CN105734424A - Alloy material for offshore drilling platform freshwater cooling system and preparation method thereof - Google Patents
Alloy material for offshore drilling platform freshwater cooling system and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- 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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/002—Heat treatment of ferrous alloys containing Cr
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- C—CHEMISTRY; METALLURGY
- 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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/005—Heat treatment of ferrous alloys containing Mn
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- C—CHEMISTRY; METALLURGY
- 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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/008—Heat treatment of ferrous alloys containing Si
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/32—Ferrous alloys, e.g. steel alloys containing chromium with boron
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/60—Ferrous alloys, e.g. steel alloys containing lead, selenium, tellurium, or antimony, or more than 0.04% by weight of sulfur
Abstract
The invention provides an alloy material for an offshore drilling platform freshwater cooling system and a preparation method thereof. The alloy material comprises the following raw materials: C, Mn, P, S, B, Mg, Sb, Si, Cr, Mo, Be, La, Er and the balance of Fe; and the preparation method comprises the following steps: adding the to-be-melted Fe, Mn, Mg, Sb, Cr, Mo, Be and Re into a vacuum chamber of a water-cooling copper crucible according to the proportion of material components; vacuumizing; melting at a sintering temperature of 940-960 DEG C; adding C, P, S, B and Si in the metal melting condition, preserving heat and stirring uniformly; cooling to 630 DEG C in an inert gas pressurizing condition, and preserving heat for 30-40min; and cooling again to room temperature to obtain a finished product of the alloy material for the offshore drilling platform freshwater cooling system. The product prepared in the invention has good properties of rust prevention, pressure resistance, high-temperature resistance, rare deformation in heat and light mass.
Description
Technical field
The invention belongs to ferrous alloy field, be specifically related to a kind of marine drilling platform cooling system of fresh water alloy material and preparation method thereof.
Background technology
In the past few decades, petroleum industry is constantly expanded to ultra-deep sea from shallow sea to deep-sea again.Marine oil and gas total output accounts for the ratio of global Oil Gas total output and rises to current more than 40% from 20% in 1997, and wherein deep-sea oil gas yield accounts for more than the 30% of marine oil and gas yield.In the Recoverable oil and gas reserves that the world has been found that, marine oil and gas accounts for 41%.The degree of prospecting of especially deep-sea, some marine sites and Arctic is also very low, and therefore the potentiality of Marine oil and gas resource are still very big.The yield of marine oil and gas and reserves are always maintained at very fast growth, have also driven the development in marine drilling platform market.Last century, the forties barge was first for offshore survey drilling well, within 1956, occurred in that drill ship, and within 1961, semisubmersible drilling platform comes out.Current marine drilling platform substantially can be divided into 8 classes, namely drilling barge, drill ship, inland refute, self-elevating drilling platform, platform rig, semisubmersible drilling platform, submercible unit and drilling module.
Marine drilling platform cooling system of fresh water is the important component part that platform cooling system is crept in ocean, in the centralized of whole marine drilling platform in cooling system, is exactly cooled with seawater fresh water in fact, and the fresh water after cooling goes cooling plant equipment again.With salt water cooling system the difference is that, cooling system of fresh water is a closed circulation system.At sea, sea water is almost inexhaustible.From drawing up in the sea, directly discharge after being finished and gone in the sea.But fresh water is different, fresh water is at sea that comparison is precious.And be usually treated soft water for the fresh water of cooling system, but also can inside put into a lot of additive, it is to avoid the elemental release in water, or the cavitation pitting of equipment is avoided in anti-foaming etc..Cooling system of fresh water, particularly says generating set, point high temperature cooling system of fresh water and low temperature cooling system of fresh water.Therefore, the material of other system can be different from for the material of the cooling system of fresh water of marine drilling platform.But, marine drilling platform this still in constantly perfect technology, the material of the cooling system of fresh water of marine drilling platform is in a great extent to be groped and continuous experimental stage, how to select and to manufacture excellent, not only anticorrosion but also heat-resisting marine drilling platform cooling system of fresh water material, being when previous urgent problem.
Summary of the invention
In order to overcome above-mentioned deficiency, it is an object of the invention to provide a kind of marine drilling platform cooling system of fresh water alloy material and preparation method thereof, consider the cost of each composition, optimize the ratio between each composition, find the material prescription that cost performance is the highest, add rare earth metal, it is possible to efficiently solve the problems referred to above.
