CN102768154A - Method for characterizing apparent strength of carbon foam layer - Google Patents
Method for characterizing apparent strength of carbon foam layer Download PDFInfo
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- CN102768154A CN102768154A CN2012102827147A CN201210282714A CN102768154A CN 102768154 A CN102768154 A CN 102768154A CN 2012102827147 A CN2012102827147 A CN 2012102827147A CN 201210282714 A CN201210282714 A CN 201210282714A CN 102768154 A CN102768154 A CN 102768154A
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Abstract
A method for characterizing an apparent strength of a carbon foam layer comprises mounting or replacing a probe at a middle part of a lower surface of a depression unit in a common material compression testing instrument, testing at different positions of a surface of the carbon foam layer, calculating pressure intensities withstood by the surface of the carbon foam layer according to tested pressures, calculating an average pressure intensity, and characterizing the apparent strength of the carbon foam layer with the average pressure intensity. The inventive method substitutes a pressure intensity method for a pressure method, and can reduce a contact area of compression test to a value without being affected by a shape of the carbon foam layer by mounting or replacing the probe, hence the inventive method significantly improves accuracy and repeatability of measurement results compared with the prior characterization method, and can provide reliable analysis means for research of expansive type flame retardant materials.
Description
Technical field
The present invention relates to expanding flame-proof material, particularly a kind of characterizing method of Carbon foam layer apparent intensity of expanding flame-proof material.
Background technology
Material is the pillar of modern science and social development, and macromolecular material has the incomparable performance of many other materials especially.But no matter natural macromolecular material, or synthetic macromolecular material, great majority all belong to inflammable, combustible material, in case burning, burning rate is fast, is difficult for extinguishing.The fire that takes place in the world in recent ten years, quite a few rises because of macromolecular material.And the flame-retardant modified fire preventing just of macromolecular material fire spread is taken place, delays, reduces one of important measures of fire damage.
Got into since 21 century, the whole world is more and more tighter to the requirement of flame retardant products, and its relevant criterion and rules are also more and more abundanter and perfect, especially efficient to fire retardant, low toxicity, lacks the pursuit of cigarette, and people are to the research pay attention to day by day of halogen-free flameproof.In order to cater to the requirements of the times of preserving the ecological environment now, expansion type flame retardant is because of its unique fire-retardant mechanism, and low cigarette, low toxicity, addition advantages such as other halogen-free flame retardants are low relatively become the emphasis of various flame-retarded resins researchs.
The expansion type flame-retarding technique functions comes from the thirties in 20th century, first piece of patent (US, 2106938) that Tramm proposed in 1938 about expanding fire-proof paint, and this fire-type coating is made up of diammonium hydrogen phosphate, dicyandiamide, formaldehyde resin.Expansion type flame retardant can produce gas and charcoal layer in the polymer combustion process, and gas can inflation charcoal layer, and charcoal layer cooling back coated polymer interrupts burning thereby stop oxygen to get into.The decomposition that comes from matrix resin that wherein the charcoal layer has (fixing of the residue of charing and cigarette), the decomposition that comes from fire retardant that has (the acid source decomposes, and the catalytic carbon source forms the charcoal layer).Can see that in the expansion type flame-retarding system, the charcoal layer is most important.
Chinese scholars is more extensive to the expandable flame retardant architectural study at present, and many documents have reported that all the quality of charcoal layer has bigger influence [1-5] to fire resistance.Propose charcoal layer intensity like J.E.J.Stags and depended on its porous structure; Cevdet Kaynak etc. has studied nano imvite to epoxy resin charcoal layer effect on structure, with and to the contact of blocking oxygen; Fabienne Samyn etc. has discussed its nano shape of polymer nanocomposites to charcoal layer structure and fire-retardant influence; Takashi Kashiwagi etc. are explaining that fire resistance has been concerned about the crackle that the charcoal layer produces when changing; Zhenyu Wang etc. has proposed adjuvant makes its littler aperture of inierpeneirating network structure and the thicker hole layer of the generation of charcoal layer can improve fire resistance.Therefore, the sign to Carbon foam layer character becomes more and more important.
