CN106996840B - A kind of force-responsive type fluorescent optical sensor and preparation method thereof based on dissaving polymer - Google Patents
A kind of force-responsive type fluorescent optical sensor and preparation method thereof based on dissaving polymer Download PDFInfo
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- CN106996840B CN106996840B CN201710251499.7A CN201710251499A CN106996840B CN 106996840 B CN106996840 B CN 106996840B CN 201710251499 A CN201710251499 A CN 201710251499A CN 106996840 B CN106996840 B CN 106996840B
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- 229920000642 polymer Polymers 0.000 title claims abstract description 42
- 230000003287 optical effect Effects 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920001971 elastomer Polymers 0.000 claims abstract description 34
- 239000005060 rubber Substances 0.000 claims abstract description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 229920006254 polymer film Polymers 0.000 claims description 9
- 244000043261 Hevea brasiliensis Species 0.000 claims description 8
- 229920003052 natural elastomer Polymers 0.000 claims description 8
- 229920001194 natural rubber Polymers 0.000 claims description 8
- -1 poly amino ester Chemical class 0.000 claims description 7
- 229920002614 Polyether block amide Polymers 0.000 claims description 6
- 229920000962 poly(amidoamine) Polymers 0.000 claims description 5
- 229920002379 silicone rubber Polymers 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000005062 Polybutadiene Substances 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 238000007872 degassing Methods 0.000 claims description 2
- 239000007791 liquid phase Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229920002857 polybutadiene Polymers 0.000 claims description 2
- 229920003225 polyurethane elastomer Polymers 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 claims 1
- 150000004767 nitrides Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 16
- 230000004044 response Effects 0.000 abstract description 8
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 6
- 230000002441 reversible effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- 230000000638 stimulation Effects 0.000 description 3
- JLZUZNKTTIRERF-UHFFFAOYSA-N tetraphenylethylene Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)=C(C=1C=CC=CC=1)C1=CC=CC=C1 JLZUZNKTTIRERF-UHFFFAOYSA-N 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920002873 Polyethylenimine Polymers 0.000 description 2
- 239000004433 Thermoplastic polyurethane Substances 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 2
- RMXVNDUWESWVKI-UHFFFAOYSA-N 3-(1-adamantyl)dioxetane Chemical group C1OOC1C1(C2)CC(C3)CC2CC3C1 RMXVNDUWESWVKI-UHFFFAOYSA-N 0.000 description 1
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229920000547 conjugated polymer Polymers 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920000587 hyperbranched polymer Polymers 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- HRGDZIGMBDGFTC-UHFFFAOYSA-N platinum(2+) Chemical group [Pt+2] HRGDZIGMBDGFTC-UHFFFAOYSA-N 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/24—Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Force Measurement Appropriate To Specific Purposes (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Laminated Bodies (AREA)
Abstract
The invention discloses a kind of force-responsive type fluorescent optical sensor and preparation method thereof based on dissaving polymer, wherein force-responsive type fluorescent optical sensor is the laminated film assembled by dissaving polymer and transparent rubber, is followed successively by transparent rubber layer, dissaving polymer layer and transparent rubber layer from top to bottom.The mass ratio of dissaving polymer layer and transparent rubber layer is 10~1:1 in force-responsive type fluorescent optical sensor.Force-responsive type fluorescent optical sensor of the present invention stimulates external force very sensitive: with the increase of material strain caused by external force, the fluorescence intensity of sensor can be gradually increased；Moreover, this fluorescence intensity change has invertibity, with the reduction of strain, fluorescence intensity can be gradually decreased.Moreover, this force-responsive type fluorescent optical sensor also has many advantages, such as fast response time.
Description
Technical field
The present invention relates to a kind of force-responsive type fluorescent optical sensor and preparation method thereof based on dissaving polymer, belongs to and answers
Power or strain-responsive fluorescent optical sensor technical field.
Background technique
Force-responsive fluorescent material refer to mechanical force stimulation under, the photoluminescent property (for example, fluorescence intensity and color) of material
Can reversibly it be regulated and controled.Due to external strength our daily life be readily available with it is easy-to-handle,
This material with force-responsive fluorescence capability has potential application in fields such as sensor, display and safe-guarding and anti-counterfeiting materials
Prospect.Force-responsive type fluorescent optical sensor is constructed based on force-responsive fluorescent material has been subjected to the extensive of researcher in recent years
Concern.
