CN107573073A - Graphite product and preparation method thereof - Google Patents
Graphite product and preparation method thereof Download PDFInfo
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- CN107573073A CN107573073A CN201710573406.2A CN201710573406A CN107573073A CN 107573073 A CN107573073 A CN 107573073A CN 201710573406 A CN201710573406 A CN 201710573406A CN 107573073 A CN107573073 A CN 107573073A
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Abstract
The present invention relates to a kind of graphite product and preparation method thereof, preparation method comprises the following steps：S1：Graphite material is crushed, is then well mixed with binding agent；S2：The obtained mixtures of step S1 are put into mould, are heated to 50~100 DEG C of progress rigid mould compactings；S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product.The graphite product that the present invention is prepared, has that density is big, surface accuracy is high, thermal coefficient of expansion is small, thermal diffusivity and thermal conductivity are high, heat transfer is fast, resistance to compression and the anti-excellent properties such as roll well；And preparation method is simple, production cost is low.
Description
Technical field
The present invention relates to graphite material technical field, and in particular to a kind of graphite product and preparation method thereof.
Background technology
Graphite (graphite) is a kind of crystalline carbon, hexagonal crystal system, is iron mass colour to Dark grey；Matter is soft, have soapy feeling,
It is electrically conductive.Pot be household implements the most frequently used in people's daily life, pot on the market is largely iron pan, but its have it is resistance to
The shortcomings of heat rating is small, and thermal coefficient of expansion is big, thermal diffusivity and thermal conductivity are small；There is also use pot, ceramic pan made of ceramics
Although thermal conductivity is high and thermal coefficient of expansion is small, its resistance to heat rating is small and easily rupturable；The health pot made of high borosilicate also be present,
Although it has relatively low thermal coefficient of expansion, it is insensitive to heat.Therefore, it is also desirable to develop the pot system of excellent combination property
Product, to meet consumer demand.
The content of the invention
For in the prior art the defects of, present invention aims at a kind of graphite product and preparation method thereof is provided, to carry
The density and surface accuracy of high graphite product, thermal coefficient of expansion is reduced, improves thermal diffusivity and thermal conductivity, accelerate rate of heat transfer,
Strengthen resistance to compression and fracture resistance.
To achieve the above object, technical scheme provided by the invention is：
In a first aspect, the invention provides a kind of preparation method of graphite product, comprise the following steps：S1：By graphite material
Feed powder is broken, is then well mixed with binding agent；S2：The obtained mixtures of step S1 are put into mould, it is heated to 50~
100 DEG C of progress rigid mould compactings；S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product.
In the further embodiment of the present invention, in step S1, the mass ratio of graphite material and binding agent is 100:(5
~10)；Particle diameter after graphite material crushes is less than 100 μm.It should be noted that graphite material includes graphite.
In the further embodiment of the present invention, in step S2, the time of rigid mould compacting is 25~35min.
In the further embodiment of the present invention, in step S3, hot pressed sintering includes the first temperature-rise period, second successively
Increasing temperature and pressure and constant temperature and pressure process and temperature-fall period：In first temperature-rise period, mechanical pressure is 20~22MPa, and with 20~
40 DEG C/min heating rate is warming up to 2500 DEG C；During second increasing temperature and pressure and constant temperature and pressure, mechanical pressure is linearly risen
Up to 26~28MPa, temperature linearity is increased to 2900~3100 DEG C, and makes temperature and pressure while reach maximum, afterwards
22~26h of constant temperature and pressure；Wherein, heating rate is 10~15 DEG C/min；In temperature-fall period, holding mechanical pressure is maximum,
15~30 DEG C are cooled to 120~150 DEG C/h rate of temperature fall.
In the further embodiment of the present invention, in step S2, mould includes：Frying pan mould, slaughterhouse mould, iron
One or more in cake pot mould and Barbecuing plate mould.
In the further embodiment of the present invention, in step S1, the preparation method of graphite material comprises the following steps：
S101：Graphite powder is added in ethanol eugenol mixed solution, it is ultrasonic after being uniformly dispersed；S102：Step S101 is obtained mixed
Compound, alumina powder and nickel powder are added in dibutyl hydroxy toluene cloves phenol solution, and preset time is stood after well mixed；
S103：In the product drying that step S102 is obtained, the solid of collection and the pig iron, calcium oxide, zirconium oxide are well mixed, obtain stone
Ink material.
