CN102364323B - 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 PDF

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CN102364323B
CN102364323B CN201110315926.6A CN201110315926A CN102364323B CN 102364323 B CN102364323 B CN 102364323B CN 201110315926 A CN201110315926 A CN 201110315926A CN 102364323 B CN102364323 B CN 102364323B
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steel
temperature
metallographic
control unit
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CN102364323A (en
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钟万里
王伟
李正刚
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Wuhan University WHU
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Wuhan University WHU
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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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

A kind of display packing of tempered martensite steel carbonide colour metallograpy and special-purpose electrothermal metallographic chromogenic device thereof
Technical field
The display packing that the present invention relates to a kind of colour metallograpy of steel carbonide, belongs to technical field of metallographic sample preparation, relates in particular to a kind of display packing of tempered martensite steel carbonide colour metallograpy.The invention still further relates to the electrothermal metallographic chromogenic device of the method special use.
Background technology
After the high-temperature metal parts high temperature long-time running of power station, all can there is continuous aging and macro property deteriorated gradually of microstructure in the metal material of these parts, thereby promptly and accurately judge metal material microstructure Aging Damage degree under effect when high temperature is long, to understanding and grasp the quality condition of high-temperature metal parts, all kinds of accidents that reduce material aging in operational process and cause, and the reliability of raising high-temperature metal parts safe operation has important theory value and practical significance.At present, to the failure check of the non-pearlitic steel of this class of tempered martensite steel and evaluation, the failure assessment method of the relevant non-pearlitic steel of Main Basis power industry proposed standard DL/T 884-2004 " thermal power plant's metal inspection and assessment technology guide rule " and the aging tissue signature of non-pearlitic steel considers intracrystalline and grain boundary carbide changes to evaluate.
T91 steel (Chinese trade mark 10Cr9Mo1VNbN, U.S. ASME SA-213 T91), with its excellent combination property, becomes the steel grade that represents 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's development supercritical generating unit, 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 class steel contains a large amount of alloying elements, in high tempering after normalizing, recrystallization does not occur and form ferrite matrix, but deformation while discharging martensite phase transformation with the lath fragmentation of high-temperature reply and the formation of metastable state dislocation network stores energy.The typical organization of T91 steel is tempering lath martensitic stucture, and the carbonitride being distributed by martensite lath, highdensity dislocation and disperse is formed.In T91 steel, separate out sediment mainly by the M that is positioned at martensite lath circle and original austenite crystal prevention 23c 6the MX type Nb/V carbonitride that (M is mainly Cr) type carbonide and disperse are distributed in lath matrix forms.
The tempered martensite heat-resisting steel original structure state that the T91 steel of take is representative is tempered martensite, metallographic structure is more tiny and complicated than pearlite heatproof steel in the past, in long term high temperature use procedure, there will be high temperature ageing, tempered martensite in T91 steel is replied, and carbide particle is separated out the tendency that alligatoring is grown up and had crystal boundary agglomeration is occurred, but Carbide Precipitation is 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 less, only has tens nanometers, even if there is the agglomeration of carbonide, the precipitated phase after failure, alligatoring is still tiny.From DL/T 884 appendix B(standardization appendix) T91 structure of steel aging evaluation rank figure (Fig. 5 a ~ 5d) be not difficult to find out, the method that " thermal power plant's metal inspection and assessment technology guide rule " adopts 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, in tradition metallographic microstructure, the demonstration of carbonide is to rely on etch Faxian to show the phase boundary between two-phase, during etch method display organization, the shallow phase border that is difficult for showing is crossed in etch, etch is crossed and is deeply easily caused again coming off or phase obscurity boundary of tiny phase, therefore, in microstructure prepared by tempered martensite steel classic method, Carbide Phases obscure boundary is clear, between carbonide and matrix the too low distinguishing ability of carbonide that makes of contrast limited.