In order to solve above-mentioned technical problem, the present invention takes following technical scheme:
A kind of marine drilling platform cooling system of fresh water alloy material, the material composition of described alloy material and mass percent thereof be: C:0.10%～0.30%, Mn:0.50%～0.80%, P:0.03%～0.05%, S:0.03%～0.05%, B:0.40%～0.60%, Mg:0.40%～0.60%, Sb:0.30%～0.40%, Si:0.50%～1.50%, Cr:0.50%～0.80%, Mo:0.90%～1.20%, Be:3.0%～4.0%, RE:0.20%～0.80%, all the other are Fe.
Further, RE includes: Pr:0.10%～0.40%, Yb:0.10%～0.40%.
Further, material composition and mass percent thereof are: C:0.20%, Mn:0.70%, P:0.04%, S:0.045%, B:0.50%, Mg:0.50%, Sb:0.30%, Si:1.0%, Cr:0.50%, Mo:1.20%, Be:3.40%, Pr:0.10%, Yb:0.40%, all the other are Fe.
Hereinafter, the restriction reason that the one-tenth of the alloy of employing in the present invention is grouped into illustrates, and becomes the % related in being grouped into refer to quality %.
C:0.10%～0.30%, C can form solid solution tissue in steel, improve the intensity of steel, forms carbide tissue, can improve hardness and the wearability of steel.Therefore, C is in steel, and phosphorus content is more high, and the intensity of steel, hardness are more high, but plasticity, toughness also can decrease.Otherwise, phosphorus content is more low, and the plasticity of steel, toughness are more high, its intensity, hardness also can decrease, for adapting to ocean condition and job requirements effect, C content in marine drilling platform cooling system of fresh water material is defined as 0.10%～0.30% by the present invention, it is preferred to 0.20%.
Mn:0.50%～0.80%, Mn is a kind of weak deoxidizer, adds Mn, be not only advantageous to the corrosion stability of steel, and the intensity of steel can also be made to improve, and can reduce hot cracking tendency, improve corrosion resistance and the welding performance of steel in steel.Along with Mn content increases, steel strength increases, and for adapting to the concrete actual specific demand of marine drilling platform cooling system of fresh water, Mn content is defined as 0.50%～0.80% by the present invention, it is preferred to 0.70%.
P:0.03%～0.05%, the tensile strength improving steel is had certain effect by phosphorus, but all increases again the fragility of steel simultaneously.For adapting to the specific demand of ocean condition and marine drilling platform cooling system of fresh water, P content is defined as 0.03%～0.05% by the present invention, it is preferred to 0.03%.
S:0.03%～0.05%, S can cause steel hot-short, reduces the plasticity of steel, impact flexibility, fatigue strength and rust quality etc., and common buildings steel sulfur content requires less than 0.055%, should less than 0.050% in Welding Structure.A certain amount of S and Mn forms MnS in steel, is favorably improved the element of machinability.When lower than 0.001%, additive effect is insufficient, saturated more than 0.15% additive effect, and S can reduce the mobility of molten iron, stops Fe3C decomposes, and makes foundry goods produce pore, is difficult to cutting and reduces its toughness.Therefore S is defined as 0.03%～0.05%, it is preferred to 0.03%.
B:0.40%～0.60%, B is referred to as " vitamin " in steel, can increase hardenability exponentially, increases hardness and the tension stress of steel, improves the welding performance of steel, add a certain amount of B in mild steel, has the function absorbing neutron.For adapting to the specific demand of ocean condition and marine drilling platform cooling system of fresh water, B content in material is defined as 0.40%～0.60% by the present invention, it is preferred to 0.50%.
Mg:0.40%～0.60%, adds a small amount of magnesium in the alloy, can improve intensity and yield limit, improves the machinability of alloy.Alloy containing magnesium has excellent corrosion resistance.For adapting to the specific demand of ocean condition and marine drilling platform cooling system of fresh water, Mg content in alloy material is defined as 0.40%～0.60% by the present invention, it is preferred to 0.40%.
