CN101921959A - Hot working tool steel and the steel work that uses it to make - Google Patents
Hot working tool steel and the steel work that uses it to make Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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- C21D6/002—Heat treatment of ferrous alloys containing Cr
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D7/00—Modifying the physical properties of iron or steel by deformation
- C21D7/13—Modifying the physical properties of iron or steel by deformation by hot working
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Abstract
The invention provides a kind of hot working tool steel, it contains: 0.20 quality %≤C≤0.50 quality %, 0.01 quality %≤Si＜0.25 quality %, 0.50 quality %＜Mn≤1.50 quality %, 5.24 quality %＜Cr≤9.00 quality %, 1.24 quality %＜Mo＜2.95 quality % and 0.30 quality %＜V＜0.70 quality %, surplus is Fe and unavoidable impurities.The present invention also provides the steel work that utilizes this hot working tool steel to make.Hot working tool steel of the present invention has reliable machinability, guarantees to be processed to mold shape industrial, and compares with general die steel (for example JIS SKD61), and its thermal conductivity and impact value are improved.
Description
Technical field
The steel work that the present invention relates to hot working tool steel and make with it.More particularly, the steel work that the present invention relates to such hot working tool steel and make with it, this hot working tool steel has reliable machinability, guarantee to be processed to mold shape industrial, and compare with general die steel (for example JIS SKD61), its thermal conductivity and impact value are improved.
Background technology
About the moulding stock that die casting, forge hot and warm forging are used, use the JIS SKD61 of machinability excellence usually.Yet the thermal conductivity of JIS SKD61 is low, thereby brings such problem: die temperature is often higher, and owing to continually sticking to mould (soldering) or hot tearing take place, and makes the lost of life of mould.In addition, along with the increase of die size, because the transition temperature height (so-called hardening capacity) that JIS SKD61 changes at low rate of cooling condition lower bainite, so it is difficult to carry out structure refinement, and this can cause toughness significantly to reduce.Therefore, JIS SKD61 has such disadvantage: promoted hot tearing, thereby further shorten the life-span of mould.In this case, a kind of thermal conductivity of industrial needs and impact value all are better than the hot working tool steel of JIS SKD61.
In this respect, the someone has proposed the multiple steel that are suitable for this kind application.
For example, patent documentation 1 discloses a kind of transformation behavior (hardening capacity) and creep properties excellence and hot working tool steel alternative JIS SKD61, this hot working tool steel is to contain the steel of following column element as main component: C:0.30 to 0.38 weight %, Si:0.10 to 0.40 weight %, Mn:0.60 to 0.80 weight %, Cr:5.40 to 5.70 weight %, Mo:1.50 to 1.70 weight %, V:0.70 to 0.85 weight %, surplus is Fe and unavoidable impurities.
[patent documentation 1] JP-A-06-322483 (term used herein " JP-A " is meant " uncensored Japanese Patent Application Publication ")
[patent documentation 2] JP-A-03-000402
[patent documentation 3] JP-A-07-062494
[patent documentation 4] JP-A-60-059053
[patent documentation 5] JP-A-08-100239
[patent documentation 6] JP-A-2008-056982
[patent documentation 7] JP-A-2004-183008
[patent documentation 8] JP-A-2005-307242
[patent documentation 9] JP-A-64-062444
[patent documentation 10] JP-A-2008-121032
Yet disclosed steel are not the steel that can satisfy thermal conductivity and impact value simultaneously that the present invention is devoted to obtain in the patent documentation 1 to 10.
For example, in patent documentation 1, both hint did not disclose its thermal conductivity yet, and may cause impact value to reduce owing to excessive V.
In patent documentation 2, may cause thermal conductivity to reduce owing to excessive Si, perhaps since Mn very little or Cr cause the impact value reduction very little.
In patent documentation 3 to 5, yet do not hint or disclose its thermal conductivity.In patent documentation 3, may cause the insufficient and impact value reduction of transformation behavior (hardening capacity) very little owing to the amount of Mn.In patent documentation 4, may owing to the amount of Cr very little or the amount of V is very few or too much cause impact value to reduce.In patent documentation 5, may cause the insufficient and impact value of transformation behavior (hardening capacity) to reduce owing to the amount of Mn very little, because it is the amount of Mo causes hot strength to reduce very little, perhaps very few or too much cause the impact value reduction owing to the amount of V.
In patent documentation 6 to 8, may be owing to the very few transformation behavior that causes of the amount of Cr
(hardening capacity) deterioration or hardness or impact value reduce.
In patent documentation 9 and 10, may cause thermal conductivity to reduce owing to excessive Si, perhaps the amount of Cr is very few and cause impact value to reduce.
Summary of the invention
The present invention makes under these situations of consideration, the steel work that an object of the present invention is to provide such hot working tool steel and make with it, this hot working tool steel has reliable machinability, guarantee to be processed to mold shape industrial, and compare with general die steel (for example JIS SKD61), its thermal conductivity and impact value are improved.
General die steel (JIS SKD61) is though have excellent machinability, and its thermal conductivity and impact value are lower.Therefore, the inventor has carried out deep research so that thermal conductivity and impact value are increased to thermal conductivity and the impact value that is higher than general die steel, and keep simultaneously can be in the industrial machinability that is processed to mold shape.Found that,, can improve impact value by amount, the amount of Cr, the amount of Mo and the amount of V of regulating Mn simultaneously by the amount of Si being set to such an extent that can improve thermal conductivity than low.Finished the present invention based on these discoveries.
To achieve these goals, the invention provides a kind of hot working tool steel, comprise:
0.20 quality %≤C≤0.50 quality %,
0.01 quality %≤Si＜0.25 quality %,
0.50 quality %＜Mn≤1.50 quality %,
5.24 quality %＜Cr≤9.00 quality %,
1.24 quality %＜Mo＜2.95 quality %, and
0.30 quality %＜V＜0.70 quality %,
Surplus is Fe and unavoidable impurities.
Herein, the example of unavoidable impurities comprises: W＜0.30 quality %, Co＜0.30 quality %, Nb＜0.004 quality %, Ta＜0.004 quality %, Ti＜0.004 quality %, Zr＜0.004 quality %, Al＜0.004 quality %, N＜0.004 quality %, Cu＜0.15 quality %, Ni＜0.15 quality %, B＜0.0010 quality %, S＜0.010 quality %, Ca＜0.0005 quality %, Se＜0.03 quality %, Te＜0.005 quality %, Bi＜0.01 quality %, Pb＜0.03 quality %, Mg＜0.005 quality %, and O＜0.0080 quality %.