According to the classification of material type, force-responsive fluorescent material can be divided into polymer type and small organic molecule class
Type.In current report, the force-responsive fluorescent material in relation to polymer type is relatively fewer, and most polymers type
Force-responsive fluorescent material belong to conjugated system.For example, in the report of Rowan et al., 4- dodecane oxygen that they utilize
(N- methylbenzene imidazoles-the 2)-pyridine of base -2,6- bis- and platinum (II) form complex, are mixed into polymethyl methacrylate and make
At force-responsive fluorescent optical sensor.When by scraping, Red Shift Phenomena (Journal of is had occurred in the wavelength of fluorescence of this sensor
Materials Chemistry,2012,22,14196).Xin et al. utilizes the double benzoxazolyl hexichol second of aromatic dyestuff
Alkene (BBS) and thermoplastic polyurethane (TPU) are mixed with force-responsive fluorescence elastomer sensor.Under different strained conditions,
Variation (ACS applied materials&interfaces, 2013,5,4625) has occurred in its wavelength of fluorescence.A small number of is non-total
Although conjugated polymer system can show force-responsive photoluminescent property, this property is often irreversible.For example, Sijbesma etc.
Power has been made using the acrylate polymer in molecular skeleton with two (adamantyl) -1,2- dioxetanes groups in people
Response type fluorescent optical sensor.Can be issued when by external force bright blue-fluorescence (Nature Chemistry, 2012,
4,559).Trace it to its cause is because irreversible variation has occurred in chemical structure.The force-responsive fluorescent material of small organic molecule type
Refer to the fluorescent crystal that those organic molecules are formed after orderly accumulation.These fluorescent crystals not only have force-responsive characteristic, and
And photoluminescent property is reversible.For example, in Jia et al. by tetraphenylethylene (TPE) building unit force-responsive fluorescence of single crystal form
Sensor.Primary crystalline can emit navy blue fluorescence.After grinding, TPE unit is converted into amorphous phase by crystal phase, material thus
Become blue-green.Although the fluorescence response of this material can be reversible, outside stimulus is needed, for example use solvent vapo(u)r
Or it is just able to achieve after heat treatment.In the report of Jia et al., TPE crystal needs after Overheating Treatment, the luminous spy of crystal
Property can return to original state (Angewandte Chemie International Edition, 2016,55,519).With
Upper report is force-responsive type fluorescent optical sensor made of physical method.Only in report few in number, chemistry has been used
Method constructs force-responsive type fluorescent optical sensor.For example, Jia et al. has synthesized a kind of novel functional molecular based on rhodamine.
It, which is covalently embedded into elastic polyurethane, can form force-responsive sensor.Under the stimulation of mechanical force, rhodamine has occurred different
Structure, the spirolactams closed loop states distorted from one form open loop situations, and variation (Advanced has occurred in fluorescence color
Materials,2015,27,6469).But the fluorescent optical sensor of this force-responsive type is still based on conjugated system.By mesh
Before, it does not find based on aliphatic non-conjugated polymeric object, and the force-responsive fluorescent optical sensor with reversible fluorescence response
Report.
Summary of the invention
The force-responsive type fluorescent optical sensor and its preparation that the purpose of the present invention is to provide a kind of based on dissaving polymer
Method.The sensor can be to stress or strain stimulation generates significant fluorescence response and fluorescence response is reversible.
The fluorescence response of force-responsive type fluorescent optical sensor of the present invention has invertibity, and the fluorescence intensity of component can be with deformation quantity
Reduce and reduces.
The present invention is based on the force-responsive type fluorescent optical sensors of dissaving polymer, are by dissaving polymer and transparent rubber
The laminated film assembled is followed successively by transparent rubber layer, dissaving polymer layer and transparent rubber layer from top to bottom.
The mass ratio of dissaving polymer layer and transparent rubber layer is 10~1 in force-responsive type fluorescent optical sensor of the present invention:
1, wherein the quality of transparent rubber layer refers to the gross mass of upper layer and lower layer transparent rubber layer.
Transparent rubber layer with a thickness of 10~100 μm, dissaving polymer layer with a thickness of 100~1000 μm.
The dissaving polymer is over-branched polyamidoamine, hyperbranched poly amino ester, hyperbranched poly ether amide or over-expense
Change the blend or copolymer of one or more of polyethyleneimine.
Wherein, over-branched polyamidoamine is self-control, and preparation method is referring to document Zhang Y, Huang W, Zhou Y, et
al.A physical gel made from hyperbranched polymer gelator[J].Chemical
Communications,2007(25):2587-2589；Hyperbranched poly amino ester is self-control, and preparation method is referring to document Wu D
C,Liu Y,He C B,et al.Blue photoluminescence from hyperbranched poly(amino
ester)s[J].Macromolecules,2005,38(24):9906-9909；Hyperbranched poly ether amide is self-control, preparation method
Referring to document Lin Y, Gao J W, Liu H W, et al.Synthesis and characterization of
hyperbranched poly(ether amide)s with thermoresponsive property and
unexpected strong blue photoluminescence[J].Macromolecules,2009,42(9):3237-
3246；Hyperbranched polyethyleneimine is commercially available acquisition.
