KR102121130B1 - PAN-Fe2O3 magnetic composites amd manufacturing method thereof - Google Patents
PAN-Fe2O3 magnetic composites amd manufacturing method thereof Download PDFInfo
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Abstract
Description
본 발명은 PAN-Fe2O3 자성복합체 및 그 제조방법에 관한 것으로서, 특히 자기특성이 우수한 PAN-Fe2O3 자성복합체을 제조할 수 있는 제조방법에 관한 것이다.The present invention relates to a production method capable of producing PAN-Fe 2 O 3 magnetic composite, and as it relates to a process for the preparation, in particular magnetic properties are excellent PAN-Fe 2 O 3 magnetic bokhapcheeul.
에너지 생산 및 정보 통신 기술의 급속한 발전은 원하는 장비를 제조하는데 사용되는 재료의 특성에 대한 요구 사항의 수를 증가시킨다. 자성 섬유는 주로 전자 및 전자기 분야에서 응용 분야를 찾는다.The rapid development of energy production and information and communication technology increases the number of requirements for the properties of the materials used to manufacture the desired equipment. Magnetic fibers find applications mainly in the fields of electronics and electromagnetics.
폴리 아크릴로 니트릴 (PAN)로 제조된 탄소 나노 섬유는 에너지 분야에서 다양한 응용 분야를 가지고 있다. 이들 섬유의 복합체는 양호한 가역성 및 보유 용량으로 인하여 전지 및 다른 에너지 저장 장치 용 양극으로 제조될 수 있다.Carbon nanofibers made of polyacrylonitrile (PAN) have a variety of applications in the energy field. Composites of these fibers can be made into positive electrodes for batteries and other energy storage devices due to their good reversibility and storage capacity.
탄소 나노 섬유는 유연성, 기계적 강도, 고 종횡비, 제어 가능한 섬유 직경 및 저밀도와 같은 뛰어난 특성을 가지고 있다. 탄소 나노 섬유의 더 많은 특성은 다른 나노 크기의 재료로 강화함으로써 조정할 수 있다.Carbon nanofibers have excellent properties such as flexibility, mechanical strength, high aspect ratio, controllable fiber diameter and low density. More properties of the carbon nanofibers can be adjusted by strengthening with other nano-sized materials.
화학 공정은 PAN-기반 탄소 나노 섬유를 제조하는 가장 일반적으로 사용되는 방법이다. 그러나 electrospinning과 같은 물리적인 방법은 그 섬유를 생산하는 데 사용될 수 있다.Chemical processes are the most commonly used method of making PAN-based carbon nanofibers. However, physical methods such as electrospinning can be used to produce the fiber.
탄소 나노 섬유가 전자기 및 전자 분야에서 사용되기 위해서는 전자기 특성이 일정 수준의 특성 성능을 만족시켜야 한다.In order for carbon nanofibers to be used in the electromagnetic and electronic fields, the electromagnetic properties must satisfy a certain level of performance.
본 발명은 자기특성이 우수하여 전자기 및 전자 분야에서 널리 사용할 수 있는 PAN-Fe2O3 자성복합체을 제조할 수 있는 PAN-Fe2O3 자성복합체의 제조방법을 제공하는 것을 목적으로 한다.An object of the present invention is to provide a manufacturing method of the magnetic properties is PAN-Fe 2 O 3 magnetic composite capable of producing superior to well-Fe 2 O 3 magnetic bokhapcheeul PAN that can be used in the electronic and electronic fields.
상기와 같은 목적을 달성하기 위한 본 발명은,The present invention for achieving the above object,
a) DMF(Dimethylformamide)에 PAN(polyacrylonitrile) 및 Fe2O3 나노입자를 혼합한 후 교반하여 방사용액을 제조하는 단계와;a) mixing PAN (polyacrylonitrile) and Fe 2 O 3 nanoparticles in DMF (Dimethylformamide) and stirring to prepare a spinning solution;
b) 상기 방사용액을 전기방사시켜 자성복합체을 얻는 단계와;b) obtaining a magnetic complex by electrospinning the spinning solution;
c) 상기 자성복합체을 가열하여 안정화시키는 안정화 단계와;c) a stabilization step of stabilizing the magnetic complex by heating;
d) 상기 안정화된 자성복합체을 탄화시키는 탄화 단계를 포함하는 것을 특징으로 하는 PAN-Fe2O3 자성복합체의 제조방법을 제공한다.d) It provides a method for producing a PAN-Fe 2 O 3 magnetic composite comprising a carbonization step of carbonizing the stabilized magnetic composite.
그리고 상기 a)단계는 DMF 100중량부에 PAN 12~15중량부 및 Fe2O3 나노입자 5~9중량부를 혼합하는 것이 좋다.In the step a), it is preferable to mix 12 to 15 parts by weight of PAN and 5 to 9 parts by weight of Fe 2 O 3 nanoparticles in 100 parts by weight of DMF.
또한 상기 a)단계는 DMF(Dimethylformamide)에 PAN(polyacrylonitrile) 및 Fe2O3 나노입자를 혼합한 후 70℃에서 800rpm으로 6시간동안 교반하여 방사용액을 제조하는 것이 좋다.In addition, in step a), it is good to prepare a spinning solution by mixing PAN (polyacrylonitrile) and Fe 2 O 3 nanoparticles in DMF (Dimethylformamide) and stirring at 70° C. for 800 hours for 6 hours.
