WO2012036538A2 - 탄소나노튜브를 이용한, ntc 특성이 감소된 ptc 소자용 전도성 중합체조성물 - Google Patents
탄소나노튜브를 이용한, ntc 특성이 감소된 ptc 소자용 전도성 중합체조성물 Download PDFInfo
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- WO2012036538A2 WO2012036538A2 PCT/KR2011/006919 KR2011006919W WO2012036538A2 WO 2012036538 A2 WO2012036538 A2 WO 2012036538A2 KR 2011006919 W KR2011006919 W KR 2011006919W WO 2012036538 A2 WO2012036538 A2 WO 2012036538A2
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- resin
- ptc
- conductive polymer
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- ethylene
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Definitions
- the present invention relates to a conductive polymer composition for PTC devices having reduced NTC properties using carbon nanotubes, and to PTC devices, circuits, and planar heating elements using the same.
- the PTC (positive temperature coefficient) characteristic is a characteristic in which the resistance is low at a low temperature at room temperature and thus has conductivity, but the electrical resistance rapidly increases in a relatively narrow temperature range as the temperature increases. Accordingly, the PTC conductive polymer composition having such a property is suitable for use as an electric device such as a circuit protection device that varies with ambient temperature and current conditions.
- a typical PTC device structure includes a resistor made of a conductive polymer composition, two electrodes attached to the resistor and connected to a power supply, and an electrolyte metal foil on the electrodes.
- Circuit protection devices are usually connected in series with the load in electrical circuits to maintain low and low resistance states. However, when exposed to overcurrent or overtemperature conditions, the device increases resistance and effectively blocks current flow to the load in the circuit. These devices regain low resistance when they return to low-temperature and low-temperature conditions at room temperature, but when the melting point lasts longer or rises to higher temperatures, browning of the conductive filler and reagglomeration by van der Waals forces cause There was a problem that the NTC phenomenon that the resistance is reduced.
- carbon black, graphite, and the like are generally used as conductive polymers used in the conventional PTC composition.
- These are spherical particles having a ratio of shorter diameter to longer diameter of 80% or more. There was a problem that the short-circuited particles do not contact again when bending occurs due to a normal impact (FIG. 1).
- the inventors of the present invention while studying a PTC device that maintains conductivity even when external impact, when using a carbon nanotube having a long thin shape as a conductive polymer as a conductive polymer, even if bending occurs, the carbon nanotubes are resilient, even in the external impact It was confirmed that the conductivity can be maintained continuously.
- a crystalline polymer having a large volume change can be used as a PTC binder (i.e., the first resin) to disperse the carbon nanotubes that have a strong bond between molecules. ) To find out how to use.
- the present invention also aims to provide a circuit with reduced NTC phenomena and having PTC characteristics.
- the present invention provides a conductive polymer composition for a PTC (positive temperature coefficient) device comprising a carbon nanotube, the first resin and the second resin.
- the first resin and the second resin are as follows:
- a first resin which is any one selected from the group consisting of polyolefin resins and silicone resins;
- a second resin which is any one selected from the group consisting of cellulose resins and polyester resins.
- the present invention also provides a PTC device comprising the conductive polymer composition for the PTC device, a planar heating element and the circuit comprising the composition.
- the present invention provides a method for manufacturing a PTC device comprising the step of laminating an electrode and an electrolyte metal foil on a resistor thin film comprising the composition.
- the conductive polymer composition for a PTC device of the present invention does not easily change the contact resistance of a circuit, a heating element (heater), a PTC device, etc. using the same, even when external impact or bending, and excellent resilience even when the temperature is increased and then lowered again.
- Figure 1 is printed carbon black and CNT on a 150mm * 300mm BOPET, dried, and subjected to a 180 degree bending test while connecting the Digital Multimeter (YOKOGAWA 733) to the electrode and measured the resistance change, the bending of the carbon black and CNT Resistance change and durability change against repeated impact.
- YOKOGAWA 733 Digital Multimeter
- the present invention provides a conductive polymer composition for a positive temperature coefficient (PTC) device comprising a carbon nanotube, a first resin and a second resin.