Sb:0.30%～0.40%, adds a certain amount of antimony in steel, understands the resistance to corrosion improving steel in various degree and wearability.For adapting to aviation climate condition and engine calls, Sb content in alloy material is defined as 0.30%～0.40% by the present invention, it is preferred to 0.30%.
Si:0.50%～1.50%, Si can improve thermostability and the corrosion resistance of steel, reduces toughness and plasticity, can reduce fusing point, improve mobility in steel.For adapting to the specific demand of ocean condition and marine drilling platform cooling system of fresh water, Si content is defined as 0.50%～1.50% by the present invention, it is preferred to 1.0%.
Cr:0.50%～0.80%, Cr is in steel, and chromium can significantly improve intensity, hardness and wearability, but reduce plasticity and toughness simultaneously.Chromium can improve again non-oxidizability and the corrosion resistance of steel, thus is the important alloying element of steel.For adapting to the specific demand of ocean condition and marine drilling platform cooling system of fresh water, Cr content is defined as 0.50%～0.80% by the present invention, it is preferred to 0.50%.
Mo:0.90%～1.20%, the Mo energy reinforced ferrite of low content, improve intensity and the hardness of steel, reduce the critical cooling rate of steel, improve the quenching degree of steel, improve thermostability and the elevated temperature strength of steel, for adapting to the specific demand of ocean condition and marine drilling platform cooling system of fresh water, Mo content in material is defined as 0.90%～1.20% by the present invention, it is preferred to 1.20%.
Be:3.0%～4.0%, when adding people higher amount Be in the alloy, it is possible to accelerates above alloy aging process and improves timeliness hardness.Add Be in the alloy, it is possible to accelerated ag(e)ing curing progress, improve nearly 1 times of hardness, also can increase Age-prrcipitation Phase number simultaneously, reduce its size.Be content in alloy material is defined as 3.0%～4.0% by the present invention, it is preferred to 3.40%.
RE:0.20%～0.80%, rare earth element adds in alloy, it is possible to increase the mechanical strength of alloy material and corrosion resistance, increase constitutional supercooling, crystal grain thinning when making alloy casting, reduce secondary intergranular from, reduce the gas in alloy and be mingled with, and making constituent phases tend to nodularization.Also can reduce smelt surface tension, increase mobility, be conducive to casting ingot-forming, processing performance is had obvious impact, rare earth metal can also eliminate the harmful effect to marine drilling platform cooling system of fresh water of the hydrological environment of magnetic field and complexity, thus improve the service life of marine drilling platform, simultaneously when load is identical, hence it is evident that alleviate structural member weight.For adapting to the specific demand of ocean condition and marine drilling platform cooling system of fresh water, RE content in material is defined as 0.20%～0.80% by the present invention, including Pr:0.10%～0.40%, Yb:0.10%～0.40%, it is preferably Pr:0.10%, Yb:0.40%.The rare earth metal content used in the present invention is less, but is able to play good demagnetization and increase the effect of the strength of materials, wearability, advantageously reduces cost.
Another object of the present invention, is in that to provide the preparation method adopting a kind of marine drilling platform cooling system of fresh water alloy material, and making step is as follows:
Step S01, will treat that Fe, Mn, Mg, Sb, Cr, Mo, Be, RE of melting are according to material composition ratio, add in the vacuum chamber of water jacketed copper crucible, evacuation, sintering temperature be under 940 DEG C～960 DEG C conditions melted；
Step S02, add C, P, S, B, Si when metal melting according to material composition ratio, and be incubated 30min～40min, stir；
Step S03, under noble gas pressurized conditions, it is cooled to 630 DEG C, is incubated 30min～40min, then is cooled to room temperature, obtain marine drilling platform cooling system of fresh water alloy material finished product.
Further, in step S01, when the temperature of sintering is 940 DEG C～950 DEG C, RE consists of Pr.
Further, in step S01, when the temperature of sintering is 950 DEG C～960 DEG C, RE consists of Pr and Yb.
Further, in step S03, the speed of cooling is 60 DEG C/min～70 DEG C/min.
Further, in step S03, the speed of cooling is 60 DEG C/min～70 DEG C/min.
Further, in step S03, noble gas is helium or neon.
Further, in step S03, the pressure of pressurization is 60Mpa～70Mpa.
