CN106979903A - A kind of analysis method tested for ferrous materials spontaneous combustion with oxygen-enriched erosion - Google Patents
A kind of analysis method tested for ferrous materials spontaneous combustion with oxygen-enriched erosion Download PDFInfo
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 239000001301 oxygen Substances 0.000 title claims abstract description 81
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 81
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000004458 analytical method Methods 0.000 title claims abstract description 25
- 230000002269 spontaneous effect Effects 0.000 title claims abstract description 23
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 230000003628 erosive effect Effects 0.000 title claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000010453 quartz Substances 0.000 claims abstract description 12
- 230000008859 change Effects 0.000 claims abstract description 6
- 239000000470 constituent Substances 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- 244000137852 Petrea volubilis Species 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000007747 plating Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000035772 mutation Effects 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 7
- 230000035939 shock Effects 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000000956 alloy Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000006378 damage Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- -1 Oxonium ion Chemical class 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 244000144985 peep Species 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
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- Biodiversity & Conservation Biology (AREA)
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Abstract
The invention discloses a kind of analysis method tested for ferrous materials spontaneous combustion with oxygen-enriched erosion, belong to ferrous materials performance detection analysis field.When carrying out autoignition test, sample is processed into the bar of one end sharpening, is fixed in atmosphere furnace, 700 900 DEG C are heated to, opened oxygen valve, be mutated by infrared detecting set registration, determine the oxygen pressure gate threshold value of sample spontaneous combustion at such a temperature；In oxygen-enriched erosion test, sample is processed into square piece, sample is placed in small quartz boat, outside is covering one layer of sleeve pipe, is then placed in atmosphere furnace, the weight change of test sample different temperatures and oxygen pressure, and pattern and constituent analysis are carried out to oxide layer.Spontaneous combustion test is not added with ignition substance, it is to avoid influence of the ignition substance to combustibility；The oxygen attack situation of high-temperature oxygen-enriched erosion experiment more can truly reflect the workpiece prepared with ferrous materials phase under arms, this provides a kind of new method for the failure analysis and life prediction of workpiece.
Description
Technical field
The invention belongs to ferrous materials performance detection analysis field, and in particular to one kind be used for ferrous materials spontaneous combustion test and
The analysis method of oxygen-enriched erosion.
Background technology
U.S. spaceflight rocket engine mostly makees fuel using liquid hydrogen, liquid oxygen, since the seventies, and many cases fire occurs in the U.S.
Arrow and shuttle motor explosion phenomenon.Because the problem directly affects the safety and reliability of rocket engine, the U.S.
The research work in this field, NASA (NASA), Kennedy Space Center are attached great importance to the former Soviet Union
Units such as (Kennedy Space Center) has put into substantial amounts of man power and material and has carried out a series of exploration in this field
Journal of Sex Research.
The U.S. has carried out system research for metal burning, and has formulated relevant criterion by ASTM, and there are several tests in the U.S.
The method of metal burning, be respectively：
(1) mechanical shock of normal pressure liquid (LOX) oxygen is tested
In this experiment, the plummet of freely falling body gives the examination being immersed in liquid oxygen by striker certain energy transmission
Sample, weight strikes Ф 1.75cm striker for 9.09kg plummet from 1.1m height freely falling body, and 98Nm energy is passed
Pass Ф 1.75cm test sample, occur the burning of visible ray (in dark room) or sample, burn and be considered as its combustion
Burn, 20 Secondary Shocks will be carried out in each test.
(2) high-pressure gaseous oxygen (GOX) mechanical shock is tested
The experiment instead of the striker pin device in liquid oxygen experiment with special experiment generator, due to experimental facilities sound-proofing
Can be excellent, it is seen that flash of light, the burning of sample or burn the generation for being considered as reaction.For more careful observing response, reative cell peace
Generation of the special optical monitoring system to observe any intensity light is filled, the pressure used in an experiment is shown in Table 1.
The GOX mechanical shock tests pressure of table 1
(3) it is high-pressure oxygen-enriched to light experiment
This experiment process be：A diameter of Ф 3.2mm sample one end is hung under ceramic style platform, the other end
Combustion generator is connected, is ignited tested alloy sample by combustible metal (such as aluminium, magnesium, iron) silk, if sample is complete
Burning, pressure reduction is tested again, until tested sample is not burnt continuously for 5 times under this pressure condition, this pressure then makes this
Material combustion critical pressure.
