CN102275905A - EXT454 ultrafine-grained structure graphite and preparation method thereof - Google Patents
EXT454 ultrafine-grained structure graphite and preparation method thereof Download PDFInfo
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- CN102275905A CN102275905A CN201110151261XA CN201110151261A CN102275905A CN 102275905 A CN102275905 A CN 102275905A CN 201110151261X A CN201110151261X A CN 201110151261XA CN 201110151261 A CN201110151261 A CN 201110151261A CN 102275905 A CN102275905 A CN 102275905A
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Abstract
The invention discloses EXT454 ultrafine-grained structure graphite and a preparation method thereof. The EXT454 ultrafine-grained structure graphite is prepared from the following raw materials in a certain percentage: petroleum coke powder, pitch coke powder and graphite powder. The preparation method comprises the steps: A, mixing the petroleum coke powder, pitch coke powder and L399 graphite powder with a 500 L mixer while controlling the temperature and time in a certain range; B, rolling: placing the uniformly mixing material paste in a roll machine for rolling; C, milling: milling with a 4R mill; D, pressing: pressurizing with a 500 t press machine, exhausting and carrying out press molding; E, baking: heating and baking in a reverberating furnace to completely bake the inside of a product; F, immersing; and G, graphitizing: carrying out high-temperature graphitization. The preparation method is feasible and simple to operate. The ultrafine-grained structure graphite with average particle size of only 3-10 mu m can be used as a mold for hot pressed sintering of a tool bit of a diamond saw blade, and because of more compact microscopic structure, smaller pores, higher processing finish degree and strong oxidation resistance of the graphite, the mold has longer life.
Description
Technical field
The present invention relates to the carbon-graphite product technique field, relate more specifically to the ultra-fine granularity structure of a kind of EXT454 graphite, also relate to the preparation method of the ultra-fine granularity structure of a kind of EXT454 graphite simultaneously.
Background technology
China is man-made diamond big producing country, and tempo is exceedingly fast, and output ranks first in the world for years.In huge at home artificial diamond tool and the goods industry, the hot pressed sintering operation of diamond head and saw blade tip all is to adopt graphite to make mould.This is that at high temperature its physical strength can not reduce because the carbon-graphite goods have the fusing point height, and a series of excellent specific properties such as can raise on the contrary.
Traditional diamond hot pressed sintering graphite jig, general all is to adopt the high purity graphite blank of common fine-grain structure to process. the median size of such graphite is between 45～55 μ m, thereby its microstructure is fine and close inadequately, pore is bigger, it is lower to process smooth finish, oxidation-resistance is not strong, and work-ing life is shorter, is generally 4～6 times.
Summary of the invention
The objective of the invention is to be to provide the ultra-fine granularity structure of a kind of EXT454 graphite, prescription rationally, result of use is good, the microstructure densification, pore is small, can process highly polishedly, oxidation-resistance is strong.
Another object of the present invention is the preparation method who has been to provide the ultra-fine granularity structure of a kind of EXT454 graphite.Easy to implement the method, easy and simple to handle, the employing median size only is the hot pressed sintering mould that the ultra-fine granularity structure graphite of 3～10 μ m is made diamond saw blade, fine and close more because of its microstructure, pore is more small, and it is higher to process smooth finish, oxidation-resistance is strong, so longer service life.
In order to realize above-mentioned goal of the invention, the present invention adopts following technical scheme:
Adopt the ultra-fine granularity structure of EXT454 graphite to make the hot pressed sintering mould of diamond saw blade, its advantage is outstanding especially. because its particulate median size only is 1/5th to 1/15th of a traditional technology graphite, thereby make its microstructure fine and close more, pore is more small, it is higher to process smooth finish, oxidation-resistance is strong, and longer service life can reach 18～20 times.
The preparation method of the ultra-fine granularity structure of a kind of EXT454 graphite comprises following steps: is the carbon element powder such as refinery coke, pitch coke of 3～10 μ m with median size,, pricks sheet through mixing, and abrasive dust, compacting, roasting, dipping makes after the greying:
The ultra-fine granularity structure of a kind of EXT454 graphite, it is made by following raw materials by weight percent:
By the molten asphalt that modified pitch and mid-temperature pitch are half-and-half prepared burden and melted, and 46～48wt% (add---refer to petroleum coke powder, the pitch coke powder, dry powder proportionings such as L399 Graphite Powder 99 amount to 100%, and molten asphalt plays the binding agent effect in this batching, in roasting, in the high temperature treating processess such as greying, major part all vapors away, therefore,, molten asphalt proportioning adopt and to add per-cent, molten asphalt does not account for weight ratio of the present invention, and this scheme is made by prior art).
