CN102051530B - 48MnV nitrogenous steel and nitrogen adding process thereof - Google Patents
48MnV nitrogenous steel and nitrogen adding process thereof Download PDFInfo
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Abstract
The invention belongs to the field of metallurgy and relates to 48MnV nitrogenous steel and a nitrogen adding process thereof. The 48MnV nitrogenous steel comprises the following components: 0.45-0.51% of C, 0.17-0.37% of Si, 1.00-1.20% of Mn, 0.06-0.11% of V, 0.000-0.025% of Ti, 0.05-0.25% of Cr, 0.00-0.06% of Mo, 0.00-0.06% of Ni, 0.00-0.20% of Cu, 0.0080-0.0150% of N, at most 0.035% of P, at most 0.035% of S, at most 0.020% of O, 0.087-0.097% of Ceq and the balance of Fe and impurities; and the nitrogen adding process is carried out while the N content is controlled to be 0.0080-0.0150%, preferably 0.0090-0.0120%, wherein the target value is 0.0110%, and a manganese nitride iron wire is fed into the steel according to the calculated quantity in one step after a vacuum process is completed. By changing the pre-vacuum nitrogen adding and alloying into the post-vacuum nitrogen adding and alloying, the invention changes the technological process of pre-vacuum nitrogen alloying and post-vacuum slight nitrogen regulation in the metallurgy field, thereby enabling the 48MnV nitrogenous steel to obtain good comprehensive mechanical properties, and improving the strength and toughness.
Description
Technical field
The invention belongs to field of metallurgy, relate to a kind of nitrogenous steel and add nitrogen technology, a kind of specifically 48MnV nitrogenous steel and add nitrogen technology.
Background technology
The 48MnV nitrogenous steel is that non-hardened and tempered steel is used in forge hot, is mainly used in the manufacturing crankshaft of diesel engine, and the 48MnV steel is that Mn-V is perlite+ferrite type non-hardened and tempered steel.The accurate control of the nitrogen content of high level nitrogenous steel such as 48mnV is a difficult problem on metallurgical boundary always.Though it is multiple that the control method of the nitrogen content of steel has, nitrogen blowing can be described as the easiest most economical a kind of method in molten steel, and the prerequisite of this method is: the nitrogen killer that more amount is arranged in the molten steel.We have all carried out strict control to C, Mn, Cr, V, Nb, Ti, S, Al, O, N, H and residual element and Ceq this steel of 48MnV when composition designs; Require very narrow steel for this requirement of 48MnV very strictness and composition; As take the way of nitrogen blowing, will bring the very great fluctuation process of composition, material, performance.
The current at present nitrogen pick-up way that adopts in the metallurgical boundary of the nitrogenous steel of 48MnV is in stove, to add iron alloys such as nitrogenized manganese, chromium nitride, vanadium nitride, the back nitrogen pick-up but this way tap before vacuum, concrete technology be before the vacuum in the LF station toward steel in adding nitrogenized manganese and nitrogen flushing realize; Yet after vacuum outgas, nitrogen is also still often got back to the nitrogen content level when not adding nitrogen before the vacuum, has to after VD stove vacuum, add the nitrogenized manganese of equal amts again; Cause the waste of nitrogen-containing alloy, if the control of manganese, chromium is improper, then consequence is very serious; On the low side at N content, when Cr or Mn have reached target value, add alloy again; It is more then can to cause Cr or Mn to exceed target value; And this type to contain the N steel grade basically all be narrow Composition Control steel, generally all be strict by a Composition Control, contain the N alloy in case mend again; Basically be difficult to realize a some Composition Control target, user's use is affected.Under this kind situation, cannot add nitrogen-containing alloy again, nitrogen will be transferred to enter.
Summary of the invention
Technical problem to be solved by this invention is: the shortcoming to above prior art exists, and propose a kind of 48MnV nitrogenous steel and add nitrogen technology,
The technical scheme that the present invention solves above technical problem is:
A kind of 48MnV nitrogenous steel comprises following composition: C:0.45～0.51% by weight percentage, Si:0.17～0.37%, Mn:1.00～1.20%; V:0.06～0.11%, Ti:0.000～0.025, Cr:0.05～0.25%, Mo:0.00～0.06%; Ni:0.00～0.06%, Cu:0.00～0.20%, N:0.080～0.0150%, P≤0.035%; S≤0.035%, O≤0.020%, Ceq:0.087～0.097%, surplus is Fe and inevitably is mingled with.