In the further embodiment of the present invention, in step S101, the matter of graphite powder and ethanol eugenol mixed solution
Amount is than being 1:(8~10), in ethanol eugenol mixed solution, the mass ratio of ethanol and eugenol is 1:(0.8~1.0), ultrasound
Power be 500~600W, the ultrasonic time is 45~60min.
In the further embodiment of the present invention, in step S102, graphite powder, alumina powder, nickel powder and dibutyl hydroxyl
The mass ratio of base toluene cloves phenol solution is 1:(0.1~0.15):(0.02~0.05):(15~20), time of standing for 5~
6h, in dibutyl hydroxy toluene cloves phenol solution, the mass ratio of dibutyl hydroxy toluene and eugenol is 1:(0.5~0.6).
In the further embodiment of the present invention, in step S103, graphite powder, the pig iron, calcium oxide, the quality of zirconium oxide
Than for 1:(0.02~0.03):(0.02~0.06):(0.01~0.02).
Second aspect, the present invention also protect the graphite product being prepared according to above-mentioned preparation method.
Technical scheme provided by the invention, there is following beneficial effect：(1) graphite product density provided by the invention is high
And it is evenly distributed；And surface accuracy is high, because sintering process raises green density, and in viscous state in sintering
Binding agent has good " leveling " effect, so as to so that graphite product surface accuracy grade improves；(2) it is provided by the invention
Graphite product ejection pressure is small, can reduce die wear, so as to extend its service life；(3) graphite system provided by the invention
The green strength of product significantly improves, and side and arrisdefect equivalent risk so as to substantially reduce that product occurs in transfer process；
(4) the resistance to heat rating of graphite product provided by the invention is big, and thermal coefficient of expansion is small, and thermal diffusivity and thermal conductivity are high, and heat transfer is fast, resistance to compression
It is good with fracture resistance；(5) preparation method of graphite product provided by the invention is simple, and production cost is low.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Embodiment
Below in conjunction with the embodiment of the present invention, technical scheme is clearly and completely described.Implement below
Example is only used for clearly illustrating technical scheme, therefore be intended only as example, and can not limit this hair with this
Bright protection domain.
Experimental method in following embodiments, it is conventional method unless otherwise specified.Examination used in following embodiments
Material is tested, is to be commercially available from regular shops unless otherwise specified.Quantitative test in following examples, is respectively provided with three
Secondary to repeat to test, data are to repeat the average value or mean+SD of experiment three times.
The present invention provides a kind of preparation method of graphite product, comprises the following steps：
S1：Graphite material is crushed to particle diameter less than 100 μm, then with binding agent with 100:The mass ratio of (5~10) mixes
Close uniform；
S2：The obtained mixtures of step S1 are put into mould, are heated to 50~100 DEG C of progress rigid mould compactings,
The time of rigid mould compacting is 25~35min；Wherein, mould includes：Frying pan mould, slaughterhouse mould, pancake pan mould and
One or more in Barbecuing plate mould；
S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product；Wherein, hot pressed sintering
Include the first temperature-rise period, the second increasing temperature and pressure and constant temperature and pressure process and temperature-fall period successively：In first temperature-rise period, machinery
Pressure is 20~22MPa, and is warming up to 2500 DEG C with 20~40 DEG C/min heating rate；Second increasing temperature and pressure and constant temperature and pressure
During, mechanical pressure is linearly increased to 26~28MPa, temperature linearity is increased to 2900~3100 DEG C, and make temperature and
Pressure reaches maximum simultaneously, afterwards 22~26h of constant temperature and pressure；Wherein, heating rate is 10~15 DEG C/min；Temperature-fall period
In, holding mechanical pressure is maximum, and 15~30 DEG C are cooled to 120~150 DEG C/h rate of temperature fall.
