CN115626826B - Low-density wear-resistant carbon graphite material with independent micropores and preparation method thereof - Google Patents
Low-density wear-resistant carbon graphite material with independent micropores and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-density wear-resistant carbon graphite material with independent micropores and a preparation method thereof, wherein the preparation method comprises the following steps: weighing 60-80 parts of graphite fine powder, 1-10 parts of superfine artificial graphite powder, 1-10 parts of superfine modified raw coke powder, 1-10 parts of carbon black, 1-2 parts of dispersing agent, 40-50 parts of asphalt, 1-5 parts of coupling agent and 100-250 parts of ethanol-acetone mixed solution; adding a dispersing agent into an ethanol acetone mixed solution, uniformly stirring, and sequentially adding superfine artificial graphite powder and carbon powder for ultrasonic dispersion to obtain mixed slurry; placing the graphite fine powder and the superfine raw coke powder into a Raymond mill for mixing and grinding to obtain mixed fine powder; and (3) putting the mixed fine powder and the mixed slurry into a kneading pot for kneading, putting a coupling agent and asphalt in a molten state into the kneading pot when the temperature of the mixture rises to 180-200 ℃, closing a cover for kneading, and performing sheet rolling, crushing, grinding, sieving, compression molding and roasting after the kneading is finished to obtain the carbon graphite material. The prepared carbon graphite material has good mechanical strength, wear resistance, homogeneity and stability.
Description
Technical Field
The invention belongs to the technical field of carbon graphite materials, and particularly relates to a low-density wear-resistant carbon graphite material with independent micropores and a preparation method thereof.
Background
Carbon graphite materials are widely used in aeroengine bearing sealing systems, hydraulic sealing systems and fuel sealing systems due to their excellent mechanical properties, high temperature resistance and self-lubricating properties. However, with the continuous expansion of the aviation industry, the practical working condition puts higher demands on the comprehensive performance of the graphite sealing material. At present, the traditional process for preparing the carbon-graphite sealing material adopts calcined coke with larger particle size and artificial graphite as aggregate, asphalt as binder, and the green carbon-graphite material is prepared through kneading, sheet rolling, crushing, forming and multiple dipping and roasting treatments. The carbon graphite material prepared by the process has large pore diameter and easy communication among pores because the selected aggregate granularity is large and the aggregate collocation design is to be optimized, so that the carbon graphite material has poor comprehensive properties such as mechanical strength, wear resistance, homogeneity, stability and airtightness, and further the carbon graphite material is difficult to meet the requirements of the existing sealing materials.
In addition, the poor homogeneity and stability are also due to the fact that the primary structure of the original blank graphite material is affected to a certain extent by the late-stage impregnation densification process, meanwhile, the impregnant asphalt is difficult to fully infiltrate the wall of the blank hole, so that gradient density difference between the surface and the inside of the blank graphite material is caused, and the homogeneity and the stability of the blank graphite material are finally affected.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a low-density wear-resistant carbon graphite material with independent micropores and a preparation method thereof, wherein the carbon graphite material has good mechanical strength, wear resistance, homogeneity and stability, and the preparation method can effectively shorten the production period, realize short-flow production and preparation and reduce the production cost.
The technical scheme of the invention is realized as follows:
the preparation method of the low-density wear-resistant carbon graphite material with independent micropores specifically comprises the following steps:
s1: accurately weighing 60-80 parts of graphite fine powder, 1-10 parts of superfine artificial graphite powder, 1-10 parts of superfine modified raw coke powder, 1-10 parts of carbon black, 1-2 parts of dispersing agent, 40-50 parts of asphalt, 1-5 parts of coupling agent and 100-250 parts of ethanol-acetone mixed solution for later use; the volume ratio of the ethanol to the acetone in the ethanol-acetone mixed solution is 1:1-4:1;
s2: adding a dispersing agent into an ethanol acetone mixed solution, uniformly stirring, and then sequentially adding superfine artificial graphite powder and carbon black for ultrasonic dispersion to obtain mixed slurry;
s3: placing the graphite fine powder and the superfine modified raw coke powder into a Raymond mill for mixing and grinding for 1-10 min to obtain mixed fine powder;
s4: mixing and kneading the mixed fine powder and the mixed slurry in a kneading pot, adding a coupling agent and asphalt in a molten state into the kneading pot when the temperature of the mixture rises to 180-200 ℃, closing a cover and kneading, rolling, crushing, grinding, sieving to obtain pressed powder after the kneading is finished, pressing and forming to obtain a green body block, and finally roasting to obtain the carbon graphite material.