But because the charcoal layer quality that expanding flame-proof material forms is unbodied, shape is irregular, show bubble and very easily broken, thereby all the time not preferably means to characterize the charcoal layer good and bad.Though have document in its research, to carry out the sign of charcoal layer intensity, there are many defectives [6] in used pressure application, and is changeable like charcoal layer shape; Local meeting stress is concentrated and is caused the charcoal layer broken; Differ with the hold-down devices surface of contact, problems such as difficult quality control cause pressure measurements contingency big; Poor repeatability comes call for Votes obviously to remain to be discussed with its measurement result.
List of references
[1]J.E.J.Staggs.Heat?and?mass?transport?in?developing?chars[J].Polymer?Degradation?and?Stability.2003，82：297-307
[2]Cevdet?Kaynak，etal.Mechanical?properties，flammability?and?char?morphology?of?epoxy?resin/montmorillonite?nanocomposites[J].Applied?Clay?Science.2009，46：319-324
[3]Fabienne?Samyn，etal.Fire?retardancy?of?polymer?clay?nanocomposites：Is?there?an?influence?of?the?nanomorphology?[J].Polymer?Degradation?and?Stability.2008.93：2019-2024
[4]Takashi?Kashiwagi，etal.Enhancement?of?char?formation?of?polymer?nanocomposites?using?a?catalyst[J].Polymer?Degradation?and?Stability.2009，94：2028-2035
[5]Zhenyu?Wang，etal.Influence?of?nano-LDHs?on?char?formation?and?fire-resistant?properties?of?flame-retardant?coating[J].Progress?in?Organic?Coatings.2005，53：29-37
[6]The?Investigation?of?melamine?Polyphosphate?Flame?Retardant?Polyamide-6/Inorganic?Siliciferous?Filler?with?Different?Geometrical?Form[J].J?Appl?Polym?Sci.2009，113：2046-2051
[7]Alberto
etal.A?study?of?the?surface?morphology?of?poly(p-phenylene?terephthalamide).Polymer?Degradation?and?Stability.2010，95：702-707
Summary of the invention
The object of the invention is to overcome the problems referred to above that prior art exists, and a kind of characterizing method of Carbon foam layer apparent intensity is provided.
The objective of the invention is to realize like this: a kind of characterizing method of Carbon foam layer apparent intensity; Be that lower surface in material compression verification instrument hold-down devices commonly used installs or replace a probe between two parties additional; Select the diverse location of Carbon foam laminar surface to test; The pressure that this place's Carbon foam laminar surface of calculation of pressure that obtains according to test can bear, and calculate the average pressure of repeatedly measuring, characterize the apparent intensity of Carbon foam layer with this average pressure.
Described probe is the cylinder of high length-diameter ratio, and the bottom surface is the plane, and length L is 0.5-5cm, and floorage S is 1-30mm
2If probe length is not enough, can cause pressing down the outstanding position that the process probe mount might touch irregular charcoal layer, the long meeting of length causes popping one's head in crooked easily; Floorage S too conference causes charcoal layer bearing area too big, produce with repacking before similar instability problem, the too little meeting of S causes the charcoal layer under minimum pressure, to be pierced, instrument is to the measurement of factor of pressure.Measure simple charcoal layer, often intensity is medium, selects for use less S can guarantee its accuracy; The complicated charcoal layer intensity of adding inorganic mineral is very big, should select for use big slightly S to avoid the issuable deviation of particle agglomeration and the excessive probe that causes of bulk strength crooked; Add the complicated charcoal layer of lipid or non-rigid filler such as N, P-compound and also should select big slightly S because these charcoal layers often the surface is comparatively smooth, but intensity is very low, the too little meeting of S makes the measurement of factor of instrument to pressure; The charcoal layer that shape is peculiar need be used long L.The synoptic diagram of method of modifying is seen Fig. 1, and modified header 3D model is seen Fig. 2, and charcoal layer typical compressed curve is as shown in Figure 3.Among Fig. 3, A is former data, and smoothed A is through level and smooth data.Former data ordinate is a pressure, and unit is N, changes pressure into pressure during mapping, unit 10
3Pa, horizontal ordinate are reduction length.
The specific practice of described test is; Place the Carbon foam layer and make the more smooth place of probe over against the charcoal layer; Observe pressure curve, write down the mutation pressure value F of this place Carbon foam layer when broken, the pressure that can bear according to this place of floorage S calculating of pressure P=pressure F/ probe.
