CN103978221B - A kind of oxide-dispersed alloy raw powder's production technology - Google Patents
A kind of oxide-dispersed alloy raw powder's production technology Download PDFInfo
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- CN103978221B CN103978221B CN201410245626.9A CN201410245626A CN103978221B CN 103978221 B CN103978221 B CN 103978221B CN 201410245626 A CN201410245626 A CN 201410245626A CN 103978221 B CN103978221 B CN 103978221B
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- 239000000843 powder Substances 0.000 title claims abstract description 156
- 239000000956 alloy Substances 0.000 title claims abstract description 69
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 69
- 238000005516 engineering process Methods 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 58
- 235000012054 meals Nutrition 0.000 claims abstract description 42
- 239000003595 mist Substances 0.000 claims abstract description 32
- 238000009413 insulation Methods 0.000 claims abstract description 24
- 238000007872 degassing Methods 0.000 claims abstract description 14
- 238000010792 warming Methods 0.000 claims abstract description 12
- 229910052786 argon Inorganic materials 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims description 21
- 239000006104 solid solution Substances 0.000 claims description 7
- 238000000889 atomisation Methods 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 24
- 239000001301 oxygen Substances 0.000 description 24
- 229910052760 oxygen Inorganic materials 0.000 description 24
- 239000007789 gas Substances 0.000 description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 15
- 239000001257 hydrogen Substances 0.000 description 15
- 229910052739 hydrogen Inorganic materials 0.000 description 15
- 230000007704 transition Effects 0.000 description 13
- 230000001603 reducing effect Effects 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 238000005245 sintering Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 238000003701 mechanical milling Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 230000001681 protective effect Effects 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000005261 decarburization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003534 oscillatory effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
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Abstract
The invention provides a kind of oxide-dispersed alloy raw powder's production technology, comprising: raw meal is put into the first tube type vacuum stove, pass into CO-CO
2mist, be warming up to 600 ~ 750 DEG C of insulation 0.5 ~ 1h, be evacuated to lower than 0.01Pa, insulation 0.3 ~ 0.8h, keeps vacuum and is cooled to room temperature; Nano-oxide powder is placed in the second tube type vacuum stove, temperature 400 ~ 600 DEG C, low vacuum carries out the bakeout degassing of 1 ~ 3h under 0.01Pa; Raw meal after process and the mixing of nano-oxide powder are placed in vacuum sphere grinding jar, and passing into pressure is 0.1 ~ 0.3MPa, and volume ratio is Ar and CO-CO of 1:0.5 ~ 1:1
2mist, obtains alloyed powder by ball milling; Alloyed powder is placed in three-tube type vacuum drying oven, and at low vacuum in 0.01Pa, temperature is be incubated 0.3 ~ 0.8h at 250 ~ 350 DEG C; Be warming up to 400 ~ 600 DEG C, pass into the CO that vacuum is 1000 ~ 5000Pa
2gas, insulation 0.5 ~ 1.5h; Be evacuated to lower than 0.01Pa, insulation 1 ~ 3h, keeps vacuum and is cooled to room temperature, obtaining oxide-dispersed alloy powder.
Description
Technical field
The present invention relates to technical field of material, particularly relate to a kind of oxide-dispersed alloy raw powder's production technology.
Background technology
Oxide-dispersed alloy is the nano-oxide particles adding high thermal stability and chemical stability in the alloy, makes it in the base dispersed, is produced a class alloy of strengthening by obstruction dislocation and grain boundary.Oxide-dispersed alloy can extensive use but be not limited to nuclear reactor, Aero-Space engine, gas turbine, energy industry and auto industry etc.Oxide-dispersed alloy compared to not adding the iron-based of dispersed oxide phase, nickel-base alloy has good high-temerature creep fatigue behaviour, radioresistance injury reinforcing and decay resistance, but also there is the problem that percentage elongation reduces, ductile-brittle transition temperature raises simultaneously.Its performance can be partly improved by follow-up thermomechanical treatment, but complex procedures, with high costs, and easily cause the anisotropy of material.
The researcher of prior art, by analyzing the microstructure of oxide-dispersed alloy, thinks to there is primary granule border and grain boundaries enrichment large scale oxide brittlement phase in the block materials after due to sintering (as TiO
2), result in that material percentage elongation is low, ductile-brittle transition temperature is high.The excess of oxygen solid solution caused in micron-sized powder surface adsorbed oxygen and mechanical milling process is the main cause that above-mentioned phenomenon occurs.