Described hot working tool steel of the present invention also can comprise:
0.30 quality %≤W≤4.00 quality %.
Described hot working tool steel of the present invention also can comprise:
0.30 quality %≤Co≤3.00 quality %.
Described hot working tool steel of the present invention also can comprise at least a element that is selected from the group of being made up of following column element:
0.004 quality %≤Nb≤0.100 quality %,
0.004 quality %≤Ta≤0.100 quality %,
0.004 quality %≤Ti≤0.100 quality %,
0.004 quality %≤Zr≤0.100 quality %,
0.004 quality %≤Al≤0.050 quality %, and
0.004 quality %≤N≤0.050 quality %.
Described hot working tool steel of the present invention also can comprise at least a element that is selected from the group of being made up of following column element:
0.15 quality %≤Cu≤1.50 quality %,
0.15 quality %≤Ni≤1.50 quality %, and
0.0010 quality %≤B≤0.0100 quality %.
Described hot working tool steel of the present invention also can comprise at least a element that is selected from the group of being made up of following column element:
0.010 quality %≤S≤0.500 quality %,
0.0005 quality %≤Ca≤0.2000 quality %,
0.03 quality %≤Se≤0.50 quality %,
0.005 quality %≤Te≤0.100 quality %,
0.01 quality %≤Bi≤0.30 quality %, and
0.03 quality %≤Pb≤0.50 quality %.
Hot working tool steel of the present invention thermal conductivity at room temperature is preferably more than or equals 28W/m/K.
Steel work of the present invention has used described hot working tool steel of the present invention.
Term used herein " steel work " is meant (for example) transfer mold, hot forged mould or warm forging mould, but the present invention is not limited thereto.
Hot working tool steel of the present invention and use the steel work of this hot working tool steel manufacturing to have above-mentioned one-tenth to be grouped into, therefore it has produced such effect: keep can industrial be processed to the machinability of mold shape in, compare with general die steel (for example JISSKD61), it guarantees to have high thermal conductivity and high impact value.
That is to say, amount to Si in hot working tool steel of the present invention is optimized, produced such effect thus: keep can industrial be processed to the machinability of mold shape in, compare with general die steel (for example JIS SKD61), it guarantees to have higher thermal conductivity.In addition, in described hot working tool steel, the amount of Mn, the amount of Cr, the amount of Mo and the amount of V are optimized, produced such effect thus: it is low and have a high impact value to change the transition temperature of (so-called hardening capacity) at low rate of cooling condition lower bainite.Therefore, hot working tool steel of the present invention can cause sticking to mould or hot tearing hardly, thereby can obtain long die life and reduce production cost, and the productivity can improve die casting, forge hot and/or warm forging the time.
Brief Description Of Drawings
Fig. 1 is the figure that the relation between machinability and the Si content is shown.
Fig. 2 is the figure that the relation between thermal conductivity and the Si content is shown.
Fig. 3 is the figure that the relation between impact value and the Mn content is shown.
Fig. 4 is the figure that the relation between thermal conductivity and the Mn content is shown.
Fig. 5 is the figure that the relation between impact value and the Cr content is shown.
Fig. 6 is the figure that the relation between thermal conductivity and the Cr content is shown.
Fig. 7 is the intensity (hot strength) when illustrating 600 ℃ and the figure of the relation between the Mo content.
Fig. 8 is the figure that the relation between impact value and the V content is shown.
Embodiment
Describe below according to hot working tool steel of one embodiment of the invention and the steel work that uses this hot working tool steel to make.
(one-tenth of hot working tool steel is grouped into and limits reason)
The hot working tool steel of the present embodiment contains down, and column element is Fe and unavoidable impurities as principal element: C, Si, Mn, Cr, Mo and V, surplus.Hot working tool steel according to the present embodiment contains (for example) W, Co, Nb, Ta, Ti, Zr, Al, N, Cu, Ni, B, S, Ca, Se, Te, Bi, Pb, Mg and O as unavoidable impurities.Herein, in this manual, all mass percents are identical with weight percent respectively.
(1) 0.20 quality %≤C≤0.50 quality %
C is the required principal element of intensity of regulating steel.If the amount of C is lower than 0.20 quality %, be difficult to obtain needed hardness, yet if the amount of C is higher than 0.50 quality %, then hardness is tending towards saturated more than or equal to 36HRC, the quantitative change of carbide simultaneously gets too much, thereby makes fatigue strength or impact value deterioration.Therefore, the amount with C is set at 0.20 quality %≤C≤0.50 quality %.In order to obtain excellent balance between hardness, fatigue strength and impact value, the amount of C is preferably 0.24 quality %≤C≤0.46 quality %, more preferably 0.28 quality %≤C≤0.42 quality %.
(2) 0.01 quality %≤Si＜0.25 quality %
Si is machinability and the required principal element of thermal conductivity of regulating steel.If the amount of Si is lower than 0.01 quality %, thereby then the remarkable deterioration of machinability is very difficult to be processed into the shape of mould.If the amount of Si is 0.25 quality % or higher, then thermal conductivity significantly reduces.Therefore, the amount with Si is set at 0.01 quality %≤Si＜0.25 quality %.The amount of Si is preferably Si≤0.20 quality %, Si＜0.10 quality % more preferably, and this can obtain high thermal conductivity.
(3) 0.50 quality %＜Mn≤1.50 quality %
Mn is the principal element that is used to improve transformation behavior (hardening capacity).If the amount of Mn is less than or equal to 0.50 quality %, then reduce transformation temperature and make the effect of structure refinement insufficient, therefore be difficult to guarantee hardness or impact value.If the amount of Mn surpasses 1.50 quality %, not only impact value greatly reduces, and almost can not keep high thermal conductivity.Therefore, the amount with Mn is set at 0.50 quality %＜Mn≤1.50 quality %.The amount of Mn is preferably 0.66 quality %＜Mn≤1.20 quality %, and this can guarantee hardness and impact value, can obtain high thermal conductivity simultaneously.
