CN106829916B - A kind of preparation method of pure pyrolytic carbon tensile property test sample - Google Patents
A kind of preparation method of pure pyrolytic carbon tensile property test sample Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of pure pyrolytic carbon tensile property test sample, using SiO2Fibre bundle prepares pyrolytic carbon and SiO2Bundle of composite fibers, corroded with hydrofluoric acid aqueous solution, obtain pure tubulose pyrolytic carbon fiber beam；It is subsequently placed in cvd furnace, the solid pyrolytic carbon fiber beam of varying cross-section product is prepared.The beneficial effects of the present invention are: when (1) prepares pure pyrolytic carbon Tensile test specimens, the period is short, simple process, and made pyrolytic carbon test sample globality is strong, destroys without layering etc.；(2) the pyrolytic carbon fiber beam prepared by belongs to the material of macroscopical scope, can accurately test its mechanical property；(3) this method can get different structure pyrolytic carbon, including smooth layer, rough layer, isotropic layer pyrolytic carbon accurate tensile property data.
Description
Technical field
The present invention relates to a kind of preparation methods of pure pyrolytic carbon tensile property test sample, more particularly to a kind of utilization
SiO2Fibre bundle is the preparation method that template prepares pure pyrolytic carbon fiber bundle drawing sample.
Background technique
The tensile mechanical properties of pyrolytic carbon are analyzing carbon/carbon, carbon ceramic composite material residual thermal stress, are predicting its macromechanics
Performance etc. is of great significance, but in practical applications, and there is a serious shortage of and only low volume data cannot be abundant for the data
The mechanical characteristics for reflecting different structure pyrolytic carbon (such as rough layer, smooth layer, isotropic layer pyrolytic carbon), cause analytical error.
For example, in document Magali Rollin, St é phane Jouannigot, Jacques Lamon, Ren é
Pailler.Characterization of fibre/matrix interfaces in carbon/carbon
Composite.Composites Science and Technology, 2009,69 (9), in 1442-1446., author's application
Mechanical Datas such as the stretch modulus of pyrolytic carbon, but do not consider the structure species of pyrolytic carbon, i.e. author are by different structure pyrolytic carbon
Mechanical property lump together, lead to biggish calculating error, affect analysis conclusion.In document Craig A.Taylor,
Mark F.Wayne,and Wilson KS Chiu.Heat treatment of thin carbon films and the
effect on residual stress,modulus,thermal expansion and
Microstructure.Carbon, 2003,41 (10), in 1867-1875. using stretch modulus of the forefathers in relation to pyrolytic carbon and
Thermal expansion coefficients are according to the residual thermal stress for calculating certain class pyrolysis C film that it is voluntarily prepared, because not considering to be pyrolyzed carbon structure to mechanics
The influence of feature, analysis result are inaccurate.
In order to obtain the stretching mechanical data of pyrolytic carbon, researcher can enhance pyrolytic carbon composite wood based on unidirectional carbon fiber
The tensile property of material is tested, and using mixing principle as foundation, calculates the stretching mechanical data of pyrolytic carbon, such as the mixing of modulus indirectly
Rule formula is Ec=EfVf+Em(1-Vf), wherein Ec、Ef、EmThe respectively elasticity modulus of composite material, fiber and matrix, Vf、
VmThe respectively volume content of Fiber In Composite Material and matrix.But unidirectionally pyrolysis carbon composite tensile property remove with
Fiber and matrix have outside the Pass, and the influence of interfacial structure and property is also quite large, it is sufficient to the tensile property for substantially changing material, because
This, the stretching mechanical data error for calculating pyrolytic carbon using mixing principle is also larger.
In order to obtain the stretching mechanical data of accurate Mechanical Data, especially different structure pyrolytic carbon, need to prepare big
The pure pyrolytic carbon Tensile test specimens of size.On the basis of carrying out extension test to it, the stretching for calculating analysis pyrolytic carbon is strong
The stretching mechanicals parameter such as degree, modulus.But it is limited to domestic and international existing pyrolytic carbon preparation process, i.e. chemical vapor deposition, prepares
Large scale is pyrolyzed carbon material, it is necessary to which experience is up to 1000 hours or more manufacturing cycles, and large scale pyrolysis carbon material easily produces
Layering on raw different scale, seriously affects the accuracy of extension test result.As it can be seen that it is necessary to develop a kind of novel pyrolytic carbon
The preparation method of tensile property test sample.