Owing to generally using argon gas as protective atmosphere in existing ball-milling technology, obtained oxide-dispersed alloy powder oxygen content is higher.Some researchers in Europe attempt adopting hydrogen as ball milling reducing atmosphere in addition, and under result of study shows nitrogen atmosphere, gained powder oxygen content obviously reduces, but can produce the material hydrogen embrittlement problem because hydrogen solid solution causes, thus causes toughness of material to reduce.
Summary of the invention
The invention provides a kind of oxide-dispersed alloy raw powder's production technology, higher in order to solve oxide-dispersed alloy powder oxygen content in prior art, cause the defect that material percentage elongation is low, ductile-brittle transition temperature is high, can also toughness of material be ensured simultaneously.
The invention provides a kind of oxide-dispersed alloy raw powder's production technology, comprise the steps:
Raw meal is put into the first tube type vacuum stove, pass into CO-CO
2mist, be warming up to 600 ~ 750 DEG C of insulation 0.5 ~ 1h, and be evacuated to lower than 0.01Pa, insulation 0.3 ~ 0.8h, keeps vacuum and is cooled to room temperature; Described raw meal be according to required element proportioning simple metal powder or atomization prealloy powder;
Nano-oxide powder is placed in the second tube type vacuum stove, temperature 400 ~ 600 DEG C, low vacuum carries out the bakeout degassing of 1 ~ 3h under 0.01Pa;
By the described raw meal after above-mentioned process and the mixing of described nano-oxide powder, be placed in vacuum sphere grinding jar, passing into pressure is 0.1 ~ 0.3MPa, and volume ratio is Ar and CO-CO of 1:0.5 ~ 1:1
2mist, obtains the uniform alloyed powder of solid solution by ball milling;
The described alloyed powder of gained is placed in three-tube type vacuum drying oven, and at low vacuum in 0.01Pa, temperature is be incubated 0.3 ~ 0.8h at 250 ~ 350 DEG C; Be warming up to 400 ~ 600 DEG C, pass into the CO that vacuum is 1000 ~ 5000Pa
2gas, insulation 0.5 ~ 1.5h; Be evacuated to lower than 0.01Pa, insulation 1 ~ 3h, keeps vacuum and is cooled to room temperature, obtaining oxide-dispersed alloy powder.
In method described above, described nano-oxide powder comprises Y
2o
3, Al
2o
3or ThO
2.
In method described above, described CO-CO
2cO and CO in mist
2volume ratio is 1:0.5 ~ 1:0.8, containing H
2o amount is less than 50ppm; Its flow velocity is 1 ~ 30mL/min.
In method described above, the ball mill that ball milling uses in described vacuum sphere grinding jar is high energy ball mill; Milling protection atmosphere adopts Ar-CO-CO
2mist fills row 2 ~ 3 times repeatedly, and before each inflation, in tank, vacuum should lower than 1Pa.
In method described above, described by the described raw meal after above-mentioned process and described nano-oxide powder mixing before also comprise:
The described raw meal after process is taken out from described first tube type vacuum stove;
And the described nano-oxide powder taken out from described second tube type vacuum stove after process.
In method described above, the described raw meal after process is taken out from described first tube type vacuum stove, the described nano-oxide powder after process is taken out from described second tube type vacuum stove, and the process of the described raw meal after above-mentioned process and the mixing of described nano-oxide powder is all completed in the glove box of ar gas environment, in described glove box, pressure is 0.1 ~ 3MPa, H
2o and O
2content is all less than 1ppm.
