CN107721426A - A kind of processing method for the graphite material for preparing mould - Google Patents
A kind of processing method for the graphite material for preparing mould Download PDFInfo
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- CN107721426A CN107721426A CN201711083818.4A CN201711083818A CN107721426A CN 107721426 A CN107721426 A CN 107721426A CN 201711083818 A CN201711083818 A CN 201711083818A CN 107721426 A CN107721426 A CN 107721426A
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Abstract
A kind of processing method for the graphite material for preparing mould is to dissolve to obtain thermosetting resin impregnating agent by thermosetting resin and solvent；Mould is placed in impregnating equipment with graphite blank after vacuumizing and adds thermosetting resin impregnating agent and impregnated, dipping rear mold is solidified with graphite blank, after calcination process under inert atmosphere, obtain mould graphite blank.The present invention has that technique is simple, and cost is low, and the advantages of can be mass-produced.
Description
Technical field
The invention belongs to a kind of manufacture method of graphite material, and in particular to a kind of processing for the graphite material for preparing mould
Method.
Background technology
Due to graphite material have easy processing, radiation proof, corrosion-resistant, thermoelectricity capability is good, heat shock resistance, red hardness and good
The characteristic such as processed surface smoothness, be widely used in mould especially die material field.At present, commercialized graphite
Mould sorting requires high (it is required that graphite raw material purity is high, density is big, granularity is as small as possible), and this undoubtedly increases graphite jig
Manufacture difficulty and processing cost.At present, can be used for processing the graphite species of high terminal mould and few, graphite jig in domestic graphite
Raw material supply external dependence degree is high, and (the main supplier of high-end graphite has in the world：Japan, POCO, Xi Geli, excellent card, step are high, smart
The well-known Tan Su enterprises such as Supreme Being, the East Sea, U.S. Ademilson).
In graphite material manufacturing process, hole defect is inevitably resulted from inside base substrate, these defects will be tight
The mechanical performance and processed surface smoothness of graphite material are had influence on again, and this will significantly limit its answering in mould manufacture field
With.In order to reduce the quantity and size of base substrate inner void defect in graphite manufacturing process, generally use reduces aggregate Jiao's particle
Spend (submicron order), increase the methods of briquetting pressure and hot pressure sintering.These methods considerably increase mould graphite material system
Standby difficulty and cost.
The content of the invention
The technical problems to be solved by the invention are for above shortcomings in the prior art, there is provided a kind of technique letter
Single, cost is low, and the processing method for the graphite material for preparing mould that can be mass-produced.
The present invention is by thermosetting resin impregnated graphite die blank, is then solidified the graphite blank after dipping
And high-temperature roasting processing, to obtain low compactness height, percent opening, surfacing and the graphite jig blank of excellent in mechanical performance.
Due to thermosetting resin is cured and high-temperature heat treatment caused by carbon residue be filled in graphite jig blank hole, can be effectively
Reduce graphite surface and internal void number and size, improve the density and mechanical performance of graphite base substrate, slow down made graphite mo(u)ld
Structural collapse and degree of oxidation during tool use, extend die life.
The processing method of the present invention, comprises the following steps：
(1) among thermosetting resin, is added into solvent, warming while stirring is to 50-80 DEG C and is completely dissolved resin,
Obtain thermosetting resin impregnating agent；
(2), mould is placed in impregnating equipment with after graphite blank drying process, and impregnating equipment is impregnated into cavity liter
Warm 60-70 DEG C, and 0.01MPa is evacuated to, persistently vacuumize 1-3h；
(3) thermosetting resin impregnating agent is added into impregnating equipment, its addition must ensure that pressurization terminates rear thermosetting tree
Fat impregnating agent liquid level is higher by 10-20mm than graphite blank top, and high pressure inert gas-pressure is passed through then to impregnating equipment inside
To impregnation pressure 0.5-8MPa, constant high-pressure 3-5h is kept, graphite blank is taken out after pressure release, and wipes the adhesion of graphite blank surface
Thermosetting resin impregnating agent, obtain impregnation mold graphite blank, and be placed on ventilation dry 8-24h solvent is volatilized
Totally；
(4) impregnation mold need to be higher than impregnation pressure in step (3) with graphite blank in inert atmosphere, solidifying pressure
0.05-0.2MPa, 130-150 DEG C of solidification temperature, and constant temperature 3-4h are warming up to 1-10 DEG C/h heating rate, obtain curing mold
Tool uses graphite blank；
(5) curing mold under inert atmosphere is warming up to 800- with graphite blank with 2-5 DEG C/min heating rate
2500 DEG C, and constant temperature 1-3h completes calcination process, obtains mould graphite blank；
(6) gained graphite blank in step (5) is detected, works as porosity<5%th, average pore size<It is at 1 μm
It is qualified, when not reaching index, repeat step (1)-(5), until touching the mark.