(4) 5.24 quality %＜Cr≤9.00 quality %
Cr be used to improve transformation behavior (hardening capacity), simultaneously by forming the principal element that carbide improves hardness of steel.If the amount of Cr is less than or equal to 5.24 quality %, then reduces transformation temperature and make the effect of structure refinement insufficient, thereby be difficult to obtain sufficient hardness and impact value.In addition, along with the amount increase of Cr, erosion resistance also increases, and this is that the die casting that is exposed in the corrosive atmosphere is required.On the other hand, if the amount of Cr surpasses 9.00 quality %, then be difficult to the thermal conductivity that keeps high.Therefore, the amount with Cr is set at 5.24 quality %＜Cr≤9.00 quality %.In addition, the amount of Cr is preferably 5.40 quality %＜Cr≤7.00 quality %, 5.55 quality %≤Cr≤6.50 quality % more preferably, and this can guarantee hardness, impact value and erosion resistance, can obtain high thermal conductivity simultaneously.
(5) 1.24 quality %＜Mo＜2.95 quality %
Mo is not only and improves transformation behavior (hardening capacity) and be to improve the principal element of hardness of steel (especially improving hot strength) by forming carbide.If the amount of Mo is less than or equal to 1.24 quality %, can not obtain gratifying hot strength, yet if the amount of Mo more than or equal to 2.95 quality %, then hot strength is tending towards saturated, simultaneously cost significantly improves and makes earning rate impaired.Therefore, the amount with Mo is set at 1.24 quality %＜Mo＜2.95 quality %.In addition, the amount of Mo is preferably 1.37 quality %＜Mo≤2.80 quality %, more preferably 1.50 quality %≤Mo≤2.50 quality %.
(6) 0.30 quality %＜V＜0.70 quality %
V is not only and improves transformation behavior (hardening capacity) and be to improve the principal element of hardness of steel (especially improving hot strength) by forming carbide.If the amount of V is less than or equal to 0.30 quality %, thereby the easy roughening of austenite particle has reduced impact value when quenching, yet if the amount of V more than or equal to 0.70 quality %, the amount of coarse carbide is too much, this can make the impact value deterioration.Therefore, the amount with V is set at 0.30 quality %＜V＜0.70 quality %.In addition, the amount of V is preferably 0.40 quality %≤V≤0.67 quality %, 0.50 quality %≤V≤0.64 quality % more preferably, and this can guarantee softening resistance, obtains satisfied fatigue strength and impact value simultaneously.
(7) unavoidable impurities:
W＜0.30 quality %, Co＜0.30 quality %, Nb＜0.004 quality %, Ta＜0.004 quality %, Ti＜0.004 quality %, Zr＜0.004 quality %, Al＜0.004 quality %, N＜0.004 quality %, Cu＜0.15 quality %, Ni＜0.15 quality %, B＜0.0010 quality %, S＜0.010 quality %, Ca＜0.0005 quality %, Se＜0.03 quality %, Te＜0.005 quality %, Bi＜0.01 quality %, Pb＜0.03 quality %, Mg＜0.005 quality %, O＜0.0080 quality %, etc.
Respectively under the situation in above-mentioned scope, these elements are involved as unavoidable impurities in the amount of W, Co, Nb, Ta, Ti, Zr, Al, N, Cu, Ni, B, S, Ca, Se, Te, Bi, Pb, Mg, O etc.
Also can contain down column element as selectable element according to the hot working tool steel of the present embodiment:
(a)W，
(b)Co，
(c) be selected from least a element in the group of forming by Nb, Ta, Ti, Zr, Al and N,
(d) be selected from least a element in the group of forming by Cu, Ni and B, and/or,
(e) be selected from least a element in the group of forming by S, Ca, Se, Te, Bi and Pb.
(8) 0.30 quality %≤W≤4.00 quality %
W is the selective element that can add, to improve intensity (precipitation hardening) by carbide precipitate.If the amount of W is less than 0.30 quality %, the effect that then improves intensity is less, and if the amount of W surpasses 4.00 quality %, this can cause the effect of described raising intensity saturated and can cause cost to significantly improve.Therefore, the amount with W is set at 0.30 quality %≤W≤4.00 quality %.
(9) 0.30 quality %≤Co≤3.00 quality %
Co is the selective element that can add, to improve intensity (solution hardening) by the sosoloid in the matrix.If the amount of Co is less than 0.30 quality %, the effect that then improves intensity is less, and if the amount of Co surpasses 3.00 quality %, this can cause the effect of described raising intensity saturated and cause cost to significantly improve.Therefore, the amount with Co is set at 0.30 quality %≤Co≤3.00 quality %.
(10) be selected from by at least a element in the group of descending column element to form:
0.004 quality %≤Nb≤0.100 quality %,
0.004 quality %≤Ta≤0.100 quality %,
0.004 quality %≤Ti≤0.100 quality %,
0.004 quality %≤Zr≤0.100 quality %,
0.004 quality %≤Al≤0.050 quality %, and
0.004 quality %≤N≤0.050 quality %.
Nb, Ta, Ti, Zr, Al and N are the selective elements that can be added, and improve intensity and toughness with the austenite particle (grain refining) when quenching.For all these elements, if its addition is less than predetermined amount, then improve intensity and the flexible effect is less, and if its addition surpasses predetermined amount, then produce excessive carbide, nitride or oxide compound, and this can cause toughness to reduce.
(11) be selected from by at least a element in the group of descending column element to form:
0.15 quality %≤Cu≤1.50 quality %,
0.15 quality %≤Ni≤1.50 quality %, and
0.0010 quality %≤B≤0.0100 quality %.
Cu, Ni and B are the selective elements that can be added, to improve transformation behavior (hardening capacity).For all these elements, if its addition is less than predetermined amount, the effect of then improving transformation behavior (hardening capacity) is less, and if its addition surpasses predetermined amount, the then described effect of improving is saturated, and practical benefits is less.Particularly, for Cu and Ni,, can cause that thermal conductivity reduces if the amount that adds is too much.
(12) be selected from by at least a element in the group of descending column element to form:
0.010 quality %≤S≤0.500 quality %,
0.0005 quality %≤Ca≤0.2000 quality %,
0.03 quality %≤Se≤0.50 quality %,
0.005 quality %≤Te≤0.100 quality %,
0.01 quality %≤Bi≤0.30 quality %, and
0.03 quality %≤Pb≤0.50 quality %.