Summary of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of system of pure pyrolytic carbon tensile property test sample
Preparation Method, to be commercialized SiO2Fibre bundle is template, and the depositing operation based on optimization can prepare the fiber of different structure pyrolytic carbon
Pencil tensile property test sample has the advantages that short preparation period, at low cost, dimensional controllability is good, extension test error is small.
Technical solution
A kind of preparation method of pure pyrolytic carbon tensile property test sample, it is characterised in that steps are as follows:
Step 1: by SiO2Fibre bundle is placed in cvd furnace, with CH4Pyrolytic carbon is deposited for presoma, deposition partial pressure is 3-
20kPa, depositing temperature are 800-1200 DEG C, sedimentation time 1-5h, and pyrolysis carbon thickness is about 500-2000nm, and pyrolytic carbon is made
SiO2Bundle of composite fibers；
Step 2: by SiO2Bundle of composite fibers is cut into the fibre bundle section that length is not less than 100mm, lies against and fills volume
For score to be corroded in the polytetrafluoroethylene (PTFE) closed container of 20-40% hydrofluoric acid aqueous solution, corrosion temperature is 25-35 DEG C, when
Between be 5-10min；Later, solution is sucked out, pours into deionized water cleaning, after standing 5min, then deionized water is sucked out, is repeated
Cleaning 3-5 times, to remove the hydrofluoric acid on fibre bundle surface；Alcohol washes fibre bundle is then used, 1h in 60 DEG C of baking ovens is placed in, obtains
Pure tubulose pyrolytic carbon fiber beam
Step 3: tubulose pyrolytic carbon fiber beam being placed in cvd furnace, with CH4Continue to deposit for presoma, depositing temperature is
1050-1120 DEG C, partial pressure is deposited as 4-9kPa, after sedimentation time 5-40h, obtains solid pyrolytic carbon fiber beam.
The SiO2The every beam of fibre bundle is 500-1000 root.
A method of pure pyrolytic carbon tensile property is carried out using the test sample and is tested, it is characterised in that step is such as
Under:
Step (1): the solid pyrolytic carbon fiber beam that length is 50mm is placed in scanning electron microscope, and measures the ruler of cross section
It is very little, calculate cross-sectional area A；
Step (2): referring to ASTM D 3379-75 technical standard, solid pyrolytic carbon fiber Shu Jinhang tensile strength is surveyed
Examination, obtains maximum tension load FmaxAnd elongation at break εt；
Step (3): the tensile strength of pyrolytic carbon fiber beam is calculated:
Calculate pyrolytic carbon fiber modulus:
Wherein: strain when ε is fiber failure, Δ L and L are respectively that the fracture of the fibre bundle in tensile strength test is stretched
Long amount and original are long；εtFor fracture elongation, E is the stretch modulus of carbon fiber；
It repeats step (1)~step (3), to test the tensile property of 10-20 root pyrolytic carbon fiber beam material, to 10-20
A test result, i.e. tensile strength σ and modulus E carry out Weibull analysis, obtain the tensile property number of pure pyrolytic carbon fiber beam
According to.
The scanning electron microscope sem is FEI NANOSEM450.
Beneficial effect
The preparation method of a kind of pure pyrolytic carbon tensile property test sample proposed by the present invention, using SiO2Fibre bundle preparation
Pyrolytic carbon and SiO2Bundle of composite fibers, corroded with hydrofluoric acid aqueous solution, obtain pure tubulose pyrolytic carbon fiber beam；So
It is placed in cvd furnace, the solid pyrolytic carbon fiber beam of varying cross-section product is prepared.The beneficial effects of the present invention are: (1)
When preparing pure pyrolytic carbon Tensile test specimens, the period is short, simple process, and made pyrolytic carbon test sample globality is strong, without layering
Deng destruction；(2) the pyrolytic carbon fiber beam prepared by belongs to the material of macroscopical scope, can accurately test its mechanical property；(3) party
Method can get different structure pyrolytic carbon, including smooth layer, rough layer, isotropic layer pyrolytic carbon accurate tensile property data.
