CN104178744A - Deposition device and method for preparing cylindrical and columnar isotropic pyrolytic carbon - Google Patents
Deposition device and method for preparing cylindrical and columnar isotropic pyrolytic carbon Download PDFInfo
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- CN104178744A CN104178744A CN201410407180.5A CN201410407180A CN104178744A CN 104178744 A CN104178744 A CN 104178744A CN 201410407180 A CN201410407180 A CN 201410407180A CN 104178744 A CN104178744 A CN 104178744A
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Abstract
The invention provides a deposition device which comprises an upper diversion cone, a lower diversion cone, a deposition substrate and a deposition chamber, wherein the upper diversion cone and lower diversion cone are arranged inside the deposition chamber in opposite through the respective bottom surfaces; the bottom surfaces are respectively provided with a cylindrical upper lug boss and a lower lug boss which respectively extend from the upper diversion cone and lower diversion cone; the upper lug boss and lower lug boss respectively extend into the deposition substrate to be matched and fixed; the end surfaces of the deposition substrate in contact with the bottom surfaces of the upper diversion cone and lower diversion cone are non-specular surfaces; and a 0.5-1.5mm clearance is respectively left between the inner wall of the deposition substrate and the outer walls of the upper lug boss and lower lug boss. The invention also provides a method for preparing cylindrical and columnar isotropic pyrolytic carbon by using the deposition device. The deposition device forms the columnar isotropic pyrolytic carbon by the aid of the outer wall of the deposition substrate, and forms the cylindrical isotropic pyrolytic carbon by the aid of the upper lug boss and lower lug boss, thereby obtaining the isotropic pyrolytic carbon materials with two different sizes and shapes after one furnace loading process.
Description
Technical field
The present invention relates to chemical vapour deposition, relate more specifically to a kind of deposition apparatus and prepare cylindrical and method round shape isotropic pyrolytic carbon.
Background technology
Compact structure, the grain-size of isotropic pyrolytic carbon are little, each is to performance high conformity, except possessing high temperature resistant (under oxygen-free environment), the self-lubricating of common carbonaceous material, the common advantage such as wear-resistant, also have that intensity is high, good airproof performance, the good performance of processability, thereby have broad application prospects in fields such as machinery, Aeronautics and Astronautics, boats and ships, medical science.
Document " preparation of large-sized isotropic decomposition charcoal and sign < < novel charcoal material > > the 2nd phase of 21 volumes in 2006 " discloses a kind of method that adopts rotary substrate stable fluidized bed device to prepare isotropic pyrolytic carbon.Adopting this method is at 1400-1500 ℃ at depositing temperature, has prepared diameter 130mm, the isotropic pyrolytic carbon material that thickness is 5mm; Patent of invention " preparation method's application number 200810150299.3 of large-sized isotropic decomposition charcoal " discloses a kind of employing thermal gradient chemical vapor infiltration method, at 1000-1100 ℃, on charcoal fibrous matrix, prepare the method for large-sized isotropic decomposition charcoal material.
There is following shortcoming in the preparation method of above-mentioned two kinds of isotropic pyrolytic carbons: the material shape that (1) rotary substrate stable fluidized bed chemical vapor deposition method is prepared is limited, can only be round shape or tabular; (2) facility investment is large, and production cost is high; (3) fluidized state processing parameter is many, and technique controlling difficulty is large; (4) in order to form fluidization in reaction cavity, need to use Al
2o
3on bed particle; (5) consistency of performance of the isotropic pyrolytic carbon that thermal gradient chemical vapor infiltration technique is prepared is poor, and can only on tabular depositing base, prepare isotropic pyrolytic carbon material.
Summary of the invention
The problem existing in order to solve above-mentioned prior art, the present invention aims to provide a kind of deposition apparatus and prepares cylindrical and method round shape isotropic pyrolytic carbon.
Deposition apparatus of the present invention, comprise deflection cone, lower deflection cone, depositing base and sediment chamber, by it, bottom surface is separately relative puts in the inside of described sediment chamber for described upper deflection cone and lower deflection cone, has respectively from its extended columniform convex platform and lower convex platform on described bottom surface; The inside that described convex platform and lower convex platform stretch into respectively described depositing base is fixed, described depositing base is nonspecular surface with the end face that the bottom surface of described upper deflection cone and lower deflection cone contacts, and retains respectively the gap of 0.5-1.5mm between the inwall of described depositing base and described convex platform and the outer wall of lower convex platform.