Further, the D50 of the graphite fine powder is less than or equal to 6 mu m, and the graphite fine powder is prepared by taking the pitch coke after forging or the needle coke after forging as a raw material and adopting an airflow mill.
Further, the carbon black is one or two of N220 carbon black, N326 carbon black, N330 carbon black, N339 carbon black, modified carbon black and intermediate phase carbon microsphere; the asphalt is one or two of low-temperature asphalt, medium-temperature asphalt, high-temperature asphalt and modified asphalt.
Further, the dispersing agent is one or two of borate, aminopropylamine dioleate and carboxymethyl cellulose; the coupling agent is one or two of aluminate, phthalate and dioxy acetic acyl phthalate.
Further, when the mixed slurry is prepared, firstly adding ultrafine artificial graphite powder into a mixed solution of a dispersing agent and ethanol for ultrasonic dispersion for 10-30 min, and then adding carbon powder for ultrasonic dispersion for 10-30 min.
Further, during kneading, the mixed fine powder is firstly put into a kneading pot, mixed for 10-20 min at 100-110 ℃, the rotating speed of the kneading pot is 10-50 r/min, and the cover is opened to rotate forward; after the temperature of the material reaches 100-110 ℃, putting the mixed slurry into a kneading pot, kneading for 0.5-1 h, wherein the rotating speed of the kneading pot is 10-50 r/min, and uncovering is rotated forward; after the moisture is completely removed, the temperature of the materials is raised to 180-200 ℃, asphalt in a molten state is put into a kneading pot, a coupling agent is put into the kneading pot, the rotating speed of the kneading pot is 10-50 r/min, forward rotation and reverse rotation are alternately carried out, and the kneading is carried out for 0.5-1 h after the cover is closed.
Further, when preparing the pressed powder, rapidly putting the paste obtained by kneading into a sheet rolling machine, rolling sheets for 3-4 times, wherein the thickness of the rolled sheets is 1-2.5 mm, the temperature of the rolled sheets is 180-200 ℃, the rotating speed is 10-25 r/min, standing the sheet materials for 5-10 h after the rolling sheets are finished, crushing and grinding, and standing for 5-10 h after passing through a 100-400 mesh screen, thereby preparing the pressed powder.
Further, the step of compacting the green body block is: pressing the pressed powder under 1-10 MPa to form a primary blank block, vacuum packaging, and standing for 5-10 h; placing the mixture into cold isostatic pressing equipment, pressing for 0.5-1 h under 150-200 MPa, performing gradient pressure relief, taking out, removing the packaging bag, and placing for 5-10 h to obtain the product with the density of 1.59-1.62 g/cm 3 Is a green body block of (c).
Further, the roasting process is as follows: placing the green body block in a stainless steel crucible, filling a buried firing material, placing the crucible in a roasting furnace, introducing argon, roasting for 2-4 hours at 900-1200 ℃, performing program control cooling to 150-300 ℃, and naturally cooling to room temperature to obtain the product with the volume density of 1.60-1.64 g/cm 3 The baked block is the carbon graphite material.
The invention also provides a low-density wear-resistant carbon graphite material with independent micropores, which is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, graphite fine powder (D50 is less than or equal to 6 mu m) is used as main aggregate, superfine artificial graphite powder (D50=6 mu m), superfine modified raw coke powder (D50=5 mu m containing specific volatile matters and activity) and carbon black (primary particle size is 30 nm) are used as secondary aggregate, and the carbon black is used as an antiwear agent to increase the mechanical property and wear resistance of the carbon graphite material. The main aggregate and the secondary aggregate with different particle sizes are matched, and a homogeneous carbon skeleton is formed in a particle size stacking mode, so that the homogeneous carbon skeleton is of a primary skeleton structure. Simultaneously, arch bridge effect can be generated when large and small particles are piled up, welding spots are formed among the particles to solidify, the communication of air holes is blocked in a sand bag plugging mode, the aperture of the air holes is reduced, a relatively independent non-communication micropore structure is formed, and the carbon graphite material is of a secondary welding structure, so that the aperture porosity can be effectively reduced, and the prepared carbon graphite material is low in volume density and good in air tightness.