(4) experiment is lighted in friction
Experiment is carried out under high pressure gas oxygen (6.9MPa) and up to 17000rpm rotating speeds, and is loaded with 35N/s speed, directly
Burnt to sample, experiment can be carried out under liquid oxygen (LOX) and gaseous oxygen (GOX).With Pv, (load and relative velocity multiply
Product) value size weighs the ability of different-alloy material flame resistant, and Pv values are higher, then it is more nonflammable.
Normal pressure liquid (LOX) oxygen mechanical shock experiment is merely able to qualitatively measure the complexity of different materials burning,
Qualitatively combustibility can not be characterized with physical quantity；High-pressure gaseous oxygen (GOX) mechanical shock experiment more can be observed meticulously
Process, but still do not accomplish qualitatively to measure；It is high-pressure oxygen-enriched to light experiment and qualitatively measure burning critical pressure, but survey
Amount process is relatively complicated, from metal burning key element triangle, and the influence factor of burning is a lot of, with tested sample in certain pressure
Under the conditions of do not burn for continuous 5 times, as the material combustion critical pressure under this pressure, the experimental result obtained by this standard also compares
It is rougher, it is more likely that to cause experimental result less than normal, further, since doing this experiment with the addition of ignition substance, one is introduced again
Influence factor, so can not truly reflect the process that burning is lighted；Friction is lighted experiment and is merely able to by indirect physical quantity
Pv values reflect the performance of burning, and influence of the experimental sample surface roughness to Pv values is very big.
In view of the deficiency tested above, the invention provides a kind of point for studying ferrous materials spontaneous combustion test and oxygen-enriched erosion
Analysis method, by adjusting temperature and oxygen pressure in high temperature and high pressure atmosphere stove come the ferrous materials that ignite, without drawing in experimentation
Combustion things, promote sample to burn by the way that sample one end is fined away, and sample is analyzed in difference by changing oxygen pressure and temperature
Ablation situation under temperature and pressure；If sample is in the limiting temperature (1000 DEG C) and limiting pressure of high temperature and high pressure atmosphere stove
It is also unignited under (3MPa), the oxygen attack journey of ferrous materials is just analyzed by the high-temperature oxygen-enriched experiment of transformation temperature and oxygen pressure
Degree, the combustibility of ferrous materials is reflected according to the degree of oxygen attack.This kind of spontaneous combustion test can also be measured accurately easily very much
Fire the combustibility of alloy.
The content of the invention
The present invention for existing combustibility measuring technology it is not enough there is provided one kind be used for ferrous materials spontaneous combustion test and
The analysis method of oxygen-enriched erosion, this method by adjusting temperature and oxygen pressure in high temperature and high pressure atmosphere stove come the ferrous materials that ignite,
Predict in which kind of temperature and oxygen pressure spontaneous combustion occurs for ferrous materials, and different temperatures and oxygen depress the oxygen attack journey of ferrous materials
Degree.
A kind of analysis method tested for ferrous materials spontaneous combustion, comprises the following steps：
(1) sample is prepared：Sample 1 is processed into a diameter of 1.0-2.0mm, length is 20-22mm bar, is then carried out
Wire cutting, one end of sample 1 is fined away, sophisticated a diameter of 0.1-0.25mm, and sophisticated tiltangleθ is 5-5.7 °, finally will
The outer surface of sample 1 is all milled to 2000# with sand paper, then with deionized water, acetone and ethanol is cleaned and dried respectively；
(2) sample is installed：Sample 1 is put into atmosphere furnace, one end of the non-sharpening of sample 1 is vertically tied up in support with tungsten filament
On, vertically downward, a silica ware is laid in sophisticated bottom to the sharpened end of sample 1, residual for receive that the spontaneous combustion of sample 1 falls down
Slag；
(3) vacuumize：It will be vacuumized in atmosphere furnace, vacuum 0MPa to -1MPa；
(4) autoignition test：Atmosphere in-furnace temperature is risen to 700-900 DEG C, during heating, atmosphere furnace is remained
Interior is vacuum state, after temperature reaches 700-900 DEG C, opens oxygen valve, when infrared detecting set registration is undergone mutation, now
Oxygen pressure for sample 1 in 700-900 DEG C of spontaneous combustion oxygen pressure gate threshold value；
(5) repeat step (2)-(4), can obtain the spontaneous combustion oxygen pressure gate threshold value of sample 1 under different temperatures.