Described petroleum coke powder and pitch coke powder are to select fine refinery coke and pitch coke for use, and through 1250～1300 ℃ high-temperature calcination, fragmentation and extra-fine grinding are the powder of 3～10 μ m to median size.
Described L399 Graphite Powder 99 is to select carbon content 〉=99% for use, the high purity graphite powder of-320# 〉=90%.
Described molten asphalt is to select half-and-half batching of fine modified pitch and mid-temperature pitch for use, and is heated to the liquid bitumen of 185～215 ℃ of insulations fusing in 24～26 hours.
The ultra-fine granularity structure of a kind of EXT454 graphite, it makes (preferable range) by following raw materials by weight percent:
The ultra-fine granularity structure of a kind of EXT454 graphite, it makes (optimum value) by following raw materials by weight percent:
By modified pitch and softening temperature is the half-and-half molten asphalts of batching fusing of 75～90 ℃ of mid-temperature pitches, 46～48wt% (adding).
The preparation method of the ultra-fine granularity structure of a kind of EXT454 graphite the steps include:
A, petroleum coke powder, pitch coke powder, L399 Graphite Powder 99 are mixed: carry out on 500 liters of mixing machines, Revolution Per Minute 25～34 changes, and temperature is controlled at 185～210 ℃, and mixing time 2～3 hours is wanted strict control, reaches the purpose that material fully is mixed.
The B roll: the material paste that will mix is put into Φ 400mm roller mill and is rolled sheet, and repeats once.
C abrasive dust: on the 4R pulverizing mill, carry out abrasive dust granularity-320#60 ± 5%.
D compacting: on 500 tons of pressing machinees, slowly pressurize pressure 130～150MPa, exhaust, compression molding.
The E roasting: carry out 500H super snail curve intensification roasting in down-draft furnace, 1250～1300 ℃ of top temperatures are incubated 48～60 hours, and the inside of goods is grilled thoroughly, and the cracking rate drops to bottom line.
F dipping: adopt the 2MPa high-pressure impregnation, be devoted to the core of graphite blank is soaked into.
G greying: adopt 2550～2650 ℃ of high temperature graphitizations, its degree of graphitization is reached more than 85%. its physicochemical property is splendid, and is as shown in table 1.
The present invention compared with prior art has the following advantages and effect:
The major technique of the ultra-fine granularity structure of EXT454 graphite project is embodied in two aspects: the one, and preferred by to raw-material further investigation and proportion scheme; The 2nd, carry out repeatedly process certification and the simultaneous test of its physicochemical property and trial effect, inquire into its microstructure densification, pore is small, can process highly polishedly, oxidation-resistance is strong, the making method of the ultra-fine granularity structure graphite of long service life.The advantage of this graphite is a compact structure, and pore is small, can process highly polished, the degree of graphitization height, oxidation-resistance is strong, reach 18～20 work-ing life in the hot pressed sintering of diamond tool, is 3～4 times of common graphite mould.
Major technique and the performance index such as the table 1 of the ultra-fine granularity structure of EXT454 graphite:
Table 1
Embodiment
Below providing specific embodiment further specifies.The purpose of these embodiment is illustrative, and should not be construed as limitation of the present invention.
Embodiment 1:
The ultra-fine granularity structure of a kind of EXT454 graphite, it is made by following raw materials by weight percent:
Molten asphalt 48wt% (adding) by modified pitch and double batching fusing of mid-temperature pitch.Preparation method and step: with median size is petroleum coke powder, pitch coke powder, the carbon element powder of 3～10 μ m, through mixing, pricks sheet, abrasive dust, compacting, roasting, dipping makes (molten asphalt 48wt% does not account for weight ratio of the present invention, and this scheme is made by prior art) after the greying.
The preparation method of the ultra-fine granularity structure of a kind of EXT454 graphite the steps include: raw material to prick sheet through through mixing, abrasive dust, and compacting, roasting, dipping makes after the greying.
A, petroleum coke powder, pitch coke powder, L399 Graphite Powder 99 are mixed in proportion: on 500 liters of mixing machines, carry out, Revolution Per Minute 25～34 changes, temperature is controlled at 185 or 190 or 195 or 200 or 205 or 210 ℃, mixing time 2 or 2.5 or 3 hours, want strict control, reach the purpose that material fully is mixed.
The B roll: the material paste that will mix is put into Φ 400mm roller mill and is rolled sheet, and repeats once.