Preferably, the preparation method of graphite material comprises the following steps：
S101：Graphite powder is added in ethanol eugenol mixed solution, 500~600W ultrasounds 45 after being uniformly dispersed~
60min；Wherein, the mass ratio of graphite powder and ethanol eugenol mixed solution is 1:(8~10), ethanol eugenol mixed solution
In, the mass ratio of ethanol and eugenol is 1:(0.8~1.0)；
S102：Mixture, alumina powder and the nickel powder that step S101 is obtained are added to dibutyl hydroxy toluene eugenol
In solution, 5~6h is stood after being well mixed；Wherein, graphite powder, alumina powder, nickel powder and dibutyl hydroxy toluene eugenol are molten
The mass ratio of liquid is 1:(0.1~0.15):(0.02~0.05):(15~20), in dibutyl hydroxy toluene cloves phenol solution, two
The mass ratio of butylated hydroxytoluene and eugenol is 1:(0.5~0.6)；
S103：In the product drying that step S102 is obtained, the solid of collection and the pig iron, calcium oxide, zirconium oxide are mixed equal
It is even, obtain graphite material；Wherein, graphite powder, the pig iron, calcium oxide, the mass ratio of zirconium oxide are 1:(0.02~0.03):(0.02
~0.06):(0.01~0.02).
Graphite product provided by the invention and preparation method thereof is described further with reference to specific embodiment.
Embodiment one
The present embodiment provides a kind of preparation method of graphite product, comprises the following steps：
S1：Graphite material (graphite powder) is crushed to particle diameter less than 100 μm, then with binding agent with 100:5 mass ratio
It is well mixed；
S2：The obtained mixtures of step S1 are put into shaping slaughterhouse mould, are heated to 50 DEG C of progress rigid mould compactings, just
Property molding system time be 25min；
S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product；Wherein, hot pressed sintering
Include the first temperature-rise period, the second increasing temperature and pressure and constant temperature and pressure process and temperature-fall period successively：In first temperature-rise period, machinery
Pressure is 20MPa, and is warming up to 2500 DEG C with 20 DEG C/min heating rate；During second increasing temperature and pressure and constant temperature and pressure,
Mechanical pressure is linearly increased to 26MPa, temperature linearity is increased to 2900 DEG C, and makes temperature and pressure while reaches maximum
It is worth, afterwards constant temperature and pressure 22h；Wherein, heating rate is 10 DEG C/min；In temperature-fall period, holding mechanical pressure is maximum, with
120 DEG C/h rate of temperature fall is cooled to 15 DEG C.
Embodiment two
The present embodiment provides a kind of preparation method of graphite product, comprises the following steps：
S1：Graphite material (graphite powder) is crushed to particle diameter less than 100 μm, then with binding agent with 100:10 mass ratio
It is well mixed；
S2：The obtained mixtures of step S1 are put into shaping slaughterhouse mould, are heated to 100 DEG C of progress rigid mould compactings,
The time of rigid mould compacting is 35min；
S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product；Wherein, hot pressed sintering
Include the first temperature-rise period, the second increasing temperature and pressure and constant temperature and pressure process and temperature-fall period successively：In first temperature-rise period, machinery
Pressure is 22MPa, and is warming up to 2500 DEG C with 40 DEG C/min heating rate；During second increasing temperature and pressure and constant temperature and pressure,
Mechanical pressure is linearly increased to 28MPa, temperature linearity is increased to 3100 DEG C, and makes temperature and pressure while reaches maximum
It is worth, afterwards constant temperature and pressure 26h；Wherein, heating rate is 15 DEG C/min；In temperature-fall period, holding mechanical pressure is maximum, with
150 DEG C/h rate of temperature fall is cooled to 30 DEG C.
Embodiment three
The present embodiment provides a kind of preparation method of graphite product, comprises the following steps：
S1：Graphite material (graphite powder) is crushed to particle diameter less than 100 μm, then with binding agent with 100:8 mass ratio
It is well mixed；
S2：The obtained mixtures of step S1 are put into shaping slaughterhouse mould, are heated to 80 DEG C of progress rigid mould compactings, just
Property molding system time be 30min；
S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product；Wherein, hot pressed sintering
Include the first temperature-rise period, the second increasing temperature and pressure and constant temperature and pressure process and temperature-fall period successively：In first temperature-rise period, machinery
Pressure is 21MPa, and is warming up to 2500 DEG C with 30 DEG C/min heating rate；During second increasing temperature and pressure and constant temperature and pressure,
Mechanical pressure is linearly increased to 27MPa, temperature linearity is increased to 3000 DEG C, and makes temperature and pressure while reaches maximum
It is worth, afterwards constant temperature and pressure 24h；Wherein, heating rate is 13 DEG C/min；In temperature-fall period, holding mechanical pressure is maximum, with