The transparent rubber is silicon rubber, in natural rubber, polyurethane rubber, butadiene rubber, butadiene-styrene rubber, EP rubbers
One or more.
The present invention is based on the force-responsive type fluorescent optical sensors of dissaving polymer can be by physical method or chemical method system
It is standby to obtain:
Physical method includes the following steps:
It will be directly attached at normal temperature with a thickness of 100~1000 μm of dissaving polymer film with a thickness of 10~100 μ
Then the surface of the transparent rubber of m is bonded the transparent rubber of one layer of 10~100 μ m-thick again on the surface of dissaving polymer film
Glue can be obtained force-responsive type fluorescent optical sensor.
Chemical method includes the following steps:
Dissaving polymer is dissolved in methanol, N is then utilized2Plasma gas handles the surface of transparent rubber to draw
Enter amino group, transparent rubber film be completely immersed in the solution of dissaving polymer using degassing liquid phase method and is graft-polymerized,
Reaction temperature is 50 DEG C, and the reaction time is 3 days；Then it is bonded one layer 10~100 μm again on the surface of dissaving polymer film
Thick transparent rubber, can be obtained force-responsive type fluorescent optical sensor.
Force-responsive type sensor laminated film of the present invention is symmetrical structure, is not necessarily to consider front and back sides in use process.
The beneficial effects of the present invention are embodied in:
1, the present invention is based on the force-responsive type sensors of fluorescence dissaving polymer, and fluorescence intensity and external force size are at just
Proportionate relationship, and can with external force size variation generate can reverse response.
It 2, is aliphatic the present invention is based on the dissaving polymer in the force-responsive type sensor of fluorescence dissaving polymer
Non-conjugated polymeric object has good biocompatibility and environment friendly.
Detailed description of the invention
Fig. 1 is fluorescence spectrum of the fluorescent optical sensor based on dissaving polymer under different stress, and excitation wavelength is
365nm；As can be seen from Figure 1 the fluorescence intensity of the sensor based on fluorescence dissaving polymer with the raising of stress and by
Gradually rise.
Fig. 2 is the relationship of fluorescence intensity and stress of the fluorescent optical sensor based on dissaving polymer under different stress.
As can be seen from Figure 2 the fluorescence intensity and stress of the sensor based on fluorescence dissaving polymer are substantially in a linear relationship.
Fig. 3 is the reversible force responsiveness of the fluorescent optical sensor based on dissaving polymer.Fig. 3 a is based on hyperbranched polymerization
Fluorescence spectrum of the fluorescent optical sensor of object in stress (2MPa) and the multiple cyclic process of release stress (0MPa), excitation wavelength
For 365nm；Fig. 3 b is that the fluorescent optical sensor based on dissaving polymer is multiple in stress (2MPa) and release stress (0MPa)
In cyclic process, the relationship of fluorescence intensity and cycle-index.From can be seen that in Fig. 3 a and Fig. 3 b after repeatedly recycling based on glimmering
Light dissaving polymer force-responsive sensor still has good invertibity.
Specific embodiment
The present invention is described in detail in following embodiment, it is to be understood that this only to it is of the invention it is exemplary enumerate, rather than
For limiting the present invention, more not intended to limit present invention protection scope as claimed in claim.
Embodiment 1:
1, the over-branched polyamidoamine for weighing 1.0g, is added in the sample bottle of 5mL, and 2mL methanol is then added and is dissolved,
Dissaving polymer solution can be obtained.
2, the dissaving polymer solution that step 1 obtains is cast on polyfluortetraethylene plate, dries, obtains at room temperature
To the dissaving polymer film with a thickness of 200 μm.
3, the dissaving polymer obtained step 2 is film adhered on the surface of the silicon rubber with a thickness of 20 μm, then
It is bonded the silicon rubber of one layer of 20 μ m-thick again on the surface of dissaving polymer film, force-responsive fluorescent optical sensor can be obtained.
The force-responsive type sensor of obtained fluorescence dissaving polymer is carried out under different stress corresponding glimmering
Optical tests, the result is shown in Figure 1 and Fig. 2.
Embodiment 2:
1, the natural rubber for weighing 1.0g, is dissolved in normal heptane, is then poured on the glass substrate and drying obtains 50 μ
Then the natural rubber films of m thickness utilize N2Plasma gas handles the surface of natural rubber, introduces amino group, operation
Process is to be passed through nitrogen, flow 50mL/min, operating pressure 30Pa, power 60W, day using plasma gas processing instrument
The amino group of right rubber surface increases.