Described depositing base has chamfering at contiguous described convex platform and lower convex platform place.
Described chamfering is 45～60 °.
On the end face that described depositing base contacts with the bottom surface of described upper deflection cone and lower deflection cone, have groove.
Described upper deflection cone and lower deflection cone are conical structure, and cone angle is 45～60 °.
The outer wall of described depositing base and the inwall of described sediment chamber keep being radially spaced, outlet side and inlet end around described upper deflection cone and lower deflection cone setting keeps being radially spaced with described upper deflection cone and lower deflection cone respectively, and described outlet side and inlet end form air outlet and inlet mouth around the place, summit of described upper deflection cone and lower deflection cone.
Deposition apparatus described in utilization of the present invention is prepared cylindrical and method round shape isotropic pyrolytic carbon, containing carbon matrix precursor round the columnar isotropic pyrolytic carbon of outer wall formation of deposits of described depositing base, containing carbon matrix precursor enter described depositing base inner and on described convex platform and lower convex platform the columniform isotropic pyrolytic carbon of formation of deposits.
Described method is further comprising the steps of: S1, under atmosphere of inert gases, is warming up to 950-1050 ℃ by described sediment chamber from room temperature gradually; S2 passes into containing carbon matrix precursor in described sediment chamber; S3, stops passing into containing carbon matrix precursor, continues to pass into rare gas element, and described sediment chamber is cooled to room temperature from 950-1050 ℃.
Described rare gas element is argon gas, and described is methane containing carbon matrix precursor.
Temperature rise rate in described step S1 is 100～200 ℃/h, and the flow containing carbon matrix precursor in described step S2 is 500～1000mL/h.
The present invention utilizes the refluence effect of deflection cone and the diffusional effect of gas, when forming round shape isotropic pyrolytic carbon on the outer wall of depositing base, gas enters with the end face that lower deflection cone contacts with upper deflection cone along depositing base, and the cylinder interior that enters depositing base along inwall and the interstitial diffusion between upper and lower outer wall of boss of depositing base, thereby on upper and lower boss the cylindrical isotropic pyrolytic carbon of formation of deposits.By deposition apparatus provided by the present invention and method primary depositing, can obtain two kinds of different sizes, difform isotropic pyrolytic carbon material simultaneously; And depositing temperature is also reduced to 950-1050 ℃ by 1400-1500 ℃ of fluidized-bed chemical vapor deposition technology, reduced energy consumption, saved preparation cost, depositing temperature is low, and sedimentation effect is high.
Accompanying drawing explanation
Fig. 1 is according to the sectional view of the deposition apparatus of a preferred embodiment of the present invention;
The stereoscan photograph of the isotropic pyrolytic carbon that Fig. 2 embodiment 1 prepares;
The stereoscan photograph of the isotropic pyrolytic carbon that Fig. 3 embodiment 2 prepares;
The stereoscan photograph of the isotropic pyrolytic carbon that Fig. 4 embodiment 3 prepares.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.Should be appreciated that following examples are only for the present invention is described but not for limiting the scope of the invention.
As shown in Figure 1, according to the deposition apparatus of a preferred embodiment of the present invention, comprise: upper deflection cone 1, lower deflection cone 2, depositing base 3, sediment chamber 4, outlet side 5 and inlet end 6.Wherein, upper deflection cone 1 and lower deflection cone 2 are conical structures of being made by high purity graphite, and cone angle is 60 °, with bottom surface, relatively put, on bottom surface, having respectively one from its extended columniform convex platform 11 and lower convex platform 21, is sediment chamber 4 between described upper deflection cone 1 and lower deflection cone 2.The internal diameter of sediment chamber is depicted as 57mm, high 45mm.Depositing base 3 is cylindrical structures of being made by high purity graphite equally, external diameter 47mm, internal diameter 37mm, high 35mm, the external diameter of this depositing base 3 respectively with the bottom surface equal diameters of upper deflection cone 1 and lower deflection cone 2, this depositing base 3 is located at the inside of sediment chamber 4 and is coordinated with convex platform 11 and lower convex platform 21.Outlet side 5 and inlet end 6 form gas port 51 and inlet mouth 61 around the summit of upper deflection cone 1 and lower deflection cone 2 respectively.Wherein, the cone surface of outlet side 5 and upper deflection cone 1 is, keep successively the interval of perforation continuously between the outer wall of the inwall of sediment chamber 4 and depositing base 3 and inlet end 6 and the cone surface of lower deflection cone 2.So, when this deposition apparatus is for the preparation of isotropic pyrolytic carbon time, the columnar isotropic pyrolytic carbon of outer wall formation of deposits round depositing base 3 containing carbon matrix precursor of heat.