A kind of analysis method for the oxygen-enriched erosion of ferrous materials, comprises the following steps：
(1) sample is prepared：Sample 2 is processed into (9-10) × (9-10) × (1.5-1.6) mm3Square piece, then use sand
Paper is milled to 2000#, then with deionized water, acetone and ethanol is cleaned and dried respectively；
(2) sample is installed：Sample 2 is placed in small quartz boat, outside is covering one layer of sleeve pipe, prevents other residues in stove
Sample 2 is fallen into, sample 2 is together put into atmosphere furnace together with small quartz boat and sleeve pipe；
(3) oxygen-enriched erosion test：The maximum temperature of atmosphere furnace is set as 700~900 DEG C, oxygen pressure be set as 0.5MPa~
3MPa, sample 2 is incubated 1 hour, 3 hours, 5 hours, 7 hours at such a temperature, and the balance for being respectively 0.0001g with precision is weighed
Weight change of the sample 2 together with small quartz boat；
(4) layer analysis is aoxidized：Sample 2 is subjected to Nickel Plating Treatment, then polishing carries out oxide layer shape observation and composition point
Analysis；
(5) repeat step (2)-(4), can obtain sample 2 under the conditions of high-temperature oxygen-enriched as temperature and time changes oxygen-enriched
The situation of erosion.
The advantage of the invention is：
1st, the oxygen pressure gate that ferrous materials burn at different temperatures can relatively accurately be measured from burning method using this kind
Threshold value, while this kind of spontaneous combustion method of testing is simple and easy to apply, experimental period is short；
2nd, sample one end is fined away, is conducive to sample dieseling to occur, it is also possible to stop combustion by observing sample
The size at sample tip presses the burning threshold size with a temperature of to estimate sample in this kind of oxygen during burning, in addition, being not added with ignition substance
Also influence of the ignition substance to combustibility can be avoided.
3rd, the workpiece prepared with ferrous materials more can be truly reflected using this high-temperature oxygen-enriched erosion experiment to exist
The oxygen attack situation of service phase, this provides a kind of new method for the failure analysis and life prediction of workpiece.By to oxidation
The shape characteristic of layer and the analysis of component distributing, a kind of new approaches are provided for designing new high temperature resistance oxygen-rich oxide material.
Brief description of the drawings
Fig. 1 is the schematic shapes of sample 1；
Fig. 2 is the experimental rig schematic diagram of autoignition test, and 101 be that, into oxygen outlet, 102 be tungsten filament, and 103 be sample 1 in figure,
104 be infrared detecting set, and 105 be peep hole, and 106 be silica dish, and 107 be venthole；
Fig. 3 is the placement figure of oxygen-enriched erosion test sample 2, and 201 be sleeve pipe in figure, and 202 be that sample 2,203 is small quartz
Boat；
Fig. 4, which is that stainless steel 30SiMn2MoV is high-temperature oxygen-enriched, corrodes rear oxidation layer pattern (a) and component-part diagram (b)；
Fig. 5, which is that stainless steel PCrNi3MoV is high-temperature oxygen-enriched, corrodes rear oxidation composition of layer pattern (a) and component-part diagram (b).
Embodiment
It is used for the analysis method of ferrous materials spontaneous combustion test and oxygen-enriched erosion the invention provides a kind of, below in conjunction with the accompanying drawings
The invention will be further described with embodiment, but not limitation of the present invention.
Embodiment 1：Autoignition test
(1) sample is prepared：Sample 1 is processed into a diameter of 1.0-2.0mm, length is 20-22mm bar, is then carried out
Wire cutting, one end of sample 1 is fined away, sophisticated a diameter of 0.1-0.25mm, and sophisticated tiltangleθ is 5-5.7 °, such as Fig. 1 institutes
Show, the outer surface of sample 1 is all milled to 2000# with sand paper, then with deionized water, acetone and ethanol cleaned and dried respectively；
(2) sample is installed：Sample 1 is put into atmosphere furnace, one end of the non-sharpening of sample 1 vertically tied up with tungsten filament 102
On support, vertically downward, a silica dish 106 is laid in sophisticated bottom to the sharpened end of sample 1, is fallen down for receiving the spontaneous combustion of sample 1
The residue come, experimental provision is as shown in Figure 2；
(3) vacuumize：It will be vacuumized in atmosphere furnace, vacuum 0MPa to -1MPa；
(4) autoignition test：Atmosphere in-furnace temperature is risen to 700 DEG C, during heating, remains in atmosphere furnace and is
Vacuum state, after temperature reaches 700 DEG C, opens oxygen valve, when the registration of infrared detecting set 104 is undergone mutation, oxygen now
Press the oxygen pressure gate threshold value in 700 DEG C of spontaneous combustions for sample 1；
(5) repeat step (2)-(4), are set to 750 DEG C, 800 DEG C, 850 DEG C ... by maximum temperature in stove and can obtain not
The spontaneous combustion oxygen pressure gate threshold value of synthermal lower sample 1.