The invention have the advantage that
Marine drilling platform cooling system of fresh water alloy material finished product provided by the present invention, the material of preparation has the performance of good diamagnetic, anticorrosive, pressure, high temperature resistant, not easily deformation of being heated.
Detailed description of the invention
Specific embodiments of the invention given below, are used for the present invention is described in further detail.
Embodiment 1
Raw material components:
C:0.20%, Mn:0.70%, P:0.04%, S:0.045%, B:0.50%, Mg:0.50%, Sb:0.30%, Si:1.0%, Cr:0.50%, Mo:1.20%, Be:3.40%, Pr:0.10%, Yb:0.40%, all the other are Fe.
It is prepared via a method which:
Step S01, will treat that Fe, Mn, Mg, Sb, Cr, Mo, Be, Pr, Yb of melting are according to material composition ratio, add in the vacuum chamber of water jacketed copper crucible, evacuation, sintering temperature be under 955 DEG C of conditions melted；
Step S02, add C, P, S, B, Si when metal melting according to material composition ratio, and be incubated 36min, stir；
Step S03, when helium pressurizes 67Mpa, be cooled to 630 DEG C with the rate of temperature fall of 64 DEG C/min, be incubated 36min, then be down to room temperature with the rate of temperature fall of 64 DEG C/min, obtain marine drilling platform cooling system of fresh water alloy material finished product.
Embodiment 2
Raw material components:
C:0.10%, Mn:0.50%, P:0.03%, S:0.03%, B:0.40%, Mg:0.40%, Sb:0.30%, Si:0.50%, Cr:0.50%, Mo:0.90%, Be:3.0%, Pr:0.20%, all the other are Fe.
It is prepared via a method which:
Step S01, will treat that Fe, Mn, Mg, Sb, Cr, Mo, Be, Pr of melting are according to material composition ratio, add in the vacuum chamber of water jacketed copper crucible, evacuation, sintering temperature be under 940 DEG C of conditions melted；
Step S02, add C, P, S, B, Si when metal melting according to material composition ratio, and be incubated 30min, stir；
Step S03, when helium pressurizes 60Mpa, be cooled to 630 DEG C with the rate of temperature fall of 60 DEG C/min, be incubated 30min, then be down to room temperature with the rate of temperature fall of 60 DEG C/min, obtain marine drilling platform cooling system of fresh water alloy material finished product.
Embodiment 3
Raw material components:
C:0.30%, Mn:0.80%, P:0.05%, S:0.05%, B:0.60%, Mg:0.60%, Sb:0.40%, Si:1.50%, Cr:0.80%, Mo:1.20%, Be:4.0%, Pr:0.40%, Yb:0.40%, all the other are Fe.
It is prepared via a method which:
Step S01, will treat that Fe, Mn, Mg, Sb, Cr, Mo, Be, Pr, Yb of melting are according to material composition ratio, add in the vacuum chamber of water jacketed copper crucible, evacuation, sintering temperature be under 960 DEG C of conditions melted；
Step S02, add C, P, S, B, Si when metal melting according to material composition ratio, and be incubated 40min, stir；
Step S03, when neon pressurizes 70Mpa, be cooled to 630 DEG C with the rate of temperature fall of 70 DEG C/min, be incubated 40min, then be down to room temperature with the rate of temperature fall of 70 DEG C/min, obtain marine drilling platform cooling system of fresh water alloy material finished product.
Embodiment 4
Raw material components:
C:0.20%, Mn:0.65%, P:0.04%, S:0.04%, B:0.50%, Mg:0.50%, Sb:0.35%, Si:1.0%, Cr:0.65%, Mo:1.05%, Be:3.50%, Pr:0.25%, Yb:0.25%, all the other are Fe.
It is prepared via a method which:
Step S01, will treat that Fe, Mn, Mg, Sb, Cr, Mo, Be, Pr, Yb of melting are according to material composition ratio, add in the vacuum chamber of water jacketed copper crucible, evacuation, sintering temperature be under 950 DEG C of conditions melted；
Step S02, add C, P, S, B, Si when metal melting according to material composition ratio, and be incubated 35min, stir；
Step S03, when neon pressurizes 65Mpa, be cooled to 630 DEG C with the rate of temperature fall of 65 DEG C/min, be incubated 35min, then be down to room temperature with the rate of temperature fall of 65 DEG C/min, obtain marine drilling platform cooling system of fresh water alloy material finished product.