Specific embodiment
Now in conjunction with embodiment, the invention will be further described:
Example 1:
(1) by the SiO of purchase2Fibre bundle is directly placed into cvd furnace, with CH4Equal alkane, C3H6The alcohol such as equal alkene, ethyl alcohol
Class is that presoma deposits pyrolytic carbon, and deposition partial pressure is 15kPa, and depositing temperature is 1150 DEG C, and sedimentation time 3h measures pyrolytic carbon
Thickness is about 700-900nm, and pyrolytic carbon and SiO is made2Bundle of composite fibers.
(2) bundle of composite fibers prepared by step (1) is cut into the fibre bundle section that length is not less than 100mm, lain against
It filling and is corroded in the polytetrafluoroethylene (PTFE) closed container that volume fraction is 40% hydrofluoric acid aqueous solution, corrosion temperature is 30 DEG C,
Time is 5min, and later, solution is sucked out with suction pipe.Deionized water cleaning is poured into, after standing 5min, then deionized water is inhaled
Out, and repeated washing 5 times.With alcohol washes fibre bundle, it is placed in 1h in 60 DEG C of baking ovens, obtains pure tubulose pyrolytic carbon fiber
Beam.
(3) tubulose pyrolytic carbon fiber beam prepared by step (2) is placed in cvd furnace, with CH4Continue to sink for presoma
Product sets depositing temperature as 1100 DEG C, and deposition partial pressure is 8kPa.In sedimentation time 20h, the solid pyrolytic carbon fiber of rough layer is obtained
Beam.
(4) by step (3) preparation the sample preparation of rough layer pyrolytic carbon and do multiplicating test, obtain tensile strength σ be 227-
240MPa, modulus E are 22-24GPa.
Example 2:
(1) by the SiO of purchase2Fibre bundle is directly placed into cvd furnace, with CH4Pyrolytic carbon, deposition partial pressure are deposited for presoma
For 15kPa, depositing temperature is 1000 DEG C, sedimentation time 2h, and pyrolysis carbon thickness is about 1500-1700nm, be made pyrolytic carbon and
SiO2Bundle of composite fibers.
(2) bundle of composite fibers prepared by step (1) is cut into the fibre bundle section that length is not less than 100mm, lain against
It filling and is corroded in the polytetrafluoroethylene (PTFE) closed container that volume fraction is 30% hydrofluoric acid aqueous solution, corrosion temperature is 35 DEG C,
Time is 7min, and later, solution is sucked out with suction pipe.Deionized water cleaning is poured into, after standing 5min, then deionized water is inhaled
Out, repeated washing 3 times.With alcohol washes fibre bundle, it is placed in 1h in 60 DEG C of baking ovens, obtains pure tubulose pyrolytic carbon fiber beam.
(3) tubulose pyrolytic carbon fiber beam prepared by step (2) is placed in cvd furnace, with CH4Continue to sink for presoma
Product sets depositing temperature as 1050 DEG C, and deposition partial pressure is 9kPa.After sedimentation time 30h, the solid pyrolysis carbon fiber of smooth layer is obtained
Tie up beam.
(4) by step (3) preparation the sample preparation of smooth layer pyrolytic carbon and do multiplicating test, obtain tensile strength σ be 252-
282MPa, modulus E are 20-22GPa.
The method that the test sample carries out pure pyrolytic carbon tensile property test, it is characterised in that steps are as follows:
Step (1): the solid pyrolytic carbon fiber beam that length is 50mm is placed in scanning electron microscope, and measures the ruler of cross section
It is very little, calculate cross-sectional area A；
Step (2): referring to ASTM D 3379-75 technical standard, solid pyrolytic carbon fiber Shu Jinhang tensile strength is surveyed
Examination, obtains maximum tension load FmaxAnd elongation at break εt；
Step (3): the tensile strength of pyrolytic carbon fiber beam is calculated:
Calculate pyrolytic carbon fiber modulus:
Wherein: strain when ε is fiber failure, Δ L and L are respectively that the fracture of the fibre bundle in tensile strength test is stretched
Long amount and original are long；εtFor fracture elongation, E is the stretch modulus of carbon fiber；
It repeats step (1)~step (3), to test the tensile property of 10-20 root pyrolytic carbon fiber beam material, to 10-20
A test result, i.e. tensile strength σ and modulus E carry out Weibull analysis, obtain the tensile property number of pure pyrolytic carbon fiber beam
According to.
The scanning electron microscope sem is FEI NANOSEM450.