C abrasive dust: on the 4R pulverizing mill, carry out abrasive dust granularity-320#60 ± 5%.
D compacting: on 500 tons of pressing machinees, slowly pressurize pressure 130 or 135 or 140 or 145 or 150MPa, exhaust, compression molding.
The E roasting: carry out 500H super snail curve intensification roasting in down-draft furnace, top temperature 1250 or 1260 or 1270 or 128 or 1290 or 1300 ℃ are incubated 48 or 50 or 52 or 54 or 56 or 58 or 60 hours, and the inside of goods is grilled thoroughly, and the cracking rate drops to bottom line.
F dipping: adopt the 2MPa high-pressure impregnation, be devoted to the core of graphite blank is soaked into.
G greying: adopt 2550 or 2560 or 2570 or 2585 or 2595 or 2 610 or 2625 or 2635 or 2645 or 2650 ℃ of high temperature graphitizations, its degree of graphitization is reached more than 85%.
Embodiment 2:
The ultra-fine granularity structure of a kind of EXT454 graphite, it is made by following raw materials by weight percent:
By the molten asphalt that modified pitch and mid-temperature pitch are half-and-half prepared burden and melted, 48wt% (add, molten asphalt 48wt% does not account for weight ratio of the present invention, and this scheme is made by prior art).The preparation method is identical with embodiment 1 with step.
Embodiment 3:
The ultra-fine granularity structure of a kind of EXT454 graphite, it is made by following raw materials by weight percent:
By the molten asphalt that modified pitch and mid-temperature pitch are half-and-half prepared burden and melted, 48wt% (add, molten asphalt 48wt% does not account for weight ratio of the present invention, and this scheme is made by prior art).The preparation method is identical with embodiment 1 with step.
Embodiment 4:
The ultra-fine granularity structure of a kind of EXT454 graphite, it is made by following raw materials by weight percent:
By the molten asphalt that modified pitch and mid-temperature pitch are half-and-half prepared burden and melted, 48wt% (add, molten asphalt 48wt% does not account for weight ratio of the present invention, and this scheme is made by prior art).The preparation method is identical with embodiment 1 with step.
Embodiment 5:
The ultra-fine granularity structure of a kind of EXT454 graphite, it is made by following raw materials by weight percent:
By the molten asphalt that modified pitch and mid-temperature pitch are half-and-half prepared burden and melted, 48wt% (add, molten asphalt 48wt% does not account for weight ratio of the present invention, and this scheme is made by prior art).The preparation method is identical with embodiment 1 with step.
The used equipment of the present invention has: 1. airflow strikes formula superfine mill; 2. 500 liters of multiple twin cutter mixing machines; 3. Φ 400mm roller mill; 4. 500T pressing machine; 5. 12T down-draft furnace.6. 2.3MPa high-pressure impregnation jar. 7. 1500KVA direct-current graphitization stove.
Major technique and the performance such as the table 2 of the ultra-fine granularity structure graphite of embodiment 1～5 gained:
Table 2
Product performance are compared as follows:
The ultra-fine granularity structure of EXT454 graphite is made the hot pressed sintering mould of diamond saw blade, its advantage is outstanding especially. because its particulate median size only is 1/5th to 1/15th of a traditional technology graphite, thereby make its microstructure fine and close more, pore is more small, and it is higher to process smooth finish, and oxidation-resistance is strong, longer service life, it is on probation that it is processed as on the graphite jig pressure head of 2.8～3.2mm machine, can reach work-ing life 18～20 times, and Yet-have does not see apparent damage.And the graphite jig of processing with the high purity graphite blank of common fine-grain structure. its microstructure is fine and close inadequately, and pore is bigger, and it is lower to process smooth finish, and oxidation-resistance is not strong, and work-ing life is shorter, and it only is 4～6 times that last machine is tried out the life-span.
EXT454 is that a kind of median size is the ultra-fine granularity structure graphite of 3～10 μ m, the batch process of such graphite, Yet-have beyond example at home. its excellent physicochemical property and the suitability in the hot pressed sintering of diamond segment, be on close level with American-European product.
The ultra-fine granularity structure of EXT454 graphite can be used for the hot pressed sintering mould of diamond saw blade, Graphite Electrodes is used in spark discharge processing, and the directed ingot casting graphite boat of polysilicon, and its use properties can significantly improve, this product has the extremely strong market competitiveness, has a extensive future.
More than the preparation method of the ultra-fine granularity structure of EXT454 provided by the present invention graphite is described in detail, used specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof; Simultaneously, for one of ordinary skill in the art, according to thought of the present invention, the part that all can change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.