S, Ca, Se, Te, Bi and Pb are the selective elements that can be added into, to improve machinability (mechanical workout property improvement).For all these elements, if its addition is less than predetermined amount, the effect that then improves machinability is less, and if its addition surpasses predetermined amount, then thereby the remarkable deterioration of hot workability causes the living crack of frequent real estate when plastic working, so productivity and output reduction.
In this respect, about each element that is contained in the steel of the present invention, according to an embodiment, the minimum quantity that they exist in steel be developed as table 1 and table 2 in employed smallest non-zero quantity in the example of the steel of being summed up.According to further embodiment, the maximum amount that they exist in steel be developed as table 1 and table 2 in employed maximum in the example of the steel of being summed up.
(preparation method)
For example, can obtain the steel of this embodiment, but the present invention is not limited thereto by following operation.
(1) casting
Raw material is mixed to obtain above-mentioned predetermined composition,, and in mold, melt is cast to obtain steel ingot this raw materials melt.
(2) thermal treatment/hot-work that homogenizes
Homogenize thermal treatment and hot-work so that the composition of the steel ingot that is obtained homogenize and destroy as-cast structure.About thermal treatment and the hot worked condition of homogenizing, preferably assign to select to be used for the top condition of each processing according to each one-tenth.
Usually by steel ingot is kept the thermal treatment that homogenizes in about 10 to 30 hours down at 1,100 ℃ to 1,500 ℃.
Usually under 1,000 ℃ to 1,300 ℃, carry out hot-work, and after machining, steel ingot is carried out air cooling.
(3) tempering/Spheroidizing Annealing/roughing
Steel according to the present embodiment have transformation behavior (hardening capacity) relatively preferably, therefore, because bainitic transformation or martensitic transformation have taken place, after hot-work, the hardening when being everlasting air cooling of these steel.Therefore, preferably,, make this material softening by after described hot-work, carrying out tempering and Spheroidizing Annealing, carrying out roughing then.
About the tempered condition, preferably assign to select optimal conditions according to each one-tenth.Usually by this material is kept carrying out in about 1 to 10 hour tempering down at 600 to 750 ℃.
Preferably carry out Spheroidizing Annealing so that the hardness of steel is approximately 90 to 97HRB.Usually by with described material 800 to 950 ℃ keep down about 1 to 10 hour, with 5 to 30 ℃ speed per hour it is cooled off and carries out Spheroidizing Annealing then.
Be processed into predetermined shape by the material mechanical after will softening and carry out roughing.
(4) thermal treatment (quenching/tempering)
Heat-treat so that the material after the roughing is adjusted to required hardness.About quenching conditions and tempered condition, preferably select to be used for the top condition that each is handled according to each composition and required characteristic.
Usually pass through fast it to be cooled off with the maintenance 0.5 to 5 hour under 1,000 to 1,050 ℃ of described material, then and quench.Rapid cooling method is had no particular limits, preferably select the best approach according to purpose.The example of method for rapid cooling comprises water-cooled, oil cooling and air blowing cooling.
Usually by described material is kept carrying out in 1 to 10 hour tempering down at 500 to 650 ℃.
Pass through above-mentioned step (1) to (4), can obtain such steel, these steel keep can industrial be processed to the machinability of mold shape in, compare with general die steel (for example JIS SKD61), it can guarantee high thermal conductivity and high impact value.
(5) precision work
The material that is heat-treated to required hardness is carried out precision work.
Through step (5), the steel work made from regard to the hot working tool steel that has obtained adopting the present embodiment.
(operating method)
In the hot working tool steel according to the present embodiment, the amount of Si is optimised, make these steel keep can industrial be processed to the machinability of mold shape in, have than the high thermal conductivity of general die steel (for example JIS SKD61).And in the hot working tool steel according to the present embodiment, the amount of the amount of Mn, the amount of Cr, Mo, the amount of V etc. are also optimised, make the transformation behavior of these steel can improve and have high impact value.Therefore, the hot working tool steel according to the present embodiment can cause sticking to mould or hot tearing hardly.As a result, the life-span of mould prolongs, and in die casting or heat is forged and/or the preparation cost of temperature when forging can reduce and productivity can improve.
Embodiment
(embodiment A)
In order to make each steel of the present invention among the following examples B, carry out embodiment 1 to 5 to study preferred Si amount, Mn amount, Cr amount, Mo amount and V amount.
(embodiment 1:Si Study on content)
The preferred amounts of Si is studied and is described with reference to figure 1 and Fig. 2.
When Fig. 1 shows the steel that is made of the Si of the V of Mo, the 0.62 quality % of Cr, the 1.63 quality % of Mn, the 5.73 quality % of C, the 0.82 quality % of 0.33 quality % and x quality % in cutting, with respect to the amount of Si, adopt cutting tool to process the distance of when its end-of-life, being cut.In Fig. 1, about the numerical value on each graphical pointv, the distance (mm) that the numeric representation x value (quality %) of upside, the numeric representation of downside are cut.The sample that is used to estimate machinability is that (it is to make according to the operation identical with Embodiment B to the square bar of 55mm * 55mm * 200mm, and by Spheroidizing Annealing with its softening to hardness be 90 to 97HRB), the time when the greatest wear amount on the splaying face of cutting tool is reached 300 μ m is judged as the terminal point in its life-span.The distance of being cut is big more, and the expression processibility is good more, thereby is preferred.
According to Fig. 1, along with the increase of the amount of Si, the distance of being cut also increases, and therefore, considers that from the viewpoint of improving machinability preferably the amount of Si is bigger.According to Fig. 1, when the amount of Si during less than 0.01 quality %, the distance of being cut is extremely short, so in order to ensure machinability, suitable is that the amount of Si is more than or equal to 0.01 quality %.According to Fig. 1, when the amount of Si was 0.01 to 0.24 quality % (less than 0.25 quality %), the effect of improving machinability was very remarkable, and when the amount of Si surpassed 0.24 quality %, the effect of improving machinability slowed down.