And the carbon black surface contains rich oxygen-containing functional groups such as hydroxyl, carboxyl, carbonyl and the like, is easy to act with other aggregate particles, promotes the formation of sintering necks among particles, and realizes synchronous thermal contraction among different particles. The superfine modified raw coke powder has self-sintering property, has larger volume shrinkage in the heat treatment process, and is beneficial to densification. The mode of carbon black chain sealing and raw coke powder plugging is adopted, and the three-stage protective structure is adopted, so that the welding spot combination among particles is further enhanced, and the formation of an independent non-communicated microporous structure is promoted.
2. According to the invention, a liquid phase mixing process is adopted, and dispersing agents are added to disperse ultrafine particles such as carbon black, so that the agglomeration phenomenon of the carbon black is effectively avoided, and meanwhile, a coupling agent is introduced in the mixing and kneading process, so that the fluidity of binder asphalt can be effectively improved, the formation of sintering necks among aggregate particles during roasting is further promoted, the synchronous volume heat shrinkage capability of different components of the carbon graphite material is improved, and the structure-function integration is realized.
Ultrafine particles such as carbon black are uniformly dispersed in the aggregate, so that the homogeneity of the carbon graphite material can be effectively improved, crack propagation can be prevented, the bonding strength among the aggregate particles is improved, the wear rate is reduced, and the wear resistance and stability of the carbon graphite material are improved.
3. The invention adopts the mixed solution of ethanol and acetone as the solvent, the ethanol and the acetone are low boiling point solvents, contain polar molecules and are easy to volatilize, and when the ethanol and the acetone are mixed, the volatilization degree can be reduced due to the hydrogen bond action between the ethanol and the acetone molecules. And acetone is easy to dissolve oil and lipid substances, and ethanol contains nonpolar hydroxyl groups and can dissolve some nonpolar substances, so that weak polar fine powder such as graphite powder and lipid dispersing agents can be effectively dissolved.
4. The boric acid ester, aminopropylamine dioleate, carboxymethyl cellulose and the like adopted by the invention have good matching property with the carbonaceous aggregate, and the boric acid ester, aminopropylamine dioleate, carboxymethyl cellulose and the like are adsorbed on the surfaces of particles to form a compact adsorption layer so as to prevent flocculation and coalescence among the particles, thereby achieving the dispersion stabilization effect. In addition, it can reduce the surface tension or interfacial tension to make the liquid droplet smaller, so as to attain the dispersing action.
5. The invention does not need to be impregnated and roasted for multiple times, has simple process, can effectively reduce the production cost, shortens the production period and realizes the production and preparation in a short flow.
Drawings
FIG. 1-A plot of flexural and compressive strength and corresponding cross-sectional microtopography for the carbon graphite material prepared in example 1.
FIG. 2-A graph of the friction coefficient and a scanning electron microscope of the surface of the carbon graphite material produced in example 1.
FIG. 3-A plot of flexural and compressive strength and corresponding cross-sectional microtopography for the carbon graphite material prepared in example 2.
FIG. 4-Scanning Electron Microscope (SEM) graph of friction coefficient curve and surface of the carbon graphite material prepared in example 2.
FIG. 5-A plot of flexural and compressive strength and corresponding cross-sectional microtopography for the carbon graphite material prepared in example 3.
FIG. 6-Scanning Electron Microscope (SEM) graph of friction coefficient curve and surface of the carbon graphite material prepared in example 3.
Detailed Description
The invention is described in further detail below with reference to the drawings and the detailed description.
Example 1
1) The calcined pitch coke is purchased from raw material factories, and then the graphite fine powder with the D50 less than or equal to 6 mu m is prepared by adopting an airflow mill for standby.
2) 70 parts of graphite fine powder prepared in the step 1), 10 parts of superfine artificial graphite powder, 10 parts of superfine modified raw coke powder, 5 parts of N339 carbon black and 5 parts of N326 carbon black respectively and 1 part of borate dispersing agent are accurately weighed.
3) 200 parts of a 1:1 ethanol acetone mixed solution is weighed and placed in a container, meanwhile, a borate dispersing agent is added and fully stirred until uniform, superfine artificial graphite powder is added and placed in an ultrasonic pool for ultrasonic vibration for 15min, and then N220 carbon black and N326 carbon black are added and subjected to ultrasonic vibration for 15min, so that mixed slurry is prepared.
4) And (3) placing the graphite fine powder and the superfine modified raw coke powder into a Raymond mill, mixing and grinding for 1min, and preparing the mixed fine powder.