Claims (4)
1. a kind of preparation method of pure pyrolytic carbon tensile property test sample, it is characterised in that steps are as follows:
Step 1: by SiO2Fibre bundle is placed in cvd furnace, with CH4Pyrolytic carbon is deposited for presoma, deposition partial pressure is 3-20kPa,
Depositing temperature is 800-1200 DEG C, sedimentation time 1-5h, and the SiO of pyrolytic carbon is made with a thickness of 500-2000nm in pyrolytic carbon2It is multiple
Condensating fiber beam；
Step 2: by SiO2Bundle of composite fibers is cut into the fibre bundle section that length is not less than 100mm, lies against and fills volume fraction and be
Corroded in the polytetrafluoroethylene (PTFE) closed container of 20-40% hydrofluoric acid aqueous solution, corrosion temperature is 25-35 DEG C, time 5-
10min；Later, solution is sucked out, pours into deionized water cleaning, after standing 5min, then deionized water is sucked out, repeated washing 3-
5 times, to remove the hydrofluoric acid on fibre bundle surface；Alcohol washes fibre bundle is then used, 1h in 60 DEG C of baking ovens is placed in, obtains pure
Tubulose pyrolytic carbon fiber beam；
Step 3: tubulose pyrolytic carbon fiber beam being placed in cvd furnace, with CH4Continue to deposit for presoma, depositing temperature 1050-
1120 DEG C, partial pressure is deposited as 4-9kPa, after sedimentation time 5-40h, obtains solid pyrolytic carbon fiber beam.
2. the preparation method of pure pyrolytic carbon tensile property test sample according to claim 1, it is characterised in that: the SiO2
The every beam of fibre bundle is 500-1000 root.
3. a kind of method for carrying out pure pyrolytic carbon tensile property test using test sample described in claim 1, it is characterised in that
Steps are as follows:
Step (1): the solid pyrolytic carbon fiber beam that length is 50mm is placed in scanning electron microscope, and measures the size of cross section, is counted
Calculate cross-sectional area A；
Step (2): referring to ASTM D 3379-75 technical standard, solid pyrolytic carbon fiber Shu Jinhang tensile strength is tested, is obtained
To maximum tension load FmaxAnd fracture elongation εt；
Step (3): the tensile strength of pyrolytic carbon fiber beam is calculated:
Calculate pyrolytic carbon fiber modulus:
Wherein: strain when ε is fiber failure, △ L and L are respectively the extension at break amount of the fibre bundle in tensile strength test
It is long with original；εtFor fracture elongation, E is the stretch modulus of carbon fiber；
It repeats step (1)~step (3), to test the tensile property of 10-20 root pyrolytic carbon fiber beam material, 10-20 is surveyed
Test result, i.e. tensile strength σ and modulus E carry out Weibull analysis, obtain the tensile property data of pure pyrolytic carbon fiber beam.
4. the method for pure pyrolytic carbon tensile property test according to claim 3, it is characterised in that: the scanning electron microscope sem
For FEI NANOSEM450.
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Citations (4)
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|---|---|---|---|---|
| CN101477009A (en) * | 2009-01-21 | 2009-07-08 | 哈尔滨工业大学 | Method for testing boundary strength between fiber bundle and substrate of carbon fiber reinforced carbon materials |
| US20110002086A1 (en) * | 2009-07-01 | 2011-01-06 | Feaver Aaron M | Ultrapure synthetic carbon materials |
| EP2322474A1 (en) * | 2009-11-16 | 2011-05-18 | Evonik Degussa GmbH | Method for pyrolysis of carbohydrates |
| CN104211045A (en) * | 2014-09-04 | 2014-12-17 | 江南大学 | Method for easily and fast preparing rice hull-based porous carbon/silicon dioxide composite material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101477009A (en) * | 2009-01-21 | 2009-07-08 | 哈尔滨工业大学 | Method for testing boundary strength between fiber bundle and substrate of carbon fiber reinforced carbon materials |
| US20110002086A1 (en) * | 2009-07-01 | 2011-01-06 | Feaver Aaron M | Ultrapure synthetic carbon materials |
| EP2322474A1 (en) * | 2009-11-16 | 2011-05-18 | Evonik Degussa GmbH | Method for pyrolysis of carbohydrates |
| CN104211045A (en) * | 2014-09-04 | 2014-12-17 | 江南大学 | Method for easily and fast preparing rice hull-based porous carbon/silicon dioxide composite material |
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