135 DEG C/h rate of temperature fall is cooled to 25 DEG C.
Example IV
The present embodiment provides a kind of preparation method of graphite product, comprises the following steps：
S1：Graphite material is crushed to particle diameter less than 100 μm, then with binding agent with 100:5 mass ratio is well mixed；
Wherein, the preparation method of graphite material comprises the following steps：
S101：Graphite powder is added in ethanol eugenol mixed solution, 500W ultrasounds 45min after being uniformly dispersed；Wherein, stone
The mass ratio of ink powder and ethanol eugenol mixed solution is 1:8, in ethanol eugenol mixed solution, the quality of ethanol and eugenol
Than for 1:0.8；
S102：Mixture, alumina powder and the nickel powder that step S101 is obtained are added to dibutyl hydroxy toluene eugenol
In solution, 5h is stood after well mixed；Wherein, graphite powder, alumina powder, nickel powder and dibutyl hydroxy toluene cloves phenol solution
Mass ratio is 1:0.1:0.02:15, in dibutyl hydroxy toluene cloves phenol solution, the quality of dibutyl hydroxy toluene and eugenol
Than for 1:0.5；
S103：In the product drying that step S102 is obtained, the solid of collection and the pig iron, calcium oxide, zirconium oxide are mixed equal
It is even, obtain graphite material；Wherein, graphite powder, the pig iron, calcium oxide, the mass ratio of zirconium oxide are 1:0.02:0.02:0.01.
S2：The obtained mixtures of step S1 are put into shaping slaughterhouse mould, are heated to 50 DEG C of progress rigid mould compactings, just
Property molding system time be 25min.
S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product；Wherein, hot pressed sintering
Include the first temperature-rise period, the second increasing temperature and pressure and constant temperature and pressure process and temperature-fall period successively：In first temperature-rise period, machinery
Pressure is 20MPa, and is warming up to 2500 DEG C with 20 DEG C/min heating rate；During second increasing temperature and pressure and constant temperature and pressure,
Mechanical pressure is linearly increased to 26MPa, temperature linearity is increased to 2900 DEG C, and makes temperature and pressure while reaches maximum
It is worth, afterwards constant temperature and pressure 22h；Wherein, heating rate is 10 DEG C/min；In temperature-fall period, holding mechanical pressure is maximum, with
120 DEG C/h rate of temperature fall is cooled to 15 DEG C.
Embodiment five
The present embodiment provides a kind of preparation method of graphite product, comprises the following steps：
S1：Graphite material is crushed to particle diameter less than 100 μm, then with binding agent with 100:10 mass ratio mixing is equal
It is even；
Wherein, the preparation method of graphite material comprises the following steps：
S101：Graphite powder is added in ethanol eugenol mixed solution, 600W ultrasounds 60min after being uniformly dispersed；Wherein, stone
The mass ratio of ink powder and ethanol eugenol mixed solution is 1:10, in ethanol eugenol mixed solution, the matter of ethanol and eugenol
Amount is than being 1:0.8；
S102：Mixture, alumina powder and the nickel powder that step S101 is obtained are added to dibutyl hydroxy toluene eugenol
In solution, 6h is stood after well mixed；Wherein, graphite powder, alumina powder, nickel powder and dibutyl hydroxy toluene cloves phenol solution
Mass ratio is 1:0.15:0.05:20, in dibutyl hydroxy toluene cloves phenol solution, the matter of dibutyl hydroxy toluene and eugenol
Amount is than being 1:0.6；
S103：In the product drying that step S102 is obtained, the solid of collection and the pig iron, calcium oxide, zirconium oxide are mixed equal
It is even, obtain graphite material；Wherein, graphite powder, the pig iron, calcium oxide, the mass ratio of zirconium oxide are 1:0.03:0.06:0.02.
