CN106829916A - 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
- Publication number
- CN106829916A CN106829916A CN201710155477.0A CN201710155477A CN106829916A CN 106829916 A CN106829916 A CN 106829916A CN 201710155477 A CN201710155477 A CN 201710155477A CN 106829916 A CN106829916 A CN 106829916A
- Authority
- CN
- China
- Prior art keywords
- pyrolytic carbon
- carbon fiber
- pure
- tensile property
- fiber beam
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/28—Investigating ductility, e.g. suitability of sheet metal for deep-drawing or spinning
Abstract
The present invention relates to a kind of preparation method 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, prepares the solid pyrolytic carbon fiber beam of varying cross-section product.The beneficial effects of the invention are as follows：(1) when preparing pure pyrolytic carbon Tensile test specimens, cycle is short, process is simple, made pyrolytic carbon test sample globality are destroyed by force, without layering etc.；(2) the pyrolytic carbon fiber beam prepared by belongs to the material of macroscopical category, can accurately test its mechanical property；(3) the method can obtain different structure pyrolytic carbon, including smooth layer, rough layer, isotropic layer pyrolytic carbon accurate tensile property data.
Description
Technical field
It is more particularly to a kind of to utilize the present invention relates to a kind of preparation method of pure pyrolytic carbon tensile property test sample
SiO2Fibre bundle is the preparation method that template prepares pure pyrolytic carbon fiber bundle drawing sample.
Background technology
The tensile mechanical properties of pyrolytic carbon are analyzing carbon/carbon, carbon ceramic composite material residual thermal stress, are predicting its macromechanics
The aspects such as performance are significant, but in actual applications, the data famine, and only low volume data can not be abundant
The mechanical characteristics of reflection 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
The Mechanical Datas such as the stretch modulus of pyrolytic carbon, but do not consider the structure species of pyrolytic carbon, i.e. author by different structure pyrolytic carbon
Mechanical property lump together, cause larger calculation error, have impact on analytical conclusions.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 forefathers about pyrolytic carbon stretch modulus and
Thermal expansion coefficients are pyrolyzed the residual thermal stress of C film according to its certain class for voluntarily preparing is calculated, because not considering pyrolysis carbon structure to mechanics
The influence of feature, analysis result is not accurate enough.
In order to obtain the stretching mechanical data of pyrolytic carbon, researcher can strengthen pyrolytic carbon composite wood based on unidirectional carbon
The tensile property test of material, with mixing principle as foundation, calculates the stretching mechanical data of pyrolytic carbon, the mixing of such as modulus indirectly
Rule formula is Ec=EfVf+Em(1-Vf), wherein Ec、Ef、EmThe respectively elastic modelling quantity of composite, fiber and matrix, Vf、
VmThe respectively volume content of Fiber In Composite Material and matrix.But, the tensile property of unidirectional pyrolysis carbon composite remove with
Fiber and matrix have outside the Pass, and interfacial structure is also quite big with the influence of property, it is sufficient to significantly change the tensile property of 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, particularly different structure pyrolytic carbon, it is necessary to prepare big
The pure pyrolytic carbon Tensile test specimens of size.On the basis of extension test is carried out to it, the stretching for calculating analysis pyrolytic carbon is strong
The stretching mechanical parameter such as degree, modulus.But it is limited to domestic and international existing pyrolytic carbon preparation technology, i.e. chemical vapor deposition, prepares
Large scale is pyrolyzed carbon material, it is necessary to manufacturing cycle of the experience up to more than 1000 hours, and large scale pyrolysis carbon material is easily produced
Layering on raw different scale, has a strong impact on the accuracy of extension test result.It can be seen that, it is necessary to develop a kind of novel pyrolytic carbon
The preparation method of tensile property test sample.
The content of the invention
The technical problem to be solved
In order to avoid the deficiencies in the prior art part, 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, possesses the advantages of short preparation period, low cost, dimensional controllability are good, extension test error is small.