Embodiment 2：The high-temperature oxygen-enriched erosion tests of stainless steel 30SiMn2MoV
(1) sample is prepared：Using 9~10 × 9~10 × 1.5~1.6mm3Square piece sample 2, the outer surface of sample 2 is all
2000# is milled to sand paper, is cleaned and is dried with deionized water, acetone and ethanol respectively.
(2) sample is installed：Sample 2 is placed in small quartz boat 203, outside is covering one layer of sleeve pipe 201, prevents its in stove
He is fallen on sample residue, as shown in Figure 3.
(3) oxygen-enriched erosion test：The maximum temperature of atmosphere furnace is set as 700 DEG C, oxygen pressure is set as 1MPa, and sample is existed
Constant temperature is incubated 1 hour, 3 hours, 5 hours, 7 hours at this temperature, and the balance for being respectively 0.0001g with precision weighs sample 2 and connected
With the weight change of small quartz boat；
(4) layer analysis is aoxidized：Sample 2 is carried out into Nickel Plating Treatment (can so be effectively protected the pattern of oxide layer, make examination
Sample is unlikely to damage sample in polishing), then polishing carries out oxide layer shape observation and constituent analysis.
The oxide layer shape Fig. 4 (a) of sample 2 and composition are shown in Fig. 4 (b), it can be seen that oxide skin(coating) mainly contains Fe
Oxide, oxide layer and matrix combine not fine and close, also, the concentration of oxygen is held essentially constant in oxide layer, in oxygen
The concentration of the near interface oxygen of compound and matrix drastically declines, due to occurring in that one again at oxide layer and mother metal alloy interface
The elevated peak of oxygen concentration, it is seen then that 30SiMn2MoV alloys are under the conditions of 700 DEG C high-temperature oxygen-enriched, and the generation type of oxide-film is
Oxonium ion is spread with metal with reference to formed by the inside.
Embodiment 3：The high-temperature oxygen-enriched erosion tests of stainless steel PCrNi3MoV
(1) sample is prepared：Using 9~10 × 9~10 × 1.5~1.6mm3Square piece sample 2, the outer surface of sample 2 is all
2000# is milled to sand paper, is cleaned and is dried with deionized water, acetone and ethanol respectively；
(2) sample is installed：Sample 2 is placed in small quartz boat 203, outside is covering one layer of sleeve pipe 201, prevents its in stove
He is fallen on sample residue, as shown in Figure 2；
(3) oxygen-enriched erosion test：The maximum temperature of atmosphere furnace is set as 800 DEG C, oxygen pressure is set as 2MPa, and sample is existed
Constant temperature is incubated 1 hour, 3 hours, 5 hours, 7 hours at this temperature, and the balance for being respectively 0.0001g with precision weighs sample 2 and connected
With the weight change of small quartz boat；
(3) layer analysis is aoxidized：Sample 2 is carried out into Nickel Plating Treatment (can so be effectively protected the pattern of oxide layer, make examination
Sample is unlikely to damage sample in polishing), then polishing carries out oxide layer shape observation and constituent analysis.
Oxide layer shape is shown in that Fig. 5 (a) and composition are shown in Fig. 5 (b), it can be seen that oxide layer is main by the oxygen containing Fe
Compound is constituted, and oxide is combined finer and close with matrix, in addition, the concentration of oxygen is held essentially constant in the oxide layer, in oxygen
The near interface of compound and matrix, the concentration of oxygen drastically declines, and observation oxide/basal body interface can be seen that the height at 800 DEG C
Under warm excess oxygen, oxygen constantly into matrix " infiltration ", sweeps picture it can be seen that PCrNI3MoV due to external pressure by scan line
Alloy is under the conditions of 800 DEG C are high-temperature oxygen-enriched, and oxygen preferential oxidation Fe, Cr etc. are easy to the element of oxidation, then reoxidize Ni elements, from
And make oxide/basal body interface layer that similar " feeler " shape is presented.