The 48MnV nitrogenous steel add nitrogen technology, carry out according to the following steps: the supplementary material examination → batching → electrosmelting → LF refining → VD degassing → feeding nitrification gold thread → calcium processing → quiet stirring → continuous casting → strand cooling check → blank examination → heating → de-scaling → rolling → cooling in heap → aligning → pickling → reconditioning → chamfered edge → inside and outside flaw detection → inspection after construction → packing indicates → weighs → put in storage;
In the feeding nitroalloy line procedures, press N 0.0080～0.0150% control, target value 0.0110%, press calculated amount after the vacuum flow process in steel disposable feeding nitrogenized manganese line.
The technical scheme that the present invention further limits:
Aforesaid 48MnV nitrogenous steel add nitrogen technology, the nitrogenized manganese cored-wire composition that feeding nitrogenized manganese iron wire adopts require be: C≤1.0%, S≤0.03%; N:4.5～6.0%, P≤0.30%, Mn:75.0～80.0%; Si≤2.5, surplus are Fe and and inevitably are mingled with.Nitrogenized manganese cored-wire iron sheet quality≤180g/m, core opaque amount>=500g/m, every km joint number≤2.
Aforesaid 48MnV nitrogenous steel add nitrogen technology, electrosmelting: eaf tapping point carbon>=0.10%, P≤0.010%, the freeboard of ladle 660mm is guaranteed in T>=1640 ℃; Add slag charge and steel alloy: Si-Mn:9～12Kg in the tapping process in the ladle, compound middle aluminium: 3～4Kg, V-Fe:1～1.5Kg, lime: 5～6Kg, modification refining slag: 3～4Kg.
Aforesaid 48MnV nitrogenous steel add nitrogen technology, LF refining: refining time >=40min, process is added CaO according to the slag condition, uses SiAlCa or calcium carbide deoxidation, guarantees white slag >=30 minute.
Aforesaid 48MnV nitrogenous steel add nitrogen technology, in order to ensure oxygen content in steel≤20ppm, hydrogen richness≤3ppm, molten steel must carry out vacuum outgas at the VD stove to be handled;
Advance the VD reference temperature: continuous casting first stove: 1675～1695 ℃, connect and water stove: 1675～1685 ℃, advance the VD reference temperature and can return LF adjustment composition or intensification as arranging according to the adjustment of organization of production situation, can suitably adjust temperature;
VD composition %:C:0.46, Mn:0.90, Cr:0.13, Si:0.21, Alt:0.020～0.030 are entered in control;
Vacuum tightness＜1 millibar maintenance down, hold-time 10～15min, vacuum breaker promptly keep the quiet state that stirs.
Aforesaid 48MnV nitrogenous steel add nitrogen technology, feeding nitrification gold thread → calcium processings → quiet stirring: according to target be worth according to the appearance result and finely tune, add hello C line behind the TiFe; Fed and can feed the Al line immediately, fed the MnN line then: according to N content, 100m=26ppm N; 100m=0.037%Mn stirs the above feeding of 2min CaFe line: 80～120m, and the back that finishes keeps the above feeding of the quiet 3min of stirring SFe line: feed quantity: 1m/t; Get two appearance more than the quiet 3min of stirring and analyze, continue to keep quiet stirring, according to waiting appearance result to continue to finely tune; Finely tune qualified after, get after the finished product appearance continuous casting on the bull ladle; The quiet process of stirring adds heat preserving agent 100～150kg according to temperature.
The effect of each element:
(1) C carbon in all elements improves the ability maximum of intensity; Carbon is approximately 5 times of silicon to the strengthening effect of steel; 9 times of chromium with manganese 18 times, institute thinks that assurance 48MnV steel has enough intensity, hardness, performances such as antifatigue; Must contain quite high carbon content in the steel, so carbon content is controlled at 0.45～0.51%.
(2) Si solution strengthening, precipitation strength and refined crystalline strengthening can both make the dislocation moving difficulty, can effectively improve the intensity of steel, and silicon also is prone to reduce the plasticity and the toughness of steel, so Si content is controlled at 0.17～0.37%.