Will by use with Fig. 1 in the pole of Φ 11mm * 50mm of making of identical materials 1,030 ℃ of heating down, by quick cooling and tempering it is handled hardness to 48HRC then.Make the sample of the Φ 10mm * 2mm that is used to measure thermal conductivity by this pole.Fig. 2 shows the thermal conductivity at room temperature measured by the laser scintillation method and the relation of Si content.In Fig. 2, about the numerical value on each graphical pointv, the numeric representation x value (quality %) of upside and the numeric representation thermal conductivity (W/m/K) of downside.Thermal conductivity is high more, represents that the cooling power of formed mould is high more, thereby is preferred.
According to Fig. 2, increase along with Si content, thermal conductivity reduces, but when the content of Si surpasses 0.09 quality % (less than 0.10 quality %), can obtain the thermal conductivity more than or equal to 28W/m/K, this makes its cooling power be significantly higher than general die steel (JIS SKD61 (thermal conductivity: 24W/m/K)).Incidentally, according to Fig. 2, when the content of Si is 0.007 to 0.09 quality %, can obtain high like this thermal conductivity more than or equal to 30.7W/m/K, and when the content of Si is 0.09 to 0.24 quality %, can obtain good like this thermal conductivity more than or equal to 28.1W/m/K.
In view of keep can be in the industrial machinability that is processed to mold shape, the content of Si can be less than 0.25 quality %.
(embodiment 2:Mn Study on content)
The preferred content of Mn is studied and is described with reference to figure 3 and Fig. 4.
Fig. 3 has drawn out the situation of steel impact value at room temperature with respect to the content of Mn, and described steel are made of the V of Mo, the 0.60 quality % of Cr, the 1.60 quality % of Si, the 5.75 quality % of C, the 0.08 quality % of 0.33 quality % and the Mn of x quality %.In Fig. 3, about the numerical value on each graphical pointv, the numeric representation x value (quality %) of upside and the numeric representation impact value (J/cm of downside
2).The sample that is used to estimate impact value is that (it is to make according to the operation identical with Embodiment B to the square bar of 11mm * 11mm * 55mm, and by Spheroidizing Annealing with its softening to hardness be 90 to 97HRB), with it 1,030 ℃ of down heating is handled hardness to 49HRC by quick cooling and tempering with it then.Make the JIS No.3 Impact Test sample of 10mm * 10mm * 55mm by above-mentioned square bar, and be used to measure impact value.Impact value is big more, represents that the resistance to fracture of formed mould is high more, thereby is preferred.
According to Fig. 3, can know that when the content of Mn was 0.45 quality % and 0.55 quality %, the impact value that is obtained was more than or equal to 30J/cm
2Therefore, be to be located at the lower limit that 0.50 quality % between 0.45 quality % and the 0.55 quality % is considered as Mn content with the content of Mn.In addition, according to Fig. 3, when the content of Mn during more than or equal to 0.7 quality %, the impact value that is obtained is more than or equal to 34.5J/cm
2Therefore, can the situation when containing this element that surpasses 0.66 quality % (this numerical value is between 0.55 quality % and 0.7 quality %) select as embodiment preferred.Yet as seen from Figure 3, when the content of Mn surpassed 1.50 quality %, though the numerical value of impact value still remains on good horizontal, impact value had reduced.
Fig. 4 drawn out with Fig. 3 in identical materials thermal conductivity at room temperature with respect to the situation of the content of Mn.In Fig. 4, about the numerical value on each graphical pointv, the numeric representation x value (quality %) of upside and the numeric representation thermal conductivity (W/m/K) of downside.By with embodiment 1 in the similar laser flickering method measure thermal conductivity.
According to Fig. 4, along with the increase of Mn content, thermal conductivity reduces, and when Mn content surpasses 1.50 quality %, do not obtain more than or equal to 28W/m/K thermal conductivity (with the thermal conductivity of JISSKD61: 24W/m/K compares, and this thermal conductivity makes cooling power significantly improve).According to Fig. 4, in order to obtain the thermal conductivity more than or equal to 28W/m/K, the content of Mn can be less than or equal to 1.50 quality %, and in order to obtain the thermal conductivity more than or equal to 29W/m/K, the content of Mn can be less than or equal to 1.20 quality %.
(embodiment 3:Cr Study on content)
The preferred content of Cr is studied and is described with reference to figure 5 and Fig. 6.
Fig. 5 has drawn out the situation of steel impact value at room temperature with respect to the content of Cr, described steel constitute by the Cr of the V of Mo, the 0.61 quality % of Mn, the 1.62 quality % of Si, the 0.84 quality % of C, the 0.08 quality % of 0.33 quality % and x quality % and handled to hardness be 49HRC.In Fig. 5, about the numerical value on each graphical pointv, the numeric representation x value (quality %) of upside and the numeric representation impact value (J/cm of downside
2).Prepare sample and measure impact value according to the mode identical with embodiment 2.
According to Fig. 5, along with the increase of Cr content, impact value also increases.Especially, when the content of Cr surpassed 5 quality %, the effect of this element was remarkable.Be understandable that by Fig. 5, in order to obtain more than or equal to 27.8J/cm
2Impact value, the content of Cr can be higher than 5.24 quality %.Therefore, in view of guaranteeing impact value, can be 5.24 quality % or higher with the lower limit set of Cr content.In addition, according to Fig. 5, when the content of Cr was lower than 5 quality %, impact value significantly reduced.
Fig. 6 has drawn out the situation of steel thermal conductivity at room temperature with respect to the content of Cr, and described steel are made of the V of Mo, the 0.61 quality % of Mn, the 1.62 quality % of Si, the 0.52 quality % of C, the 0.22 quality % of 0.22 quality % and the Cr of x quality %.In Fig. 6, about the numerical value on each graphical pointv, the numeric representation x value (quality %) of upside and the numeric representation thermal conductivity (W/m/K) of downside.By with embodiment 1 in the similar laser flickering method measure thermal conductivity.
According to Fig. 6, along with the increase of Cr content, thermal conductivity reduces.According to Fig. 6, for obtain more than or equal to 27.5W/m/K thermal conductivity (with the thermal conductivity of JIS SKD61: 24W/m/K compares, this thermal conductivity makes cooling power improve), the content of Cr can be more than or equal to 9.00 quality %, in order to obtain thermal conductivity (this thermal conductivity makes cooling power significantly improve) more than or equal to 30.1W/m/K, the content of Cr can be less than or equal to 7.00 quality %, and in order to obtain the thermal conductivity more than or equal to 31W/m/K, the content of Cr can be less than or equal to 6.50 quality %.