Technical scheme
A kind of preparation method of pure pyrolytic carbon tensile property test sample, it is characterised in that step is as follows：
Step 1：By SiO2Fibre bundle is inserted in cvd furnace, with CH4For presoma deposits pyrolytic carbon, deposition partial pressure is 3-
20kPa, depositing temperature is 800-1200 DEG C, and sedimentation time is 1-5h, and pyrolysis carbon thickness is about 500-2000nm, and pyrolytic carbon is obtained
SiO2Bundle of composite fibers；
Step 2：By SiO2Bundle of composite fibers is cut into fibre bundle section of the length not less than 100mm, lies against and fills volume
To be corroded in the polytetrafluoroethylene (PTFE) closed container of 20-40% hydrofluoric acid aqueous solutions, corrosion temperature is 25-35 DEG C to fraction, when
Between be 5-10min；Afterwards, solution is suctioned out, pours into deionized water cleaning, after standing 5min, then deionized water suctioned out, repeated
Cleaning 3-5 times, to remove the hydrofluoric acid on fibre bundle surface；Alcohol washes fibre bundle then is used, 1h in 60 DEG C of baking ovens is placed in, obtained
Pure tubulose pyrolytic carbon fiber beam
Step 3：Tubulose pyrolytic carbon fiber beam is placed in cvd furnace, with CH4For presoma continues to deposit, depositing temperature is
1050-1120 DEG C, deposition partial pressure is 4-9kPa, after sedimentation time 5-40h, obtains solid pyrolytic carbon fiber beam.
The SiO2Fibre bundle is 500-1000 roots per beam.
It is a kind of to carry out the method that pure pyrolytic carbon tensile property is tested using the test sample, it is characterised in that step is such as
Under：
Step (1)：By length for the solid pyrolytic carbon fiber beam of 50mm is placed in ESEM, and measure the chi of cross section
It is very little, calculate cross-sectional area A；
Step (2)：With reference to ASTM D 3379-75 technical standards, solid pyrolytic carbon fiber Shu Jinhang tensile strengths are surveyed
Examination, obtains maximum tension load FmaxAnd elongation at break εt；
Step (3)：Calculate the tensile strength of pyrolytic carbon fiber beam：
Calculate pyrolytic carbon fiber modulus：
Wherein：Strain when ε is fiber failure, the fracture of the fibre bundle that Δ L and L are respectively in tensile strength test is stretched
Amount long and original are long；εtIt is fracture elongation, E is the stretch modulus of carbon fiber；
Repeat step (1)~step (3), to test the tensile property of 10-20 root pyrolytic carbon fiber beam materials, to 10-20
Individual 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 SiO2It is prepared by fibre bundle
Pyrolytic carbon and SiO2Bundle of composite fibers, corroded with hydrofluoric acid aqueous solution, obtain pure tubulose pyrolytic carbon fiber beam；So
After be placed in cvd furnace, prepare varying cross-section product solid pyrolytic carbon fiber beam.The beneficial effects of the invention are as follows：(1)
When preparing pure pyrolytic carbon Tensile test specimens, cycle is short, process is simple, 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 category, can accurately test its mechanical property；(3) party
Method can obtain different structure pyrolytic carbon, including smooth layer, rough layer, isotropic layer pyrolytic carbon accurate tensile property data.
Specific embodiment
In conjunction with embodiment, the invention will be further described：
Example 1：
(1) SiO that will be bought2Fibre bundle is directly placed into cvd furnace, with CH4Deng alkane, C3H6Deng alcohol such as alkene, ethanol
Class is that presoma deposits pyrolytic carbon, and deposition partial pressure is 15kPa, and depositing temperature is 1150 DEG C, and sedimentation time is 3h, measures pyrolytic carbon
Thickness is about 700-900nm, and pyrolytic carbon and SiO is obtained2Bundle of composite fibers.
(2) bundle of composite fibers prepared by step (1) is cut into fibre bundle section of the length not less than 100mm, is lain against
Fill and 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, afterwards, solution is suctioned out with suction pipe.Deionized water cleaning is poured into, after standing 5min, then deionized water is inhaled
Go out, and repeated washing 5 times.Alcohol washes fibre bundle is used, 1h in 60 DEG C of baking ovens is placed in, pure tubulose pyrolytic carbon fiber is obtained
Beam.
(3) the tubulose pyrolytic carbon fiber beam prepared by step (2) is placed in cvd furnace, with CH4For presoma continues heavy
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) prepare the sample preparation of rough layer pyrolytic carbon and test is repeated several times, obtain tensile strength σ be 227-
240MPa, modulus E are 22-24GPa.