Claims (2)
1. a kind of analysis method tested for ferrous materials spontaneous combustion, it is characterised in that comprise the following steps：
(1) sample is prepared：Sample 1 is processed into a diameter of 1.0-2.0mm, length is 20-22mm bar, then enters line and cuts
Cut, one end of sample 1 is fined away, sophisticated a diameter of 0.1-0.25mm, sophisticated inclination angle is 5-5.7 °, finally by sample 1
Outer surface be all milled to 2000# with sand paper, then with deionized water, acetone and ethanol cleaned and dried respectively；
(2) sample is installed：Sample 1 is put into atmosphere furnace, one end of the non-sharpening of sample 1 is vertically tied up on support with tungsten filament,
Vertically downward, a silica ware is laid in sophisticated bottom to the sharpened end of sample 1, for receiving the residue that the spontaneous combustion of sample 1 is fallen down；
(3) vacuumize：It will be vacuumized in atmosphere furnace, vacuum 0MPa to -1MPa；
(4) autoignition test：Atmosphere in-furnace temperature is risen to 700-900 DEG C, during heating, remains in atmosphere furnace and is
Vacuum state, after temperature reaches 700-900 DEG C, opens oxygen valve, when infrared detecting set registration is undergone mutation, oxygen now
Press is sample 1 in 700-900 DEG C of spontaneous combustion oxygen pressure gate threshold value；
(5) repeat step (2)-(4), can obtain the spontaneous combustion oxygen pressure gate threshold value of sample 1 under different temperatures.
2. a kind of analysis method for the oxygen-enriched erosion of ferrous materials, it is characterised in that comprise the following steps：
(1) sample is prepared：Sample 2 is processed into (9-10) × (9-10) × (1.5-1.6) mm3Square piece, be then milled to sand paper
2000#, then with deionized water, acetone and ethanol cleaned and dried respectively；
(2) sample is installed：Sample 2 is placed in small quartz boat, outside is covering one layer of sleeve pipe, prevents other residues in stove from falling into
Sample 2, sample 2 is together put into atmosphere furnace together with small quartz boat and sleeve pipe；
(3) oxygen-enriched erosion test：The maximum temperature of atmosphere furnace is set as 700~900 DEG C, oxygen pressure be set as 0.5MPa~
3MPa, sample 2 is incubated 1 hour, 3 hours, 5 hours, 7 hours at such a temperature, and the balance for being respectively 0.0001g with precision is weighed
Weight change of the sample 2 together with small quartz boat；
(4) layer analysis is aoxidized：Sample 2 is subjected to Nickel Plating Treatment, then polishing carries out oxide layer shape observation and constituent analysis；
(5) repeat step (2)-(4), can obtain sample 2 and are corroded under the conditions of high-temperature oxygen-enriched as temperature and time change is oxygen-enriched
Situation.
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Cited By (7)
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| CN107998985A (en) * | 2017-12-20 | 2018-05-08 | 北京科技大学 | A kind of method and reaction unit for simulating working condition measurement metal material burning behavior |
| CN108279281A (en) * | 2018-01-29 | 2018-07-13 | 北京科技大学 | A kind of method and device of control metal Rich Oxygen Combustion |
| CN111781086A (en) * | 2020-08-11 | 2020-10-16 | 中钢集团洛阳耐火材料研究院有限公司 | Method for rapidly detecting high-temperature oxidation resistance of silicon carbide refractory material |
| CN111929231A (en) * | 2020-08-20 | 2020-11-13 | 江苏君澄空间科技有限公司 | Liquid oxygen compatibility testing arrangement |
| CN112578073A (en) * | 2019-09-29 | 2021-03-30 | 中国石油化工股份有限公司 | Experimental device for survey gaseous spontaneous combustion induction time |
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| CN108279281B (en) * | 2018-01-29 | 2022-02-15 | 北京科技大学 | Method and device for controlling oxygen-enriched combustion process of metal |
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| CN111781086A (en) * | 2020-08-11 | 2020-10-16 | 中钢集团洛阳耐火材料研究院有限公司 | Method for rapidly detecting high-temperature oxidation resistance of silicon carbide refractory material |
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| CN113049633A (en) * | 2021-03-05 | 2021-06-29 | 浙江省应急管理科学研究院 | Device and method for testing spontaneous combustion of metal dust in water |
| CN113624909A (en) * | 2021-08-30 | 2021-11-09 | 山东誉信工程检测有限公司 | Building material flammability detection method of waste gas treatment structure |
| CN113624909B (en) * | 2021-08-30 | 2024-05-14 | 山东誉信工程检测有限公司 | Method for detecting combustibility of building materials of waste gas treatment structure |
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