The demonstration of tempered martensite steel tradition metallographic microstructure is to rely on etch method, its principle is to utilize various tissues to be subject to the difference of etch degree to be shown as different gray scales, this black and white contrast is a kind of univariate contrast, often obvious not, for those reflecting powers only have nuance microstructure, on the metallographic of the faint variation of gray scale, be difficult to distinguish, even covered.And color contrast is the contrast of the ternary of brightness, color harmony color saturation.Therefore by color contrast, different objects is had to higher distinguishing ability.Heat tinting method is that the steel samples preparing is placed under oxidizing atmosphere and is heated, and makes metal surface generate one deck and interferes oxide film.Wherein, oxidation rate to composition difference and crystal degree to very sensitive, thereby in sample not homophase due to oxidation rate difference, at specimen surface, deposited the oxide film of different-thickness, under microscope illumination condition, can be observed many different form and aspect.Utilize the thin film interference effects of light, make the microstructure of metal and alloy present different colors, thereby go the method for identifying microstructure to be called colour metallograpy by color.Mosaic gold is on good terms and is made in black and white metallographic some be difficult for the phases that show and organize details fully to show, colour metallograpy not only bright-coloured, contrast and sharpness high, and made up the deficiency of black and white metallographic.
The method that Color Metallographic Technology is prepared the film interference display organization of metal microstructure test sample has Physical 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 alloy.Heat tinting method heating-up temperature (generally not higher than 500 ℃) is lower than the normal serviceability temperature of heat-resisting steel (550 ℃ of >), applicable to this tempered martensite heat-resisting steel of T91.While utilizing the ready-made interference oxide film of heat tinting method, the variation of heat tinting color generally presents pale yellow-deep yellow-reddish brown-purplish red-blueness-light blue (green grass or young crops)-green-grey Changing Pattern, but heat tinting color depends on the thickness of film, interference thin film thickness is relevant with alloying component and the institutional framework of heating-up temperature, temperature retention time and metal material again.As can be seen here, select suitable heat tinting parameter, make tempered martensite steel matrix and carbonide present the key that larger color contrast and sharpness become problem.
In addition, generally, the heating metallographic structure display device of heat tinting method adopts common heat treatment resistance furnace, but heat tinting method is used resistance furnace to process, and has the following disadvantages: (1)resistance furnace is comprised of heating, masonry, metal shell, fire door and electric control system etc., and for the metal lographic examination sample of reduced size, resistance furnace volume is large, operation inconvenience; (2)resistance furnace is divided into by serviceability temperature scope: working temperature is in the low temperature oven below 650 ℃, the moderate oven that working temperature is 650~1000 ℃, 1000 ℃ of above high temperature furnaces of working temperature, it is high that their working temperature is less than or equal to the heating-up temperature of 500 ℃ compared with heat tinting method, in the temperature range of heat tinting method, conventional, electric-resistance furnace temperature control accuracy is low, and error is larger; (3)with resistance furnace heating colour developing, cannot observe directly the situation of change of oxide film color in heating process color; (4)resistance furnace heating is not easy to mobile, cannot be to on-the-spot metal lographic examination sample heating colour developing; (5)the resistance furnace using at present needs the manual control heat time, is difficult to control experiment effect.
Summary of the invention
First object of the present invention is intended to overcome the deficiency that 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, the method can effectively show and improve contrast between T91 steel carbonide and matrix, to effectively observe the microstructure morphology of martensite steel.
Second object of the present invention is to provide the dedicated electric-thermal metallographic chromogenic device of above-mentioned tempered martensite steel carbonide colour metallograpy display packing.
Goal of the invention of the present invention is achieved through the following technical solutions: a kind of display packing of tempered martensite steel carbonide colour metallograpy, comprises the following 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, on tempered martensite steel sample surface, form the interference oxide film that presents different colors under the effect of microstructure at light that makes metal and alloy, to show tempered martensite steel carbonide colour metallograpy.