Oxide-dispersed alloy raw powder's production technology of the present invention, adopts CO-CO
2mist, as reducing atmosphere, first carries out reduction and degassed process to raw meal, guarantees the purity of original powder; Secondly, in mechanical milling process, Ar-CO-CO is kept
2reproducibility environment, stop further the generation of oxidation; Finally at high-purity CO of rough vacuum
2remove the carbon that powder surface may exist under atmosphere, then degasification reduce powder micro-hardness under a high vacuum, avoids CO, CO
2adsorb at powder surface or enter alloyed powder inside and cause pore, improve the percentage elongation after sintering, reduce ductile-brittle transition temperature.Experiment proves, the oxide-dispersed alloy powder excess of oxygen content obtained by this method is lower than 100ppm (namely 0.01%).Therefore, oxide-dispersed alloy raw powder's production technology of the present invention, can from reducing oxygen content and avoiding the angle proposition CO-CO of hydrogen embrittlement
2mist substitutes argon gas or hydrogen as reduction and protective atmosphere; and adopt corresponding salvo for the different phase in oxide-dispersed alloy powder preparation process; both reduce excess of oxygen content, turn avoid hydrogen embrittlement, and also make powder have lower containing H simultaneously
2o amount and phosphorus content.Therefore the oxide-dispersed alloy powder prepared of oxide-dispersed alloy raw powder's production technology of the present invention, compared with the oxide-dispersed alloy powder obtained with existing method, possess that excess of oxygen content is low, the feature such as percentage elongation raising, ductile-brittle transition temperature reduction after sintering.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
The flow chart of the oxide-dispersed alloy raw powder's production technology that Fig. 1 provides for one embodiment of the invention.
The flow chart of the oxide-dispersed alloy raw powder's production technology that Fig. 2 provides for another embodiment of the present invention.
The flow chart of the oxide-dispersed alloy raw powder's production technology that Fig. 3 provides for yet another embodiment of the invention.
Detailed description of the invention
For making the object of the embodiment of the present invention, technical scheme and advantage clearly, below in conjunction with the accompanying drawing in the embodiment of the present invention, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The flow chart of the oxide-dispersed alloy raw powder's production technology that Fig. 1 provides for one embodiment of the invention.As shown in Figure 1, the oxide-dispersed alloy raw powder's production technology of the present embodiment, comprises the steps:
100, raw meal is put into the first tube type vacuum stove, pass into CO-CO
2mist, be warming up to 600 ~ 750 DEG C of insulation 0.5 ~ 1h, and be evacuated to lower than 0.01Pa, insulation 0.3 ~ 0.8h, keeps vacuum and is cooled to room temperature;
Wherein raw meal is according to the simple metal powder (as Fe powder, Cr powder, W powder) of required element proportioning or atomization prealloy powder (be the alloyed powder of different element proportioning, as by the Fe-9Cr-2W powder, Fe-14Cr-2W-0.3Ti powder etc. of quality proportioning).CO-CO
2namely mist represents CO and CO
2mist.CO-CO is adopted in this step
2mist, as reducing atmosphere, carries out reduction and degassed process to raw meal, guarantees the purity of original powder, obtains high-purity low gas raw meal.Namely this step can be implemented in strong reducing property atmosphere and rough vacuum environment respectively raw meal is reduced, degassing processing.
101, nano-oxide powder is placed in the second tube type vacuum stove, temperature 400 ~ 600 DEG C, low vacuum carries out the bakeout degassing of 1 ~ 3h under 0.01Pa;
Such as, nano-oxide powder in this step comprises Y
2o
3, Al
2o
3or ThO
2.This step is used for realizing carrying out degassing processing to nano-oxide powder, guarantees its purity.
102, by the raw meal after above-mentioned process and the mixing of nano-oxide powder, be placed in vacuum sphere grinding jar, passing into pressure is 0.1 ~ 0.3MPa, and volume ratio is Ar and CO-CO of 1:0.5 ~ 1:1
2mist, obtains the uniform alloyed powder of solid solution by ball milling;
The mechanical milling process of this step occurs in the Ar-CO-CO of low reproducibility
2in mixed atmosphere, by adopting Ar-CO-CO
2the reproducibility environment of mist, stop the generation of oxidation further.
103, the alloyed powder of gained is placed in three-tube type vacuum drying oven, at low vacuum in 0.01Pa, temperature is be incubated 0.3 ~ 0.8h at 250 ~ 350 DEG C; Be warming up to 400 ~ 600 DEG C, pass into the CO that vacuum is 1000 ~ 5000Pa
2gas, insulation 0.5 ~ 1.5h; Be evacuated to lower than 0.01Pa, insulation 1 ~ 3h, keeps vacuum and is cooled to room temperature, obtaining oxide-dispersed alloy powder.