(3) Mn, Cr play strengthening effect to steel, so content is controlled at Mn 1.00～1.20%, and Cr0.05～0.25%.
(4) V, T all are strong carbide forming elements, and the effect of precipitation strength and refined crystalline strengthening is arranged in steel, so content is controlled at V 0.06～0.11%, Ti 0.000～0.025.
(5) N and V, Nb, Ti are compound, play the refined crystalline strengthening effect, so content is controlled at N 0.080～0.0150%.
Advantage of the present invention is: the present invention changes that to add nitrogen alloying before the vacuum be to add nitrogen alloying after the vacuum; Changed the preceding nitrogen alloying of metallurgical boundary vacuum; Finely tune the technical process of nitrogen after the vacuum again, can make the 48MnV nitrogenous steel obtain better comprehensive mechanical property, improve intensity and toughness.
Embodiment
Embodiment one
Present embodiment is a kind of 48MnV nitrogenous steel, comprises following composition: C:0.45% by weight percentage, Si:0.17%, Mn:1.00%; V:0.06%, Cr:0.05%, Mo:0.016%, Ni:0.01%; Cu:0.02%, N:0.080%, P:0.005%, S:0.015%; O:0.010%, Ceq:0.087%, surplus is Fe and inevitably is mingled with.
The 48MnV nitrogenous steel add nitrogen technology, carry out according to the following steps: the supplementary material examination → batching → electrosmelting → LF refining → VD degassing → feeding nitrification gold thread → calcium processing → quiet stirring → continuous casting → strand cooling check → blank examination → heating → de-scaling → rolling → cooling in heap → aligning → pickling → reconditioning → chamfered edge → inside and outside flaw detection → inspection after construction → packing indicates → weighs → put in storage;
In the feeding nitroalloy line procedures, controlled target value 0.0110%, by calculated amount after the vacuum flow process in steel disposable feeding 239m nitrogenized manganese line.
The nitrogenized manganese cored-wire composition that feeding nitrogenized manganese iron wire adopts requires:
Table 1
The nitrogenized manganese cored wire technology requires:
Table 2
Actual contain Mn75% with the heavy 500g of the every ground rice of nitrogenized manganese line, nitrogenous 5%, reserve in the LF station and to add the nitrogenized manganese line and increase Mn and measure.
The actual production process major control is following:
EAF: tap is allocated molten iron 40t into for the 100t electric furnace, with addition of the high-quality steel scrap.New new three stoves of stove, newly build preceding 3 stoves of steel and must not produce this steel grade.Eaf tapping point carbon>=0.10%, P≤0.010%, the freeboard of ladle 660mm is guaranteed in T>=1640 ℃.Add slag charge and alloy Kg/t steel: Si-Mn:9Kg in the tapping process in the ladle, compound middle aluminium: 3Kg, V-Fe:1Kg, lime: 5Kg, modification refining slag: 3Kg.
LF: more than refining time >=40min, process is added CaO according to the slag condition, uses SiAlCa, calcium carbide deoxidation, guarantees white slag >=30 minute.
VD: advance the VD reference temperature, continuous casting first stove: 1675 ℃, connect and water stove: 1675 ℃.Annotate: advancing the VD reference temperature can return LF adjustment composition or intensification as arranging according to the adjustment of organization of production situation, can suitably adjust temperature; Guarantee the omnidistance Alt of refining >=more than 0.020%; VD composition %:C:0.46, Mn:0.90, Cr:0.13, Si:0.21, Alt:0.020 are advanced in control; Vacuum tightness＜1 millibar maintenance down, hold-time 10min, vacuum breaker promptly keep the quiet state that stirs; Vacuum breaker is got lollipop appearance and is analyzed full composition, uses the nitrogen pick-up of MnN line.
Line feeding is grasped: according to target be worth according to the appearance result and finely tune, feed the C line behind the adding TiFe, fed and can feed the Al line immediately; Feed then the MnN line (according to N content, 100m=26ppm N, 100m=0.037%Mn); Stir the above feeding of 2min CaFe line: 80m, the back that finishes keeps the above feeding of the quiet 3min of stirring SFe line, and (feed quantity: 1m/t is according to molten steel actual [S]; Get two appearance more than the quiet 3min of stirring and analyze, continue to keep quiet stirring, according to waiting appearance result to continue to finely tune; Finely tune qualified after, get after the finished product appearance continuous casting on the bull ladle; The quiet process of stirring adds heat preserving agent 100kg according to temperature.