5) 25 parts of high-temperature asphalt (softening point 112 ℃) and 15 parts of modified asphalt (softening point 105 ℃) are accurately weighed, and 5 parts of phthalate coupling agent are weighed.
6) Putting the mixed fine powder obtained in the step 4) into a kneading pot, mixing for 10min at 110 ℃, wherein the rotating speed of the kneading pot is 15r/min, and opening the cover to rotate positively; after the temperature of the material reaches 100 ℃, putting the slurry prepared in the step 3) into a kneading pot, kneading for 30min, wherein the rotating speed of the kneading pot is 25r/min, and opening the cover to rotate forward; after the moisture is completely removed, the temperature of the materials is raised to 185 ℃, asphalt in a molten state is put into a kneading pot, a coupling agent is put into the kneading pot, the kneading is carried out for 1h, the rotating speed of the kneading pot is 50r/min, the forward rotation and the reverse rotation are alternately carried out, and the cover is closed for kneading. After the kneading is finished, rapidly putting the paste obtained by kneading into a sheet rolling machine, rolling for 3 times, wherein the thickness of the rolled sheet is 1.5mm, the temperature of the rolled sheet is 185 ℃, the rotating speed is 25r/min, standing the sheet material for 10h after the rolling is finished, crushing, grinding, sieving with a 200-mesh screen, and standing for 10h to obtain pressed powder.
7) Pressing the pressed powder prepared in the step 6) into a primary blank block under 5MPa, vacuum packaging, and standing for 10 hours; placing in cold isostatic pressing equipment, pressing under 200MPa for 0.5 hr, gradient pressure relieving, taking out sample, removing packaging bag, and standing for 10 hr to obtain product with density of 1.59g/cm 3 Is a green body block of (c).
8) Placing the green body block prepared in the step 7) in a stainless steel crucible, filling a buried firing material, adjusting the green body block to a proper position, placing the crucible in a roasting furnace, introducing argon in the roasting process, roasting for 4 hours at 1200 ℃, naturally cooling to room temperature after the temperature is reduced to 150 ℃ in a program control manner, and obtaining the product with the density of 1.60g/cm 3 Is a baked block (carbon graphite material).
The fracture resistance and compression resistance diagrams and the corresponding section morphology diagrams of the carbon graphite material prepared in the embodiment are shown in fig. 1, fig. 1 (a) and fig. 1 (c) are respectively fracture resistance and compression resistance diagrams of the carbon graphite material, and fig. 1 (b) and fig. 1 (d) are respectively section microscopic morphology diagrams of the carbon graphite material. As can be seen from fig. 1 (a) and 1 (c), the flexural strength and compressive strength of the carbon graphite material were 79.69MPa and 235.77MPa, respectively. As can be seen from fig. 1 (b) and fig. 1 (d), the structure between the aggregates is compact, the pore size between the particles is small, and no obvious cracks are generated, so that the prepared carbon graphite material has excellent fracture and compression strength.
The coefficient of friction curve of the carbon graphite material obtained in this example is shown in fig. 2 (a), and the load is 500 g. As can be seen from FIG. 2 (a), the carbon graphite material of the present example gradually decreased from 0.165 to 0.13 in friction coefficient over a period of 30min at room temperature, and had an average friction coefficient of 0.1382, and the wear rate was 5.107 ×10 calculated after measuring the loss of wear mass -6 cm 3 And (3) the friction and wear performance is better. As shown in FIG. 2 (b), the surface scanning electron microscope of the carbon graphite material obtained in this example has no communication channels formed between the air holes, the aperture is about 10 micrometers, and the open porosity is 3.11% as measured by a boiling method, so that the air tightness is good.
Example 2
1) The calcined pitch coke is purchased from raw material factories, and then the graphite fine powder with the D50 less than or equal to 6 mu m is prepared by adopting an airflow mill for standby.
2) 72 parts of graphite fine powder prepared in the step 1), 8 parts of superfine artificial graphite powder, 10 parts of superfine modified raw coke powder, 5 parts of N326 carbon black and mesocarbon microbeads respectively and 1 part of borate dispersing agent are accurately weighed.
3) 200 parts of a 1:1 ethanol acetone mixed solution is weighed and placed in a container, simultaneously boric acid ester dispersing agent is added and fully stirred until uniform, superfine artificial graphite powder is added and placed in an ultrasonic pool for ultrasonic vibration for 15min, and then N326 carbon black and mesophase carbon microspheres are added and subjected to ultrasonic vibration for 15min, so that mixed slurry is prepared.