The heating-up temperature of heat tinting method is affected by alloy element component and institutional framework, and alloy element component and institutional framework in iron and steel can be different because of different classes of iron and steel, thereby heat tinting temperature can be different different because of ferrous materials, in application heat tinting legal system, need to carry out groping of heating-up temperature according to concrete iron and steel kind during for metallographic sample so.Through inventor's experimental study, find 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 cannot check the actual metallurgical structure of tempered martensite steel sample exactly, and too low temperature can make to interfere oxide film formation speed excessively slow, working time is long, is unfavorable for the application of practical operation.After the heating-up temperature of heat tinting is selected, heat tinting temperature retention time will be determined according to the variation of specimen surface oxidation tint, conventionally for convenient operation is generally controlled at the heat tinting time within the scope of 6 ~ 15min and is advisable with controlling, because find by experimental study, tempered martensite steel is 400 ~ 500 ℃ of temperature range heat tintings, the control heat tinting time can make surface form the suitable interference thin film of thickness within the scope of 6 ~ 15min, under the effect of light, make matrix present bluish violet, carbonide presents yellow, and now matrix and carbonide present larger color contrast and sharpness (referring to Fig. 6).
Grinding in step of the present invention (1) refers to fine lapping after the first rough lapping in surface of tempered martensite steel sample, concrete operations are: tempered martensite steel sample is gone out to smooth flour milling with crushing, with No. 120 and No. 240 flint glass papers, carry out rough lapping successively, use successively again No. 400, No. 600, No. 800, No. 1000, No. 1500 and No. 2000 abrasive paper for metallograph carry out fine lapping, when grinding, often change one time sand paper, the grinding direction of tempered martensite steel sample will be together with upper polishing scratch direction vertical, being milled to one polishing scratch grinds off, fully remove deformation layer, and till new polishing scratch uniformity.When grinding, pressure is unsuitable excessive, when particularly last one sand paper grinds, must gently grind.
Deformation layer described in the present invention refers in buck process, and the tissue below tiny polishing scratch produces a very thin layer tissue distortion layer because of ablation.
Polishing in step of the present invention (1) adopts mechanical polishing method; that is: the tempered martensite steel sample through fine lapping is moved in the polishing disk that the even velvet of woollen cloth, nylon taffeta, velvet or other fiber finer is housed with the polishing scratch that diamond polishing cream is polished to grinding and remove completely; surface during as minute surface till; polishing afterwash dries up, make surface not have water mark or dirt residual.As a kind of optimal way, concrete operation of the present invention is: the tempered martensite steel sample through fine lapping is moved to woollen cloth is housed, nylon taffeta, in the polishing disk of the velvet that velvet or fiber finer are even, first use the diamond polishing cream polishing of 1.0 microns, polishing 3 ~ 5 minutes, after cleaning, use the diamond polishing cream polishing of 0.5 micron instead, polishing 3 ~ 5 minutes, use again clear water polishing 1 ~ 2 minute, now the polishing scratch of tempered martensite steel sample surface grinding is completely removed, surface resembles minute surface, then after cleaning, use absolute ethyl alcohol wiping, dry up the processing of carrying out again next step.
Described tempered martensite steel sample is applied absolute ethyl alcohol before in moving to polishing disk and is carried out wiping, makes surface not have dirt residual.
Described tempered martensite steel sample is T91 steel after original supply of material state T91 steel, 700 ℃ of high temperature ageing timeliness, the T91 steel after hot operation 85000h, the T91 steel after hot operation booster.
Second object of the present invention is to realize by following technical measures: the special-purpose electrothermal metallographic chromogenic device of the display packing of tempered martensite steel carbonide colour metallograpy, comprise well heater, for the temperature control unit of control heater temperature with for controlling the time control unit of heat time, described temperature control unit and time control unit are electrically connected to, and the output control terminal of described temperature control unit is connected with the input control end of well heater.Temperature control unit is controlled and is started the temperature that well heater is heated to setting by the temperature parameter of setting, time control unit starts and starts timing, the predetermined value that arrives the heating and thermal insulation time of setting is to cut off the electricity supply, and stops detecting the heating and thermal insulation of metal metallographic specimen.
As one of them embodiment of the present invention, described well heater forms by heating with for heating the heating element of the metal metallographic sample of different size, described heating has hollow chamber, 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 extend out to outside heating, for heating of metal metallographic sample.
The installation portion of described heating element has the passage for detection of temperature, and that one end that this passage is positioned at working end is in communication with the outside, and can inject different atmosphere gas from this passage, reserved controlled atmospher electric heating coloring function; In the passage of described heating element, be provided with temperature measuring equipment, the signal output part of this temperature measuring equipment is connected with the signal input part of temperature control unit, then the temperature that this temperature measuring equipment detects heating element feeds back to temperature control unit, if temperature is lower than predetermined value, temperature control unit startup well heater heats, if temperature is higher than predetermined value, temperature control unit is closed well heater and is stopped heating.