Example 2：
(1) SiO that will be bought2Fibre bundle is directly placed into cvd furnace, with CH4For presoma deposits pyrolytic carbon, partial pressure is deposited
Be 15kPa, depositing temperature is 1000 DEG C, and sedimentation time is 2h, pyrolysis carbon thickness is about 1500-1700nm, be obtained pyrolytic carbon and
SiO2Bundle of composite fibers.
(2) bundle of composite fibers prepared by step (1) is cut into fibre bundle section of the length not less than 100mm, is lain against
Fill and 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, afterwards, solution is suctioned out with suction pipe.Deionized water cleaning is poured into, after standing 5min, then deionized water is inhaled
Go out, repeated washing 3 times.Alcohol washes fibre bundle is used, 1h in 60 DEG C of baking ovens is placed in, pure tubulose pyrolytic carbon fiber beam is obtained.
(3) the tubulose pyrolytic carbon fiber beam prepared by step (2) is placed in cvd furnace, with CH4For presoma continues heavy
Product, sets depositing temperature as 1050 DEG C, and deposition partial pressure is 9kPa.After sedimentation time 30h, the solid pyrolytic carbon of smooth layer is obtained fine
Dimension beam.
(4) by step (3) prepare the sample preparation of smooth layer pyrolytic carbon and test is repeated several times, 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 step is as follows：
Step (1)：By length for the solid pyrolytic carbon fiber beam of 50mm is placed in ESEM, and measure the chi of cross section
It is very little, calculate cross-sectional area A；
Step (2)：With reference to ASTM D 3379-75 technical standards, solid pyrolytic carbon fiber Shu Jinhang tensile strengths are surveyed
Examination, obtains maximum tension load FmaxAnd elongation at break εt；
Step (3)：Calculate the tensile strength of pyrolytic carbon fiber beam：
Calculate pyrolytic carbon fiber modulus：
Wherein：Strain when ε is fiber failure, the fracture of the fibre bundle that Δ L and L are respectively in tensile strength test is stretched
Amount long and original are long；εtIt is fracture elongation, E is the stretch modulus of carbon fiber；
Repeat step (1)~step (3), to test the tensile property of 10-20 root pyrolytic carbon fiber beam materials, to 10-20
Individual 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 step is as follows：
Step 1：By SiO2Fibre bundle is inserted in cvd furnace, with CH4For presoma deposits pyrolytic carbon, deposition partial pressure is 3-20kPa,
Depositing temperature is 800-1200 DEG C, and sedimentation time is 1-5h, and pyrolysis carbon thickness is about 500-2000nm, and the SiO of pyrolytic carbon is obtained2
Bundle of composite fibers；
Step 2：By SiO2Bundle of composite fibers is cut into fibre bundle section of the length 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 solutions, corrosion temperature is 25-35 DEG C, and the time is 5-
10min；Afterwards, solution is suctioned out, pours into deionized water cleaning, after standing 5min, then deionized water suctioned out, repeated washing 3-
5 times, to remove the hydrofluoric acid on fibre bundle surface；Alcohol washes fibre bundle then is 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 is placed in cvd furnace, with CH4For presoma continues to deposit, depositing temperature is 1050-
1120 DEG C, deposition partial pressure is 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
Fibre bundle is 500-1000 roots per beam.