4) And (3) placing the graphite fine powder and the superfine modified raw coke powder into a Raymond mill, mixing and grinding for 1min, and preparing the mixed fine powder.
5) 25 parts of high-temperature asphalt (softening point 112 ℃) and 20 parts of modified asphalt (softening point 105 ℃) are accurately weighed, and 5 parts of phthalate coupling agent are weighed.
6) Putting the mixed fine powder obtained in the step 4) into a kneading pot, mixing for 10min at 110 ℃, wherein the rotating speed of the kneading pot is 15r/min, and opening the cover to rotate positively; after the temperature of the material reaches 110 ℃, putting the slurry prepared in the step 3) into a kneading pot, kneading for 30min, wherein the rotating speed of the kneading pot is 25r/min, and opening the cover to rotate forward; after the moisture is completely removed, the temperature of the materials is raised to 185 ℃, asphalt in a molten state is put into a kneading pot, a coupling agent is put into the kneading pot, the kneading is carried out for 1h, the rotating speed of the kneading pot is 50r/min, the forward rotation and the reverse rotation are alternately carried out, and the cover is closed for kneading. After the kneading is finished, rapidly putting the paste obtained by kneading into a sheet rolling machine, rolling for 3 times, wherein the thickness of the rolled sheet is 1.5mm, the temperature of the rolled sheet is 185 ℃, the rotating speed is 25r/min, standing the sheet material for 10h after the rolling is finished, crushing, grinding, sieving with a 200-mesh screen, and standing for 10h to obtain pressed powder.
7) Pressing the pressed powder prepared in the step 6) into a primary blank block under 5MPa, vacuum packaging, and standing for 10 hours; placing in cold isostatic pressing equipment, pressing under 200MPa for 0.5 hr, gradient pressure relieving, taking out sample, removing packaging bag, and standing for 10 hr to obtain product with density of 1.59g/cm 3 Is a green body block of (c).
8) Placing the green body block prepared in the step 7) in a stainless steel crucible, filling a buried firing material, adjusting the green body block to a proper position, placing the crucible in a roasting furnace, introducing argon in the roasting process, roasting for 4 hours at 1200 ℃, naturally cooling to room temperature after the temperature is reduced to 150 ℃ in a program control manner, and obtaining the product with the density of 1.61g/cm 3 Is a baked block (carbon graphite material).
The fracture resistance and compression resistance diagrams and the corresponding section morphology diagrams of the carbon graphite material prepared in the embodiment are shown in fig. 3, fig. 3 (a) and fig. 3 (c) are respectively fracture resistance and compression resistance diagrams of the carbon graphite material, and fig. 3 (b) and fig. 3 (d) are respectively section microscopic morphology diagrams of the carbon graphite material. As can be seen from fig. 3 (a) and 3 (c), the flexural strength and compressive strength of the carbon graphite material were 82.46MPa and 240.91MPa, respectively. As can be seen from fig. 3 (b) and fig. 3 (d), the structure between the aggregates is compact, the pore size between the particles is small, and no obvious cracks are generated, so that the prepared carbon graphite material has excellent fracture and compression strength.
The coefficient of friction curve of the carbon graphite material obtained in this example is shown in fig. 4 (a), and the load is 500 g. As can be seen from FIG. 4 (a), the carbon graphite material obtained in this example has a coefficient of friction stabilized at about 0.15 and an average coefficient of friction of 0.1580 over a period of 30 minutes at room temperature, and wear was measuredThe abrasion rate obtained by calculation after the mass loss is 5.326 multiplied by 10 -6 cm 3 And (3) the friction and wear performance is better. As shown in FIG. 4 (b), the surface scanning electron microscope image of the carbon graphite material obtained in the embodiment has no communication channels formed among the air holes, the aperture is below 10 micrometers, the open porosity is 2.85% measured by a boiling method, and the air tightness is good.
Example 3
1) The calcined pitch coke is purchased from raw material factories, and then the graphite fine powder with the D50 less than or equal to 6 mu m is prepared by adopting an airflow mill for standby.
2) 75 parts of graphite fine powder prepared in the step 1), 5 parts of superfine artificial graphite powder, 10 parts of superfine modified raw coke powder, 5 parts of modified carbon black and N339 carbon black respectively and 1 part of borate dispersing agent are accurately weighed.