S2：The obtained mixtures of step S1 are put into shaping slaughterhouse mould, are heated to 100 DEG C of progress rigid mould compactings,
The time of rigid mould compacting is 35min.
S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product；Wherein, hot pressed sintering
Include the first temperature-rise period, the second increasing temperature and pressure and constant temperature and pressure process and temperature-fall period successively：In first temperature-rise period, machinery
Pressure is 22MPa, and is warming up to 2500 DEG C with 40 DEG C/min heating rate；During second increasing temperature and pressure and constant temperature and pressure,
Mechanical pressure is linearly increased to 28MPa, temperature linearity is increased to 3100 DEG C, and makes temperature and pressure while reaches maximum
It is worth, afterwards constant temperature and pressure 26h；Wherein, heating rate is 15 DEG C/min；In temperature-fall period, holding mechanical pressure is maximum, with
150 DEG C/h rate of temperature fall is cooled to 30 DEG C.
Embodiment six
The present embodiment provides a kind of preparation method of graphite product, comprises the following steps：
S1：Graphite material is crushed to particle diameter less than 100 μm, then with binding agent with 100:8 mass ratio is well mixed；
Wherein, the preparation method of graphite material comprises the following steps：
S101：Graphite powder is added in ethanol eugenol mixed solution, 550W ultrasounds 55min after being uniformly dispersed；Wherein, stone
The mass ratio of ink powder and ethanol eugenol mixed solution is 1:9, in ethanol eugenol mixed solution, the quality of ethanol and eugenol
Than for 1:0.9；
S102：Mixture, alumina powder and the nickel powder that step S101 is obtained are added to dibutyl hydroxy toluene eugenol
In solution, 5.5h is stood after well mixed；Wherein, graphite powder, alumina powder, nickel powder and dibutyl hydroxy toluene cloves phenol solution
Mass ratio be 1:0.12:0.04:18, in dibutyl hydroxy toluene cloves phenol solution, dibutyl hydroxy toluene and eugenol
Mass ratio is 1:0.55；
S103：In the product drying that step S102 is obtained, the solid of collection and the pig iron, calcium oxide, zirconium oxide are mixed equal
It is even, obtain graphite material；Wherein, graphite powder, the pig iron, calcium oxide, the mass ratio of zirconium oxide are 1:0.025:0.04:0.015.
S2：The obtained mixtures of step S1 are put into shaping slaughterhouse mould, are heated to 80 DEG C of progress rigid mould compactings, just
Property molding system time be 30min.
S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product；Wherein, hot pressed sintering
Include the first temperature-rise period, the second increasing temperature and pressure and constant temperature and pressure process and temperature-fall period successively：In first temperature-rise period, machinery
Pressure is 21MPa, and is warming up to 2500 DEG C with 30 DEG C/min heating rate；During second increasing temperature and pressure and constant temperature and pressure,
Mechanical pressure is linearly increased to 27MPa, temperature linearity is increased to 3000 DEG C, and makes temperature and pressure while reaches maximum
It is worth, afterwards constant temperature and pressure 24h；Wherein, heating rate is 13 DEG C/min；In temperature-fall period, holding mechanical pressure is maximum, with
135 DEG C/h rate of temperature fall is cooled to 25 DEG C.
Comparative example one
This comparative example provides a kind of preparation method of graphite product, comprises the following steps：
S1：Graphite material is crushed to particle diameter less than 100 μm, then with binding agent with 100:8 mass ratio is well mixed；
Wherein, the preparation method of graphite material comprises the following steps：
S101：Graphite powder is added in ethanol eugenol mixed solution, 550W ultrasounds 55min after being uniformly dispersed；Wherein, stone
The mass ratio of ink powder and ethanol eugenol mixed solution is 1:9, in ethanol eugenol mixed solution, the quality of ethanol and eugenol
Than for 1:0.9；
S102：The obtained mixtures of step S101 are added in dibutyl hydroxy toluene cloves phenol solution, are well mixed
After stand 5.5h；Wherein, the mass ratio of graphite powder and dibutyl hydroxy toluene cloves phenol solution is 1:18, dibutyl hydroxy toluene
In cloves phenol solution, the mass ratio of dibutyl hydroxy toluene and eugenol is 1:0.55；
S103：In the product drying that step S102 is obtained, the solid of collection and the pig iron, calcium oxide, zirconium oxide are mixed equal
It is even, obtain graphite material；Wherein, graphite powder, the pig iron, calcium oxide, the mass ratio of zirconium oxide are 1:0.025:0.04:0.015.