Experimental example 1
Wear resistence contrast test:
The marine drilling platform cooling system of fresh water alloy material that the embodiment of the present invention 1～5 prepares and common cooling system of fresh water material do slurry (quartz sand+water) wet grinding test on jetting type erosive-corrosive wear testing machine, and make the corrosion resistance test of material, performance is in Table 1.
Table 1 wear resistence and hardness balance's result of the test
| Material | Anticorrosive multiplying power | The wear-resistant multiplying power of wet grinding | Hardness (HB) |
| Common cooling system of fresh water material | 1.0 | 1.0 | 149 |
| Embodiment 1 prepares alloy material | 1.16 | 1.19 | 187 |
| Embodiment 2 prepares alloy material | 1.10 | 1.17 | 180 |
| Embodiment 3 prepares alloy material | 1.14 | 1.15 | 184 |
| Embodiment 4 prepares alloy material | 1.15 | 1.16 | 180 |
Experimental example 2
The marine drilling platform cooling system of fresh water alloy material that the embodiment of the present invention 1～5 is prepared compared with the base metal characteristic of common cooling system of fresh water material, its results of property such as table 2 below.
Table 2 base metal characteristic performance compares
From above-mentioned test example, the properties of alloy material of the present invention is above common cooling system of fresh water material, and the special material consumption preparing alloy of the present invention is few, and relative cost is low, is more suitable for for marine drilling platform cooling system of fresh water alloy material.
These are only the preferred embodiments of the present invention and experimental example, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (10)
1. a marine drilling platform cooling system of fresh water alloy material, it is characterized in that, the material composition of described alloy material and mass percent thereof be: C:0.10%～0.30%, Mn:0.50%～0.80%, P:0.03%～0.05%, S:0.03%～0.05%, B:0.40%～0.60%, Mg:0.40%～0.60%, Sb:0.30%～0.40%, Si:0.50%～1.50%, Cr:0.50%～0.80%, Mo:0.90%～1.20%, Be:3.0%～4.0%, RE:0.20%～0.90%, all the other are Fe.
2. alloy material according to claim 1, it is characterised in that described RE includes: La:0.10%～0.40%, Er:0.10%～0.40%.
3. alloy material according to claim 1, it is characterised in that described material composition and mass percent thereof be: C:0.20%, Mn:0.70%, P:0.04%, S:0.045%, B:0.50%, Mg:0.50%, Sb:0.30%, Si:1.0%, Cr:0.50%, Mo:1.20%, Be:3.40%, Pr:0.10%, Yb:0.40%, all the other are Fe.
4. the preparation method of alloy material according to any one of claims 1 to 3, it is characterised in that include following making step:
Step S01, will treat that Fe, Mn, Mg, Sb, Cr, Mo, Be, RE of melting are according to material composition ratio, add in the vacuum chamber of water jacketed copper crucible, evacuation, sintering temperature be under 940 DEG C～960 DEG C conditions melted；
Step S02, add C, P, S, B, Si when metal melting according to material composition ratio, and be incubated 30min～40min, stir；
Step S03, under noble gas pressurized conditions, it is cooled to 630 DEG C, is incubated 30min～40min, then is cooled to room temperature, obtain marine drilling platform cooling system of fresh water alloy material finished product.
5. preparation method according to claim 4, it is characterised in that in step S01, when the temperature of described sintering is 940 DEG C～950 DEG C, RE consists of Pr.
6. preparation method according to claim 4, it is characterised in that in step S01, when the temperature of described sintering is 950 DEG C～960 DEG C, RE consists of Pr and Yb.
7. preparation method according to claim 4, it is characterised in that in step S03, the speed of described cooling is 60 DEG C/min～70 DEG C/min.
8. preparation method according to claim 4, it is characterised in that in step S03, the speed of described cooling is 60 DEG C/min～70 DEG C/min.
9. preparation method according to claim 4, it is characterised in that in step S03, described noble gas is helium or neon.
10. preparation method according to claim 4, it is characterised in that in step S03, the pressure of described pressurization is 60Mpa～70Mpa.
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Application publication date: 20160706 |