3) 200 parts of a 1:1 ethanol acetone mixed solution is weighed and placed in a container, meanwhile, a borate dispersing agent is added and fully stirred until uniform, superfine artificial graphite powder is added and placed in an ultrasonic pool for ultrasonic vibration for 15min, and then N326 carbon black and N339 carbon black are added and subjected to ultrasonic vibration for 15min, so that mixed slurry is prepared.
4) And (3) placing the graphite fine powder and the superfine modified raw coke powder into a Raymond mill, mixing and grinding for 1min, and preparing the mixed fine powder.
5) Accurately weighing 20 parts of high-temperature asphalt (softening point 112 ℃) and 28 parts of modified asphalt (softening point 105 ℃) and 5 parts of phthalate coupling agent.
6) Putting the mixed fine powder obtained in the step 4) into a kneading pot, mixing for 10min at 110 ℃, wherein the rotating speed of the kneading pot is 15r/min, and opening the cover to rotate positively; after the temperature of the material reaches 105 ℃, putting the slurry prepared in the step 3) into a kneading pot, kneading for 30min, wherein the rotating speed of the kneading pot is 25r/min, and opening the cover to rotate forward; after the moisture is completely removed, the temperature of the materials is raised to 185 ℃, asphalt in a molten state is put into a kneading pot, a coupling agent is put into the kneading pot, the kneading is carried out for 1h, the rotating speed of the kneading pot is 50r/min, the forward rotation and the reverse rotation are alternately carried out, and the cover is closed for kneading. After the kneading is finished, rapidly putting the paste obtained by kneading into a sheet rolling machine, rolling for 3 times, wherein the thickness of the rolled sheet is 1.5mm, the temperature of the rolled sheet is 185 ℃, the rotating speed is 25r/min, standing the sheet material for 10h after the rolling is finished, crushing, grinding, sieving with a 200-mesh screen, and standing for 10h to obtain pressed powder.
7) Pressing the pressed powder prepared in the step 6) into a primary blank block under 5MPa, vacuum packaging, and standing for 10 hours; placing in cold isostatic pressing equipment, pressing under 200MPa for 0.5 hr, gradient pressure relieving, taking out sample, removing packaging bag, and standing for 10 hr to obtain product with density of 1.61g/cm 3 Is a green body block of (c).
8) Placing the green body block prepared in the step 7) in a stainless steel crucible, filling a buried firing material, adjusting the green body block to a proper position, placing the crucible in a roasting furnace, introducing argon in the roasting process, roasting for 4 hours at 1200 ℃, naturally cooling to room temperature after the temperature is reduced to 150 ℃ in a program control manner, and obtaining the product with the density of 1.63g/cm 3 Is a baked block (carbon graphite material).
The fracture resistance and compression resistance diagrams and the corresponding section morphology diagrams of the carbon graphite material prepared in the embodiment are shown in fig. 5, fig. 5 (a) and fig. 5 (c) are respectively fracture resistance and compression resistance diagrams of the carbon graphite material, and fig. 5 (b) and fig. 5 (d) are respectively section microscopic morphology diagrams of the carbon graphite material. As can be seen from fig. 5 (a) and 5 (c), the flexural strength and compressive strength of the carbon graphite material were 86.77MPa and 259.41MPa, respectively. As can be seen from fig. 5 (b) and fig. 5 (d), the structure between the aggregates is compact, the pore size between the particles is small, and no obvious cracks are generated, so that the prepared carbon graphite material has excellent fracture and compression strength.
The coefficient of friction curve of the carbon graphite material obtained in this example is shown in fig. 6 (a), and the load is 500 g. As can be seen from FIG. 6 (a), the carbon graphite material obtained in this example has a coefficient of friction of about 0.12, an average coefficient of friction of 0.1254, and a wear rate of 4.929 ×10 calculated after measuring the loss of wear mass, in a period of 30min at room temperature -6 cm 3 And (3) the friction and wear performance is better. As shown in FIG. 6 (b), the surface scanning electron microscope image of the carbon graphite material obtained in the embodiment has no communication channels formed among the air holes, the aperture is below 10 microns, the open porosity is 2.56% measured by a boiling method, and the air tightness is good.
In summary, the proportions of the raw materials used in examples 1 to 3 and the basic performance parameters of the prepared carbon graphite materials are shown in Table 1.