(embodiment 4:Mo Study on content)
The preferred content of Mo is studied and is described with reference to figure 7.
Fig. 7 shows the situation of the hot strength (resistance to deformations in the time of 600 ℃) of steel with respect to the content of Mo, and described steel are made of the V of Cr, the 0.59 quality % of Mn, the 5.74 quality % of Si, the 0.83 quality % of C, the 0.07 quality % of 0.33 quality % and the Mo of x quality %.In Fig. 7, about the numerical value on each graphical pointv, the numeric representation x value (quality %) of upside and the numeric representation hot strength (MPa) of downside.The sample that is used to measure resistance to deformation is that (it is to make according to the operation identical with Embodiment B to the pole of Φ 15mm * 50mm, and by Spheroidizing Annealing with its softening to hardness be 90 to 97HRB), with it 1,030 ℃ of down heating is handled hardness to 45HRC by quick cooling and tempering with it then.Make the sample of the Φ 14mm * 21mm that is used to measure resistance to deformation by this pole.With this sample with 5 ℃/second speed be heated to 600 ℃ and keep 100 seconds after, be 10 seconds in strain rate
-1Condition under it is processed to measure resistance to deformation.
Term used herein " resistance to deformation " is the power of instigating on the required per unit area of material deformation.More specifically, " resistance to deformation " expression is by K
f=p
w/ a
wDetermined K
f, p wherein
wFor with 10 seconds
-1The strain rate process of processing in power, and a
wExpression and the vertical contact area of this power (hereinafter, the implication of used " resistance to deformation " is with identical herein).
The resistance to deformation that records in this way is defined as intensity (hot strength) under 600 ℃, and with the content drawing (see figure 7) of this resistance to deformation with respect to Mo.Resistance to deformation is high more, and expression intensity is high more, and wearing and tearing are just low more conversely, thereby are preferred.
According to Fig. 7, along with the raising of Mo content, hot strength also improves thereupon.Especially, when the content of Mo is higher than 1.24 quality %, the raising of hot strength make it possible to obtain higher degree hot strength (＞970MPa).According to Fig. 7, when the content of Mo for being higher than 1.24 quality % and during less than 3 quality %, the raising of hot strength slows down, and when the content of Mo during more than or equal to 3 quality %, the raising of hot strength reaches capacity.According to Fig. 7, in order to obtain hot strength more than or equal to 971MPa, the content of Mo can be higher than 1.24 quality %, in order to obtain hot strength more than or equal to 974MPa, the content of Mo can be higher than 1.37 quality %, and in order to obtain the hot strength more than or equal to 977MPa, the content of Mo can be more than or equal to 1.50 quality %.Yet the content of Mo can cause cost to significantly improve during more than or equal to 2.95 quality %.Therefore, consider to reduce production costs that the content of Mo preferably is lower than 2.99 quality %, more preferably be less than or equal to 2.80 quality %, further be more preferably less than or equal 2.50 quality %.
(embodiment 5:V Study on content)
The preferred content of V is studied and is described with reference to figure 8.
Fig. 8 shows the situation of the impact value of steel with respect to the content of V, and described steel constitute, also have been processed to 48HRC by the Mo of Cr, the 1.63 quality % of Mn, the 5.75 quality % of Si, the 0.82 quality % of C, the 0.09 quality % of 0.34 quality % and the V of x quality %.In Fig. 8, about the numerical value on each graphical pointv, the numeric representation x value (quality %) of upside and the numeric representation impact value (J/cm of downside
2).Prepare sample and measure impact value according to the mode identical with embodiment 2.
According to Fig. 8, when the content of V changes,, all obtain good impact value (20J/cm between 0.1 quality % to 1 quality % no matter how much content of V is
2Perhaps higher).According to Fig. 8, V content be 0.30 quality % near and V content be 0.70 quality % near flex point appears.Therefore, be higher than 0.30 quality % when being lower than 0.70 quality %, be considered to help to improve transformation behavior (hardening capacity) and can realize the high strength of steel by forming carbide when the content with V is set at.On the other hand, according to Fig. 8, when the content of V was less than or equal to 0.30 quality %, impact value significantly reduced, and when the content of V during more than or equal to 0.70 quality %, except impact value reduced, the increase of material cost also can become problem.Therefore, the content of V is preferably 0.30 quality %＜V＜0.70 quality %.According to Fig. 8, in order to obtain more than or equal to 31J/cm
2Impact value, the content of V can be for more than or equal to 0.40 quality %, and in order to obtain more than or equal to 34J/cm
2Impact value, the content of V can be for more than or equal to 0.50 quality %.
(Embodiment B)
Based on the result of study of embodiment A, made steel of the present invention and contrasted and estimated with steel and to them, as described below.
(manufacturing of sample and die casting)
About the embodiment shown in table 1 and the table 2 and comparative example (contrast is JISSKD61 with steel A 10),, and melt cast in mold to obtain 6 tons of steel ingots the fusion in a vacuum of each steel part.
With the processing that under 1,240 ℃, homogenizes of resulting steel ingot.Then, forging the manufacturing cross section by heat is the rectangular block of 310mm * 660mm.
Subsequently, under 700 ℃,, be heated to 900 ℃ and cooling gradually then with this rectangular block tempering, thus make this rectangular block softening to hardness be 90 to 97HRB.By the die casting of resulting rectangular block processing into about 700kg.
With this die casting be heated in a vacuum 1,030 ℃ and kept 1 hour after, make its quenching by spraying nitrogen.By under 580 to 610 ℃, carrying out tempering the hardness of this die casting is handled to about 42HRC then.
After thermal treatment, cut different sample down from this die casting.In addition, this die casting is carried out precision work, thereby make the die casting of about 650kg.
(measurement of fundamental characteristics and evaluation)
Its fundamental characteristics (hot strength, thermal conductivity, impact value, erosion resistance, cost) is measured and estimated to use from the sample that die casting cuts down.
Measure hot strength in the following manner.Cut down the sample of Φ 14mm * 21mm from die casting.With the sample that obtained with 5 ℃/second speed be heated to 600 ℃ and kept 100 seconds after, be 10 seconds in strain rate then
-1Condition under it is processed to measure resistance to deformation.The results are shown in table 3.