2, hyperbranched poly ether amide of the end with double bond for weighing 5.5g, is dissolved in methanol, will under conditions of 50 DEG C
The natural rubber films that step 1 obtains, which are completely immersed in hyperbranched polyether amide solution, to react 3 days, takes out after reaction,
It dries 2~3 days at room temperature.
3, it is bonded the natural rubber of one layer of 50 μ m-thick again on the surface of dissaving polymer film, force-responsive type can be obtained
Sensor.
The force-responsive type sensor of obtained fluorescence dissaving polymer is carried out under different stress corresponding glimmering
Optical tests.
Embodiment 3:
The preparation process of the present embodiment is with embodiment 1, the difference is that over-branched polyamidoamine is replaced with hyperbranched poly second
In addition the silicon rubber of 20 μ m-thicks is replaced with the natural rubber of 10 μ m-thicks by alkene imines, other preparation conditions are constant.It finally will preparation
Obtained force-responsive type fluorescent optical sensor is tested, and test condition is identical with embodiment 1.
Embodiment 4:
The preparation process of the present embodiment is with embodiment 2, the difference is that hyperbranched poly ether amide is replaced with hyperbranched poly ammonia
Base ester, other preparation conditions are constant.Finally the force-responsive type sensor being prepared is tested, test condition and embodiment
2 is identical.
Claims (6)
1. a kind of force-responsive type fluorescent optical sensor based on dissaving polymer, it is characterised in that: the force-responsive type fluorescence passes
Sensor is the laminated film assembled by dissaving polymer and transparent rubber, is followed successively by transparent rubber layer from top to bottom, surpasses
Branched polymeric nitride layer and transparent rubber layer；
The dissaving polymer is over-branched polyamidoamine, hyperbranched poly amino ester, hyperbranched poly ether amide or hyperbranched poly
The blend or copolymer of one or more of aziridine.
2. force-responsive type fluorescent optical sensor according to claim 1, it is characterised in that:
The mass ratio of dissaving polymer layer and transparent rubber layer is 10~1:1 in the force-responsive type fluorescent optical sensor.
3. force-responsive type fluorescent optical sensor according to claim 1, it is characterised in that:
Every layer of transparent rubber layer with a thickness of 10~100 μm, dissaving polymer layer with a thickness of 100~1000 μm.
4. force-responsive type fluorescent optical sensor according to claim 1, it is characterised in that:
The transparent rubber is silicon rubber, natural rubber, polyurethane rubber, butadiene rubber, butadiene-styrene rubber, one in EP rubbers
Kind is several.
5. a kind of preparation method of force-responsive type fluorescent optical sensor described in claim 1,2,3 or 4, includes the following steps:
It will be directly attached at normal temperature with a thickness of 100~1000 μm of dissaving polymer film with a thickness of 10~100 μm
Then the surface of transparent rubber is bonded the transparent rubber of one layer of 10~100 μ m-thick, i.e., again on the surface of dissaving polymer film
It can get force-responsive type fluorescent optical sensor.
6. a kind of preparation method of force-responsive type fluorescent optical sensor described in claim 1,2,3 or 4, includes the following steps:
Dissaving polymer is dissolved in methanol, N is then utilized2Plasma gas handles the surface of transparent rubber to introduce ammonia
Transparent rubber film is completely immersed in the solution of dissaving polymer using degassing liquid phase method and is graft-polymerized, reacted by base group
Temperature is 50 DEG C, and the reaction time is 3 days；Then it is bonded one layer of 10~100 μ m-thick again on the surface of dissaving polymer film
Transparent rubber can be obtained force-responsive type fluorescent optical sensor.
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| CA2284300A1 (en) * | 1999-09-29 | 2001-03-29 | Ian Manners | Phosphorescent oxygen sensors |
| WO2001034682A1 (en) * | 1999-11-05 | 2001-05-17 | Ian Manners | Phosphorescent oxygen sensors |
| US6565992B1 (en) * | 1996-05-03 | 2003-05-20 | Ian Manners | Phosphorescent oxygen sensors |
| CN1720275A (en) * | 2002-11-08 | 2006-01-11 | 领先技术有限责任公司 | Pressure sensitive material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070105235A1 (en) * | 2005-02-16 | 2007-05-10 | Carlson William B | Osmium-based oxygen sensor and pressure-sensitive paint |
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| US6565992B1 (en) * | 1996-05-03 | 2003-05-20 | Ian Manners | Phosphorescent oxygen sensors |
| CA2284300A1 (en) * | 1999-09-29 | 2001-03-29 | Ian Manners | Phosphorescent oxygen sensors |
| WO2001034682A1 (en) * | 1999-11-05 | 2001-05-17 | Ian Manners | Phosphorescent oxygen sensors |
| CN1720275A (en) * | 2002-11-08 | 2006-01-11 | 领先技术有限责任公司 | Pressure sensitive material |
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