S2：The obtained mixtures of step S1 are put into shaping slaughterhouse mould, are heated to 80 DEG C of progress rigid mould compactings, just
Property molding system time be 30min.
S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product；Wherein, hot pressed sintering
Include the first temperature-rise period, the second increasing temperature and pressure and constant temperature and pressure process and temperature-fall period successively：In first temperature-rise period, machinery
Pressure is 21MPa, and is warming up to 2500 DEG C with 30 DEG C/min heating rate；During second increasing temperature and pressure and constant temperature and pressure,
Mechanical pressure is linearly increased to 27MPa, temperature linearity is increased to 3000 DEG C, and makes temperature and pressure while reaches maximum
It is worth, afterwards constant temperature and pressure 24h；Wherein, heating rate is 13 DEG C/min；In temperature-fall period, holding mechanical pressure is maximum, with
135 DEG C/h rate of temperature fall is cooled to 25 DEG C.
Comparative example two
This comparative example provides a kind of preparation method of graphite product, comprises the following steps：
S1：Graphite material is crushed to particle diameter less than 100 μm, then with binding agent with 100:8 mass ratio is well mixed；
Wherein, the preparation method of graphite material comprises the following steps：
S101：Graphite powder is added in ethanol eugenol mixed solution, 550W ultrasounds 55min after being uniformly dispersed；Wherein, stone
The mass ratio of ink powder and ethanol eugenol mixed solution is 1:9, in ethanol eugenol mixed solution, the quality of ethanol and eugenol
Than for 1:0.9；
S102：Mixture, alumina powder and the nickel powder that step S101 is obtained are added to dibutyl hydroxy toluene eugenol
In solution, 5.5h is stood after well mixed；Wherein, graphite powder, alumina powder, nickel powder and dibutyl hydroxy toluene cloves phenol solution
Mass ratio be 1:0.12:0.04:18, in dibutyl hydroxy toluene cloves phenol solution, dibutyl hydroxy toluene and eugenol
Mass ratio is 1:0.55；
S103：In the product drying that step S102 is obtained, the solid of collection and the pig iron are well mixed, obtain graphite material
Material；Wherein, graphite powder, the mass ratio of the pig iron are 1:0.025.
S2：The obtained mixtures of step S1 are put into shaping slaughterhouse mould, are heated to 80 DEG C of progress rigid mould compactings, just
Property molding system time be 30min.
S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains graphite product；Wherein, hot pressed sintering
Include the first temperature-rise period, the second increasing temperature and pressure and constant temperature and pressure process and temperature-fall period successively：In first temperature-rise period, machinery
Pressure is 21MPa, and is warming up to 2500 DEG C with 30 DEG C/min heating rate；During second increasing temperature and pressure and constant temperature and pressure,
Mechanical pressure is linearly increased to 27MPa, temperature linearity is increased to 3000 DEG C, and makes temperature and pressure while reaches maximum
It is worth, afterwards constant temperature and pressure 24h；Wherein, heating rate is 13 DEG C/min；In temperature-fall period, holding mechanical pressure is maximum, with
135 DEG C/h rate of temperature fall is cooled to 25 DEG C.
Comparative example three
This comparative example provides a kind of preparation method of graphite product, comprises the following steps：
S1：Graphite material is crushed to particle diameter less than 100 μm, then with binding agent with 100:8 mass ratio is well mixed；
Wherein, the preparation method of graphite material comprises the following steps：
S101：Graphite powder is added in ethanol eugenol mixed solution, 550W ultrasounds 55min after being uniformly dispersed；Wherein, stone
The mass ratio of ink powder and ethanol eugenol mixed solution is 1:9, in ethanol eugenol mixed solution, the quality of ethanol and eugenol
Than for 1:0.9；
S102：Mixture, alumina powder and the nickel powder that step S101 is obtained are added to dibutyl hydroxy toluene eugenol
In solution, 5.5h is stood after well mixed；Wherein, graphite powder, alumina powder, nickel powder and dibutyl hydroxy toluene cloves phenol solution
Mass ratio be 1:0.12:0.04:18, in dibutyl hydroxy toluene cloves phenol solution, dibutyl hydroxy toluene and eugenol
Mass ratio is 1:0.55；
S103：In the product drying that step S102 is obtained, the solid of collection and the pig iron, calcium oxide, zirconium oxide are mixed equal
It is even, obtain graphite material；Wherein, graphite powder, the pig iron, calcium oxide, the mass ratio of zirconium oxide are 1:0.025:0.04:0.015.