Wherein pass into the CO that vacuum is 1000 ~ 5000Pa
2gas is high-purity CO
2gas.This step can by alloyed powder in three-tube type vacuum drying oven, at high-purity CO of rough vacuum
2remove the carbon that powder surface may exist under atmosphere, then degasification reduce powder micro-hardness under a high vacuum, avoids CO, CO
2adsorb at powder surface or enter alloyed powder inside and cause pore, thus degreasing, decarburization and degassing processing can be carried out successively, improve the percentage elongation after oxide-dispersed alloy powder sintering, reduce ductile-brittle transition temperature.The oxide-dispersed alloy powder excess of oxygen content obtained by this method, lower than 100ppm (0.01%), utilizes follow-up powder metallurgy process can obtain the alloy of more high-elongation and lower ductile-brittle transition temperature.
The first tube type vacuum stove of the present embodiment, the second tube type vacuum stove and three-tube type vacuum drying oven can also be same tube type vacuum stove, but need before every use to ensure its cleannes, to ensure success rate prepared by oxide-dispersed alloy powder.
The oxide-dispersed alloy raw powder's production technology of the present embodiment, adopts CO-CO
2mist, as reducing atmosphere, first carries out reduction and degassed process to raw meal, guarantees the purity of original powder; Secondly, in mechanical milling process, Ar-CO-CO is kept
2reproducibility environment, stop further the generation of oxidation; Finally at high-purity CO of rough vacuum
2remove the carbon that powder surface may exist under atmosphere, then degasification reduce powder micro-hardness under a high vacuum, avoids CO, CO
2adsorb at powder surface or enter alloyed powder inside and cause pore, improve the percentage elongation after sintering, reduce ductile-brittle transition temperature.Experiment proves, the oxide-dispersed alloy powder excess of oxygen content obtained by this method is lower than 100ppm (namely 0.01%).Therefore, the oxide-dispersed alloy raw powder's production technology of the present embodiment, can from reducing oxygen content and avoiding the angle proposition CO-CO of hydrogen embrittlement
2mist substitutes argon gas or hydrogen as reduction and protective atmosphere; and adopt corresponding salvo for the different phase in oxide-dispersed alloy powder preparation process; both reduce excess of oxygen content, turn avoid hydrogen embrittlement, and also make powder have lower containing H simultaneously
2o amount and phosphorus content.Therefore the oxide-dispersed alloy powder prepared of the oxide-dispersed alloy raw powder's production technology of the present embodiment, compared with the oxide-dispersed alloy powder obtained with existing method, possess that excess of oxygen content is low, the feature such as percentage elongation raising, ductile-brittle transition temperature reduction after sintering.
Alternatively, in the technical scheme of above-described embodiment, CO-CO
2cO and CO in mist
2volume ratio is 1:0.5 ~ 1:0.8, containing H
2o amount is less than 50ppm; Its flow velocity is 1 ~ 30mL/min.
Further alternatively, in the technical scheme of above-described embodiment, the ball mill that ball milling uses in vacuum sphere grinding jar is high energy ball mill, and the high energy ball mill in the present embodiment is specifically as follows planetary ball mill, oscillatory type ball mill or stirring ball mill; Milling protection atmosphere adopts Ar-CO-CO
2mist fills row 2 ~ 3 times repeatedly, and before each inflation, in tank, vacuum should lower than 1Pa.
Further alternatively, in the technical scheme of above-described embodiment, can also comprise before step 102 " by the raw meal after above-mentioned process and the mixing of nano-oxide powder ":
A () takes out the raw meal after process from the first tube type vacuum stove;
And (b) takes out the nano-oxide powder after processing from the second tube type vacuum stove.
Further alternatively, in the technical scheme of above-described embodiment, step (a) takes out the raw meal after process from the first tube type vacuum stove, step (b) takes out the nano-oxide powder after process from the second tube type vacuum stove, and the process of " by the raw meal after above-mentioned process and the mixing of nano-oxide powder " in step 102 is all completed in the glove box of ar gas environment, in glove box, pressure is 0.1 ~ 3MPa, H
2o and O
2content is all less than 1ppm.
