, cause the preferential oxidation of local deformation layer and be shown, polishing scratch and mixed and disorderly color occur after making the sample heat tinting because of the heat tinting method.
Advantages such as (3) electric heating metallographic display device of the present invention has compact conformation, and in light weight, carry at the scene of being convenient to, and heating-up temperature and time are controlled automatically, and heating process can be observed, and is easy to operate.
(4) heating element of electric heating metallographic display device of the present invention removably is sleeved in the heating, can be equipped with the variform heating element in working end, in the middle of work, can change heating element according to the size of test sample.
When (5) using electric heating metallographic display device of the present invention to carry out metal metallographic color operation; Not only can observe directly oxide film change in color situation in the heating process color; And can control heating-up temperature and temperature retention time automatically; Reduce manually-operated error, control experiment effect easily, guarantee the truth of the institutional framework of the tempered martensite steel metallographic sample that prepared tempered martensite steel colour metallograpy sample ability accurate response is to be detected.
Description of drawings
Fig. 1 is the one-piece construction synoptic diagram of the embodiment of the invention one.
Fig. 2 is the well heater of the embodiment of the invention one and the structural representation of heat insulation handle portion.
Fig. 3 is the structural representation of the embodiment of the invention two.
Fig. 4 is the well heater of the embodiment of the invention two and the structural representation of heat insulation handle portion.
Fig. 5 a is 2 grades of aging evaluation rank figure (700 X) of T91 structure of steel.
Fig. 5 b is 3 grades of aging evaluation rank figure (700 X) of T91 structure of steel.
Fig. 5 c is 4 grades of aging evaluation rank figure (700 X) of T91 structure of steel.
Fig. 5 d is 5 grades of aging evaluation rank figure (700 X) of T91 structure of steel.
Fig. 6 is T91 steel heat tinting change color figure.
Fig. 7 a is the microstructure that adopts sample behind the T91 steel hot operation 85000h that method of the present invention obtains, 450 ℃ and be incubated 8 minutes matrix and carbonide metallographs (2000 X) after the colour developing.
Fig. 7 b is the microstructure metallograph (2000 X) that traditional etch Faxian shows sample behind the T91 steel hot operation 85000h.
Fig. 8 is the microstructure without the supply of material attitude T91 steel sample that uses that adopts method of the present invention to obtain, matrix after the colour developing and carbonide metallograph (2000 X).
Fig. 9 is the microstructure that adopts 700 ℃ of high temperature ageing aging samples of T91 steel of method acquisition of the present invention, matrix after the colour developing and carbonide metallograph (2000 X).
Figure 10 is the microstructure that adopts the T91 steel hot operation booster sample of method acquisition of the present invention, matrix after the colour developing and carbonide metallograph (2000 X).
Figure 11 is the microstructure that adopts sample behind the T91 steel hot operation 85000h that method of the present invention obtains, 500 ℃ and be incubated 6 minutes matrix and carbonide metallographs (2000 X) after the colour developing.
Figure 12 is the microstructure that adopts sample behind the T91 steel hot operation 85000h that method of the present invention obtains, 400 ℃ and be incubated 15 minutes matrix and carbonide metallographs (2000 X) after the colour developing.
Embodiment
Embodiment one:
Electric heating metallographic display device shown in Fig. 1 ~ 2 is one embodiment of the present of invention.This electric heating metallographic display device, by heat insulation handle, heat radiation overcoat 8, insulation shell 9, temperature measuring equipment 5, well heater, be used for the control heater temperature heating-up temperature temperature control unit 3 and be used to control the time control unit 4 of heat time heating time and constitute.Well heater, temperature control unit 3 and time control unit 4 are connected with power supply respectively.The heating-up temperature scope of temperature control unit 3 controls is at 100 ~ 600 ℃.Temperature control unit 3 is electrically connected with time control unit 4, and the output control terminal of temperature control unit 3 is connected with the input control end of well heater, is used in time controlling the keying of electric heater.Well heater is made up of heating 2 and heating element 1.Heating 2 is cylindric, has the hollow chamber that is used to install heating element 1, and heating 2 is connected with power supply.Heating element 1 is made by fine copper; Comprise installation portion and the working end that is used for heating of metal metallographic sample heating, wherein, installation portion is dismountable to be set in the chamber of heating 2; Installation portion is cylindrical, and hollow chamber's internal diameter of its external diameter and heating 2 is suitable.Installation portion has the passage 11 that is used for detected temperatures, and that end that this passage 11 is positioned at the working end is in communication with the outside, and can inject different atmosphere gas from this passage 11, reserves control electric heating colour developing atmosphere function.The working end of heating element 1 is a tabular, is positioned at outside the hollow chamber of heating 2.Be used for preparation or the preparation of on-the-spot color metal metallographic of the color metal metallographic sample of flour milling diameter phi＞15mm.