Measure thermal conductivity in the following manner.Cut down the sample of Φ 10mm * 2mm from die casting, and at room temperature measure the thermal conductivity of the sample that is obtained by the laser flickering method.The results are shown in table 3.
Measure impact value in the following manner.Cut down the JIS No.3 Impact Test sample of 10mm * 10mm * 55mm from die casting, and at room temperature measure the impact value of this sample.The results are shown in table 3.
Measure erosion resistance in the following manner.Cut down sample from die casting, be equipped with the hole in this sample, and make the flow through inside 72 hours in this hole of 45 ℃ process water with 3.5 liters/minute speed.After making the current warp, with the naked eye estimate the generating state of iron rust on the internal surface in hole.The results are shown in table 3.
Table 3
Fundamental characteristics
(evaluation of fundamental characteristics)
When hot strength is 970MPa or is decided to be " good " (being expressed as " A " in table 3) when higher, otherwise then be decided to be " poor " (in table 3, being expressed as " B ").When thermal conductivity is 28W/m/K or is decided to be " good " (being expressed as " A " in table 3) when higher, otherwise then be decided to be " poor " (in table 3, be expressed as " C ", but when the thermal conductivity value approaches 28W/m/K, then be expressed as " B ").When impact value is higher than 20J/cm
2Shi Dingwei " good " (being expressed as " A " in table 3) otherwise then is decided to be " poor " (being expressed as " B " in table 3).
Steel of the present invention all demonstrate good characteristic in all items.In addition, though the machinability of steel of the present invention slightly is worse than general die steel (JIS SKD61), this machinability is in the industrial level that can be processed to mold shape, thereby can not have problems.Incidentally, by to die casting when the actual cut working (machining) efficiency and the wearing and tearing of cutting tool judge, estimate machinability thus.When the steel to the machinability difference cut, cutting tool causes local heel and toe wear easily or produces chip, this can reduce working (machining) efficiency inevitably owing to will change cutting tool continually, and this can raise the cost inevitably owing to will use a large amount of cutting tools.Compare with the steel that routine is general, working (machining) efficiency abrasion loss poor slightly or cutting tool is bigger when cutting steel of the present invention, but the bad degree of this change is not remarkable, and, confirmablely be, in the Mould Machining of reality, the machinability of steel of the present invention is industrial no problem.
Surpass in the steel of the present invention of 30W/m/K in its thermal conductivity, the content of Si is that the content of 0.04 to 0.09 quality %, Mn is that 0.70 to 1.15 quality % is (except steel A12 of the present invention, other is 0.70 to 0.95 quality %) and the content of Cr be that 5.55 to 6.06 quality % are (except steel A08 of the present invention, other is 5.55 to 5.89 quality %, and further, except steel A12 of the present invention, other is 5.64 to 5.89 quality %).
In its impact value more than or equal to 35J/cm
2Steel of the present invention in, the content of Mn is that 0.52 to 1.31 quality % is (except steel A05 of the present invention, other is 0.70 to 1.31 quality %), the content of Cr is that 5.25 to 6.28 quality % are (except steel A05 of the present invention, other is 5.71 to 6.28 quality %) and the content of V be 0.61 to 0.69 quality % (except steel A05 of the present invention, other is 0.61 to 0.66 quality %).
On the other hand, under the situation of contrast with steel A10, except cost, other all items all is evaluated as " poor ".Used sample is the sample that cuts down from big die casting (its quench rates is reduced).Therefore, contrast is low especially with the impact value of steel A10.
Other contrasts are compared with steel A10 (JISSKD61) much better in some assessment item with steel, but the none steel part all is cited as " good " in all items.
For example, use among the steel A01 in contrast, because the content of C is too low, its hot strength reduces.In addition, because the content of V hangs down austenite particle generation roughening when causing quenching excessively, and impact value reduces.
Than using among the steel A02, because the content of Si is too much, its thermal conductivity reduction.In addition, use among the steel A02 in contrast, because the content of C content too much or V too much causes the amount of carbide excessive, and impact value reduces.
Use among the steel A03 in contrast, because the content of Si too much causes thermal conductivity to reduce.
Use among the steel A04 in contrast, cause the hardenability deficiency, and impact value reduces because the content of Mn is too low.Contrast uses the thermal conductivity of steel A04 a little less than steel of the present invention.Its reason it is believed that and is: contrast is relatively large with the Si content among the steel A04, and contrast is with the composition of steel A04 balance not too on the whole.
Use among the steel A05 in contrast, because the too high levels of Mn causes its thermal conductivity to reduce.
With among the steel A06,, under the low condition of rate of cooling, make the effect of effect that transformation temperature reduces and structure refinement insufficient, and impact value reduce in contrast because the content of Cr is too low.
Use among the steel A07 in contrast, because Cr too much causes thermal conductivity to reduce.
Use among the steel A08 in contrast, because Mo causes hot strength to reduce very little.
Use among the steel A09 in contrast, because Mo too much causes cost to significantly improve.
Use among the steel A10 in contrast, because Si too much causes thermal conductivity to reduce.In addition, because Mo causes contrasting the hot strength reduction with steel A10 very little.And, use among the steel A10 in contrast, because V too much causes carbonitride too much, and impact value reduces.
(real machine test that utilizes die casting to carry out)
According to following manner, utilize die casting to carry out real machine test.Prepared die casting is installed in the machine, and aluminium alloy is cast.ADC 12 is used as aluminium alloy, and the temperature of fusion and holding furnace is set at 680 ℃.The weight of die casting product is about 7kg, and a circulation is 60 seconds.After casting 10,000 times, the corrosion failure of hot tearing on the die surface and internal cooling circuit is estimated.In addition, also will be to when finishing 10,000 castings, whether owing to breaking of internal cooling circuit causes tangible sticking to mould or leak estimating.Real machine test the results are shown in table 4.Thermal conductivity shown in the table 3 and impact value directly are inserted in the table 4.
Table 4
The die casting test-results
Table 4 (continuing)
The die casting test-results
(evaluation of real machine test)
With the naked eye judge breaking of hot tearing, sticking to mould, wearing and tearing and water hole one by one, when producing above-mentioned situation, it is not chosen as " good " (in table 4, being expressed as " A "); When having produced above-mentioned situation a little, it is chosen as " slightly poor " (in table 4, being expressed as " B "); When having produced above-mentioned situation, it is chosen as " poor " (in table 4, being expressed as " C ").