The flow chart of the oxide-dispersed alloy raw powder's production technology that Fig. 2 provides for another embodiment of the present invention.The oxide-dispersed alloy raw powder's production technology of the present embodiment introduces technical scheme of the present invention in further detail further on above-mentioned basis embodiment illustrated in fig. 1.As shown in Figure 2, the oxide-dispersed alloy raw powder's production technology of the present embodiment, comprises the steps:
200, according to mass percent be Cr9.0%, W2%, V0.2%, surplus be Fe prepare raw meal, raw meal is placed in the first tube type vacuum stove, passes into CO and CO with the flow velocity of 10mL/min
2volume ratio is the mist of 1:0.8, and be warming up to 650 DEG C of insulation 0.8h, be then evacuated to lower than 0.01Pa, insulation 0.5h, keeps vacuum and be cooled to room temperature;
The simple metal powder that raw meal in the present embodiment is mass percent is Cr9.0%, W2%, V0.2%, surplus are Fe.
201, by nanometer Y
2o
3powder is placed in the second tube type vacuum stove, and temperature 400 DEG C, low vacuum carries out the bakeout degassing of 1.5h under 0.01Pa;
The nano-oxide powder of the present embodiment is nanometer Y
2o
3.
202, step 200 is processed the raw meal obtained and step 201 processes the nanometer Y obtained
2o
3powder mixes, and be placed in vacuum sphere grinding jar, passing into pressure is 0.2MPa, and volume ratio is Ar and CO-CO of 1:0.5
2mist, obtains the uniform alloyed powder of solid solution by planetary ball mill ball milling;
Wherein CO-CO
2cO and CO in mist
2volume ratio is 1:0.8.It should be noted that, from the first tube type vacuum stove, take out the raw meal after process, from the second tube type vacuum stove, take out the nanometer Y after process
2o
3powder, and " by the raw meal after above-mentioned process and nanometer Y
2o
3powder mix " process all complete in the glove box of ar gas environment, in glove box, pressure is 0.1 ~ 3MPa, H
2o and O
2content is all less than 1ppm.
203, step 202 alloyed powder gained alloyed powder is placed in three-tube type vacuum drying oven, at low vacuum in 0.01Pa, temperature is be incubated 0.5h at 300 DEG C; Be warming up to 500 DEG C, pass into high-purity CO that vacuum is 1000 ~ 5000Pa
2gas, insulation 0.5h; Be evacuated to lower than 0.01Pa, insulation 2h, keeps vacuum and is cooled to room temperature, obtaining oxide-dispersed alloy powder;
It should be noted that, when needs take out oxide-dispersed alloy powder, need equally in the glove box of ar gas environment, get powder and preserve.The oxide-dispersed alloy powder obtained by the preparation method of employing the present embodiment is the alloy powder of ultra low oxygen content, and its excess of oxygen content is 90ppm.
The oxide-dispersed alloy raw powder's production technology of the present embodiment, adopts CO-CO
2mist, as reducing atmosphere, first carries out reduction and degassed process to raw meal, guarantees the purity of original powder; Secondly, in mechanical milling process, Ar-CO-CO is kept
2reproducibility environment, stop further the generation of oxidation; Finally at high-purity CO of rough vacuum
2remove the carbon that powder surface may exist under atmosphere, then degasification reduce powder micro-hardness under a high vacuum, avoids CO, CO
2adsorb at powder surface or enter alloyed powder inside and cause pore, improve the percentage elongation after sintering, reduce ductile-brittle transition temperature.Therefore, the oxide-dispersed alloy raw powder's production technology of the present embodiment, can from reducing oxygen content and avoiding the angle proposition CO-CO of hydrogen embrittlement
2mist substitutes argon gas or hydrogen as reduction and protective atmosphere; and adopt corresponding salvo for the different phase in oxide-dispersed alloy powder preparation process; both reduce excess of oxygen content, turn avoid hydrogen embrittlement, and also make powder have lower containing H simultaneously
2o amount and phosphorus content.Therefore the oxide-dispersed alloy powder prepared of the oxide-dispersed alloy raw powder's production technology of the present embodiment, compared with the oxide-dispersed alloy powder obtained with existing method, possess that excess of oxygen content is low, the feature such as percentage elongation raising, ductile-brittle transition temperature reduction after sintering.