Preferably, the thermosetting resin in the step (1) can be thermosetting phenolic resin and/or epoxy resin, more
Preferably, to use thermosetting phenolic resin as impregnating agent.
Solvent as described above is toluene and/or absolute ethyl alcohol.Preferably, in the step (1) thermosetting resin with it is molten
The volume ratio of agent is 0.5-1.5:1, it is 65-75 DEG C that maceration extract, which prepares temperature,.
Preferably, the graphite blank used in the step (2) is density>1.7g/cm3Fine grained graphite.
Preferably, the inert gas used in the step (3) is nitrogen or argon gas, impregnation pressure 0.5-0.6MPa,
Maintain 4h.
Preferably, the inert atmosphere used in the step (4) is nitrogen or argon gas, and cure under pressure pressure is 0.6-
0.8MPa, solidification heating rate are 1-5 DEG C/h, hardening time 3.5-3.8h.
Preferably, the inert atmosphere used in the step (5) is argon gas, and heating rate is 2-4 DEG C/min, sintering temperature
For 1800-2200 DEG C, roasting time 1.5-2.5h.
Compared with existing mould makes processing method with graphite material, the present invention has advantages below：
(1) present invention fills mould graphite blank table by carbon residue caused by high fixing carbon thermosetting resin high temperature pyrolysis
Face and internal void, and avoid in conventional method by reducing mould graphite particle degree, increasing briquetting pressure and hot pressure sintering
Etc. process bands come long fabrication cycle, high manufacture difficulty, high processing cost the defects of.
(2) present invention can reduce to mould graphite material sorting requirement to a certain extent, can be suitably low from price
Honest and clean slightly coarse-grain graphite also can reach mould as mould graphite material candidate materials after the PROCESS FOR TREATMENT through the present invention
Has the index request for using low graphite material compactness height, percent opening, surfacing and excellent in mechanical performance.
(3) present invention fills mould graphite blank table by carbon residue caused by high fixing carbon thermosetting resin high temperature pyrolysis
Face and internal void, to obtain low compactness height, percent opening, surfacing and the graphite jig blank of excellent in mechanical performance.By
In thermosetting resin is cured and high-temperature heat treatment caused by carbon residue be filled in graphite jig blank hole, can effectively subtract
Small graphite surface and internal void number and size, the density and mechanical performance of graphite base substrate are improved, slows down made graphite jig
Structural collapse and degree of oxidation during use, extend die life.
(4) heretofore described technique can effectively improve mould graphite material density about 1.6%-8.5%, compression strength
About 10%-17%, porosity about 65%-80%, the average pore size about 62- of mould graphite material can be effectively reduced
80%.
Brief description of the drawings
Fig. 1 is the flow chart of the present invention.
Embodiment
For the ease of the understanding of those skilled in the art, with reference to example, the present invention is further illustrated；And this
The scope of the claims of invention is not limited by the example.
Embodiment 1
1st, formulated phenolic resin maceration extract：By thermosetting phenolic resin and absolute ethyl alcohol according to volume ratio 0.5:After 1 mixing,
It is put into water-bath to heat while stirring to resin and is completely dissolved and stand-by in 50 DEG C of constant temperature.
2nd, by after the ISEM-8 graphite blank drying process for preparing mould, it is placed in impregnating equipment, it is permanent after being warming up to 70 DEG C
Temperature simultaneously starts to vacuumize and dipping inside cavity air pressure is reduced to 0.01MPa (persistently vacuumizing 1h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 10mm than graphite blank top), it is passed through high pressure nitrogen then to impregnating equipment inside and is forced into 0.5MPa,
Constant high-pressure 4h is kept, graphite blank is taken out after pressure release and wipes the resin maceration extract of graphite blank surface adhesion, impregnated
Graphite blank and being placed on ventilation and drying 8h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into nitrogen in high-tension apparatus to be forced into 0.55MPa and be warming up to 140 DEG C according to 1 DEG C/h
And constant temperature 3h, obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 800 DEG C under argon gas atmosphere with 2 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 2h completes calcination process, graphite jig blank is obtained.