Steel of the present invention all demonstrate good characteristic in all items, and contrast does not all meet judgement criteria with steel in any one project.This is because steel of the present invention have above-mentioned one-tenth and are grouped into, thereby has guaranteed high thermal conductivity and high impact value, and contrast does not have above-mentioned one-tenth with steel and is grouped into, thereby thermal conductivity and/or impact value are low.
That is to say, in steel of the present invention, because the thermal conductivity height so thermal stresses is little, and hardly hot tearing can take place.In addition, under the situation of steel of the present invention, high thermal conductivity has suppressed the overheated of mould, and has reduced the sticking to mould between aluminium alloy and the mould significantly.In addition, inject the caused wearing and tearing of aluminium alloy at a high speed and can ignore, this is corresponding with the hot strength height.Under the situation of steel of the present invention, the corrosion of internal cooling circuit is not too obvious, and produces because leaking of causing of the infiltration in crack (it originates from the part that is corroded).
On the other hand, as can be seen, contrast is better than JIS SKD61 (relatively using steel A10) with steel A01 to A09, but poorer than steel of the present invention.In all lower steel part of its thermal conductivity and impact value (contrast with steel A02, A04 and A10), hot tearing takes place easily.In addition, in the lower steel part of thermal conductivity (contrast steel A02, A03, A05, A07 and A10), sticking to mould takes place continually.In the lower steel part of hot strength (contrast steel A01 and A08), wearing and tearing obviously.Though contrast has guaranteed to have high mold performance with steel A09, because the content height of Mo is considered cost or saved resource, so do not recommend this material.
Especially, contrast except cost, all is cited as " poor " with steel A10 (JIS SKD61) in other all project, and this situation when estimating at fundamental characteristics is similar.Contrast causes mould overheated with steel A10 because its thermal conductivity is low, and between aluminium alloy and mould sticking to mould takes place continually.In addition, because thermal conductivity is lower, thermal stresses is bigger conversely, a lot of hot tearings have been produced.The wearing and tearing that high speed is injected aluminium alloy and caused are remarkable, and this is low with hot strength to be corresponding.In addition, the corrosion of internal cooling circuit is very serious, and originate from be corroded the part the crack spread out.
The mould that is used for real machine test is a large mould.This test-results shows: although the die size that utilizes steel of the present invention to make is bigger, it can have high impact value, and can have high thermal conductivity and hot strength.
Though described the present invention hereinbefore, it should be understood that the present invention is not limited to these embodiments.
Hot working tool steel of the present invention and the steel work that utilizes this hot working tool steel to make have high thermal conductivity and high impact value, therefore, and industrial very valuable for die casting producer and mould user.
Claims (8)
1. hot working tool steel comprises:
0.20 quality %≤C≤0.50 quality %,
0.01 quality %≤Si＜0.25 quality %,
0.50 quality %＜Mn≤1.50 quality %,
5.24 quality %＜Cr≤9.00 quality %,
1.24 quality %＜Mo＜2.95 quality %, and
0.30 quality %＜V＜0.70 quality %,
Surplus is Fe and unavoidable impurities.
2. the described hot working tool steel of claim 1 also comprises:
0.30 quality %≤W≤4.00 quality %.
3. claim 1 or 2 described hot working tool steels also comprise:
0.30 quality %≤Co≤3.00 quality %.
4. any described hot working tool steel in the claim 1 to 3 also comprises at least a element that is selected from the group of being made up of column element down:
0.004 quality %≤Nb≤0.100 quality %,
0.004 quality %≤Ta≤0.100 quality %,
0.004 quality %≤Ti≤0.100 quality %,
0.004 quality %≤Zr≤0.100 quality %,
0.004 quality %≤Al≤0.050 quality %, and
0.004 quality %≤N≤0.050 quality %.
5. any described hot working tool steel in the claim 1 to 4 also comprises at least a element that is selected from the group of being made up of column element down:
0.15 quality %≤Cu≤1.50 quality %,
0.15 quality %≤Ni≤1.50 quality %, and
0.0010 quality %≤B≤0.0100 quality %.
6. any described hot working tool steel in the claim 1 to 5 also comprises at least a element that is selected from the group of being made up of column element down:
0.010 quality %≤S≤0.500 quality %,
0.0005 quality %≤Ca≤0.2000 quality %,
0.03 quality %≤Se≤0.50 quality %,
0.005 quality %≤Te≤0.100 quality %,
0.01 quality %≤Bi≤0.30 quality %, and
0.03 quality %≤Pb≤0.50 quality %.
7. any described hot working tool steel in the claim 1 to 6, its thermal conductivity at room temperature is more than or equal to 28W/m/K.
8. steel work, it comprises any described hot working tool steel in the claim 1 to 7.
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| JP2009-143376 | 2009-06-16 | ||
| JP2009143376A JP2011001572A (en) | 2009-06-16 | 2009-06-16 | Tool steel for hot work and steel product using the same |
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| CN101921959A true CN101921959A (en) | 2010-12-22 |
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| JPS6059053A (en) | 1983-09-09 | 1985-04-05 | Daido Steel Co Ltd | Hot working tool steel |
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| AU2003292572A1 (en) * | 2003-12-19 | 2005-07-14 | Daido Steel Co., Ltd | Hot work tool steel and mold member excellent in resistance to melting |
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| JP2008121032A (en) | 2006-11-08 | 2008-05-29 | Daido Steel Co Ltd | Die steel superior in spheroidizing annealing property and hardenability |
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2009
- 2009-06-16 JP JP2009143376A patent/JP2011001572A/en active Pending
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2010
- 2010-06-12 CN CN2010102035115A patent/CN101921959A/en active Pending
- 2010-06-14 EP EP10006151A patent/EP2270246A1/en not_active Withdrawn
- 2010-06-16 KR KR1020100057288A patent/KR20100135205A/en not_active Application Discontinuation
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Also Published As
| Publication number | Publication date |
|---|---|
| EP2270246A1 (en) | 2011-01-05 |
| JP2011001572A (en) | 2011-01-06 |
| KR20100135205A (en) | 2010-12-24 |
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