Heat insulation handle comprises connecting pipe 6 and heat-barrier material 7, and an end of connecting pipe 6 is threaded with the heating 2 of well heater.Heat-barrier material 7 is coated on the connecting pipe 6 part outer surface of tube body and forms the grip part.Temperature control unit 3 is provided with on the grip part with time control unit 4.8 in overcoat of heat radiation is arranged on the outside surface of exposed connecting pipe 6 bodys between grip part and the well heater, and to promote heat radiation, quickening reduces the temperature of the link of heat insulation handle, avoids high temperature to damage connecting pipe, temperature control unit and time control unit.The passage 11 of the installation portion of heating element 1 is communicated with the official jargon of connecting pipe 6.Temperature measuring equipment 5 adopts thermopair; The signal output part of this thermopair is connected with the signal input part of temperature control unit 3, and its thermometric working end then stretches in the passage 11 of heating element 1 installation portion through the tube chamber of connecting pipe 6, detects the temperature of heating element 1; If temperature is lower than predetermined value; Then start heating 2 and heat,, then close heating 2 and stop heating if temperature is higher than predetermined value.
When using this electric heating metallographic display device to carry out heating operation; Temperature control unit 3 heats the temperature that makes heating element 1 by the temperature parameter control startup well heater of setting and reaches to the temperature of setting; Heat sample with contacting on the surface of the working end of heating element and the metallographic sample of T91 steel; Thermopair is monitored the temperature of heating element 1 in real time, so that the duty of real-time control heater.When the temperature of heating element 1 arrived design temperature, time control unit 4 startups picked up counting, and the predetermined value that arrives the heat tracing time of setting is to cut off the electricity supply, and stops the heat tracing to the metallographic sample of T91 steel.
Embodiment two:
Different with embodiment one is: shown in Fig. 3 ~ 4; The working end of the heating element 1 of electric heating metallographic display device is a tubular; Plenum chamber is used to place metal sample therein; The color metal metallographic sample that is used for flour milling diameter phi≤15mm, its plenum chamber opening part can cover a quartz glass plate 10 than its somewhat larger in diameter, are used for insulation and observation.
Following examples three ~ eight use the foregoing description one and two electric heating metallographic display device to carry out the colour metallograpy sample of T91 steel.
Embodiment three
(1)Tempered martensite steel T91 steel sample to behind the hot operation 85000h goes out smooth flour milling with crushing; Carry out rough lapping with No. 120 and No. 240 flint glass papers successively, carry out fine lapping with No. 400, No. 600, No. 800, No. 1000, No. 1500 and No. 2000 abrasive paper for metallograph successively again, when grinding, whenever change one time sand paper; The grinding direction of T91 steel sample is vertical with last polishing scratch direction; Be milled to one polishing scratch and grind off, fully remove deformation layer, and till the new polishing scratch uniformity.Pressure is unsuitable excessive when grinding, and particularly last one sand paper must gently grind when grinding.