6th, detection case is carried out to gained graphite blank in step (5), its porosity is 4.2%, average pore size is
0.8 μm, reach the purpose for effectively reducing graphite blank porosity machine average pore size in step (1), obtained graphite jig blank.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Porosity | Average pore size |
| ISEM-8 (untreated) | 1.78 | 106 | 16.6% | 2.4μm |
| ISEM-8 (after processing) | 1.86 | 120 | 4.2% | 0.8μm |
Embodiment 2
1st, formulated phenolic resin maceration extract：By thermosetting phenolic resin and absolute ethyl alcohol according to volume ratio 0.7:After 1 mixing,
It is put into water-bath to heat while stirring to resin and is completely dissolved and stand-by in 70 DEG C of constant temperature.
2nd, by after the ISEM-8 graphite blank drying process for preparing mould, it is placed in impregnating equipment, it is permanent after being warming up to 70 DEG C
Temperature simultaneously starts to vacuumize and dipping inside cavity air pressure is reduced to 0.01MPa (persistently vacuumizing 2h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 15mm than graphite blank top), it is passed through high pressure nitrogen then to impregnating equipment inside and is forced into 0.6MPa,
Constant high-pressure 4h is kept, graphite blank is taken out after pressure release and wipes the resin maceration extract of graphite blank surface adhesion, impregnated
Graphite blank and being placed on ventilation and drying 12h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into nitrogen in high-tension apparatus to be forced into 0.7MPa and be warming up to 140 DEG C according to 2 DEG C/h
And constant temperature 3.6h, obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 1000 DEG C under argon gas atmosphere with 3 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 2h completes calcination process, graphite jig blank is obtained.
6th, detection case is carried out to gained graphite blank in step (5), its porosity is 4.1%, average pore size is
0.7 μm, reach the purpose for effectively reducing graphite blank porosity machine average pore size in step (1), obtained graphite jig blank.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Porosity | Average pore size |
| ISEM-8 (untreated) | 1.78 | 106 | 16.6% | 2.4μm |
| ISEM-8 (after processing) | 1.88 | 123 | 4.1% | 0.7μm |
Embodiment 3
1st, formulated phenolic resin maceration extract：By thermosetting phenolic resin and absolute ethyl alcohol according to volume ratio 1:After 1 mixing, put
Enter to heat while stirring to resin in water-bath and be completely dissolved and stand-by in 60 DEG C of constant temperature.
2nd, by after the ISEM-8 graphite blank drying process for preparing mould, it is placed in impregnating equipment, it is permanent after being warming up to 70 DEG C
Temperature simultaneously starts to vacuumize and dipping inside cavity air pressure is reduced to 0.01MPa (persistently vacuumizing 3h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 20mm than graphite blank top), it is passed through high pressure nitrogen then to impregnating equipment inside and is forced into 2MPa, protects
Constant high-pressure 4h is held, graphite blank is taken out after pressure release and wipes the resin maceration extract of graphite blank surface adhesion, obtains impregnating stone
Black blank and being placed on ventilation and drying 24h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into nitrogen in high-tension apparatus to be forced into 2.1MPa and be warming up to 140 DEG C according to 2 DEG C/h
And constant temperature 4h, obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 1200 DEG C under argon gas atmosphere with 5 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 1h completes calcination process, graphite jig blank is obtained.
6th, detection case is carried out to gained graphite blank in step (5), its porosity is 3.9%, average pore size is
0.6 μm, reach the purpose for effectively reducing graphite blank porosity machine average pore size in step (1), obtained graphite jig blank.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Porosity | Average pore size |
| ISEM-8 (untreated) | 1.78 | 106 | 16.6% | 2.4μm |
| ISEM-8 (after processing) | 1.89 | 121 | 3.9% | 0.6μm |
Embodiment 4
1st, formulated phenolic resin maceration extract：By thermosetting phenolic resin and absolute ethyl alcohol according to volume ratio 1.2:After 1 mixing,
It is put into water-bath to heat while stirring to resin and is completely dissolved and stand-by in 80 DEG C of constant temperature.
