CN104325135A - Nanometer iron powder sintering body containing nano iron trioxide and preparation method of nanometer iron powder sintering body - Google Patents
Nanometer iron powder sintering body containing nano iron trioxide and preparation method of nanometer iron powder sintering body Download PDFInfo
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- CN104325135A CN104325135A CN201410648712.4A CN201410648712A CN104325135A CN 104325135 A CN104325135 A CN 104325135A CN 201410648712 A CN201410648712 A CN 201410648712A CN 104325135 A CN104325135 A CN 104325135A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000005245 sintering Methods 0.000 title claims abstract description 22
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title abstract 3
- 239000000843 powder Substances 0.000 claims abstract description 147
- 239000000654 additive Substances 0.000 claims abstract description 38
- 230000000996 additive effect Effects 0.000 claims abstract description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 28
- 239000001257 hydrogen Substances 0.000 claims abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 229910052718 tin Inorganic materials 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 238000003825 pressing Methods 0.000 claims abstract description 3
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 claims description 43
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 40
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000011863 silicon-based powder Substances 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 6
- 239000000956 alloy Substances 0.000 abstract description 6
- 229910000831 Steel Inorganic materials 0.000 abstract description 5
- 239000010959 steel Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 229910000976 Electrical steel Inorganic materials 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 150000002506 iron compounds Chemical class 0.000 abstract 1
- 238000000462 isostatic pressing Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 16
- 230000014759 maintenance of location Effects 0.000 description 11
- 238000000748 compression moulding Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 239000002184 metal Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910002551 Fe-Mn Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The invention discloses a nanometer iron powder sintering body containing nano iron trioxide and a preparation method of the nanometer iron powder sintering body. The nanometer iron powder sintering body is prepared from the following raw materials in mass percentage: 80%-100% of nano iron trioxide powder and 0-20% of additive powder, wherein the additive powder is the powder containing one of C, Al, Si, Mn, Sn, Ni, Co, Cr, Mo, Sb and Bi, or compound powder containing two or more of C, Al, Si, Mn, Sn, Ni, Co, Cr, Mo, Sb and Bi. The preparation method comprises the following steps: fully mixing the raw materials; then carrying out mold pressing, isostatic pressing or vibration molding; finally sintering in high-purity hydrogen or a mixed atmosphere of the high-purity hydrogen and nitrogen at 700-1,000 DEG C; carrying out heat preservation for 30-600 minutes. The preparation method is simple in process, rapid sintering of iron compound powder is achieved at a relatively low temperature, wear-resistant alloy, high-temperature alloy, silicon steel, high-strength spare parts for automobiles and other special steel products can be manufactured, and the production cost is low.
Description
Technical field
The present invention relates to nanometer iron powder sintered body, refer to a kind of nanometer iron powder sintered body containing nanometer di-iron trioxide and preparation method thereof particularly.
Background technology
In field of powder metallurgy, metal powder is pressurizeed in metal pattern, shaping after, carry out sintering and the sintered body made, precision can manufacture the mechanical part of complicated shape well.Therefore, in the manufacture requiring the automobile component of high dimensional accuracy, antifriction alloy, high temperature alloy and other specific use parts, sintered body can be applied widely.
Publication number is that the Chinese invention patent of CN101772389A discloses " powder used in metallurgy iron system's mixed-powder and iron powder sintering body ", be with containing iron-based powder, graphite powder, copper powder and composite oxides for raw material, realize below 1000 DEG C sintering.Publication number is that the Chinese invention patent of CN101733400A discloses " high-strength composition iron powder and its sintered component of use ", with iron powder primary raw material, add a certain amount of Mn, Fe-Mn (particle diameter less than 45 microns), Cu and powdered graphite, more than the fusing point of Cu, in less than 1300 DEG C temperature ranges, realize sintering.Publication number is that the Chinese utility model patent of CN201141401Y discloses " a kind of bimetallic bearing of copper-clad iron powder sintering ", sintering has the wearing layer of copper-clad iron powder on a surface of a steel sheet, form stacked composite, and make axle sleeve or flat board with this composite, sintering has the surface of copper-clad iron powder to be the rubbing surface of bearing.
In sum, the research of iron system composite powder sintered body, mainly concentrates on the relatively low copper powder of employing fusing point as sintering aid aspect, cannot meet the use needs of high strength parts and other steel for special purposes products.
Summary of the invention
Object of the present invention is exactly to overcome the deficiency existing for prior art, nanometer iron powder sintered body providing a kind of nanometer to contain nanometer di-iron trioxide and preparation method thereof.
The fusing point of general material is, under a certain pressure, pure material solid-state and liquid in balance time temperature, that is, under this pressure and melting temperature, pure material be that solid-state chemical potential is equal with the chemical potential be in a liquid state.Concerning the pure object of bulk, its chemical potential is the function of temperature and pressure.