Described Carbon foam layer is meant expanding flame-proof material through after the combustion process, residual irregular unbodied Carbon foam layer.Combustion process wherein comprises vertical combustion test, oxygen index test or the test of taper calorimeter.The charcoal layer that expanding flame-proof material produces is a show bubble, and is loose and very easily broken, irregular shape often cause to its whole when bearing pressure test local stress excessive and break, test result is extremely inaccurate; And because the combustion testing temperature often is lower than 1000 ℃, therefore the charcoal layer degree of graphitization that form low, belong to amorphous carbon, the pressure that isotropy makes its surface can bear is more consistent.Therefore it is higher to characterize charcoal layer feasibility with the pressure method.Especially for the most frequently used, the easiest, but the standard batten is thinner, the most uneven oxygen index test of charcoal layer after the burning; Use the pressure method can greatly make things convenient for the researchist; Not only cost is low, and sample preparation is easy, and has guaranteed the accuracy and the repeatability of the strength test of charcoal layer.
Described Carbon foam layer comprises simple charcoal layer or complicated charcoal layer, and the carbon element content of simple charcoal layer is greater than 90%; Carbon element content≤90% of complicated charcoal layer, all the other are various inorganicss and/or organic substance residues.Therefore the intensity of complicated charcoal layer is actually the intensity of apparent charcoal layer.Inorganics and the organic intensity that can influence the charcoal layer to a certain extent that remains in, many bibliographical informations the added synergist of expandable flame retardant system has been changed charcoal layer character, thereby changed fire resistance, therefore the intensity to complicated charcoal layer characterizes also necessary.Through test of many times, as long as the dispersion of its synergist of fire proofing is more even, the charcoal layer intensity that is produced is also comparatively unified, and measured data repeatability is very high.
The measuring accuracy of described material compression verification instrument is≤0.1N.Like HY-0230 system controlled by computer electronics universal testing machine.Because the present invention measures pressure and need use the less probe of area, and the pressure that loose Carbon foam layer can bear is not too large, and this just causes less pressure just can puncture the charcoal layer, if measurement of factor will cause the inaccurate of experimental data.
The characterizing method of Carbon foam layer apparent intensity of the present invention changes the pressure method into by pressure application; Promptly install or replace a probe between two parties additional through lower surface in original material compression verification instrument hold-down devices; Can the contact area of compression verification be narrowed down to the influence that does not receive charcoal layer shape; Thereby the present invention compares with original characterizing method, and its measurement result accuracy and repeatability significantly improve, and the research that can be expanding flame-proof material improves reliable analysis means.
Description of drawings
Fig. 1 is the material compression verification instrument and repacking front and back contrast synoptic diagram through repacking;
Fig. 2 is the 3D illustraton of model of modified header;
Fig. 3 is a charcoal layer typical compressed curve.
Embodiment
The characterizing method of Carbon foam layer apparent intensity of the present invention; Be that hold-down devices lower surface at material compression verification instrument commonly used installs or replace a probe between two parties additional; Select the diverse location of Carbon foam laminar surface to test; The pressure that this place's Carbon foam laminar surface of calculation of pressure that obtains according to test can bear, and calculate the average pressure of repeatedly measuring, characterize the apparent intensity of Carbon foam layer with this average pressure.
Further specify characterizing method of the present invention through embodiment below.But the protection domain that the following example does not limit the present invention in any way.
Oxygen index test (hereinafter to be referred as the LOI test) is the most simple, with low cost; The easiest acquisition of its charcoal layer, convenient repeatedly measurement, and shape is the most complicated and changeable; Can more be expressly understood the quality of pressure application and pressure method, thereby following examples all adopt the sample after oxygen index is tested.Pressure application and pressure method are all tested on the universal material test machine, adopt the speed that presses down of 5mm/min, and repeatedly measure calculating mean value and standard deviation.Because pressure application is different with pressure method unit, directly to use the standard deviation stability of comparing data intuitively, thereby compare with coefficient of dispersion (standard deviation/mean value), its test result is seen table 1-4.
Embodiment 1
Adopt APP/pentaerythrite/polyacrylic flame-retardant material composite; Wherein fire retardant accounts for 25% (fire retardant is APP and pentaerythrite; APP/pentaerythrite is respectively: 1: 1,1.5: 1,2: 1,3: 1,4: 1); More complete some pressure application and the pressure methods of adopting respectively of charcoal layer (simple charcoal layer) that produce after the collection LOI test are carried out strength test, wherein the S=3.14mm of the probe of pressure method employing
2, L=1cm.The pressure application test result is as shown in table 1, and pressure method test result is as shown in table 2.