2nd, by after the ISEM-8 graphite blank drying process for preparing mould, it is placed in impregnating equipment, it is permanent after being warming up to 70 DEG C
Temperature simultaneously starts to vacuumize and dipping inside cavity air pressure is reduced to 0.01MPa (persistently vacuumizing 2h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 10mm than graphite blank top), it is passed through high pressure nitrogen then to impregnating equipment inside and is forced into 5MPa, protects
Constant high-pressure 4h is held, graphite blank is taken out after pressure release and wipes the resin maceration extract of graphite blank surface adhesion, obtains impregnating stone
Black blank and being placed on ventilation and drying 12h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into nitrogen in high-tension apparatus to be forced into 5.2MPa and be warming up to 140 DEG C according to 3 DEG C/h
And constant temperature 3.6h, obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 1500 DEG C under argon gas atmosphere with 3 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 2h completes calcination process, graphite jig blank is obtained.
6th, detection case is carried out to gained graphite blank in step (5), its porosity is 3.6%, average pore size is
0.58 μm, reach the purpose for effectively reducing graphite blank porosity machine average pore size in step (1), obtained graphite jig base
Material.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Porosity | Average pore size |
| ISEM-8 (untreated) | 1.78 | 106 | 16.6% | 2.4μm |
| ISEM-8 (after processing) | 1.91 | 124 | 3.6% | 0.58μm |
Embodiment 5
1st, formulated phenolic resin maceration extract：By thermosetting phenolic resin and absolute ethyl alcohol according to volume ratio 1.5:After 1 mixing,
It is put into water-bath to heat while stirring to resin and is completely dissolved and stand-by in 80 DEG C of constant temperature.
2nd, by after the ISEM-8 graphite blank drying process for preparing mould, it is placed in impregnating equipment, it is permanent after being warming up to 70 DEG C
Temperature simultaneously starts to vacuumize and dipping inside cavity air pressure is reduced to 0.01MPa (persistently vacuumizing 1h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 15mm than graphite blank top), it is passed through high pressure nitrogen then to impregnating equipment inside and is forced into 8MPa, protects
Constant high-pressure 4h is held, graphite blank is taken out after pressure release and wipes the resin maceration extract of graphite blank surface adhesion, obtains impregnating stone
Black blank and being placed on ventilation and drying 8h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into nitrogen in high-tension apparatus to be forced into 8.1MPa and be warming up to 140 DEG C according to 5 DEG C/h
And constant temperature 3.6h, obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 2000 DEG C under argon gas atmosphere with 2 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 1h completes calcination process, graphite jig blank is obtained.
6th, detection case is carried out to gained graphite blank in step (5), its porosity is 3.4%, average pore size is
0.5 μm, reach the purpose for effectively reducing graphite blank porosity machine average pore size in step (1), obtained more preferable graphite mo(u)ld
Has blank.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Porosity | Average pore size |
| ISEM-8 (untreated) | 1.78 | 106 | 16.6% | 2.4μm |
| ISEM-8 (after processing) | 1.93 | 124 | 3.4% | 0.5μm |
Embodiment 6
1st, epoxy phenolics maceration extract is prepared：By thermosetting phenolic resin, epoxy resin, toluene and absolute ethyl alcohol according to
Volume ratio 1:2:1:After 2 mixing, it is put into water-bath to heat while stirring to resin and is completely dissolved and stand-by in 65 DEG C of constant temperature.
2nd, mould is placed in impregnating equipment with after ISEM-8 graphite blank drying process, constant temperature is simultaneously after being warming up to 65 DEG C
Starting to vacuumize makes dipping inside cavity air pressure be reduced to 0.01MPa (persistently vacuumizing 2h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 20mm than graphite blank top), it is passed through high-pressure inert gas then to impregnating equipment inside and is forced into
0.6MPa, constant high-pressure 4h is kept, take out graphite blank after pressure release and wipe the resin maceration extract of graphite blank surface adhesion, obtain
To impregnated graphite blank and being placed on ventilation drying 24h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into inert gas in high-tension apparatus to be forced into 0.7MPa and be warming up to according to 1 DEG C/h
140 DEG C and constant temperature 3.6h (ensureing that the resin solidification in graphite blank hole is complete), obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 2200 DEG C under argon gas atmosphere with 3 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 2h completes calcination process, graphite jig blank is obtained.