And nano particle due to particle diameter little, specific surface free energy is high, therefore its chemical potential is higher than the blocks of solid under the same terms a lot, and result causes its fusing point and sintering temperature to be significantly less than the blocks of solid of same material, and the particle diameter of particle is less, its fusing point and sintering temperature lower.Such as, the fusing point of bulk Pb is 600K, and the fusing point of 20 nanometer spherical Pb particles reduces 288K, and nano-Ag particles is starting fusing lower than 373K, and the fusing point of conventional Ag is up to 1273K.
We are found by experimental study, when the particle diameter of nanometer iron powder is less than 100 nanometer, its fusing point can reduce, simultaneously, under the specific condition of high-purity hydrogen or high-purity hydrogen and nitrogen mixture atmosphere, after metal oxide back becomes simple substance particle, its activity is higher, more easily and other metals or oxide react, sinter.Utilize this principle to design, produce various metals sintered powder, to meet the use needs of high strength parts and other steel for special purposes products.
For achieving the above object, the nanometer iron powder sintered body containing nanometer di-iron trioxide designed by the present invention, it is formulated by following raw material by mass percentage: nanometer ferric oxide powder 80 ~ 100%, additive powder 0 ~ 20%, described additive powder is containing a kind of powder in C, Al, Si, Mn, Sn, Ni, Co, Cr, Mo, Sb, Bi element or two kinds and two or more composite powders.
Preferably, the nanometer iron powder sintered body containing nanometer di-iron trioxide is formulated by following raw material by mass percentage: nanometer ferric oxide powder 90 ~ 95%, graphite powder 0.05 ~ 0.5%, Al powder 1.0 ~ 5.0%, Si powder 1.0 ~ 5.0%, Mn powder 1.0 ~ 4.5%.
Preferably, the nanometer iron powder sintered body containing nanometer di-iron trioxide is formulated by following raw material by mass percentage: nanometer ferric oxide powder 80 ~ 93%, Ni powder 5 ~ 15%, Co powder 2 ~ 10%.
Preferably, the nanometer iron powder sintered body containing nanometer di-iron trioxide is formulated by following raw material by mass percentage: nanometer ferric oxide powder 80 ~ 90%, Ni powder 5 ~ 15%, Cr powder 5 ~ 10%, Mn powder 0 ~ 5%.
Preferably, the nanometer iron powder sintered body containing nanometer di-iron trioxide is formulated by following raw material by mass percentage: nanometer ferric oxide powder 90 ~ 95%, Al powder 1.0 ~ 1.5%, Si powder 2.0 ~ 5.0%, Mn powder 1.0 ~ 3.5%, Sn powder 0.1 ~ 1.0%, Sb powder 0.2 ~ 0.8%, Bi powder 0.1 ~ 0.5%.
Preferably, the nanometer iron powder sintered body containing nanometer di-iron trioxide is formulated by following raw material by mass percentage: nanometer ferric oxide powder 80 ~ 90%, graphite powder 0.1 ~ 0.5%, Mn powder 1.0 ~ 3.5%, Cr powder 5 ~ 15%, Mo powder 2 ~ 8%.
In the present invention, the average grain diameter of described nanometer ferric oxide powder is less than 100 nanometers, purity more than 98%.
In the present invention, the average grain diameter of described additive powder is less than 10 microns, purity more than 99%.
The preparation method of the above-mentioned nanometer iron powder sintered body containing nanometer di-iron trioxide: first raw material is fully mixed, then mold pressing, isostatic pressed or vibration moulding is carried out, finally in the mixed atmosphere of high-purity hydrogen or high-purity hydrogen and nitrogen, sinter at sintering temperature 700 ~ 1000 DEG C, be incubated 30 ~ 600 minutes.
In mixed atmosphere of the present invention, hydrogen volume percent concentration is 30 ~ 99%, and nitrogen concentration of volume percent is 1 ~ 70%.
Found by experimental study, when the particle diameter of nanometer ferric oxide powder is less than 100 nanometer, its fusing point can reduce, simultaneously, under the specific condition of the mixed atmosphere of high-purity hydrogen or high-purity hydrogen and nitrogen, after nanometer ferric oxide powder is reduced into fe, its activity is higher, even occurs liquid phase, more easily and other metals or oxide react, sinter, utilize this principle to design, produce various metals sintered powder.
Beneficial effect of the present invention is: adopt technique scheme, present invention process is simple, under low temperature, realize the sintering of quick iron system composite powder, antifriction alloy, high temperature alloy, silicon steel, automobile high-strength parts and other steel for special purposes products can be manufactured, low production cost.
Detailed description of the invention
In order to explain the present invention better, below in conjunction with specific embodiment, the present invention is described in further detail, but they do not form restriction to the present invention.