S2：The obtained mixtures of step S1 are put into shaping slaughterhouse mould, are heated to 80 DEG C of progress rigid mould compactings, just
Property molding system time be 30min.
S3：The mechanograph that step S2 is obtained is taken out, then 3000 DEG C of hot pressed sintering 24h, obtain graphite product.
The graphite product (graphite slaughterhouse) that the embodiment of the present invention one is prepared to embodiment six, carry out correlated performance ginseng
Several tests, and the graphite product (graphite slaughterhouse) being prepared with comparative example one to comparative example three is as a comparison.Obtained knot
Shown in fruit Tables 1 and 2 specific as follows.
The graphite slaughterhouse performance parameter table -1 of table 1
The graphite slaughterhouse performance parameter table -2 of table 2
| Group | Thermal coefficient of expansion (/K) | Thermal diffusivity (m2/s) | Thermal conductivity (w/mk) |
| Embodiment one | 4.97×10-6 | 76.28 | 126.7 |
| Embodiment two | 5.09×10-6 | 75.81 | 125.1 |
| Embodiment three | 4.86×10-6 | 76.43 | 127.4 |
| Example IV | 1.07×10-7 | 98.38 | 150.9 |
| Embodiment five | 1.12×10-7 | 98.25 | 149.7 |
| Embodiment six | 1.03×10-7 | 99.61 | 152.8 |
| Comparative example one | 4.39×10-5 | 66.28 | 120.4 |
| Comparative example two | 6.57×10-5 | 53.97 | 111.6 |
| Comparative example three | 3.21×10-6 | 72.16 | 135.8 |
It should be noted that except the situation that above-described embodiment one is enumerated to embodiment six, from other preparation methods
Parameter is also feasible.
Technical scheme provided by the invention, there is following beneficial effect：(1) graphite product density provided by the invention
It is high and be evenly distributed；And surface accuracy is high, because sintering process raises green density, and viscous state is in sintering
Binding agent there is good " leveling " effect, so as to so that the raising of graphite product surface accuracy grade；(2) present invention provides
Graphite product ejection pressure it is small, die wear can be reduced, so as to extend its service life；(3) graphite provided by the invention
The green strength of product significantly improves, and the wind such as side and arrisdefect so as to substantially reduce that product occurs in transfer process
Danger；(4) the resistance to heat rating of graphite product provided by the invention is big, and thermal coefficient of expansion is small, and thermal diffusivity and thermal conductivity are high, and heat transfer is fast,
Resistance to compression and fracture resistance are good；(5) preparation method of graphite product provided by the invention is simple, and production cost is low.
It should be noted that unless otherwise indicated, technical term or scientific terminology used in this application should be this hair
The ordinary meaning that bright one of ordinary skill in the art are understood.Unless specifically stated otherwise, otherwise illustrate in these embodiments
Part and relative step, numerical expression and the numerical value of step are not limit the scope of the invention.It is illustrated and described herein
In all examples, unless otherwise prescribed, any occurrence should be construed as merely exemplary, not as limitation, because
This, other examples of exemplary embodiment can have different values.
In the description of the invention, it is to be understood that term " first ", " second " are only used for describing purpose, and can not
It is interpreted as indicating or implies relative importance or imply the quantity of the technical characteristic indicated by indicating.Thus, define " the
One ", one or more this feature can be expressed or be implicitly included to the feature of " second ".In the description of the invention,
" multiple " are meant that two or more, unless otherwise specifically defined.
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, either which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme, it all should cover among protection scope of the present invention.