As can be seen from table 1: 1) The carbon graphite material prepared by the invention meets the following performance indexes of the aviation carbon graphite sealing material of standard HB 5366-86: the flexural strength is more than or equal to 49MPa, the compressive strength is more than or equal to 118MPa, the Shore hardness is more than or equal to 60HS, the volume density is more than or equal to 1.60g/cm < 3 >, and the friction coefficient is less than or equal to 0.25. And compared with the M106 material mentioned in HB5366-86, the flexural strength and the compressive strength of the carbon graphite material prepared by the invention are respectively improved by 1.62 times and 2 times.
2) It is understood from examples 1 to 3 that the bulk density of the material is 1.6g/cm or more 3 The flexural strength and compressive strength are excellent, and the high strength is attributed to the following 2 reasons: a. the superfine modified raw coke powder and the carbon black have rich marginal carbon atoms and high chemical activity and rich hetero atoms. The high chemical activity is beneficial to promoting the formation of sintering necks among the aggregate particles of the green body material, thereby promoting the self-sintering performance, the self-bonding performance and the mechanical performance; the abundant hetero atoms are beneficial to increasing the wettability of asphalt to aggregate and increasing the interfacial binding force. b. The fine aggregate selected by the invention has large surface area and defects, is beneficial to increasing the interfacial binding force and endows the material with excellent mechanical properties.
The method is characterized in that a homogeneous carbon skeleton (primary skeleton structure) is formed in a mode of stacking different particle sizes, welding spots are formed among particles to solidify, pore communication is blocked in a mode similar to sand bag plugging, a secondary welding structure is adopted, meanwhile, a mode of carbon black chain sealing and raw coke powder plugging is adopted, welding spot combination among particles is further enhanced, pore diameters of the pores are reduced, a tertiary protection structure is adopted, and the formation of an independent non-communicated microporous structure is promoted, so that the homogeneity, stability, air tightness, yield and mechanical strength of a carbon graphite material are improved. The Shore hardness of the carbon graphite material prepared by the method is about 100HS, and the friction coefficient is about 0.12-0.15, which also shows that the wear resistance of the carbon graphite material can be effectively improved by introducing superfine modified raw coke powder and carbon black.
Table 1 the raw material ratios used in examples 1 to 3 and the basic performance parameters of the prepared carbon graphite materials
| Example 1 | Example 2 | Example 3 | |
| Graphite fine powder/part | 70 | 72 | 75 |
| Superfine artificial graphite powder | 10 | 8 | 5 |
| Superfine modified raw coke powder | 10 | 10 | 10 |
| Carbon black/part | 10 | 10 | 10 |
| Dispersing agent/part | 1 | 1 | 1 |
| Bitumen/portion | 40 | 45 | 48 |
| Coupling agent/portion | 5 | 5 | 5 |
| Compressive Strength/MPa | 235.77 | 240.91 | 259.41 |
| Flexural Strength/MPa | 79.69 | 82.46 | 86.77 |
| Shore hardness/HS | 99 | 101 | 105 |
| Bulk Density/g/cm 3 | 1.60 | 1.61 | 1.63 |
| Resistivity/. Mu.OMEGA.m | 33.42 | 34.19 | 30.14 |
| Coefficient of friction/. Mu. | 0.1382 | 0.1580 | 0.1254 |
Finally, it should be noted that the above-mentioned examples of the present invention are only illustrative of the present invention and are not limiting of the embodiments of the present invention. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. Not all embodiments are exhaustive. Obvious changes and modifications which are extended by the technical proposal of the invention are still within the protection scope of the invention.
Claims (10)
1. The preparation method of the low-density wear-resistant carbon graphite material with independent micropores is characterized by comprising the following steps of:
s1: 60-80 parts of graphite fine powder, 1-10 parts of superfine artificial graphite powder, 1-10 parts of superfine modified raw coke powder, 1-10 parts of carbon black, 1-2 parts of dispersing agent, 40-50 parts of asphalt, 1-5 parts of coupling agent and 100-250 parts of ethanol-acetone mixed solution for later use; the volume ratio of the ethanol to the acetone in the ethanol-acetone mixed solution is 1:1-4:1; the dispersing agent is one or two of boric acid ester and aminopropylamine dioleate; wherein d50 of the graphite fine powder is less than or equal to 6 mu m, d50=6 mu m of the superfine artificial graphite powder, d50=5 mu m of the superfine modified raw coke powder, and the primary particle size of the carbon black is 30 nm;
s2: adding a dispersing agent into an ethanol acetone mixed solution, uniformly stirring, and then sequentially adding superfine artificial graphite powder and carbon black for ultrasonic dispersion to obtain mixed slurry;
s3: placing the graphite fine powder and the superfine modified raw coke powder into a Raymond mill, mixing and grinding for 1-10 min to obtain mixed fine powder;
s4: and (3) putting the mixed fine powder and the mixed slurry into a kneading pot for kneading, putting a coupling agent and asphalt in a molten state into the kneading pot when the temperature of the materials rises to 180-200 ℃, closing a cover for kneading, rolling, crushing, grinding, sieving to obtain pressed powder after the kneading is finished, pressing and forming to obtain a green body block, and finally roasting to obtain the carbon graphite material.