Table 1
Table 2
Can see simple its variation tendency basically identical of charcoal layer intensity that pressure application and pressure method record by table 1, table 2.The pressure method is to reduce gradually, and 2: 1 sample data of pressure application has a deviation.Relatively coefficient of dispersion can be known and sees that pressure method data stability more increases, and standard deviation and coefficient of dispersion are less relatively; And the pressure application coefficient of dispersion is bigger, thereby its its fiduciary level of data that record is also lower, and 2: 1 sample data does not meet trend and becomes yet and be appreciated that.Therefore, during research charcoal layer intensity, adopt the pressure method can make the data that record more accurate, find more correct rule.
Adopt APP/pentaerythrite/silicon dioxide/polyacrylic flame-retardant material composite; Wherein fire retardant accounts for 25% (APP/pentaerythrite=2: 1); Synergist silica comprises 2% or 4%; Collect more complete some pressure application and the pressure methods of adopting respectively of charcoal layer (complicated charcoal layer) that produce after the LOI test and carry out strength test, wherein the probe of pressure method employing probe S=12.56mm
2, L=2cm.The pressure application test result is as shown in table 3, and pressure method test result is as shown in table 4.
Embodiment 3
Adopt the flame-retardant material composite of orthophosphoric acid melamine/neopentyl glycol/talcum powder/poly terephthalic acid diethylester; Wherein fire retardant IFR accounts for 30%; Fire retardant ratio APP/neopentyl glycol=1: 1; The synergist talcum powder accounts for 2% or 4%, collect more complete some pressure application and the pressure methods of adopting respectively of charcoal layer (complicated charcoal layer) that produce after the LOI test and carry out strength test, wherein the probe of pressure method employing probe S=12.56mm
2, L=2cm.The pressure application test result is as shown in table 3, and pressure method test result is as shown in table 4.
Embodiment 4
Adopt the flame-retardant material composite of dicyandiamide/phosphoguanidine/zeolite/wood powder; Wherein fire retardant accounts for 15% (dicyandiamide/phosphoguanidine=1: 2); The synergist zeolite accounts for 2% or 4%; Collect more complete some pressure application and the pressure methods of adopting respectively of charcoal layer (complicated charcoal layer) that produce after the LOI test and carry out strength test, wherein the probe of pressure method employing probe S=12.56mm
2, L=4cm.The pressure application test result is as shown in table 3, and pressure method test result is as shown in table 4.
Embodiment 5
Adopt urea/pyrophosphoric acid two melamines/monoethylene glycol/lime carbonate/poly flame-retardant material composite; Wherein fire retardant accounts for 30% (urea/pyrophosphoric acid two melamines/monoethylene glycol=1: 3: 2); Synergist lime carbonate accounts for 2% or 4%; Collect more complete some pressure application and the pressure methods of adopting respectively of charcoal layer (complicated charcoal layer) that produce after the LOI test and carry out strength test, wherein the probe of pressure method employing probe S=12.56mm
2, L=4cm.The pressure application test result is as shown in table 3, and pressure method test result is as shown in table 4.
Adopt the flame-retardant material composite of melamine cyanurate/triphenyl phosphate/glycerine/polystyrene; Fire retardant accounts for 30% (melamine cyanurate/glycerine=3: 1); The synergist triphenyl phosphate accounts for 2% or 4%; Collect more complete some pressure application and the pressure methods of adopting respectively of charcoal layer (complicated charcoal layer) that produce after the LOI test and carry out strength test, wherein the probe of pressure method employing probe S=19.63_mm
2, L=4cm.The pressure application test result is as shown in table 3, and pressure method test result is as shown in table 4.
Table 3
Table 4
Can be seen that by table 3, table 4 for the ionization meter of various complicated charcoal layers, the coefficient of dispersion of pressure method still is controlled at small range, the coefficient of dispersion of pressure application then fluctuates in bigger scope.