To use the absolute ethyl alcohol wiped clean through the T91 of fine lapping steel sample, the diamond polishing cream that moves in the polishing disk that the even velvet of woollen cloth, nylon taffeta, velvet or other fiber finer is housed earlier with 1.0 microns polishes, and polishes 3 ~ 5 minutes; Use 0.5 micron diamond polishing cream polishing after the cleaning instead; Polish after 3 ~ 5 minutes, with clear water polishing 1 ~ 2 minute, polishing scratch and deformation layer that this moment, the T91 steel sample ground were removed fully; The surface resembles minute surface; With after the ultrasonic cleaning with absolute ethyl alcohol wiping 3 times, dry up then, obtain the metallographic sample of T91 steel.
The metallographic sample of T91 steel with under oxidizing atmosphere, be heated to 450 ℃ and be incubated 8 minutes; Form the interference oxide film that demonstrates various colors under the effect of microstructure that makes metal and alloy on T91 steel metallographic sample surface, with the metallographic sample carbonide colour metallograpy of the T91 steel behind the demonstration hot operation 85000h at light.Its in the microstructure of the microscopically of 2000X shown in Fig. 7 a.Fig. 7 b provides the microstructure metallograph that identical T91 steel sample adopts traditional etch method to show behind the hot operation 85000h, compare with Fig. 7 b from Fig. 7 a, among Fig. 7 a the demonstration of the microstructure of tempered martensite steel and carbonide more clear, resolution is higher.
Embodiment four:
Different with embodiment three is that without the supply of material attitude martensite steel T91 steel sample that uses, its microstructure at the microscopically of 2000X is as shown in Figure 8.
Embodiment five:
Different with embodiment three is that through 700 ℃ of high temperature ageing aged martensite steel T91 steel samples, its microstructure at the microscopically of 2000X is as shown in Figure 9.
Embodiment six:
Different with embodiment three is, martensite steel T91 steel hot operation booster sample, and its microstructure at the microscopically of 2000X is shown in figure 10.
Embodiment seven:
Different with embodiment three is; T91 steel behind the martensite steel samples using hot operation 85000h; Step (3) is heated to 500 ℃ and be incubated 6 minutes with the metallographic sample of T91 steel under oxidizing atmosphere; Form the interference oxide film that demonstrates various colors under the effect of microstructure that makes metal and alloy on T91 steel surface behind the hot operation 85000h at light; With the metallographic sample carbonide colour metallograpy of the T91 steel behind the demonstration hot operation 85000h, its microstructure at the microscopically of 2000X is shown in figure 11.
Embodiment eight:
Different with embodiment three is; T91 steel behind the martensite steel samples using hot operation 85000h; Step (3) is heated to 400 ℃ and be incubated 15 minutes with the metallographic sample of T91 steel under oxidizing atmosphere; Form the interference oxide film that demonstrates various colors under the effect of microstructure that makes metal and alloy on T91 steel surface behind the hot operation 85000h at light; With the metallographic sample carbonide colour metallograpy of the T91 steel behind the demonstration hot operation 85000h, its microstructure at the microscopically of 2000X is shown in figure 12.
The present invention can summarize with other the concrete form without prejudice to spirit of the present invention or principal character.Above-mentioned embodiment of the present invention all can only be thought explanation of the present invention rather than restriction; As be not limited to embodiment and adopt electric heating metallographic display device to carry out the heat treated of tempered martensite steel sample; Also can adopt resistance furnace of the prior art; Therefore every foundation essence technology of the present invention all belongs in the scope of technical scheme of the present invention any trickle modification, equivalent variations and modification that above embodiment did.
Claims (10)
1. the display packing of a tempered martensite steel carbonide colour metallograpy is characterized in that, may further comprise the steps:
(1) surface of tempered martensite steel sample is ground and polishing, obtain tempered martensite steel metallographic sample;
(2) tempered martensite steel metallographic sample is heated to 400 ~ 500 ℃ under oxidizing atmosphere; Insulation 6 ~ 15min; Form the interference oxide film that demonstrates various colors under the effect of microstructure that makes metal and alloy on tempered martensite steel sample surface, to show tempered martensite steel carbonide colour metallograpy at light.