The vacuum out-station temperature: the bull ladle reference temperature (℃) continuous casting first stove: 1560, connect and water stove: 1550; VD fine setting composition can allow to return LF adjustment or intensification according to the organization of production situation; T liquid=1490 ℃, middle bag storing time meets the Technology rules requirement of electric furnace factory, best superheating temperature: 15 ℃; CC: continuous casting becomes the 320mm*480mm bloom.
Embodiment two
Present embodiment is a kind of 48MnV nitrogenous steel, comprises following composition: C:0.49% by weight percentage, Si:0.25%, Mn:1.10%; V:0.09%, Ti:0.015%, Cr:0.15%, Mo:0.04%; Ni:0.04%, Cu:0.10%, N:0.010%, P:0.025%; S:0.020%, O:0.010%, Ceq:0.091%, surplus is Fe and inevitably is mingled with.
The 48MnV nitrogenous steel add nitrogen technology, carry out according to the following steps: the supplementary material examination → batching → electrosmelting → LF refining → VD degassing → feeding nitrification gold thread → calcium processing → quiet stirring → continuous casting → strand cooling check → blank examination → heating → de-scaling → rolling → cooling in heap → aligning → pickling → reconditioning → chamfered edge → inside and outside flaw detection → inspection after construction → packing indicates → weighs → put in storage;
In the feeding nitroalloy line procedures, controlled target value 0.0110%, by calculated amount after the vacuum flow process in steel disposable feeding 239m nitrogenized manganese line.
The nitrogenized manganese cored-wire composition that feeding nitrogenized manganese iron wire adopts requires:
Table 3
The nitrogenized manganese cored wire technology requires:
Table 4
Actual contain Mn75% with the heavy 500g of the every ground rice of nitrogenized manganese line, nitrogenous 5%, reserve in the LF station and to add the nitrogenized manganese line and increase Mn and measure.
The actual production process major control is following:
EAF: tap is allocated molten iron 40t into for the 100t electric furnace, with addition of the high-quality steel scrap.New new three stoves of stove, newly build preceding 3 stoves of steel and must not produce this steel grade.Eaf tapping point carbon>=0.10%, P≤0.010%, the freeboard of ladle 660mm is guaranteed in T>=1640 ℃.Add slag charge and alloy Kg/t steel: Si-Mn:10Kg in the tapping process in the ladle, compound middle aluminium: 3.5Kg, V-Fe:1.2Kg, lime: 5.5Kg, modification refining slag: 3.5Kg.
LF: more than refining time >=40min, process is added CaO according to the slag condition, uses SiAlCa, calcium carbide deoxidation, guarantees white slag >=30 minute.
VD: advance the VD reference temperature, continuous casting first stove: 1680 ℃, connect and water stove: 1679 ℃.Annotate: advancing the VD reference temperature can return LF adjustment composition or intensification as arranging according to the adjustment of organization of production situation, can suitably adjust temperature; Guarantee the omnidistance Alt of refining >=more than 0.020%; VD composition %:C:0.46, Mn:0.90, Cr:0.13, Si:0.21, Alt:0.030 are advanced in control; Vacuum tightness＜1 millibar maintenance down, hold-time 12min, vacuum breaker promptly keep the quiet state that stirs; Vacuum breaker is got lollipop appearance and is analyzed full composition, uses the nitrogen pick-up of MnN line.
Line feeding is grasped: according to target be worth according to the appearance result and finely tune, feed the C line behind the adding TiFe, fed and can feed the Al line immediately; Feed then the MnN line (according to N content, 100m=26ppm N, 100m=0.037%Mn); Stir the above feeding of 2min CaFe line: 100m, the back that finishes keeps the above feeding of the quiet 3min of stirring SFe line, and (feed quantity: 1m/t is according to molten steel actual [S]; Get two appearance more than the quiet 3min of stirring and analyze, continue to keep quiet stirring, according to waiting appearance result to continue to finely tune; Finely tune qualified after, get after the finished product appearance continuous casting on the bull ladle; The quiet process of stirring adds heat preserving agent 120kg according to temperature.