- PTC positive temperature coefficient
- the first resin and the second resin are as follows:
- a first resin which is any one selected from the group consisting of polyolefin resins and silicone resins;
- a second resin which is any one selected from the group consisting of cellulose resins and polyester resins.
- the present invention also provides a PTC device comprising the conductive polymer composition for the PTC device, a planar heating element and the circuit comprising the composition.
- the present invention provides a method for manufacturing a PTC device comprising the step of laminating an electrode and an electrolyte metal foil on a resistor thin film comprising the composition.
- the carbon nanotubes of the present invention are general carbon nanotubes, and may be single-walled nanotubes (SWNTs) or multi-walled nanotubes (MWNTs).
- the carbon nanotubes have a diameter of 10 to 60 nm and an aspect ratio of 1,000 or more, but may have a high-efficiency exothermic property that can be heated to 10 ° C. or more at 12 V even with a small amount, but is not limited thereto. .
- the mass ratio of the carbon nanotubes: the first resin and the second resin is preferably 1: 4 to 1:16, which is poor in flowability and inferior in printability, low in resin dispersibility, and low in adhesion. Without excessively high, the sheet resistance value is a sufficient amount of CNTs enough to enable a high-efficiency heat generated by the appropriate size.
- the carbon nanotube: first resin has a mass ratio of 1: 2 to 1: 9 (ie, the first resin is 200 to 900 parts by weight based on 100 parts by weight of carbon nanotubes), and the carbon nanotubes: first 2 resins are in a mass ratio of 1: 2 to 1: 7 (ie, the second resin is 200 to 700 parts by weight based on 100 parts by weight of carbon nanotubes), but is not limited thereto.
- the first resin serves as a PTC binder that functions as a PTC.
- the polyolefin-based resins are all common polyolefin-based resins known in the art.
- the polyolefin resin may be a polyethylene resin or a polypropylene resin, and may be a modified polyethylene resin, a modified polypropylene resin, an ethylene copolymer or a propylene copolymer.
- the polyethylene includes high density polyethylene (HDPE), medium density polyethylene (MDPE), low density polyethylene (LDPE), linear low density polyethylene (LLDPE), and mixtures thereof. Grafted high density polyethylene (m-HDPE), maleic anhydride-grafted low density polyethylene (m-LDPE), and the like can also be used.
- the ethylene copolymer and the propylene copolymer may be a copolymer of ethylene and a monomer having a polar group, a copolymer of propylene and a monomer having a polar group, or a mixture thereof, but is not limited thereto.
- ethylene copolymers or propylene copolymers examples include ethylene / acrylic acid copolymers, ethylene / methacrylic acid copolymers, ethylene / ethylacrylates, ethylene-butylacrylate copolymers, ethylene-vinylacetate copolymers, ethylene / itaconic acid copolymers.
- the silicone resin may be used as long as it is a general silicone resin, and includes a modified silicone resin.
- the silicone resin may be a silicone wax.
- the silicone resin may be silicone rubber Dow Corning, Inc. Silastic, silicon Wax, Wacker E32, or the like.
- the second resin prevents the CNTs from flowing during repeated temperature changes by fixing the CNTs and the first resin, and prevents the NTC phenomenon that the resistance is lowered during continuous temperature rise. Therefore, the second resin should use a thermosetting resin or higher Tm or softening point than the first resin.
- the softening point of the second resin is 130 ° C. or higher, or the Tm or softening point is 1.5 times higher than the first resin. Preferred but not limited to.
- the second resin is preferably higher molecular weight than the first resin in order to reduce the flowability of the CNT after coating drying, more preferably the molecular weight of the second resin is 10,000 ⁇ 50,000, considering the cost-effectiveness 10,000 ⁇ 30,000 is even more preferred.
- the cellulose resin may be used as long as it is a general cellulose resin, and may be nitrocellulose and acetylcellulose.
- ethyl cellulose, butyl cellulose, Dow's STD-10, etc. may be used as the cellulose resin of the present invention.
- the polyester resin can be used as long as it is a general polyester resin.
- the polyester of the present invention may be used, such as polyester binder KSA SP-1, K150.
- the said 1st resin has a molecular weight of 3,000 or more, and a softening point is 45-150 degreeC, More preferably, a softening point is 120-150 degreeC, but it is not limited to this.
