CN106908474B - Utilize the method for carbon nanometer paper sensor monitoring polymer based composites curing degree - Google Patents
Utilize the method for carbon nanometer paper sensor monitoring polymer based composites curing degree Download PDFInfo
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Abstract
The invention belongs to technical field of composite materials, and in particular to a method of utilize carbon nanometer paper sensor monitoring polymer based composites curing degree.The present invention is that carbon nanometer paper sensor is embedded to the inside of polymer matrix composite prepreg to be measured, obtain carbon nanometer paper resistance variations-Temperature-time relation curve of solidification process, linear fit is carried out to the carbon nanometer paper resistance variations-temperature curve for solidifying cooling stage, obtain the temperature-coefficient of electrical resistance of the carbon nanometer paper of cooling stage, the curing degree of DSC method measurement polymer matrix composite under standard cure process system is utilized simultaneously, obtain corresponding temperature-coefficient of electrical resistance and curing degree respectively at a temperature of other, obtain curing degree-temperature-coefficient of electrical resistance relation curve of polymer matrix composite.Technical solution of the present invention, which can deploy to ensure effective monitoring and control of illegal activities, carries out the monitoring of real-time online engineer application in composite material different location, has very high precision and operability, while sensor and demodulating system are at low cost.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of to utilize carbon nanometer paper sensor monitoring polymer base
The method of composite material curing degree.
Background technique
The performance of thermosetting material depends not only on the structure and performance of resin matrix, curing agent and additive, also depends on
It is closely related with its curing degree in the curing molding course between them.Curing degree is one for reflecting resin solidification degree
Important indicator.Composite material heating temperature, heating time, soaking time, cooling velocity and machine condition in the curing process,
Structure design etc. factors composite material curing degree can all be had an impact, thus influence composite material the quality of production and size it is steady
It is qualitative.The measurement method of traditional composite material curing degree be all it is non-online, pass through the remaining reaction in measurement material system
The method of heat measures curing degree (i.e. DSC, differential scanning calorimetery), is that one kind takes a long time, and material loss is serious, higher cost
Measurement method.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of multiple using carbon nanometer paper sensor monitoring polymer base
The method of condensation material curing degree, it is therefore an objective to shorten the time of measuring of curing degree, reduce measurement cost, improve measurement accuracy.
Realize that the method using carbon nanometer paper sensor monitoring polymer based composites curing degree of the object of the invention is pressed
It is carried out according to following steps:
(1) four copper conductors are fixed on rectangle carbon nanometer paper surface, carbon nanometer paper sensor are formed, by this carbon nanometer
Paper sensor is embedded to the inside of polymer matrix composite prepreg to be measured, according to the standard of polymer matrix composite prepreg
Curing process system curing molding obtains polymer matrix composite；
(2) in solidification process, the carbon nanometer paper sensor inside embedment prepreg is measured using four probe resistance measuring instruments
Resistance variations the carbon nanometer paper electricity of solidification process is obtained using the temperature change of fiber grating measurement prepreg solidification process
Resistive-Temperature-time relation curve carries out Linear Quasi to the carbon nanometer paper resistance variations-temperature curve for solidifying cooling stage
It closes, obtains the temperature-coefficient of electrical resistance of the carbon nanometer paper of cooling stage；
The curing degree of DSC method measurement polymer matrix composite under standard cure process system is utilized simultaneously；
(3) it is being lower than 5 DEG C of standard cure temperature, 10 DEG C, 15 DEG C, 20 DEG C, 25 DEG C respectively, and is being higher than standard cure temperature
Polymer matrix composite prepreg cure test is carried out at 5 DEG C, 10 DEG C, is repeated step (2), is obtained corresponding resistance temperature respectively
Coefficient and curing degree are spent, curing degree-temperature-coefficient of electrical resistance relation curve of polymer matrix composite is obtained；
(4) when practical engineering application, by the cooling stage carbon nanometer for monitoring the polymer matrix composite solidification process
Paper temperature-coefficient of electrical resistance obtains corresponding curing degree according to the curing degree in step (3)-temperature-coefficient of electrical resistance relation curve.
Wherein, the copper conductor is fixed on rectangle carbon nanometer paper surface using conducting resinl.
Compared with prior art, the features of the present invention and beneficial effect are:
Carbon nanometer paper in the present invention is interacted and shape with gap therebetween by intermolecular van der Waals by carbon nanotube
At three-dimensional net structure, gap belongs to typical mesoporous material, resin is received with carbon between 20-100nm between carbon nanometer paper
Rice paper has excellent imbibition characteristic, has very high sensitivity to resin phase-state change.It is solid in polymer matrix composite
During change, resin crosslinking curing forms three-dimensional net structure, more sensitive to temperature change when resin solidification degree is lower.