Therefore; Measurement for charcoal layer intensity; The reliability of pressure method is higher than pressure application far away, especially research charcoal layer intensity and flame-retardant system in some or during the concerning of the outer addition of variable, employing pressure method just can make research meanses such as measurement result, quantification calculating, analysis modeling more convincing.
Claims (7)
1. the characterizing method of a Carbon foam layer apparent intensity; It is characterized in that: the lower surface in material compression verification instrument hold-down devices commonly used installs or replaces a probe between two parties additional; Select the diverse location of Carbon foam laminar surface to test; The pressure that this place's Carbon foam laminar surface of calculation of pressure that obtains according to test can bear, and calculate the average pressure of repeatedly measuring, characterize the apparent intensity of Carbon foam layer with this average pressure.
2. the characterizing method of Carbon foam layer apparent intensity as claimed in claim 1 is characterized in that: described probe is the cylinder of high length-diameter ratio, and the bottom surface is the plane, and length L is 0.5-5cm, and floorage S is 1-30mm
2
3. the characterizing method of Carbon foam layer apparent intensity as claimed in claim 1; It is characterized in that: the specific practice of described test is; Place the Carbon foam layer and make the more smooth place of probe over against the charcoal layer; Observe pressure curve, write down the mutation pressure value F of this place Carbon foam layer when broken, the pressure that can bear according to this place of floorage S calculating of pressure P=pressure F/ probe.
4. the characterizing method of Carbon foam layer apparent intensity as claimed in claim 1 is characterized in that: described Carbon foam layer is meant expanding flame-proof material through after the combustion process, residual irregular unbodied Carbon foam layer.
5. the characterizing method of Carbon foam layer apparent intensity as claimed in claim 4 is characterized in that: described combustion process comprises vertical combustion test, oxygen index test or the test of taper calorimeter.
6. the characterizing method of Carbon foam layer apparent intensity as claimed in claim 1 is characterized in that: described Carbon foam layer comprises simple charcoal layer or complicated charcoal layer, and the carbon element content of simple charcoal layer is greater than 90%; Carbon element content≤90% of complicated charcoal layer, all the other are various inorganicss and/or organic substance residues.
7. the characterizing method of Carbon foam layer apparent intensity as claimed in claim 1 is characterized in that: the measuring accuracy of described material compression verification instrument is≤0.1N.
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Citations (5)
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|---|---|---|---|---|
| JPS5520472A (en) * | 1978-07-31 | 1980-02-13 | Shimadzu Corp | Compression testing unit |
| CN1447105A (en) * | 2002-03-22 | 2003-10-08 | 中国七砂集团有限责任公司 | Digit type device for measuring compression strengths of single grain of abrasive powders |
| CN1912571B (en) * | 2005-08-12 | 2010-05-26 | 大唐微电子技术有限公司 | Method for measuring compression strength of IC card module and measuring instrument |
| CN201828466U (en) * | 2010-10-28 | 2011-05-11 | 宝山钢铁股份有限公司 | Device for testing coke strength in high-temperature environment |
| CN102353588A (en) * | 2011-07-06 | 2012-02-15 | 北京航空航天大学 | Device and method for testing normal-temperature and high-temperature compression stress relaxation of rubber |
-
2012
- 2012-08-09 CN CN201210282714.7A patent/CN102768154B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5520472A (en) * | 1978-07-31 | 1980-02-13 | Shimadzu Corp | Compression testing unit |
| CN1447105A (en) * | 2002-03-22 | 2003-10-08 | 中国七砂集团有限责任公司 | Digit type device for measuring compression strengths of single grain of abrasive powders |
| CN1912571B (en) * | 2005-08-12 | 2010-05-26 | 大唐微电子技术有限公司 | Method for measuring compression strength of IC card module and measuring instrument |
| CN201828466U (en) * | 2010-10-28 | 2011-05-11 | 宝山钢铁股份有限公司 | Device for testing coke strength in high-temperature environment |
| CN102353588A (en) * | 2011-07-06 | 2012-02-15 | 北京航空航天大学 | Device and method for testing normal-temperature and high-temperature compression stress relaxation of rubber |
Non-Patent Citations (1)
| Title |
|---|
| YUAN LIU ET AL: "The Investigation of Melamine Polyphosphate Flame Retardant Polyamide-6/Inorganic Siliciferous Filler with Different Geometrical Form", 《JOURNAL OF APPLIED POLYMERSCIENCE》 * |
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