- the second resin preferably has a molecular weight of 10,000 or more and a softening point of 130 ° C., but is not limited thereto.
- the composition may optionally further comprise nickel powder, gold powder, copper powder, metal alloy powder, carbon powder, graphite powder, and the like, which are conventional conductive fillers.
- composition may further include polyvinyl-based polymers such as polyvinyl chloride and polyvinylidene chloride, polyvinyl fluoride and polyvinylidene fluoride, and thermoplastic polymers such as polysulfone, polyamide, and the like.
- polyvinyl-based polymers such as polyvinyl chloride and polyvinylidene chloride, polyvinyl fluoride and polyvinylidene fluoride
- thermoplastic polymers such as polysulfone, polyamide, and the like.
- composition may further include an antioxidant, a deteriorating agent or an antifoaming agent.
- the composition may be printed or coated on a substrate and manufactured into a PTC device, a planar heating element, and a circuit.
- composition of the present invention can act as a heating ink or paste, a thin dry film thickness after coating can be quickly dried to yield high productivity, and is completely dried from the surface to the inside to lower the resistance, more preferably 10 Micrometers or less, even more preferably 5 micrometers or less.
- the surface resistance of the material coated with 5 micrometers is preferably 50-1,000 ⁇ / sq, more preferably 50-800 ⁇ / sq to be. If the sheet resistance is too low, the flowability is poor, the printability is poor, and the viscosity is excessively increased, thereby reducing the efficiency of the manufacturing process. When the sheet resistance is more than 1,000 ⁇ / sq, low heat generation performance of less than 10 °C / min is shown at 12 V. When the sheet resistance is less than 50 ⁇ / sq, it reaches a temperature higher than 200 °C within 3 minutes due to the rapid heat generation phenomenon.
- this sheet resistance range is a range for the implementation of the optimum and the highest efficiency of the present invention, although the efficiency or safety is somewhat lowered outside this range, but the scope of the present invention is not limited to this range.
- CNTs are synthesized using a metal catalyst, and the resulting CNTs are acid-treated to form carboxyl groups (-COOH) on the surface, and acyl chlorination and amino functionalization give CNTs with amine groups.
- Ethylene-EVA copolymer ASTOR 538, ASTOR 635
- Ethylene-MMA copolymer WK-402, WK-307
- PE Wax 802C, 503NC, 106N
- Dow (STD-10) And dispersant BYK 9076, BYK 9077
- JUNSEI EC50, Dow STD-10) or Polyester Binder (KSA SP-1) to remove bubbles through Paste Mixer (DAE WHA TECH DDM-300) process Afterwards, the paste is manufactured through the Sambon Mill (EXAKT 80S) process.
- the prepared paste was coated with BOPET with a 5 micrometer thickness using a Gravure printing machine, and then dried at 130 ° C for 10 minutes. Then, the Pttnized Ag Paste (Large Electronic Materials, DHC-7075 or 7045) was silk screened to 7-10 microns. Printed to a thickness and dried for 10 minutes at 130 degrees to produce a low-voltage PTC heating element.
- the sheet resistance was measured by Loresta-GP (MCP-T610), and the adhesion was measured by cross-cutting 10 grids at 1mm intervals and attaching and detaching 3M SEIL TAPE, and the PTC paste made of the above prescription was 150mm * 300mm 100 micro thickness BOPET.
- the Ag electrode with 4mm intervals in succession is coated and dried on PTC-CNT dry surface, and the Digital Multimeter (YOKOGAWA 733) is separated and connected to the electrode. Change was measured.
- the temperature increases continuously, if the resistance of the Digital Multimeter continuously increases or the resistance stops, the NTC phenomenon does not appear. If the resistance decreases when the temperature of the hot plate increases, there is an NTC phenomenon. saw.
- the first resin serves as a PTC binder
- the polyester resin and the CNT, which are the second resin are used, the PTC and NTC characteristics cannot be analyzed (Comparative Example 3) and the content of the first resin is small. Also included were difficulties in analyzing PTC properties (Comparative Example 6).