6th, be 8.2% according to gained graphite blank detection case its porosity in step (5), average pore size be 1.3 μ
M, be not inconsistent standardization, to its repeat step (1)-(5) once after, its porosity is 4.7%, average pore size is 0.8 μm, is reached
To effective purpose for reducing graphite blank porosity machine average pore size in step (1), more preferable graphite jig blank has been obtained.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Porosity | Average pore size |
| ISEM-8 (untreated) | 1.78 | 106 | 16.6% | 2.4μm |
| ISEM-8 (after 2 processing) | 1.84 | 119 | 4.7% | 0.8μm |
Embodiment 7
1st, epoxy phenolics maceration extract is prepared：By thermosetting phenolic resin, epoxy resin, toluene and absolute ethyl alcohol according to
Volume ratio 1.5:2:1:After 2 mixing, it is put into water-bath to heat while stirring to resin and is completely dissolved and stand-by in 65 DEG C of constant temperature.
2nd, mould is placed in impregnating equipment with after ISEM-8 graphite blank drying process, constant temperature is simultaneously after being warming up to 65 DEG C
Starting to vacuumize makes dipping inside cavity air pressure be reduced to 0.01MPa (persistently vacuumizing 2h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 15mm than graphite blank top), it is passed through high-pressure inert gas then to impregnating equipment inside and is forced into
0.6MPa, constant high-pressure 4h is kept, take out graphite blank after pressure release and wipe the resin maceration extract of graphite blank surface adhesion, obtain
To impregnated graphite blank and being placed on ventilation drying 12h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into inert gas in high-tension apparatus to be forced into 0.65MPa and be warming up to according to 3 DEG C/h
140 DEG C and constant temperature 3h (ensureing that the resin solidification in graphite blank hole is complete), obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 2500 DEG C under argon gas atmosphere with 3 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 1h completes calcination process, graphite jig blank is obtained.
6th, be 8.2% according to gained graphite blank detection case its porosity in step (5), average pore size be 1.3 μ
M, be not inconsistent standardization, to its repeat step (1)-(5) once after, its porosity is 4.6%, average pore size is 0.6 μm, is reached
To effective purpose for reducing graphite blank porosity machine average pore size in step (1), graphite jig blank has been obtained.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Porosity | Average pore size |
| ISEM-8 (untreated) | 1.78 | 106 | 16.6% | 2.4μm |
| ISEM-8 (after 2 processing) | 1.86 | 121 | 4.6% | 0.6μm |
Embodiment 8
1st, epoxy phenolics maceration extract is prepared：By thermosetting phenolic resin, epoxy resin, toluene and absolute ethyl alcohol according to
Volume ratio 1:1.5:1.5:After 1 mixing, it is put into water-bath to heat while stirring to resin and is completely dissolved and is treated in 65 DEG C of constant temperature
With.
2nd, mould is placed in impregnating equipment with after ISEM-8 graphite blank drying process, constant temperature is simultaneously after being warming up to 65 DEG C
Starting to vacuumize makes dipping inside cavity air pressure be reduced to 0.01MPa (persistently vacuumizing 3h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 15mm than graphite blank top), it is passed through high-pressure inert gas then to impregnating equipment inside and is forced into
0.6MPa, constant high-pressure 4h is kept, take out graphite blank after pressure release and wipe the resin maceration extract of graphite blank surface adhesion, obtain
To impregnated graphite blank and being placed on ventilation drying 12h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into inert gas in high-tension apparatus to be forced into 0.7MPa and be warming up to according to 10 DEG C/h
140 DEG C and constant temperature 3.5h (ensureing that the resin solidification in graphite blank hole is complete), obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 2000 DEG C under argon gas atmosphere with 3 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 2h completes calcination process, graphite jig blank is obtained.