2. The method for preparing the low-density wear-resistant carbon graphite material with independent micropores according to claim 1, wherein the graphite fine powder is prepared from forged pitch coke or forged needle coke serving as a raw material by an air flow mill.
3. The method for preparing a low density and abrasion resistant carbon graphite material having independent micropores according to claim 1, wherein the carbon black is one or two of N220 carbon black, N326 carbon black, N330 carbon black, N339 carbon black, modified carbon black and mesophase carbon microspheres; the asphalt is one or two of low-temperature asphalt, medium-temperature asphalt, high-temperature asphalt and modified asphalt.
4. The method for preparing the low-density and wear-resistant carbon graphite material with independent micropores according to claim 1, wherein the coupling agent is one or two of aluminate, phthalate and dioxy-acetylphthalate.
5. The preparation method of the low-density wear-resistant carbon graphite material with independent micropores, which is characterized in that when the mixed slurry is prepared, ultrafine artificial graphite powder is added into a mixed solution of a dispersing agent and ethanol for ultrasonic dispersion for 10-30 min, and then carbon powder is added into the mixed solution for ultrasonic dispersion for 10-30 min.
6. The preparation method of the low-density wear-resistant carbon graphite material with independent micropores, which is characterized in that during kneading, the mixed fine powder is firstly put into a kneading pot, mixed for 10-20 min at 100-110 ℃, the rotating speed of the kneading pot is 10-50 r/min, and the cover is opened to rotate positively; after the temperature of the material reaches 100-110 ℃, putting the mixed slurry into a kneading pot, kneading for 0.5-1 h, wherein the rotating speed of the kneading pot is 10-50 r/min, and uncovering is rotated forward; after the moisture is completely removed, the temperature of the materials is raised to 180-200 ℃, asphalt in a molten state is put into a kneading pot, a coupling agent is put into the kneading pot, the rotating speed of the kneading pot is 10-50 r/min, forward rotation and reverse rotation are alternately carried out, and the kneading pot is closed and kneaded for 0.5-1 h.
7. The preparation method of the low-density wear-resistant carbon graphite material with independent micropores is characterized by comprising the steps of rapidly feeding paste obtained by kneading into a flaker during preparation of pressed powder, flaking for 3-4 times, wherein the thickness of the flaking is 1-2.5 mm, the temperature of the flaking is 180-200 ℃, the rotating speed is 10-25 r/min, standing the flaking material for 5-10 h after the flaking is finished, crushing, grinding, sieving with a 100-400-mesh screen, and standing for 5-10 h, so that pressed powder is obtained.
8. The method of preparing a low density, abrasion resistant carbon graphite material having isolated micropores according to claim 1, wherein the step of compacting the powder to prepare a green body block comprises: pressing the pressed powder at 1-10 MPa to obtain a primary blank block, vacuum packaging, and standing for 5-10 h; placing the mixture in cold isostatic pressing equipment, pressing for 0.5-1 h under 150-200 MPa, performing gradient pressure relief, taking out, removing the packaging bag, and placing for 5-10 h to obtain the product with the density of 1.59-1.62 g/cm 3 Is a green body block of (c).
9. The method for preparing the low-density wear-resistant carbon graphite material with independent micropores according to claim 1, wherein the roasting process is as follows: placing the green body block in a stainless steel crucible, filling a buried firing material, placing the crucible in a roasting furnace, introducing argon, roasting for 2-4 hours at 900-1200 ℃, performing program control cooling to 150-300 ℃, and naturally cooling to room temperature to obtain the product with the volume density of 1.60-1.64 g/cm 3 The baked block is the carbon graphite material.
10. The low-density wear-resistant carbon graphite material with independent micropores is characterized by being prepared by the preparation method according to any one of claims 1-9.
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