Embodiment 1
The composition of raw materials of the nanometer iron powder sintered body containing nanometer di-iron trioxide, is by mass percentage: nanometer ferric oxide powder 90%, additive powder 10%; Wherein, additive powder is graphite powder 0.5%, Al powder 1.0%, Si powder 5.0%, Mn powder 3.5%.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: first nanometer ferric oxide powder is fully mixed with additive powder, then compression molding is carried out, last in high-purity hydrogen atmosphere, sinter at 850 DEG C, temperature retention time 60 minutes.
Embodiment 2
The composition of raw materials of the nanometer iron powder sintered body containing nanometer di-iron trioxide, is by mass percentage: nanometer ferric oxide powder 95%, additive powder 5%; Wherein, additive powder is graphite powder 0.1%, Al powder 2.0%, Si powder 1.4%, Mn powder 1.5%.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: first nanometer ferric oxide powder is fully mixed with additive powder, then compression molding is carried out, last in high-purity hydrogen atmosphere, sinter at 900 DEG C, temperature retention time 30 minutes.
Embodiment 3
The composition of raw materials of the nanometer iron powder sintered body containing nanometer di-iron trioxide, is by mass percentage: nanometer ferric oxide powder 93%, additive powder 7%; Wherein, additive powder is graphite powder 0.3%, Al powder 2.0%, Si powder 2.2%, Mn powder 2.5%.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: first nanometer ferric oxide powder is fully mixed with additive powder, then compression molding is carried out, last in high-purity hydrogen and nitrogen mixture atmosphere, hydrogen volume percent concentration is 90%, nitrogen concentration of volume percent is 10%, sinter at 850 DEG C, temperature retention time 30 minutes.
Embodiment 4
The raw material of the nanometer iron powder sintered body containing nanometer di-iron trioxide is 100% nanometer ferric oxide powder.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: nanometer ferric oxide powder is carried out compression molding, in high-purity hydrogen atmosphere, sinters at 750 DEG C, temperature retention time 60 minutes.
Embodiment 5
The raw material of the nanometer iron powder sintered body containing nanometer di-iron trioxide is 100% nanometer ferric oxide powder.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: nanometer ferric oxide powder is carried out compression molding, in high-purity hydrogen and nitrogen mixture atmosphere, hydrogen volume percent concentration is 70%, nitrogen concentration of volume percent is 30%, sinter at 850 DEG C, temperature retention time 120 minutes.
Embodiment 6
The composition of raw materials of the nanometer iron powder sintered body containing nanometer di-iron trioxide, is by mass percentage: nanometer ferric oxide powder 83%, additive powder 17%; Wherein, additive powder is Ni powder 15%, Co powder 2%.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: first nanometer ferric oxide powder is fully mixed with additive powder, then vibration moulding is carried out, last in high-purity hydrogen, sinter at 950 DEG C, temperature retention time 300 minutes.
Embodiment 7
The composition of raw materials of the nanometer iron powder sintered body containing nanometer di-iron trioxide, is by mass percentage: nanometer ferric oxide powder 85%, additive powder 15%; Wherein, additive powder is Ni powder 15%.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: first nanometer ferric oxide powder is fully mixed with additive powder, then isostatic compaction is carried out, last in high-purity hydrogen, sinter at 900 DEG C, temperature retention time 600 minutes.
Embodiment 8
The composition of raw materials of the nanometer iron powder sintered body containing nanometer di-iron trioxide, is by mass percentage: nanometer ferric oxide powder 80%, additive powder 20%; Wherein, additive powder is Ni powder 10%, Co powder 10%.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: first nanometer ferric oxide powder is fully mixed with additive powder, then compression molding is carried out, last in high-purity hydrogen and nitrogen mixture atmosphere, hydrogen volume percent concentration is 50%, nitrogen concentration of volume percent is 50%, sinter at 980 DEG C, temperature retention time 120 minutes.
Embodiment 9
The composition of raw materials of the nanometer iron powder sintered body containing nanometer di-iron trioxide, is by mass percentage: nanometer ferric oxide powder 80%, additive powder 20%; Wherein, additive powder is Ni powder 15%, Cr powder 5%, Mn powder 5%.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: first nanometer ferric oxide powder is fully mixed with additive powder, then compression molding is carried out, last in high-purity hydrogen atmosphere, sinter at 930 DEG C, temperature retention time 120 minutes.
Embodiment 10
The composition of raw materials of the nanometer iron powder sintered body containing nanometer di-iron trioxide, is by mass percentage: nanometer ferric oxide powder 80%, additive powder 20%; Wherein, additive powder is Ni powder 10%, Cr powder 10%.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: first nanometer ferric oxide powder is fully mixed with additive powder, then vibration moulding is carried out, in high-purity hydrogen and nitrogen mixture atmosphere, hydrogen volume percent concentration is 40%, nitrogen concentration of volume percent is 60%, sinter at 960 DEG C, be incubated 120 minutes.