Surprisingly, by the inwall of depositing base 3 respectively with the outer wall running fit of convex platform 11 and lower convex platform 21, heat containing carbon matrix precursor enter depositing base 3 inner and on convex platform 11 and lower convex platform 21 the columniform isotropic pyrolytic carbon of formation of deposits.In fact, existing any deposition apparatus all cannot form columniform isotropic pyrolytic carbon, by the deposition apparatus with gap L provided by the present invention initiative obtained columniform isotropic pyrolytic carbon, thereby for those, for columniform profile, have in the application of demand.
In order to form better columniform isotropic pyrolytic carbon, the place, bottom surface of the inwall of depositing base 3 deflection cone 1 and lower deflection cone 2 on closing on has chamfering 7, thereby promote gas uniform ground to the internal divergence of depositing base 3, thereby guarantee the quality of formed columniform isotropic pyrolytic carbon.
In a preferred embodiment, the gap L that retains 1.0mm between the inwall of depositing base 3 and described convex platform 11 and the outer wall of lower convex platform 21, on the end face that depositing base 3 contacts with the bottom surface of described upper deflection cone 1 and described lower deflection cone 2, have groove, so that gas diffuses into depositing base 3 inside along gap L after by this groove.
The gap L that in fact, can retain 0.5～1.5mm between the inwall of depositing base 3 and described convex platform 11 and the outer wall of lower convex platform 21.
In fact, the chamfering that the end that the inwall of depositing base 3 contacts in the bottom surface with upper deflection cone 1 and lower deflection cone 2 has can be 45～60 °.
In addition, the cone angle of upper deflection cone 1 and lower deflection cone 2 can be 45～60 °.
The present invention also provides a kind of method of utilizing this deposition apparatus to prepare isotropic pyrolytic carbon, below provides 3 preferred embodiments.
Embodiment 1
By external diameter 47mm, internal diameter 37mm, internal diameter edge is 45 ° of chamferings, the depositing base 3 that the columnar high purity graphite of high 35mm is made, cone angle are that upper deflection cone 1, the lower deflection cone 2 of 45 ° is placed in Ultrasonic Cleaners ultrasonic cleaning 15min in advance, to remove the graphite particulate that adds surface attachment in man-hour.
Upper deflection cone 1 after above-mentioned steps is cleaned, lower deflection cone 2 and depositing base 3 are put into baking oven, at 110 ℃ of dry 2h, remove moisture.
To be assemblied on the boss of upper deflection cone 1, lower deflection cone 2 through the dried depositing base 3 of above-mentioned steps, wherein, between the inwall of depositing base 3 and convex platform 11 and the outer wall of lower convex platform 21, retain the gap of 0.5mm.
Upper deflection cone 1, lower deflection cone 2 and depositing base 3 after above-mentioned steps assembling are put into internal diameter 57mm, in the isothermal CVD (Chemical Vapor Deposition) chamber 3 of high 45mm, and be connected with outlet side 5 with inlet end 6.
Close isothermal chemical vapor deposition stove fire door; confirm after cvd furnace good seal; under argon shield atmosphere; temperature rise rate with 100 ℃/h rises to 950 ℃ by device temperature, insulation 1h, and then the flow with 500mL/h passes into methane in sediment chamber; after deposition 20h; close methane, pass into argon shield gas, stop deposition.Rate of temperature fall with 100 ℃/h in temperature-fall period is down to equipment after 200 ℃, power-off cooling.At the outer wall of described depositing base 3, form round shape isotropic pyrolytic carbon, between the described convex platform 11 of deflection cone 1 and lower deflection cone 2 and lower convex platform 21, form cylindrical isotropic pyrolytic carbon on described.