Claims (9)
1. the ultra-fine granularity structure of EXT454 graphite, it is made by following raw materials by weight percent:
Raw material %
Petroleum coke powder 75 ~ 79
Pitch coke powder 16 ~ 20
Graphite Powder 99 1 ~ 6.
2. the ultra-fine granularity structure of a kind of EXT454 according to claim 1 graphite is characterized in that:
Raw material %
Petroleum coke powder 76 ~ 78
Pitch coke powder 17 ~ 19
Graphite Powder 99 2 ~ 5.
3. the ultra-fine granularity structure of a kind of EXT454 according to claim 1 graphite is characterized in that:
Raw material %
Petroleum coke powder 78
Pitch coke powder 17
L399 Graphite Powder 99 5.
4. the ultra-fine granularity structure of a kind of EXT454 according to claim 1 graphite is characterized in that:
Raw material %
Petroleum coke powder 75
Pitch coke powder 20
L399 Graphite Powder 99 5.
5. the ultra-fine granularity structure of a kind of EXT454 according to claim 1 graphite is characterized in that:
Raw material %
Petroleum coke powder 76
Pitch coke powder 19
L399 Graphite Powder 99 5.
6. the ultra-fine granularity structure of a kind of EXT454 according to claim 1 graphite is characterized in that:
Raw material %
Petroleum coke powder 77
Pitch coke powder 18
L399 Graphite Powder 99 5.
7. the ultra-fine granularity structure of a kind of EXT454 according to claim 1 graphite is characterized in that:
Raw material %
Petroleum coke powder 78
Pitch coke powder 17
L399 Graphite Powder 99 5.
8. the ultra-fine granularity structure of a kind of EXT454 according to claim 1 graphite is characterized in that:
Raw material %
Petroleum coke powder 79
Pitch coke powder 16
L399 Graphite Powder 99 5.
9. the preparation method of the ultra-fine granularity structure of the described a kind of EXT454 of claim 1 graphite the steps include:
A, petroleum coke powder, pitch coke powder, L399 Graphite Powder 99 are mixed: carry out on 500 liters of mixing machines, Revolution Per Minute 25～34 changes, and temperature is controlled at 185～210 ℃, mixing time 2～3 hours;
The B roll: the material paste that will mix is put into Ф 400 ㎜ roller mills and is rolled sheet, and repeats once;
C abrasive dust: on the 4R pulverizing mill, carry out abrasive dust granularity-320#60;
D compacting: on 500 tons of pressing machinees, pressurize pressure 130～150Mpa, exhaust, compression molding;
The E roasting: carry out 500H super snail curve intensification roasting in down-draft furnace, 1250～1300 ℃ of temperature are incubated 48～60 hours, and the inside of goods is grilled thoroughly;
F dipping: adopt the 2MPa high-pressure impregnation, be devoted to the core of graphite blank is soaked into;
G greying: adopt 2550～2650 ℃ of high temperature graphitizations, make its degree of graphitization reach 85%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103753844A (en) * | 2013-12-21 | 2014-04-30 | 湖北鄂信钻石材料有限责任公司 | Vacuum pressing method for superfine carbon green body |
Citations (2)
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|---|---|---|---|---|
| US7491421B2 (en) * | 2005-04-13 | 2009-02-17 | Kai-Yu Lin | Graphite base for heat sink, method of making graphite base and heat sink |
| CN101823707A (en) * | 2010-04-28 | 2010-09-08 | 四川广汉士达炭素股份有限公司 | Technical method for producing isostatic pressure graphite |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7491421B2 (en) * | 2005-04-13 | 2009-02-17 | Kai-Yu Lin | Graphite base for heat sink, method of making graphite base and heat sink |
| CN101823707A (en) * | 2010-04-28 | 2010-09-08 | 四川广汉士达炭素股份有限公司 | Technical method for producing isostatic pressure graphite |
Non-Patent Citations (1)
| Title |
|---|
| 缪树良: "热压金刚石地质钻头用石墨模具", 《超硬材料工程》, vol. 21, no. 5, 31 October 2009 (2009-10-31), pages 16 - 22 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103753844A (en) * | 2013-12-21 | 2014-04-30 | 湖北鄂信钻石材料有限责任公司 | Vacuum pressing method for superfine carbon green body |
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Denomination of invention: EXT454 ultra-fine-grained structured graphite and preparation method Effective date of registration: 20220815 Granted publication date: 20130904 Pledgee: Bank of China Limited Ezhou branch Pledgor: Believe diamond new material limited liability company in Hubei Province Registration number: Y2022420000257 |
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