The working end of described heating element is tabular, for the preparation of color metal metallographic sample or the preparation of on-the-spot color metal metallographic of flour milling diameter phi > 15mm.
The working end of described heating element is tubular, its hollow chamber is used for placing metal sample, color metal metallographic sample ,Qi hollow chamber opening part for flour milling diameter phi≤15mm can cover one compared with the quartz glass plate of its slightly larger in diameter, for insulation and observation.
This present invention also comprises a heat insulation handle, and this heat insulation handle comprises grip part, and described connecting portion is connected with well heater, and described temperature control unit and time control unit are arranged on grip part.
Between the grip part of described heat insulation handle and well heater, heat radiation overcoat is set, to promote heat radiation, accelerates to reduce the temperature of the link of heat insulation handle, avoid high temperature to damage temperature control unit and time control unit.
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 grip part, and described heat radiation overcoat is arranged on the outside surface of connecting pipe body exposed between grip part and well heater.
Described heating element is removably sleeved in the chamber of heating, conveniently according to actual specimen size, changes corresponding heating element.
At the outside suit of well heater one heat-insulation and heat-preservation housing, to accelerate heating head programming rate, and keep the temperature of 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, on tempered martensite steel sample surface, form and interfere oxide film, under the effect of light, make carbonide and matrix present different colors, utilize heterochromia to improve largely the contrast of carbonide, can differentiate preferably carbonide and matrix, improve the resolution of microstructure.
(2) grinding of the present invention and polishing method, can remove preferably the deformation layer occurring in process of lapping, avoid responsive especially to deformation layer because of heat tinting method, cause the preferential oxidation of local deformation layer and be shown, make to occur polishing scratch and mixed and disorderly color after sample heat tinting.
(3) electrothermal metallographic chromogenic device of the present invention has compact conformation, lightweight, and carry at the scene of being convenient to, and acid extraction is controlled automatically, heating process observable, the advantage such as easy to operate.
(4) heating element of electrothermal metallographic chromogenic device of the present invention is removably sleeved in heating, can be equipped with the variform heating element in working end, in the middle of work, can, according to the size that detects sample, change heating element.
(5) while using electrothermal metallographic chromogenic device of the present invention to carry out metal metallographic color operation, not only can observe directly the situation of change of oxide film color in heating process color, and can automatically control heating-up temperature and temperature retention time, reduce manually-operated error, easily control experiment effect, guarantee the truth of the institutional framework of the tempered martensite steel metallographic sample that prepared tempered martensite steel colour metallograpy sample energy accurate response is detected.
Accompanying drawing explanation
Fig. 1 is the one-piece construction schematic diagram of the embodiment of the present invention one.
Fig. 2 is the well heater of the embodiment of the present invention one and the structural representation of heat insulation handle portion.
Fig. 3 is the structural representation of the embodiment of the present invention two.
Fig. 4 is the well heater of the embodiment of the present invention two and the structural representation of heat insulation handle portion.
Fig. 5 a is 2 grades of aging evaluation rank figure of T91 structure of steel (700 X).
Fig. 5 b is 3 grades of aging evaluation rank figure of T91 structure of steel (700 X).
Fig. 5 c is 4 grades of aging evaluation rank figure of T91 structure of steel (700 X).
Fig. 5 d is 5 grades of aging evaluation rank figure of T91 structure of steel (700 X).
Fig. 6 is T91 steel heat tinting change color figure.
Fig. 7 a is the microstructure that adopts sample after 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 colour developing.
Fig. 7 b is the microstructure metallograph (2000 X) that traditional etch Faxian shows sample after T91 steel hot operation 85000h.
Fig. 8 is the microstructure without the supply of material state T91 steel sample using that adopts method of the present invention to obtain, the matrix after 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, the matrix after 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, the matrix after colour developing and carbonide metallograph (2000 X).
Figure 11 is the microstructure that adopts sample after 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 colour developing.