The isotropic pyrolytic carbon material of preparing through above-mentioned steps is put into medium-frequency induction furnace and carry out high temperature graphitization processing, graphitization processing temperature is 2700 ℃, and the treatment time is 2h.
Stereoscan photograph from Fig. 2 can be found out, compact structure, the homogeneous grain size of two kinds of difform isotropic pyrolytic carbons prepared by the present embodiment.The density of the material that employing Archimedes drainage records is higher, is 1.78g/cm3.
In order to ensure before forming cylindrical isotropic pyrolytic carbon, space between the outer wall of depositing base and sediment chamber's inwall is not filled, the present embodiment is defined as 0.5mm by the gap between the inwall of depositing base 3 and convex platform 11 and the outer wall of lower convex platform 21, then the flow with 500mL/h passes into methane in sediment chamber, deposition 20h, forms by controlling when this gap length, methane flow and depositing time have guaranteed difform pyrolyzed carbon materials.
Embodiment 2
By external diameter 47mm, internal diameter 37mm, internal diameter edge is 55 ° of chamferings, the depositing base 3 that the columnar high purity graphite of high 35mm is made, cone angle are that upper deflection cone 1, the lower deflection cone 2 of 45 ° is placed in Ultrasonic Cleaners ultrasonic cleaning 15min in advance, to remove the graphite particulate that adds surface attachment in man-hour.
Upper deflection cone 1 after above-mentioned steps is cleaned, lower deflection cone 2 and depositing base 3 are put into baking oven, at 110 ℃ of dry 2h to remove moisture.
To through the dried depositing base 3 of above-mentioned steps, be assemblied on the convex platform 11 and lower convex platform 21 of upper deflection cone 1, lower deflection cone 2, wherein, between the inwall of depositing base 3 and convex platform 11 and the outer wall of lower convex platform 21, retain the gap of 1.0mm.
Upper deflection cone 1, lower deflection cone 2 and depositing base 3 after above-mentioned steps assembling are put into internal diameter 57mm, in the isothermal CVD (Chemical Vapor Deposition) chamber 3 of high 45mm, and be connected with outlet side 5 with inlet end 6.
Close isothermal chemical vapor deposition stove fire door; confirm after cvd furnace good seal; under argon shield atmosphere; temperature rise rate with 150 ℃/h rises to 1000 ℃ by device temperature, insulation 1h, and then the flow with 750mL/h passes into methane in sediment chamber; after deposition 15h; close methane, pass into argon shield gas, stop deposition.Rate of temperature fall with 100 ℃/h in temperature-fall period is down to equipment after 200 ℃, power-off cooling.At the outer wall of described depositing base 3, form round shape isotropic pyrolytic carbon, between the described convex platform 11 of deflection cone 1 and lower deflection cone 2 and lower convex platform 21, form cylindrical isotropic pyrolytic carbon on described.
The isotropic pyrolytic carbon material of preparing through above-mentioned steps is put into medium-frequency induction furnace and carry out high temperature graphitization processing, graphitization processing temperature is 2700 ℃, and the treatment time is 2h.
Stereoscan photograph from Fig. 3 can be found out, compact structure, the homogeneous grain size of two kinds of difform isotropic pyrolytic carbons prepared by the present embodiment.The density of the material that employing Archimedes drainage records is higher, is 1.74g/cm3.
In order to ensure before forming cylindrical isotropic pyrolytic carbon, space between the outer wall of depositing base and sediment chamber's inwall is not filled, the present embodiment is defined as 1.0mm by the gap between the inwall of depositing base 3 and convex platform 11 and the outer wall of lower convex platform 21, then the flow with 750mL/h passes into methane in sediment chamber, deposition 15h, forms by controlling when this gap length, methane flow and depositing time have guaranteed difform pyrolyzed carbon materials.