6th, be 8.2% according to gained graphite blank detection case its porosity in step (5), average pore size be 1.3 μ
M, be not inconsistent standardization, to its repeat step (1)-(5) once after, its porosity is 4.2%, average pore size is 0.5 μm, is reached
To effective purpose for reducing graphite blank porosity machine average pore size in step (1), graphite jig blank has been obtained.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Porosity | Average pore size |
| ISEM-8 (untreated) | 1.78 | 106 | 16.6% | 2.4μm |
| ISEM-8 (after 2 processing) | 1.88 | 123 | 4.2% | 0.5μm |
Embodiment 9
1st, formulated phenolic resin maceration extract：By thermosetting phenolic resin and absolute ethyl alcohol according to volume ratio 1:After 1 mixing, put
Enter to heat while stirring to resin in water-bath and be completely dissolved and stand-by in 70 DEG C of constant temperature.
2nd, mould is placed in impregnating equipment with after R8510 graphite blank drying process, constant temperature and opened after being warming up to 70 DEG C
Beginning, which vacuumizes, makes dipping inside cavity air pressure be reduced to 0.01MPa (persistently vacuumizing 2h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 15mm than graphite blank top), it is passed through high-pressure inert gas then to impregnating equipment inside and is forced into
0.6MPa, constant high-pressure 4h is kept, take out graphite blank after pressure release and wipe the resin maceration extract of graphite blank surface adhesion, obtain
To impregnated graphite blank and being placed on ventilation drying 12h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into inert gas in high-tension apparatus to be forced into 0.8MPa and be warming up to according to 7 DEG C/h
140 DEG C and constant temperature 4h (ensureing that the resin solidification in graphite blank hole is complete), obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 2200 DEG C under argon gas atmosphere with 3 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 2h completes calcination process, graphite jig blank is obtained.
Caused resin carbon is filled in mould R8510 graphite blank inside openings after thermosetting phenolic resin pyrolytic
Among hole, the pore-size and porosity of R8510 graphite matrixs are greatly reduced.
It is as shown in the table with the performance test results before and after R8510 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Percent opening | Average pore size |
| R8510 (untreated) | 1.83 | 125 | 10% | 1.5μm |
| R8510 (after processing) | 1.88 | 140 | 3% | 0.53μm |
Embodiment 10
1st, epoxy phenolics maceration extract is prepared：By thermosetting phenolic resin, epoxy resin, toluene and absolute ethyl alcohol according to
Volume ratio 1:2:1.5:After 1 mixing, it is put into water-bath to heat while stirring to resin and is completely dissolved and stand-by in 65 DEG C of constant temperature.
2nd, mould is placed in impregnating equipment with after R8510 graphite blank drying process, constant temperature and opened after being warming up to 65 DEG C
Beginning, which vacuumizes, makes dipping inside cavity air pressure be reduced to 0.01MPa (persistently vacuumizing 2h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 15mm than graphite blank top), it is passed through high-pressure inert gas then to impregnating equipment inside and is forced into
0.6MPa, constant high-pressure 4h is kept, take out graphite blank after pressure release and wipe the resin maceration extract of graphite blank surface adhesion, obtain
To impregnated graphite blank and being placed on ventilation drying 12h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into inert gas in high-tension apparatus to be forced into 0.7MPa and be warming up to according to 5 DEG C/h
140 DEG C and constant temperature 3.6h (ensureing that the resin solidification in graphite blank hole is complete), obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 2000 DEG C under argon gas atmosphere with 3 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 3h completes calcination process, graphite jig blank is obtained.
Caused resin carbon is filled in mould R8510 graphite blank inside openings after thermosetting phenolic resin pyrolytic
Among hole, the pore-size and porosity of R8510 graphite matrixs are greatly reduced.
It is as shown in the table with the performance test results before and after R8510 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Percent opening | Average pore size |
| R8510 (untreated) | 1.83 | 125 | 10% | 1.5μm |
| R8510 (after processing) | 1.86 | 138 | 3.5% | 0.56μm |
Embodiment 11
1st, formulated phenolic resin maceration extract：By thermosetting phenolic resin and toluene according to volume ratio 1:After 1 mixing, water is put into
Heat while stirring to resin and be completely dissolved and stand-by in 50 DEG C of constant temperature in bath.
2nd, by after the ISEM-8 graphite blank drying process for preparing mould, it is placed in impregnating equipment, it is permanent after being warming up to 70 DEG C
Temperature simultaneously starts to vacuumize and dipping inside cavity air pressure is reduced to 0.01MPa (persistently vacuumizing 1h).