Figure 12 is the microstructure that adopts sample after 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 colour developing.
Embodiment
embodiment mono-:
Electrothermal metallographic chromogenic device shown in Fig. 1 ~ 2 is one embodiment of the present of invention.This electrothermal metallographic chromogenic device, by heat insulation handle, heat radiation overcoat 8, insulation shell 9, temperature measuring equipment 5, well heater, for the temperature control unit 3 of the heating-up temperature of control heater temperature with form for controlling the time control unit 4 of heat time.Well heater, temperature control unit 3 and time control unit 4 are connected with power supply respectively.The heating-up temperature scope that temperature control unit 3 is controlled is at 100 ~ 600 ℃.Temperature control unit 3 and time control unit 4 are electrically connected to, and the output control terminal of temperature control unit 3 is connected with the input control end of well heater, for controlling in time the keying of electric heater.Well heater consists of heating 2 and heating element 1.Heating 2 is cylindric, has for the hollow chamber of heating element 1 is installed, and heating 2 is connected with power supply.Heating element 1 is made by fine copper, comprise installation portion and for the working end of 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 for detection of temperature, and that one end that this passage 11 is positioned at working end is in communication with the outside, and can inject different atmosphere gas from this passage 11, the reserved electric heating colour developing atmosphere function of controlling.The working end of heating element 1 is tabular, is positioned at outside the hollow chamber of heating 2.The preparation of color metal metallographic sample or the preparation of on-the-spot color metal metallographic for flour milling diameter phi > 15mm.
Heat insulation handle comprises connecting pipe 6 and heat-barrier material 7, and one end of connecting pipe 6 is threaded with the heating of well heater 2.Heat-barrier material 7 is coated on connecting pipe 6 part outer surface of tube body and forms grip part.Temperature control unit 3 and time control unit 4 arrange on grip part.8, overcoat of heat radiation is arranged on the outside surface of exposed connecting pipe 6 bodys between grip part and well heater, to promote heat radiation, accelerates the temperature of the link of the heat insulation handle of reduction, 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, its thermometric working end stretches in the passage 11 of heating element 1 installation portion by the tube chamber of connecting pipe 6, detect the temperature of heating element 1, if temperature is lower than predetermined value, start heating 2 and heat, if temperature higher than predetermined value, is closed heating 2, stop heating.
While using this electrothermal metallographic chromogenic device to carry out heating operation, temperature control unit 3 heats the temperature of heating element 1 is reached to the temperature of setting by the temperature parameter control startup well heater 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 arrives design temperature, time control unit 4 starts and starts timing, and the predetermined value that arrives the heating and thermal insulation time of setting is to cut off the electricity supply, and stops the heating and thermal insulation to the metallographic sample of T91 steel.
embodiment bis-:
Different from embodiment mono-: as shown in Fig. 3 ~ 4, the working end of the heating element 1 of electrothermal metallographic chromogenic device is tubular, plenum chamber is for placing metal sample therein, color metal metallographic sample for flour milling diameter phi≤15mm, its plenum chamber opening part can cover one compared with the quartz glass plate of its slightly larger in diameter 10, for insulation and observation.
Following examples three ~ eight are used above-described embodiment one and two electrothermal metallographic chromogenic device to carry out the colour metallograpy sample of T91 steel.
embodiment tri-
(1)tempered martensite steel T91 steel sample after hot operation 85000h is gone out to smooth flour milling with crushing, with No. 120 and No. 240 flint glass papers, carry out rough lapping successively, with No. 400, No. 600, No. 800, No. 1000, No. 1500 and No. 2000 abrasive paper for metallograph, carry out fine lapping successively again, when grinding, often change one time sand paper, the grinding direction of T91 steel sample will be together with upper polishing scratch direction vertical, be milled to one polishing scratch and grind off, fully remove deformation layer, and till new polishing scratch uniformity.When grinding, pressure is unsuitable excessive, when particularly last one sand paper grinds, must gently grind.