Embodiment 3
By external diameter 47mm, internal diameter 37mm, internal diameter edge is 60 ° of chamferings, the depositing base 3 that the columnar high purity graphite of high 35mm is made, cone angle are that upper deflection cone 1, the lower deflection cone 2 of 45 ° is placed in Ultrasonic Cleaners ultrasonic cleaning 15min in advance, to remove the graphite particulate that adds surface attachment in man-hour.
Upper deflection cone 1 after above-mentioned steps is cleaned, lower deflection cone 2 and depositing base 3 are put into baking oven, at 110 ℃ of dry 2h to remove moisture.
To through the dried depositing base 3 of above-mentioned steps, be assemblied on the convex platform 11 and lower convex platform 21 of upper deflection cone 1, lower deflection cone 2, wherein, between the inwall of depositing base 3 and convex platform 11 and the outer wall of lower convex platform 21, retain the gap of 1.5mm.
Upper deflection cone 1, lower deflection cone 2 and depositing base 3 after above-mentioned steps assembling are put into internal diameter 57mm, in the isothermal CVD (Chemical Vapor Deposition) chamber 3 of high 45mm, and be connected with outlet side 5 with inlet end 6.
Close isothermal chemical vapor deposition stove fire door; confirm after cvd furnace good seal; under argon shield atmosphere; temperature rise rate with 200 ℃/h rises to 1050 ℃ by device temperature, insulation 1h, and then the flow with 1000mL/h passes into methane in sediment chamber; after deposition 10h; close methane, pass into argon shield gas, stop deposition.Rate of temperature fall with 100 ℃/h in temperature-fall period is down to equipment after 200 ℃, power-off cooling.At the outer wall of described depositing base 3, form round shape isotropic pyrolytic carbon, between the described convex platform 11 of deflection cone 1 and lower deflection cone 2 and lower convex platform 21, form cylindrical isotropic pyrolytic carbon on described.
The isotropic pyrolytic carbon material of preparing through above-mentioned steps is put into medium-frequency induction furnace and carry out high temperature graphitization processing, graphitization processing temperature is 2700 ℃, and the treatment time is 2h.
Stereoscan photograph from Fig. 4 can find out, the relative embodiment 1 and 2 of compact structure of two kinds of difform isotropic pyrolytic carbons prepared by the present embodiment decreases.The density of the material that employing Archimedes drainage records is higher, is 1.70g/cm3.
In order to ensure before forming cylindrical isotropic pyrolytic carbon, space between the outer wall of depositing base and sediment chamber's inwall is not filled, the present embodiment is defined as 1.5mm by the gap between the inwall of depositing base 3 and convex platform 11 and the outer wall of lower convex platform 21, then the flow with 1000mL/h passes into methane in sediment chamber, deposition 10h, forms by controlling when this gap length, methane flow and depositing time have guaranteed difform pyrolyzed carbon materials.
Following table is the bending property of the isotropic pyrolytic carbon of embodiment 1,2,3 preparations.
Table 1 bending property
| Embodiment (depositing temperature) | Flexural strength (MPa) |
| Embodiment 1 (950 ℃) | 165.4 |
| Embodiment 1 (1000 ℃) | 144.8 |
| Embodiment 1 (1050 ℃) | 109.6 |
Known according to upper table 1, in embodiment 1, the flexural strength value of prepared pyrolyzed carbon materials is the highest, compact structure, homogeneous grain size, performance is best, according to contriver's research, reach a conclusion, the most critical factor of the pyrolyzed carbon materials performance impact finally obtaining for the present invention is depositing temperature.According to method provided by the present invention, under the depositing temperature of 950-1050 ℃, can obtain the pyrolyzed carbon materials that isotropic behavior is good, reduce compared to existing technology energy consumption, save preparation cost.
Above-described, be only preferred embodiment of the present invention, not in order to limit scope of the present invention, the above embodiment of the present invention can also make a variety of changes.Be that simple, the equivalence that every claims according to the present patent application and description are done changes and modify, all fall into the claim protection domain of patent of the present invention.The present invention not detailed description be routine techniques content.