3rd, thermosetting phenolic resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting phenolic resin
Maceration extract liquid level is higher by 10mm than graphite blank top), it is passed through high pressure nitrogen then to impregnating equipment inside and is forced into 0.5MPa,
Constant high-pressure 4h is kept, graphite blank is taken out after pressure release and wipes the resin maceration extract of graphite blank surface adhesion, impregnated
Graphite blank and being placed on ventilation and drying 8h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into nitrogen in high-tension apparatus to be forced into 0.55MPa and be warming up to 140 DEG C according to 1 DEG C/h
And constant temperature 3h, obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 900 DEG C under argon gas atmosphere with 2 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 2h completes calcination process, graphite jig blank is obtained.
6th, detection case is carried out to gained graphite blank in step (5), its porosity is 4.3%, average pore size is
0.9 μm, reach the purpose for effectively reducing graphite blank porosity machine average pore size in step (1), obtained graphite jig blank.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Porosity | Average pore size |
| ISEM-8 (untreated) | 1.78 | 106 | 16.6% | 2.4μm |
| ISEM-8 (after processing) | 1.84 | 118 | 4.3% | 0.9μm |
Embodiment 12
1st, epoxy resin maceration extract is prepared：By thermosetting epoxy resin and absolute ethyl alcohol according to volume ratio 0.8:After 1 mixing,
It is put into water-bath to heat while stirring to resin and is completely dissolved and stand-by in 60 DEG C of constant temperature.
2nd, by after the ISEM-8 graphite blank drying process for preparing mould, it is placed in impregnating equipment, it is permanent after being warming up to 60 DEG C
Temperature simultaneously starts to vacuumize and dipping inside cavity air pressure is reduced to 0.01MPa (persistently vacuumizing 1h).
3rd, thermosetting epoxy resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting epoxy resin
Maceration extract liquid level is higher by 10mm than graphite blank top), it is passed through high pressure nitrogen then to impregnating equipment inside and is forced into 0.5MPa,
Constant high-pressure 4h is kept, graphite blank is taken out after pressure release and wipes the resin maceration extract of graphite blank surface adhesion, impregnated
Graphite blank and being placed on ventilation and drying 10h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into nitrogen in high-tension apparatus to be forced into 0.55MPa and be warming up to 140 DEG C according to 1 DEG C/h
And constant temperature 3h, obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 1000 DEG C under argon gas atmosphere with 2 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 2h completes calcination process, graphite jig blank is obtained.
6th, detection case is carried out to gained graphite blank in step (5), its porosity is 4.1%, average pore size is
0.7 μm, reach the purpose for effectively reducing graphite blank porosity machine average pore size in step (1), obtained graphite jig blank.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
| Sample name | Density g/cm3 | Compression strength MPa | Porosity | Average pore size |
| ISEM-8 (untreated) | 1.78 | 106 | 16.6% | 2.4μm |
| ISEM-8 (after processing) | 1.85 | 120 | 4.1% | 0.7μm |
Embodiment 13
1st, epoxy resin maceration extract is prepared：By thermosetting epoxy resin and toluene according to volume ratio 1:After 1 mixing, water is put into
Heat while stirring to resin and be completely dissolved and stand-by in 60 DEG C of constant temperature in bath.
2nd, by after the ISEM-8 graphite blank drying process for preparing mould, it is placed in impregnating equipment, it is permanent after being warming up to 70 DEG C
Temperature simultaneously starts to vacuumize and dipping inside cavity air pressure is reduced to 0.01MPa (persistently vacuumizing 1h).
3rd, thermosetting epoxy resin maceration extract is added into impregnating equipment (must ensure that pressurization terminates rear thermosetting epoxy resin
Maceration extract liquid level is higher by 10mm than graphite blank top), it is passed through high pressure nitrogen then to impregnating equipment inside and is forced into 0.5MPa,
Constant high-pressure 4h is kept, graphite blank is taken out after pressure release and wipes the resin maceration extract of graphite blank surface adhesion, impregnated
Graphite blank and being placed on ventilation and drying 8h makes solvent volatilization clean.
4th, impregnated graphite blank is placed in into nitrogen in high-tension apparatus to be forced into 0.55MPa and be warming up to 140 DEG C according to 1 DEG C/h
And constant temperature 3h, obtain solidification graphite blank.