Claims (10)
1. a kind of preparation method of graphite product, it is characterised in that comprise the following steps：
S1：Graphite material is crushed, is then well mixed with binding agent；
S2：The obtained mixtures of step S1 are put into mould, are heated to 50~100 DEG C of progress rigid mould compactings；
S3：The mechanograph that step S2 is obtained is taken out, hot pressed sintering is then carried out, obtains the graphite product.
2. the preparation method of graphite product according to claim 1, it is characterised in that：
In step S1, the mass ratio of the graphite material and the binding agent is 100:(5~10)；After the graphite material crushes
Particle diameter be less than 100 μm.
3. the preparation method of graphite product according to claim 1, it is characterised in that：
In step S2, the time of the rigid mould compacting is 25~35min.
4. the preparation method of graphite product according to claim 1, it is characterised in that：
In step S3, the hot pressed sintering includes the first temperature-rise period, the second increasing temperature and pressure and constant temperature and pressure process and drop successively
Warm process：
In first temperature-rise period, mechanical pressure is 20~22MPa, and is warming up to 20~40 DEG C/min heating rate
2500℃；
During second increasing temperature and pressure and constant temperature and pressure, mechanical pressure is linearly increased to 26~28MPa, by temperature linearity
2900~3100 DEG C are increased to, and makes temperature and pressure while reaches maximum, afterwards 22~26h of constant temperature and pressure；Wherein, heat up
Speed is 10~15 DEG C/min；
In the temperature-fall period, holding mechanical pressure is the maximum, and 15 are cooled to 120~150 DEG C/h rate of temperature fall
~30 DEG C.
5. the preparation method of graphite product according to claim 1, it is characterised in that：
In step S2, the mould includes：One in frying pan mould, slaughterhouse mould, pancake pan mould and Barbecuing plate mould
Kind is a variety of.
6. the preparation method of graphite product according to claim 1, it is characterised in that
In step S1, the preparation method of the graphite material comprises the following steps：
S101：Graphite powder is added in ethanol eugenol mixed solution, it is ultrasonic after being uniformly dispersed；
S102：Mixture, alumina powder and the nickel powder that step S101 is obtained are added to dibutyl hydroxy toluene cloves phenol solution
In, stand preset time after well mixed；
S103：In the product drying that step S102 is obtained, the solid of collection and the pig iron, calcium oxide, zirconium oxide are well mixed, obtained
To the graphite material.
7. the preparation method of graphite product according to claim 1, it is characterised in that：
In step S101, the mass ratio of the graphite powder and the ethanol eugenol mixed solution is 1:(8~10), the ethanol
In eugenol mixed solution, the mass ratio of ethanol and eugenol is 1:(0.8~1.0), the ultrasonic power be 500~
600W, the ultrasonic time are 45~60min.
8. the preparation method of graphite product according to claim 1, it is characterised in that：
In step S102, graphite powder, alumina powder, the mass ratio of nickel powder and dibutyl hydroxy toluene cloves phenol solution are 1:(0.1
~0.15):(0.02~0.05):(15~20), time of the standing are 5~6h, the dibutyl hydroxy toluene eugenol
In solution, the mass ratio of dibutyl hydroxy toluene and eugenol is 1:(0.5~0.6).
9. the preparation method of graphite product according to claim 1, it is characterised in that：
In step S103, graphite powder, the pig iron, calcium oxide, the mass ratio of zirconium oxide are 1:(0.02~0.03):(0.02~
0.06):(0.01~0.02).
10. the graphite product that the preparation method described in claim any one of 1-9 is prepared.
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| CN109503169A (en) * | 2018-12-24 | 2019-03-22 | 成都阿泰克特种石墨有限公司 | A kind of special graphite and preparation method thereof |
| CN112624102A (en) * | 2020-12-27 | 2021-04-09 | 南通百大石墨设备有限公司 | Production method of graphite product |
| CN115057688A (en) * | 2022-07-01 | 2022-09-16 | 江西嘉逸陶瓷有限公司 | Method for preparing heat-resistant ceramic pot from synthetic black jade |
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| CN115057688A (en) * | 2022-07-01 | 2022-09-16 | 江西嘉逸陶瓷有限公司 | Method for preparing heat-resistant ceramic pot from synthetic black jade |
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| CN107573073B (en) | 2019-09-10 |
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