- Example 1 of Example 1 and Example 2 of preventing the NTC characteristics while excellent in PTC characteristics using a film heater 400mm (L) * 300mm (D) pattern was formed to produce, The resistance change was observed with a digital multimeter while being placed in a matiz oven similar to the heater operating conditions and rising 10 degrees / min from 25 degrees to 180 degrees. In addition, the resistance change with increasing temperature of the comparative example of Experimental Example 1 was observed in the same manner.
- Test conditions are as follows, the resistance change of the heater was measured by a multimeter.
- the PTC-CNT heater of the present invention was confirmed that the resistance increases as the temperature rises from 30 ° C to 130 ° C, and NTC phenomenon does not appear.
- the CNT heater of the comparative example did not change resistance up to 110 ° C., but was slightly lower in resistance at constant temperature rise (FIG. 2).
- the PTC-CNT heater of the present invention was found to increase resistance due to electric shock, but has excellent durability within 5% (Table 3).
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Abstract
Description
발열소재 | 제 1수지 | 제 2수지 | 첨가제 | 용제 | |||||
CNT | LDPE | 에틸렌-EVA 공중합체 | 에틸렌-MMA 공중합체 | 실리콘 왁스 | 셀룰로스계 수지 | 폴리에스터 수지 | 분산제 | DBA/Terpineol | |
실시예1 | To100 | 900 | 700 | 680 | 1000 | ||||
실시예2 | To100 | 900 | 700 | 600 | 1000 | ||||
실시예3 | To100 | 220 | 700 | 460 | 880 | ||||
실시예4 | To100 | 900 | 210 | 380 | 880 | ||||
실시예5 | To100 | 200 | 200 | 450 | 1000 | ||||
실시예6 | To100 | 200 | 200 | 330 | 660 | ||||
비교예1 | To100 | 600 | 340 | 880 | |||||
비교예2 | To100 | 600 | 600 | 1000 | |||||
비교예3 | To100 | 600 | 400 | 800 | |||||
비교예4 | To100 | 600 | 180 | 400 | 880 | ||||
비교예5 | To100 | 700 | 750 | 430 | 1000 | ||||
비교예6 | To100 | 150 | 550 | 350 | 800 | ||||
비교예7 | To100 | 1000 | 600 | 320 | 800 |
면저항(Ω/sq) | 부착력 | PTC 특성 | 면저항 증가비 | NTC 발생여부 | |
실시예1 | 195 | O | 57 | 308 | X |
실시예2 | 200 | O | 63 | 211 | X |
실시예3 | 160 | O | 67 | 305 | X |
실시예4 | 240 | O | 78 | 302 | X |
실시예5 | 210 | O | 59 | 207 | X |
실시예6 | 190 | O | 60 | 301 | X |
비교예1 | 6,000 | O | 60 | 100 | X |
비교예2 | 140,000 | X | - | - | - |
비교예3 | 200 | O | - | - | - |
비교예4 | 5150 | X | 75 | 120 | O |
비교예5 | 3800 | X | 79 | 150 | X |
비교예6 | 7000 | X | - | - | - |
비교예7 | 90,000 | X | - | - | - |
On/off 수 | 저항(Ω) | 변화율(%) |
0회 | 3.5 | 0 |
500회 | 3.5 | 0 |
1,000회 | 3.53 | 0.9 |
2,000회 | 3.56 | 1.7 |
3,000회 | 3.60 | 2.8 |
5,000회 | 3.64 | 4.0 |
8,000회 | 3.66 | 4.5 |
10,000회 | 3.66 | 4.5 |
15,000회 | 3.66 | 4.7 |
20,000회 | 3.67 | 4.9 |
Claims (12)
- 탄소나노튜브, 하기 제 1 수지 및 제 2 수지를 포함하는 PTC(positive temperature coefficient) 소자용 전도성 중합체 조성물:1) 폴리올레핀계 수지 및 실리콘계 수지로 구성되는 군으로부터 선택되는어느 하나인 제 1 수지;2) 셀룰로스계 수지 및 폴리에스터계 수지로 구성되는 군으로부터 선택되는어느 하나인 제 2 수지.