The flow chart of the oxide-dispersed alloy raw powder's production technology that Fig. 3 provides for yet another embodiment of the invention.The oxide-dispersed alloy raw powder's production technology of the present embodiment introduces technical scheme of the present invention in further detail further on above-mentioned basis embodiment illustrated in fig. 1.As shown in Figure 3, the oxide-dispersed alloy raw powder's production technology of the present embodiment, comprises the steps:
300, according to mass percent be Cr22.0%, Fe18%, Mo9%, Co1.5%, W0.6%, Mn1%, surplus be raw meal prepared by Ni, raw meal is placed in the first tube type vacuum stove, passes into CO and CO with the flow velocity of 20mL/min
2volume ratio is the mist of 1:0.6, and be warming up to 700 DEG C of insulation 1h, be then evacuated to lower than 0.01Pa, insulation 0.5h, keeps vacuum and be cooled to room temperature;
The raw meal of the present embodiment is mass percent is Cr22.0%, Fe18%, Mo9%, Co1.5%, W0.6%, Mn1%, surplus are atomization prealloy powder prepared by Ni.
301, by nanometer Al
2o
3powder is placed in the second tube type vacuum stove, and temperature 400 DEG C, low vacuum carries out the bakeout degassing of 1.5h under 0.01Pa;
The nano-oxide powder of the present embodiment is nanometer Al
2o
3.
302, the Al that raw meal step 300 obtained and step 301 obtain
2o
3powder mixes, and be placed in vacuum sphere grinding jar, passing into pressure is 0.2MPa, and volume ratio is Ar and CO-CO of 1:1
2mist, obtains the uniform alloyed powder of solid solution by vibrator ball milling;
The CO-CO of the present embodiment
2cO and CO in mist
2volume ratio is 1:0.6.It should be noted that, the raw meal after process is taken out from the first tube type vacuum stove, the nano-oxide powder after process is taken out from the second tube type vacuum stove, and the process of " by the raw meal after above-mentioned process and the mixing of nano-oxide powder " all completes in the glove box of ar gas environment, in glove box, pressure is 0.1 ~ 3MPa, H
2o and O
2content is all less than 1ppm.
303, step 302 gained alloyed powder is placed in three-tube type vacuum drying oven, at low vacuum in 0.01Pa, temperature is be incubated 0.5h at 300 DEG C; Be warming up to 550 DEG C, pass into high-purity CO that vacuum is 1000 ~ 5000Pa
2gas, insulation 1h; Be evacuated to lower than 0.01Pa, insulation 2.5h, keeps vacuum and is cooled to room temperature, to oxide-dispersed alloy powder;
It should be noted that, when needs take out oxide-dispersed alloy powder, need equally in the glove box of ar gas environment, get powder and preserve.The oxide-dispersed alloy powder obtained by the preparation method of employing the present embodiment is the alloy powder of ultra low oxygen content, and its excess of oxygen content is 50ppm.
The oxide-dispersed alloy raw powder's production technology of the present embodiment, adopts CO-CO
2mist, as reducing atmosphere, first carries out reduction and degassed process to raw meal, guarantees the purity of original powder; Secondly, in mechanical milling process, Ar-CO-CO is kept
2reproducibility environment, stop further the generation of oxidation; Finally at high-purity CO of rough vacuum
2remove the carbon that powder surface may exist under atmosphere, then degasification reduce powder micro-hardness under a high vacuum, avoids CO, CO
2adsorb at powder surface or enter alloyed powder inside and cause pore, improve the percentage elongation after sintering, reduce ductile-brittle transition temperature.Therefore, the oxide-dispersed alloy raw powder's production technology of the present embodiment, can from reducing oxygen content and avoiding the angle proposition CO-CO of hydrogen embrittlement
2mist substitutes argon gas or hydrogen as reduction and protective atmosphere; and adopt corresponding salvo for the different phase in oxide-dispersed alloy powder preparation process; both reduce excess of oxygen content, turn avoid hydrogen embrittlement, and also make powder have lower containing H simultaneously
2o amount and phosphorus content.Therefore the oxide-dispersed alloy powder prepared of the oxide-dispersed alloy raw powder's production technology of the present embodiment, compared with the oxide-dispersed alloy powder obtained with existing method, possess that excess of oxygen content is low, the feature such as percentage elongation raising, ductile-brittle transition temperature reduction after sintering.