It is 3. a kind of to carry out the method that pure pyrolytic carbon tensile property is tested using test sample described in claim 1, it is characterised in that
Step is as follows：
Step (1)：By length for the solid pyrolytic carbon fiber beam of 50mm is placed in ESEM, and the size of cross section is measured, meter
Calculate cross-sectional area A；
Step (2)：With reference to ASTM D 3379-75 technical standards, solid pyrolytic carbon fiber Shu Jinhang tensile strengths are tested, obtained
To maximum tension load FmaxAnd elongation at break εt；
Step (3)：Calculate the tensile strength of pyrolytic carbon fiber beam：
Calculate pyrolytic carbon fiber modulus：
Wherein：Strain when ε is fiber failure, Δ L and L are respectively the extension at break amount of the fibre bundle in tensile strength test
It is long with original；εtIt is fracture elongation, E is the stretch modulus of carbon fiber；
Repeat step (1)~step (3), to test the tensile property of 10-20 root pyrolytic carbon fiber beam materials, surveys to 10-20
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 that pure pyrolytic carbon tensile property is tested according to claim 2, it is characterised in that：The scanning electron microscope sem
It is FEI NANOSEM450.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710155477.0A CN106829916B (en) | 2017-03-16 | 2017-03-16 | A kind of preparation method of pure pyrolytic carbon tensile property test sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710155477.0A CN106829916B (en) | 2017-03-16 | 2017-03-16 | A kind of preparation method of pure pyrolytic carbon tensile property test sample |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106829916A true CN106829916A (en) | 2017-06-13 |
| CN106829916B CN106829916B (en) | 2018-12-28 |
Family
ID=59143956
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710155477.0A Active CN106829916B (en) | 2017-03-16 | 2017-03-16 | A kind of preparation method of pure pyrolytic carbon tensile property test sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106829916B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113029786A (en) * | 2021-03-16 | 2021-06-25 | 南京航空航天大学 | Ceramic fiber strength distribution rapid measurement method |
| CN113023726A (en) * | 2021-04-16 | 2021-06-25 | 西北工业大学 | Method for preparing high-thermal-conductivity carbon material by low-temperature CVD (chemical vapor deposition) method |
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 |
-
2017
- 2017-03-16 CN CN201710155477.0A patent/CN106829916B/en active Active
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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113029786A (en) * | 2021-03-16 | 2021-06-25 | 南京航空航天大学 | Ceramic fiber strength distribution rapid measurement method |
| CN113023726A (en) * | 2021-04-16 | 2021-06-25 | 西北工业大学 | Method for preparing high-thermal-conductivity carbon material by low-temperature CVD (chemical vapor deposition) method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106829916B (en) | 2018-12-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102435513B (en) | Prediction method of breaking strength and toughness of brittle film | |
| CN106829916B (en) | A kind of preparation method of pure pyrolytic carbon tensile property test sample | |
| Xia et al. | Study on the breaking strength of jute fibres using modified Weibull distribution | |
| CN106934168B (en) | A kind of material multi-axial creep failure strain prediction technique | |
| WO2013086933A1 (en) | Method for calibration of parameters assessing brittle fracture of material based on beremin model | |
| Xie et al. | Size effect research of tensile strength of bamboo scrimber based on boundary effect model | |
| CN102135486A (en) | Method for quickly detecting concentration of polyacrylonitrile-based free radical coagulation bath | |
| Wen et al. | Study on mechanical properties and size effect of coal gangue concrete at mesoscale | |
| CN104050387A (en) | Concrete thermal expansion coefficient prediction model construction method | |
| CN115964954A (en) | Ultrahigh-performance concrete multi-item performance prediction method and mix proportion optimization design method thereof | |
| Kong et al. | Development of micro and macro fracture properties of cementitious materials exposed to freeze-thaw environment at early ages | |
| Kai-yun et al. | Fracture propertie analysis of recycled aggregate concrete based on digital image correlation technique | |
| Jin et al. | Experimental and simulative study of bonding properties on fiber/epoxy interfaces by digital image correlation (DIC) technique and molecular dynamics | |
| Sun et al. | Multiscale collaborative process optimization method for automated fiber placement | |
| CN108204997A (en) | Normal line oil flash point online soft sensor method | |
| Eppers et al. | Autogenous shrinkage strain of ultra-high-performance concrete (UHPC) | |
| CN109711014A (en) | The model building method of wood-bending amount of deflection after a kind of microwave combined sofening treatment of hydro-thermal- | |
| CN108733861A (en) | Creep incubation period prediction technique containing residual stress under the condition of palsticity | |
| Shao et al. | Application of BP neural network model in the recycled concrete performance prediction | |
| Jin | Strength prediction method of nano ceramic composites based on nonlinear regression analysis | |
| Pan et al. | Performance of ferritic steel 16MnDR using improved local fracture criterion | |
| Gao et al. | Mechanical properties analysis of cell surface based on genetic simulated annealing optimization neural network | |
| CN113295564B (en) | Improved Beremin model parameter calibration method | |
| Mo et al. | Construction Mechanics of Nano Pva Modified Fiber Cement Soil | |
| Ali et al. | The hardened characteristics of self-compacting mortar including carbon fibers and estimation results by artificial neural networks |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221102 Address after: No. 25, Yangbei Road, Luoshe Town, Huishan District, Wuxi City, Jiangsu Province, 214154 Patentee after: Wuxi Bozhi Composite Materials Co.,Ltd. Address before: 710072 No. 127 Youyi West Road, Shaanxi, Xi'an Patentee before: Northwestern Polytechnical University |
|
| TR01 | Transfer of patent right |