The vacuum out-station temperature: the bull ladle reference temperature (℃) continuous casting first stove: 1565, connect and water stove: 1555; VD fine setting composition can allow to return LF adjustment or intensification according to the organization of production situation; T liquid=1490 ℃, middle bag storing time meets the Technology rules requirement of electric furnace factory, best superheating temperature: 20 ℃; CC: continuous casting becomes the 320mm*480mm bloom.
Embodiment three
Present embodiment is a kind of 48MnV nitrogenous steel, comprises following composition: C:0.51% by weight percentage, Si:0.37%, Mn:1.20%; V:0.11%, Ti:0.025, Cr:0.25%, Mo:0.06%; Ni:0.06%, Cu:0.20%, N:0.0150%, P:0.035%; S:0.035%, O:0.020%, Ceq:0.097%, surplus is Fe and inevitably is mingled with.
The 48MnV nitrogenous steel add nitrogen technology, carry out according to the following steps: the supplementary material examination → batching → electrosmelting → LF refining → VD degassing → feeding nitrification gold thread → calcium processing → quiet stirring → continuous casting → strand cooling check → blank examination → heating → de-scaling → rolling → cooling in heap → aligning → pickling → reconditioning → chamfered edge → inside and outside flaw detection → inspection after construction → packing indicates → weighs → put in storage;
In the feeding nitroalloy line procedures, controlled target value 0.0110%, by calculated amount after the vacuum flow process in steel disposable feeding 239m nitrogenized manganese line.
The nitrogenized manganese cored-wire composition that feeding nitrogenized manganese iron wire adopts requires:
Table 5
The nitrogenized manganese cored wire technology requires:
Table 6
Actual contain Mn75% with the heavy 500g of the every ground rice of nitrogenized manganese line, nitrogenous 5%, reserve in the LF station and to add the nitrogenized manganese line and increase Mn and measure.
The actual production process major control is following:
EAF: tap is allocated molten iron 40t into for the 100t electric furnace, with addition of the high-quality steel scrap.New new three stoves of stove, newly build preceding 3 stoves of steel and must not produce this steel grade.Eaf tapping point carbon 0.10%, P≤0.010%, the freeboard of ladle 660mm is guaranteed in T>=1640 ℃.Add slag charge and alloy Kg/t steel: Si-Mn:12Kg in the tapping process in the ladle, compound middle aluminium: 4Kg, V-Fe:1.5Kg, lime: 6Kg, modification refining slag: 4Kg.
LF: more than refining time >=40min, process is added CaO according to the slag condition, uses SiAlCa, calcium carbide deoxidation, guarantees white slag >=30 minute.
VD: advance the VD reference temperature, continuous casting first stove: 1695 ℃, connect and water stove: 1685 ℃.Annotate: advancing the VD reference temperature can return LF adjustment composition or intensification as arranging according to the adjustment of organization of production situation, can suitably adjust temperature; Guarantee the omnidistance Alt of refining >=more than 0.020%; VD composition %:C:0.46, Mn:0.90, Cr:0.13, Si:0.21, Alt:0.020-0.030 are advanced in control; Vacuum tightness＜1 millibar maintenance down, hold-time 15min, vacuum breaker promptly keep the quiet state that stirs; Vacuum breaker is got lollipop appearance and is analyzed full composition, uses the nitrogen pick-up of MnN line.
Line feeding is grasped: according to target be worth according to the appearance result and finely tune, feed the C line behind the adding TiFe, fed and can feed the Al line immediately; Feed then the MnN line (according to N content, 100m=26ppm N, 100m=0.037%Mn); Stir the above feeding of 2min CaFe line: 120m, the back that finishes keeps the above feeding of the quiet 3min of stirring SFe line, and (feed quantity: 1m/t is according to molten steel actual [S]; Get two appearance more than the quiet 3min of stirring and analyze, continue to keep quiet stirring, according to waiting appearance result to continue to finely tune; Finely tune qualified after, get after the finished product appearance continuous casting on the bull ladle; The quiet process of stirring adds heat preserving agent 150kg according to temperature.
The vacuum out-station temperature: the bull ladle reference temperature (℃) continuous casting first stove: 1570, connect and water stove: 1560; VD fine setting composition can allow to return LF adjustment or intensification according to the organization of production situation; T liquid=1490 ℃, middle bag storing time meets the Technology rules requirement of electric furnace factory, best superheating temperature: 25 ℃; CC: continuous casting becomes the 320mm*480mm bloom.