Embodiment 11
The composition of raw materials of the nanometer iron powder sintered body containing nanometer di-iron trioxide, is by mass percentage: nanometer ferric oxide powder 95%, additive powder 5%; Wherein, additive powder is Al powder 1.0%, Si powder 2.0%, Mn powder 1.0%, Sn powder 0.5%, Sb powder 0.2%, Bi powder 0.3%.
The preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide: first nanometer ferric oxide powder is fully mixed with additive powder, then compression molding is carried out, last in high-purity hydrogen atmosphere, sinter at sintering temperature 950 DEG C, temperature retention time 120 minutes.
Embodiment 12
The composition of raw materials of the nanometer iron powder sintered body containing nanometer di-iron trioxide, is by mass percentage: nanometer ferric oxide powder 81%, additive powder 19%; Wherein, additive powder is graphite powder 0.5%, Mn powder 1.0%, Cr powder 15%, Mo powder 2.5%.
Preparation technology is: first nanometer ferric oxide powder fully mixed with additive powder, then carries out compression molding, finally in high-purity hydrogen atmosphere, sinters at sintering temperature 980 DEG C, temperature retention time 300 minutes.
Claims (10)
1. the nanometer iron powder sintered body containing nanometer di-iron trioxide, it is characterized in that, it is formulated by following raw material by mass percentage: nanometer ferric oxide powder 80 ~ 100%, additive powder 0 ~ 20%, described additive powder is containing a kind of powder in C, Al, Si, Mn, Sn, Ni, Co, Cr, Mo, Sb, Bi element or two kinds and two or more composite powders.
2. the nanometer iron powder sintered body containing nanometer di-iron trioxide according to claim 1, it is characterized in that, it is formulated by following raw material by mass percentage: nanometer ferric oxide powder 90 ~ 95%, graphite powder 0.05 ~ 0.5%, Al powder 1.0 ~ 5.0%, Si powder 1.0 ~ 5.0%, Mn powder 1.0 ~ 4.5%.
3. the nanometer iron powder sintered body containing nanometer di-iron trioxide according to claim 1, it is characterized in that, it is formulated by following raw material by mass percentage: nanometer ferric oxide powder 80 ~ 95%, Ni powder 5 ~ 15%, Co powder 0 ~ 10%.
4. the nanometer iron powder sintered body containing nanometer di-iron trioxide according to claim 1, it is characterized in that, it is formulated by following raw material by mass percentage: nanometer ferric oxide powder 80 ~ 90%, Ni powder 5 ~ 15%, Cr powder 5 ~ 10%, Mn powder 0 ~ 5%.
5. the nanometer iron powder sintered body containing nanometer di-iron trioxide according to claim 1, it is characterized in that, it is formulated by following raw material by mass percentage: nanometer ferric oxide powder 90 ~ 95%, Al powder 1.0 ~ 1.5%, Si powder 2.0 ~ 5.0%, Mn powder 1.0 ~ 3.5%, Sn powder 0.1 ~ 1.0%, Sb powder 0.2 ~ 0.8%, Bi powder 0.1 ~ 0.5%.
6. the nanometer iron powder sintered body containing nanometer di-iron trioxide according to claim 1, it is characterized in that, it is formulated by following raw material by mass percentage: nanometer ferric oxide powder 80 ~ 90%, graphite powder 0.1 ~ 0.5%, Mn powder 1.0 ~ 3.5%, Cr powder 5 ~ 15%, Mo powder 2 ~ 8%.
7. the nanometer iron powder sintered body containing nanometer di-iron trioxide according to claim 1, is characterized in that: the average grain diameter of described nanometer ferric oxide powder is less than 100 nanometers, purity more than 98%.
8. the nanometer iron powder sintered body containing nanometer di-iron trioxide according to claim 1 and 2, is characterized in that: the average grain diameter of described additive powder is less than 10 microns, purity more than 99%.
9. the preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide according to claim 1, it is characterized in that: first raw material is fully mixed, then mold pressing, isostatic pressed or vibration moulding is carried out, finally in the mixed atmosphere of high-purity hydrogen or high-purity hydrogen and nitrogen, sinter at sintering temperature 700 ~ 1000 DEG C, be incubated 30 ~ 600 minutes.
10. the preparation method of the nanometer iron powder sintered body containing nanometer di-iron trioxide according to claim 4, it is characterized in that: in described mixed atmosphere, hydrogen volume percent concentration is 30 ~ 99%, and nitrogen concentration of volume percent is 1 ~ 70%.
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2014
- 2014-11-14 CN CN201410648712.4A patent/CN104325135B/en active Active
Patent Citations (7)
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| JPS50123010A (en) * | 1974-03-18 | 1975-09-27 | ||
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