By the T91 steel sample absolute ethyl alcohol wiped clean through fine lapping, move to and in the polishing disk that the even velvet of woollen cloth, nylon taffeta, velvet or other fiber finer is housed, first use the diamond polishing cream polishing of 1.0 microns, polishing 3 ~ 5 minutes, after cleaning, use the diamond polishing cream polishing of 0.5 micron instead, after polishing 3 ~ 5 minutes, with clear water polishing 1 ~ 2 minute, polishing scratch and deformation layer that now T91 steel sample grinds are removed completely, surface resembles minute surface, with using absolute ethyl alcohol wiping 3 times after Ultrasonic Cleaning, then dry up, 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, on T91 steel metallographic sample surface, form the interference oxide film that presents different colors under the effect of microstructure at light that makes metal and alloy, to show the metallographic sample carbonide colour metallograpy of the T91 steel after hot operation 85000h.Its microstructure under the microscope of 2000X as shown in Figure 7a.Fig. 7 b provides the microstructure metallograph that identical T91 steel sample adopts traditional etch method to show after hot operation 85000h, from Fig. 7 a, compares with Fig. 7 b, and in Fig. 7 a, the microstructure of tempered martensite steel and carbonide show more clearly, and resolution is higher.
embodiment tetra-:
Different from embodiment tri-, without the supply of material state martensite steel T91 steel sample using, its microstructure under the microscope of 2000X as shown in Figure 8.
embodiment five:
Different from embodiment tri-, through 700 ℃ of high temperature ageing aged martensite steel T91 steel samples, its microstructure under the microscope of 2000X as shown in Figure 9.
embodiment six:
Different from embodiment tri-, martensite steel T91 steel hot operation booster sample, its microstructure under the microscope of 2000X is as shown in figure 10.
embodiment seven:
Different from embodiment tri-is, T91 steel after martensite steel sample employing hot operation 85000h, step (3) is heated to the metallographic sample of T91 steel 500 ℃ and be incubated 6 minutes under oxidizing atmosphere, after hot operation 85000h, the formation of T91 steel surface makes the microstructure of metal and alloy under the effect of light, present the interference oxide film of different colors, to show the metallographic sample carbonide colour metallograpy of the T91 steel after hot operation 85000h, its microstructure under the microscope of 2000X as shown in figure 11.
embodiment eight:
Different from embodiment tri-is, martensite steel sample adopts the T91 steel after hot operation 85000h, step (3) is heated to the metallographic sample of T91 steel 400 ℃ and be incubated 15 minutes under oxidizing atmosphere, after hot operation 85000h, the formation of T91 steel surface makes the microstructure of metal and alloy under the effect of light, present the interference oxide film of different colors, to show the metallographic sample carbonide colour metallograpy of the T91 steel after hot operation 85000h, its microstructure under the microscope of 2000X as 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 electrothermal metallographic chromogenic 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 is done above embodiment any trickle modification, equivalent variations and modification, all belong in the scope of technical solution of the present invention.

Claims (2)

1. the dedicated electric-thermal metallographic chromogenic device of the display packing of a tempered martensite steel carbonide colour metallograpy, it is characterized in that, comprise well heater, for the temperature control unit of control heater temperature with for controlling the time control unit of heat time, described temperature control unit and time control unit are electrically connected to, and the output control terminal of described temperature control unit is connected with the input control end of well heater; Described well heater forms by heating with for heating the heating element of different size metallographic sample, described heating has hollow chamber, 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 extend out to outside heating, for heating metallographic sample; The installation portion of described heating element has the passage for detection of temperature, and that one end that this passage is positioned at working end is in communication with the outside, and from this passage, injects different atmosphere gas; In the passage of described heating element, be provided with temperature measuring equipment, the signal output part of this temperature measuring equipment is connected with the signal input part of temperature control unit.
2. the dedicated electric-thermal metallographic chromogenic device of the display packing of tempered martensite steel carbonide colour metallograpy according to claim 1, it is characterized in that, also comprise a heat insulation handle, this heat insulation handle comprises grip part, described heat insulation handle is connected with well heater, and described temperature control unit and time control unit are arranged on grip part.
CN201110315926.6A 2011-10-18 2011-10-18 Display method of tempered martensitic steel carbide colour metallography and electrothermal metallographic chromogenic device special for display method Active CN102364323B (en)

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