The present invention can also have other embodiment, and the technical scheme that equal replacement of all employings or equivalent transformation form all drops within the scope of requirement protection of the present invention.
Claims (4)
- A 48MnV nitrogenous steel add nitrogen technology, said 48MnV nitrogenous steel comprises following composition: C:0.45～0.51% by weight percentage, Si:0.17～0.37%, Mn:1.00～1.20%; V:0.06～0.11%, Ti:0.000～0.025, Cr:0.05～0.25%; Mo:0.00～0.06%, Ni:0.00～0.06%, Cu:0.00～0.20%; N:0.080～0.0150%, P≤0.035%, S≤0.035%; O≤0.020%, Ceq:0.087～0.097%, surplus is Fe and inevitably is mingled with; It is characterized in that: add nitrogen technology and carry out according to the following steps:Supplementary material examination → batching → electrosmelting → LF refining → VD the degassing → feeding nitrification gold thread → calcium processing → quiet stirring → continuous casting → strand cooling check → blank examination → heating → de-scaling → rolling → cooling in heap → aligning → pickling → reconditioning → chamfered edge → inside and outside flaw detection → inspection after construction → packing indicates → weighs → puts in storage;In the said feeding nitroalloy line procedures, press N 0.0080～0.0150% control, target value 0.0110%, by calculated amount after the vacuum flow process in steel disposable feeding nitrogenized manganese iron wire;The nitrogenized manganese cored-wire composition that said feeding nitrogenized manganese iron wire adopts requires: C≤1.0%, S≤0.03%, N:4.5～6.0%, P≤0.30%, Mn:75.0～80.0%, Si≤2.5, surplus be Fe and with inevitably be mingled with;Said nitrogenized manganese cored-wire iron sheet quality≤180g/m, core opaque amount>=500g/m, every km joint number≤2.
- 2. 48MnV nitrogenous steel as claimed in claim 1 add nitrogen technology, it is characterized in that: electrosmelting: eaf tapping point carbon>=0.10%, P≤0.010%, the freeboard of ladle 660mm is guaranteed in T>=1640 ℃; Add slag charge and steel alloy: Si-Mn:9～12kg in the tapping process in the ladle, compound middle aluminium: 3～4kg, V-Fe:1～1.5kg, lime: 5～6kg, modification refining slag: 3～4kg.
- 3. 48MnV nitrogenous steel as claimed in claim 1 add nitrogen technology, it is characterized in that: the VD degassing:Advance the VD temperature: continuous casting first stove: 1675～1695 ℃, connect and water stove: 1675～1685 ℃; VD composition %:C:0.46, Mn:0.90, Cr:0.13, Si:0.21, Alt:0.020～0.030 are entered in control;Vacuum tightness＜1 millibar maintenance down, hold-time 10～15min, vacuum breaker promptly keep the quiet state that stirs.
- 4. 48MnV nitrogenous steel as claimed in claim 1 add nitrogen technology, it is characterized in that: feeding nitrification gold thread → calcium processing → quiet stirring:According to target be worth according to the appearance result and finely tune, feed the C line after adding TiFe, fed and fed the Al line immediately, feed the MnN line then: according to N content; 100m=26ppm N, 100m=0.037%Mn stirs the above feeding of 2min CaFe line: 80～120m; The above feeding of the quiet 3min of stirring of back maintenance SFe line finishes: feed quantity: 1m/t, get two appearance analyses more than the quiet 3min of stirring, and continue to keep quiet stirring; According to etc. the appearance result continue fine setting, finely tune qualified after, get after the finished product appearance continuous casting on the bull ladle; The quiet process of stirring adds heat preserving agent 100～150kg according to temperature.
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| CN116005070B (en) * | 2022-12-23 | 2024-04-26 | 建龙北满特殊钢有限责任公司 | Production method of non-quenched and tempered steel with nitrogen content adjusted after vacuum |
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| CN101717893A (en) * | 2009-12-15 | 2010-06-02 | 南京钢铁股份有限公司 | 55Si2MnVNbN spring steel and production process thereof |
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Patent Citations (1)
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| CN101717893A (en) * | 2009-12-15 | 2010-06-02 | 南京钢铁股份有限公司 | 55Si2MnVNbN spring steel and production process thereof |
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