When the temperature decreases, the lower resin shrinkage degree of crosslinking degree is higher, the potential barrier for transmitting electronics in carbon nanometer paper conductive network
It reduces, causes carbon nanometer paper resistance variations more sensitive to the variation of temperature.So curing degree is lower, the resistance temperature of carbon nanometer paper
Degree absorbs higher.
Technical solution of the present invention, which can deploy to ensure effective monitoring and control of illegal activities, carries out the monitoring of real-time online engineer application, tool in composite material different location
There are very high precision and operability, while sensor and demodulating system are at low cost.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of carbon nanometer paper sensor of the invention；
Wherein: 1: four probe resistance measuring instrument；2: conducting resinl；3: carbon nanometer paper；4: copper conductor；
Fig. 2 is resistance variations-temperature-of carbon nanometer paper sensor monitoring composite material solidification process in the embodiment of the present invention
Time graph；
Fig. 3 is carbon nanometer paper resistance variations-temperature of cooling stage under different curing process systems in the embodiment of the present invention
Matched curve.
Specific embodiment
Carbon nanometer paper involved in the embodiment of the present invention is that patent application CN2012104391772(is based on carbon nanotube three
Tie up network thin-film temperature sensor preparation method) in prepare carbon nanometer paper；
Monitoring object in the embodiment of the present invention is glass fibre/epoxy resin, and prepreg purchase has from Weihai light prestige
Limit company (6509/G15000/33%)；
Four probe resistance measuring instrument model RTS-8 used in the present embodiment, four probe of Guangzhou science and technology；
Fiber grating used in the present embodiment selects sm125 static state (FBG) demodulator (U.S. MOI)；
Using DSC method measurement curing degree using the resistance to DSC2002F3 that speeds in the present embodiment；
Linear fit is carried out to experimental data in the present embodiment and uses Origin software.
Embodiment
The method using carbon nanometer paper sensor monitoring polymer based composites curing degree of the present embodiment is according to following
Step carries out:
(1) as shown in Figure 1, four copper conductors 4 are fixed on 3 surface of rectangle carbon nanometer paper, carbon nanometer paper sensing is formed
This carbon nanometer paper sensor is embedded to the inside of polymer matrix composite prepreg to be measured, polymerization to be measured in the present embodiment by device
Object matrix composite prepreg is glass fibre/epoxy prepreg, is that glass fibre/epoxy resin presoaks according to prepreg
The standard cure process system curing molding of material obtains glass fibre/epoxy resin, and detailed process is by glass fibre/asphalt mixtures modified by epoxy resin
Rouge prepreg is according to [0]16Ply sequence, be laid on the mold for being coated with release agent, wherein carbon nanometer paper sensor and optical fiber
Grating is placed on the 8th layer and the 9th layer centre of composite material, is covered with the die package of prepreg in vacuum bag, is placed on baking oven together
In, it vacuumizes, dynamic heats up, dynamic heating process are as follows: be increased to 120 DEG C from room temperature according to the heating rate of 1 DEG C/min, and protect
Hold 120min；
(2) in solidification process, the carbon nanometer paper sensor inside embedment prepreg is measured using four probe resistance measuring instruments
Resistance variations the carbon nanometer paper electricity of solidification process is obtained using the temperature change of fiber grating measurement prepreg solidification process
Resistive-Temperature-time relation curve, as shown in Fig. 2, the wherein initial resistance R of carbon nanometer paper sensor0, in solidification process
Resistance change value is △ R, with △ R/ R0The carbon nanometer paper resistance variations for indicating solidification process, receive the carbon for solidifying cooling stage
Rice paper resistance variations-temperature curve carries out linear fit, as shown in figure 3, the carbon for obtaining cooling stage under standard cure technique is received
The temperature-coefficient of electrical resistance of rice paper；
The curing degree of DSC method measurement polymer matrix composite under standard cure process system is utilized simultaneously；
(3) it is being lower than 5 DEG C of standard cure temperature, 10 DEG C, 15 DEG C, 20 DEG C, 25 DEG C respectively, and is being higher than standard cure temperature
Glass fibre/epoxy prepreg cure test is carried out at 5 DEG C, 10 DEG C, is repeated step (2), is obtained corresponding resistance respectively
Temperature coefficient and curing degree obtain curing degree-temperature-coefficient of electrical resistance relation curve of polymer matrix composite；
(4) when practical engineering application, by the cooling stage carbon nanometer for monitoring the polymer matrix composite solidification process
Paper temperature-coefficient of electrical resistance obtains corresponding curing degree according to the curing degree in step (3)-temperature-coefficient of electrical resistance relation curve.