2. the display packing of tempered martensite steel carbonide colour metallograpy according to claim 1; It is characterized in that the concrete operations of the grinding in the said step (1) are: the tempered martensite steel sample is gone out smooth flour milling with crushing, carry out rough lapping with No. 120 and No. 240 flint glass papers successively; Carry out fine lapping with No. 400, No. 600, No. 800, No. 1000, No. 1500 and No. 2000 fine sandpapers successively again; When grinding, whenever change sand paper one time, the grinding direction of tempered martensite steel sample is vertical with last polishing scratch direction, is milled to one polishing scratch and grinds off; Fully remove deformation layer, and till the new polishing scratch uniformity.
3. the display packing of tempered martensite steel carbonide colour metallograpy according to claim 1 and 2; It is characterized in that; The concrete operations of polishing are in the described step (1): will move in the polishing disk that the even velvet of woollen cloth, nylon taffeta, velvet or fiber finer is housed the polishing scratch that is polished to grinding with diamond polishing cream through the tempered martensite steel sample of fine lapping and remove fully; The surface during as minute surface till, the polishing afterwash dries up, make the surface not have the water mark or dirt residual.
4. the display packing of tempered martensite steel carbonide colour metallograpy according to claim 3 is characterized in that, the concrete operations of described diamond polishing cream polishing are: elder generation polishes with 1.0 microns diamond polishing cream; Polished 3 ~ 5 minutes; Use 0.5 micron diamond polishing cream polishing after the cleaning instead, polished 3 ~ 5 minutes, again with clear water polishing 1 ~ 2 minute; After cleaning, use the absolute ethyl alcohol wiping, dry up the processing of carrying out next step again.
5. the display packing of tempered martensite steel carbonide colour metallograpy according to claim 4 is characterized in that, described tempered martensite steel sample is used absolute ethyl alcohol before in moving to polishing disk and carried out wiping, and it is residual to make the surface not have a dirt.
6. the display packing of tempered martensite steel carbonide colour metallograpy according to claim 5; It is characterized in that described tempered martensite steel sample is T91 steel, the T91 steel behind the hot operation 85000h or the T91 steel behind the hot operation booster after original supply of material attitude T91 steel, the 700 ℃ of high temperature ageing timeliness.
7. the electric heating metallographic display device of the special use of the display packing of the described tempered martensite steel of the arbitrary claim of claim 1 ~ 6 a carbonide colour metallograpy; It is characterized in that; Comprise well heater, be used for the temperature control unit of control heater temperature and be used to control the time control unit of heat time heating time; Described temperature control unit and time control unit are electrically connected, and the output control terminal of described temperature control unit is connected with the input control end of well heater.
8. the dedicated electric-thermal metallographic display device of the display packing of tempered martensite steel carbonide colour metallograpy according to claim 7; It is characterized in that; Described well heater is made up of the heating element of heating with the metal metallographic sample that is used to heat different size, and described heating has hollow chamber, and described heating element has working end and installation portion; Hollow chamber's size of the size of the installation portion of heating element and heating is suitable; And be set in the hollow chamber of heating, the working end of described heating element then extend out to outside the heating, is used for the heating of metal metallographic sample.
9. the electric heating metallographic display device of the special use of the display packing of tempered martensite steel carbonide colour metallograpy according to claim 8; It is characterized in that; The installation portion of described heating element has the passage that is used for detected temperatures; That end that this passage is positioned at the working end is in communication with the outside, and injects different atmosphere gas from this passage; Be provided with temperature measuring equipment in the passage of described heating element, the signal output part of this temperature measuring equipment is connected with the signal input part of temperature control unit.
10. according to the electric heating metallographic display device of the special use of the display packing of claim 7 or 8 or 9 described tempered martensite steel carbonide colour metallograpies; It is characterized in that; Also comprise a heat insulation handle; This heat insulation handle comprises the grip part, and described connecting portion is connected with well heater, and described temperature control unit and time control unit are installed on the grip part.
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| CN109668839A (en) * | 2017-10-13 | 2019-04-23 | 中国科学院化学研究所 | A method of identifying copper sheet crystal boundary and crystal face |
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