5th, graphite blank will be solidified and is warming up to 800 DEG C under argon gas atmosphere with 2 DEG C/min temperature increasing schedule in high temperature furnace
And constant temperature 2h completes calcination process, graphite jig blank is obtained.
6th, detection case is carried out to gained graphite blank in step (5), its porosity is 4%, average pore size 0.6
μm, reach the purpose for effectively reducing graphite blank porosity machine average pore size in step (1), obtain graphite jig blank.
It is as shown in the table with the performance test results before and after ISEM-8 graphite blank impregnations to mould：
。
Claims (9)
1. a kind of processing method for the graphite material for preparing mould, it is characterised in that comprise the following steps：
(1) among thermosetting resin, is added into solvent, warming while stirring is to 50-80 DEG C and is completely dissolved resin, obtains
Thermosetting resin impregnating agent；
(2), mould is placed in impregnating equipment with after graphite blank drying process, and impregnating equipment is impregnated into cavity heating 60-
70 DEG C, and 0.01MPa is evacuated to, persistently vacuumize 1-3h；
(3) thermosetting resin impregnating agent is added into impregnating equipment, its addition must ensure that pressurization terminates rear thermosetting resin leaching
Stain agent liquid level is higher by 10-20mm than graphite blank top, and high pressure inert gas-pressure is passed through to leaching then to impregnating equipment inside
Stain pressure 0.5-8MPa, constant high-pressure 3-5h is kept, graphite blank is taken out after pressure release, and wipe the heat of graphite blank surface adhesion
Thermosetting resin impregnating agent, impregnation mold graphite blank is obtained, and being placed on ventilation drying 8-24h makes solvent volatilization dry
Only；
(4) impregnation mold need to be higher than step with graphite blank in inert atmosphere, solidifying pressure（3）Middle impregnation pressure 0.05-
0.2MPa, 130-150 DEG C of solidification temperature, and constant temperature 3-4h are warming up to 1-10 DEG C/h heating rate, obtain curing mold and use
Graphite blank；
(5) curing mold under inert atmosphere is warming up to 800-2500 DEG C with graphite blank with 2-5 DEG C/min heating rate,
And constant temperature 1-3h completes calcination process, mould graphite blank is obtained；
(6) gained graphite blank in step (5) is detected, works as porosity<5%th, average pore size<To be qualified at 1 μm,
When not reaching index, repeat step（1）-（5）, until touching the mark.
A kind of 2. processing method for the graphite material for preparing mould as claimed in claim 1, it is characterised in that the step (1)
In thermosetting resin be thermosetting phenolic resin and/or epoxy resin.
A kind of 3. processing method for the graphite material for preparing mould as claimed in claim 2, it is characterised in that the step (1)
In thermosetting resin be thermosetting phenolic resin.
A kind of 4. processing method for the graphite material for preparing mould as claimed in claim 1, it is characterised in that described solvent
For toluene and/or absolute ethyl alcohol.
A kind of 5. processing method for the graphite material for preparing mould as claimed in claim 1, it is characterised in that the step (1)
The volume ratio of middle thermosetting resin and solvent is 0.5-1.5:1, it is 65-75 DEG C that maceration extract, which prepares temperature,.
A kind of 6. processing method for the graphite material for preparing mould as claimed in claim 1, it is characterised in that the step (2)
The middle graphite blank used is density>1.7g/cm3Fine grained graphite.
A kind of 7. processing method for the graphite material for preparing mould as claimed in claim 1, it is characterised in that the step (3)
The middle inert gas used is nitrogen or argon gas, impregnation pressure 0.5-0.6MPa, maintains 4h.
A kind of 8. processing method for the graphite material for preparing mould as claimed in claim 1, it is characterised in that the step (4)
The middle inert atmosphere used is nitrogen or argon gas, and cure under pressure pressure is 0.6-0.8MPa, and solidification heating rate is 1-5 DEG C/h,
Hardening time is 3.5-3.8h.
A kind of 9. processing method for the graphite material for preparing mould as claimed in claim 1, it is characterised in that the step (5)
The middle inert atmosphere used is argon gas, and heating rate is 2-4 DEG C/min, and sintering temperature is 1800-2200 DEG C, and roasting time is
1.5-2.5h。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110372414A (en) * | 2019-07-11 | 2019-10-25 | 上海应用技术大学 | The method of phenol-formaldehyde resin modified promotion impregnated graphite performance |
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