Last it is noted that above embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (6)
1. an oxide-dispersed alloy raw powder's production technology, is characterized in that, comprises the steps:
Raw meal is put into the first tube type vacuum stove, pass into CO-CO
2mist, be warming up to 600 ~ 750 DEG C of insulation 0.5 ~ 1h, and be evacuated to lower than 0.01Pa, insulation 0.3 ~ 0.8h, keeps vacuum and is cooled to room temperature; Described raw meal be according to required element proportioning simple metal powder or atomization prealloy powder;
Nano-oxide powder is placed in the second tube type vacuum stove, temperature 400 ~ 600 DEG C, low vacuum carries out the bakeout degassing of 1 ~ 3h under 0.01Pa;
By the described raw meal after above-mentioned process and the mixing of described nano-oxide powder, be placed in vacuum sphere grinding jar, passing into pressure is 0.1 ~ 0.3MPa, and volume ratio is Ar and CO-CO of 1:0.5 ~ 1:1
2mist, obtains the uniform alloyed powder of solid solution by ball milling;
The described alloyed powder of gained is placed in three-tube type vacuum drying oven, and at low vacuum in 0.01Pa, temperature is be incubated 0.3 ~ 0.8h at 250 ~ 350 DEG C; Be warming up to 400 ~ 600 DEG C, pass into the CO that vacuum is 1000 ~ 5000Pa
2gas, insulation 0.5 ~ 1.5h; Be evacuated to lower than 0.01Pa, insulation 1 ~ 3h, keeps vacuum and is cooled to room temperature, obtaining oxide-dispersed alloy powder.
2. method according to claim 1, is characterized in that, described nano-oxide powder comprises Y
2o
3, Al
2o
3or ThO
2.
3. method according to claim 1, is characterized in that, described CO-CO
2cO and CO in mist
2volume ratio is 1:0.5 ~ 1:0.8, containing H
2o amount is less than 50ppm; Its flow velocity is 1 ~ 30mL/min.
4. method according to claim 1, is characterized in that, the ball mill that ball milling uses in described vacuum sphere grinding jar is high energy ball mill; Milling protection atmosphere adopts Ar-CO-CO
2mist fills row 2 ~ 3 times repeatedly, and before each inflation, in tank, vacuum should lower than 1Pa.
5. according to the arbitrary described method of claim 1-4, it is characterized in that, describedly also to comprise before the described raw meal after above-mentioned process and the mixing of described nano-oxide powder:
The described raw meal after process is taken out from described first tube type vacuum stove;
And the described nano-oxide powder taken out from described second tube type vacuum stove after process.
6. method according to claim 5, it is characterized in that, the described raw meal after process is taken out from described first tube type vacuum stove, the described nano-oxide powder after process is taken out from described second tube type vacuum stove, and the process of the described raw meal after above-mentioned process and the mixing of described nano-oxide powder is all completed in the glove box of ar gas environment, in described glove box, pressure is 0.1 ~ 3MPa, H
2o and O
2content is all less than 1ppm.
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| SU1579679A1 (en) * | 1988-06-29 | 1990-07-23 | Липецкий политехнический институт | Method of reconditioning rolling mill rolls |
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| JP3672903B2 (en) * | 2002-10-11 | 2005-07-20 | 核燃料サイクル開発機構 | Manufacturing method of oxide dispersion strengthened ferritic steel pipe |
| KR20120039862A (en) * | 2010-10-18 | 2012-04-26 | 한국원자력연구원 | Manufacturing method for oxide dispersion strengthened alloys |
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| US3571477A (en) * | 1968-06-21 | 1971-03-16 | Bert Phillips | Protection of oxidizable electric furnace elements at high temperatures |
| US3649242A (en) * | 1969-11-26 | 1972-03-14 | Nasa | Method for producing dispersion-strengthened alloys by converting metal to a halide, comminuting, reducing the metal halide to the metal and sintering |
| SU1579679A1 (en) * | 1988-06-29 | 1990-07-23 | Липецкий политехнический институт | Method of reconditioning rolling mill rolls |
| CN101328562A (en) * | 2008-07-17 | 2008-12-24 | 中国科学院等离子体物理研究所 | Oxide dispersion strengthening low activity martensitic steel material and preparation thereof |
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