Claims (10)
1. a deposition apparatus, described deposition apparatus comprises deflection cone (1), lower deflection cone (2), depositing base (3) and sediment chamber (4), by it, bottom surface is separately relative puts in the inside of described sediment chamber (4) for described upper deflection cone (1) and lower deflection cone (2), has respectively from its extended columniform convex platform (11) and lower convex platform (21) on described bottom surface; The inside that described convex platform (11) and lower convex platform (21) stretch into respectively described depositing base (3) is fixed, it is characterized in that, described depositing base (3) is nonspecular surface with the end face that the bottom surface of described upper deflection cone (1) and lower deflection cone (2) contacts, and retains respectively the gap (L) of 0.5-1.5mm between the inwall of described depositing base (3) and described convex platform (11) and the outer wall of lower convex platform (21).
2. deposition apparatus according to claim 1, is characterized in that, described depositing base (3) locates to have chamfering (7) at contiguous described convex platform (11) and lower convex platform (21).
3. deposition apparatus according to claim 2, is characterized in that, described chamfering (7) is 45～60 °.
4. deposition apparatus according to claim 1, is characterized in that, on the end face that described depositing base (3) contacts with the bottom surface of described upper deflection cone (1) and lower deflection cone (2), has groove.
5. deposition apparatus according to claim 1, is characterized in that, described upper deflection cone (1) and lower deflection cone (2) are conical structure, and cone angle is 45～60 °.
6. deposition apparatus according to claim 1, it is characterized in that, the inwall of the outer wall of described depositing base (3) and described sediment chamber (4) keeps being radially spaced, outlet side (5) and inlet end (6) around described upper deflection cone (1) and lower deflection cone (2) setting keeps being radially spaced with described upper deflection cone (1) and lower deflection cone (2) respectively, and described outlet side (5) and inlet end (6) form air outlet (51) and inlet mouth (61) around the place, summit of described upper deflection cone (1) and lower deflection cone (2).
7. a utilization is prepared cylindrical and method round shape isotropic pyrolytic carbon according to the deposition apparatus described in any one in claim 1-6, it is characterized in that, the columnar isotropic pyrolytic carbon of outer wall formation of deposits containing carbon matrix precursor round described depositing base (3), goes up the columniform isotropic pyrolytic carbon of formation of deposits containing carbon matrix precursor enters described depositing base (3) inside at described convex platform (11) and lower convex platform (21).
8. method according to claim 7, is characterized in that, further comprising the steps of:
S1, under atmosphere of inert gases, is warming up to 950-1050 ℃ by described sediment chamber (4) from room temperature gradually;
S2 passes into containing carbon matrix precursor in described sediment chamber (4);
S3, stops passing into containing carbon matrix precursor, continues to pass into rare gas element, and described sediment chamber (4) are cooled to room temperature from 950-1050 ℃.
9. method according to claim 8, is characterized in that, described rare gas element is argon gas, and described is methane containing carbon matrix precursor.
10. method according to claim 8, is characterized in that, the temperature rise rate in described step S1 is 100～200 ℃/h, and the flow containing carbon matrix precursor in described step S2 is 500～1000mL/h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1778671A (en) * | 2004-11-24 | 2006-05-31 | 中国科学院金属研究所 | Apparatus for producing isotropic pyrolyzed carbon materials of large-size machinery seal |
| CN101705476A (en) * | 2009-11-20 | 2010-05-12 | 中南大学 | Method for rapidly preparing high density isotropic carbon by CVD hot plate method |
| CN102115877A (en) * | 2009-12-31 | 2011-07-06 | 中国科学院金属研究所 | Equipment for preparing boron-doped isotropic pyrolytic carbon materials |
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- 2014-08-18 CN CN201410407180.5A patent/CN104178744B/en active Active
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| CN1778671A (en) * | 2004-11-24 | 2006-05-31 | 中国科学院金属研究所 | Apparatus for producing isotropic pyrolyzed carbon materials of large-size machinery seal |
| CN101705476A (en) * | 2009-11-20 | 2010-05-12 | 中南大学 | Method for rapidly preparing high density isotropic carbon by CVD hot plate method |
| CN102115877A (en) * | 2009-12-31 | 2011-07-06 | 中国科学院金属研究所 | Equipment for preparing boron-doped isotropic pyrolytic carbon materials |
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| 吴峻峰等: "大尺寸各向同性热解炭材料的制备与表征", 《新型炭材料》, vol. 21, no. 2, 30 June 2006 (2006-06-30), pages 119 - 124 * |
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