Claims (2)
1. a kind of method using carbon nanometer paper sensor monitoring polymer based composites curing degree, it is characterised in that according to
Lower step carries out:
(1) four copper conductors are fixed on rectangle carbon nanometer paper surface, form carbon nanometer paper sensor, this carbon nanometer paper is passed
Sensor is embedded to the inside of polymer matrix composite prepreg to be measured, according to the standard cure of polymer matrix composite prepreg
Process system curing molding obtains polymer matrix composite；
(2) in solidification process, the electricity of the carbon nanometer paper sensor inside embedment prepreg is measured using four probe resistance measuring instruments
Resistive, using the temperature change of fiber grating measurement prepreg solidification process, the carbon nanometer paper resistance for obtaining solidification process becomes
Change-Temperature-time relation curve carries out linear fit to the carbon nanometer paper resistance variations-temperature curve for solidifying cooling stage, obtains
To the temperature-coefficient of electrical resistance of the carbon nanometer paper of cooling stage；
The curing degree of DSC method measurement polymer matrix composite under standard cure process system is utilized simultaneously；
(3) respectively be lower than 5 DEG C of standard cure temperature, 10 DEG C, 15 DEG C, 20 DEG C, 25 DEG C, and be higher than 5 DEG C of standard cure temperature,
Polymer matrix composite prepreg cure test is carried out at 10 DEG C, is repeated step (2), is obtained corresponding resistance temperature system respectively
Several and curing degree, obtains curing degree-temperature-coefficient of electrical resistance relation curve of polymer matrix composite；
(4) when practical engineering application, by the cooling stage carbon nanometer paper electricity for monitoring the polymer matrix composite solidification process
Temperature coefficient is hindered, i.e., corresponding curing degree is obtained according to the curing degree in step (3)-temperature-coefficient of electrical resistance relation curve.
2. a kind of side using carbon nanometer paper sensor monitoring polymer based composites curing degree according to claim 1
Method, it is characterised in that the copper conductor is fixed on rectangle carbon nanometer paper surface using conducting resinl.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108181029B (en) * | 2018-01-10 | 2020-01-07 | 沈阳航空航天大学 | Method for monitoring strain of fiber reinforced composite material in multiple directions by carbon nano paper sensor |
| CN109827995B (en) * | 2019-01-17 | 2021-07-16 | 南京航空航天大学 | Online self-monitoring method for curing degree of resin-based composite material |
| CN113030191B (en) * | 2021-02-26 | 2023-03-17 | 浙江大学 | Resin curing degree in-situ monitoring method based on embedded fiber sensor |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102661930A (en) * | 2012-04-27 | 2012-09-12 | 沈阳航空航天大学 | Method used for rapidly detecting curing degrees of thermosetting materials |
| CN104732022A (en) * | 2015-03-18 | 2015-06-24 | 南京航空航天大学 | Prediction method for composite microwave curing temperature field |
| CN105136861A (en) * | 2015-06-18 | 2015-12-09 | 沈阳航空航天大学 | Carbon nano paper monitoring method of polymer-based composite material curing process |
| CN205120664U (en) * | 2015-11-09 | 2016-03-30 | 中核(天津)科技发展有限公司 | Macromolecular material curing degree nondestructive test device |
| CN106248677A (en) * | 2016-10-10 | 2016-12-21 | 广东工业大学 | The state of cure detection method of high polymer composite material and system |
-
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- 2017-03-22 CN CN201710172762.3A patent/CN106908474B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102661930A (en) * | 2012-04-27 | 2012-09-12 | 沈阳航空航天大学 | Method used for rapidly detecting curing degrees of thermosetting materials |
| CN104732022A (en) * | 2015-03-18 | 2015-06-24 | 南京航空航天大学 | Prediction method for composite microwave curing temperature field |
| CN105136861A (en) * | 2015-06-18 | 2015-12-09 | 沈阳航空航天大学 | Carbon nano paper monitoring method of polymer-based composite material curing process |
| CN205120664U (en) * | 2015-11-09 | 2016-03-30 | 中核(天津)科技发展有限公司 | Macromolecular material curing degree nondestructive test device |
| CN106248677A (en) * | 2016-10-10 | 2016-12-21 | 广东工业大学 | The state of cure detection method of high polymer composite material and system |
Non-Patent Citations (1)
| Title |
|---|
| 计算机辅助直流电分析仪监控复合材料固化过程的研究;刘刚;《玻璃钢/复合材料》;19881231;摘要以及第33页左栏第2段 |
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