- 제 1항에 있어서,상기 제 1 수지는 폴리에틸렌계 수지 또는 폴리프로필렌계 수지인 것을 특징으로 하는 PTC 소자용 전도성 중합체 조성물.
- 제 1항에 있어서,상기 제 1 수지는 변성 폴리에틸렌 수지, 변성 폴리프로필렌계 수지, 에틸렌공중합체, 프로필렌 공중합체 또는 변성 실리콘계 수지인 것을 특징으로 하는 PTC소자용 전도성 중합체 조성물.
- 제 1항에 있어서,상기 제 1 수지는 LDPE, 에틸렌-EVA 공중합체, 에틸렌-MMA 공중합체 또는 실리콘 왁스인 것을 특징으로 하는 PTC 소자용 전도성 중합체 조성물.
- 제 1항에 있어서,상기 제 2 수지는 나이트로셀룰로스 또는 아세틸셀룰로스인 것을 특징으로 하는 PTC 소자용 전도성 중합체 조성물.
- 제 1항에 있어서,상기 탄소나노튜브는 단일벽 나노튜브(SWNT) 또는 다중벽 나노튜브(MWNT)인것은 특징으로 하는 PTC 소자용 전도성 중합체 조성물.
- 제 1항에 있어서,상기 탄소나노튜브 100 중량부에 대하여 상기 제 1 수지는 200 내지 900 중량부인 것을 특징으로 하는 PTC 소자용 전도성 중합체 조성물.
- 제 1항에 있어서,상기 탄소나노튜브 100 중량부에 대하여 상기 제 2 수지는 200 내지 700 중량부인 것을 특징으로 하는 PTC 소자용 전도성 중합체 조성물.
- 제 1항 내지 제 8항 중 어느 한 항의 조성물을 포함하는 PTC 소자.
- 제 1항 내지 제 8항 중 어느 한 항의 조성물을 포함하는 면상 발열체.
- 제 1항 내지 제 8항 중 어느 한 항의 조성물을 포함하는 회로.
- 제 1항 내지 제 8항 중 어느 한 항의 조성물을 포함하는 저항체 박막에 전극및 전해질 금속박을 적층시키는 단계를 포함하는 PTC 소자의 제조 방법.
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DE112011103114T DE112011103114T5 (de) | 2010-09-17 | 2011-09-19 | Leitfähige Polymerzusammensetzung für ein PTC-Element mit verringerten NTC-Eigenschaften unter Verwendung von Kohlenstoff-Nanoröhren |
US13/814,013 US8968605B2 (en) | 2010-09-17 | 2011-09-19 | Conductive polymer composition for PTC element with decreased NTC characteristics, using carbon nanotube |
JP2013529081A JP5674947B2 (ja) | 2010-09-17 | 2011-09-19 | 炭素ナノチューブを用いた、ntc特性が減少したptc素子用伝導性重合体組成物 |
CN201180044750.3A CN103108906B (zh) | 2010-09-17 | 2011-09-19 | 利用炭纳米管的ntc特性减少的ptc元件用导电性聚合物组合物 |
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2011
- 2011-09-19 US US13/814,013 patent/US8968605B2/en not_active Expired - Fee Related
- 2011-09-19 JP JP2013529081A patent/JP5674947B2/ja not_active Expired - Fee Related
- 2011-09-19 WO PCT/KR2011/006919 patent/WO2012036538A2/ko active Application Filing
- 2011-09-19 KR KR1020110094241A patent/KR101344584B1/ko active IP Right Grant
- 2011-09-19 DE DE112011103114T patent/DE112011103114T5/de not_active Withdrawn
- 2011-09-19 CN CN201180044750.3A patent/CN103108906B/zh not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
---|---|
KR20120030030A (ko) | 2012-03-27 |
CN103108906A (zh) | 2013-05-15 |
WO2012036538A3 (ko) | 2012-06-21 |
JP5674947B2 (ja) | 2015-02-25 |
CN103108906B (zh) | 2015-08-05 |
KR101344584B1 (ko) | 2013-12-26 |
US8968605B2 (en) | 2015-03-03 |
DE112011103114T5 (de) | 2013-06-27 |
JP2013539800A (ja) | 2013-10-28 |
US20130140499A1 (en) | 2013-06-06 |
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