그리고 상기 c)단계는 상기 자성복합체을 대기와 함께 280℃에서 2시간동안 가열하여 안정화시키는 것이 좋다.In step c), it is preferable to stabilize the magnetic complex by heating at 280° C. for 2 hours with the atmosphere.
또한 상기 d)단계는 상기 안정화된 자성복합체을 비활성 분위기 내에서 750℃에서 1시간 동안 탄화시키는 것이 바람직하다.In addition, in step d), it is preferable to carbonize the stabilized magnetic complex at 750° C. for 1 hour in an inert atmosphere.
아울러 본 발명은 상기 제조방법에 의해 제조된 것을 특징으로 하는 PAN-Fe2O3 자성복합체를 제공한다.In addition, the present invention provides a PAN-Fe 2 O 3 magnetic composite, characterized in that produced by the above manufacturing method.
본 발명의 PAN-Fe2O3 자성복합체의 제조방법은 자기특성이 우수하여 전자기 및 전자 분야에서 널리 사용할 수 있는 PAN-Fe2O3 자성복합체을 제조할 수 있는 효과가 있다.Production method of the PAN-Fe 2 O 3 magnetic complex of the present invention, there is an effect that magnetic properties superior to the widely-Fe 2 O 3 magnetic manufacture PAN bokhapcheeul that can be used in the electronic and electronic fields.
도 1은 방사용액을 전기방사시켜 제조된 자성복합 나노웹을 촬영한 사진이다.
도 2는 안정화된 자성복합 나노웹을 촬영한 사진이다.
도 3은 탄화되어 완성된 PAN-Fe2O3 자성복합체을 촬영한 사진이다.
도 4는 도 1의 자성복합 나노웹의 SEM사진이다.
도 5는 도 2의 안정화된 자성복합 나노웹의 SEM사진이다.
도 6은 도 3의 탄화되어 완성된 PAN-Fe2O3 자성복합체의 SEM사진이다.1 is a photograph of a magnetic composite nanoweb prepared by electrospinning a spinning solution.
Figure 2 is a photograph of the stabilized magnetic composite nanoweb.
FIG. 3 is a photograph of a carbonized and completed PAN-Fe2O3 magnetic composite.
4 is an SEM photograph of the magnetic composite nanoweb of FIG. 1.
FIG. 5 is an SEM photograph of the stabilized magnetic composite nanoweb of FIG. 2.
FIG. 6 is an SEM photograph of the PAN-Fe2O3 magnetic composite completed by carbonization of FIG. 3.
이하, 본 발명의 PAN-Fe2O3 자성복합체 및 그 제조방법에 대해 상세히 설명하면 다음과 같다.Hereinafter, the PAN-Fe 2 O 3 magnetic composite of the present invention and its manufacturing method will be described in detail as follows.
본 발명의 PAN-Fe2O3 자성복합체의 제조방법은 크게 방사용액 혼합단계, 전기방사단계, 안정화단계 및 탄화단계를 포함한다.The method of manufacturing the PAN-Fe 2 O 3 magnetic composite of the present invention largely includes a spinning solution mixing step, an electrospinning step, a stabilization step and a carbonization step.
상기 방사용액 혼합단계는 자기 성능이 우수한 PAN-Fe2O3 자성복합체를 제조하기 위한 방사용액을 제조하기 위한 단계로서, DMF(Dimethylformamide)에 PAN(polyacrylonitrile) 및 Fe2O3 나노입자를 혼합한 후 교반하여 방사용액을 제조하는 단계이다.The spinning solution mixing step is a step for preparing a spinning solution for preparing a PAN-Fe 2 O 3 magnetic complex having excellent magnetic performance, in which PAN (polyacrylonitrile) and Fe 2 O 3 nanoparticles are mixed with DMF (Dimethylformamide). After this, it is a step of preparing a spinning solution by stirring.
그리고 전기방사시 방사용액의 방사성이 우수하고, 자기성능이 우수한 자성복합체를 제조하기 위해 DMF 100중량부에 PAN 12~15중량부 및 Fe2O3 나노입자 5~9중량부를 혼합하는 것이 좋다.And it is good to mix 12 to 15 parts by weight of PAN with 12 to 15 parts by weight of PMF and 5 to 9 parts by weight of Fe 2 O 3 nanoparticles to prepare a magnetic composite having excellent spinnability and excellent magnetic performance during spinning.
PAN이 12중량부 미만으로 혼합될 경우 전기방사시 전기분무가 일어나 비드가 관찰되고, 15중량부 초과로 혼합될 경우 리본섬유의 형성이 관찰되는 문제가 있다.When PAN is mixed with less than 12 parts by weight, electrospray occurs during electrospinning, whereby beads are observed, and when mixed with more than 15 parts by weight, formation of ribbon fibers is observed.
그리고 Fe2O3 나노입자가 5중량부 미만으로 혼합될 경우 섬유직경이 일정하지 않고 완전한 탄화가 이루어지지 않는 문제가 있고, 9중량부 초과로 혼합될 경우 Fe2O3 나노입자의 응집이 발생하여 전기방사가 원활히 이루어지지 않는 문제가 있다.In addition, when Fe 2 O 3 nanoparticles are mixed in an amount of less than 5 parts by weight, there is a problem in that the fiber diameter is not constant and complete carbonization is not performed. When mixed in excess of 9 parts by weight, aggregation of Fe 2 O 3 nanoparticles occurs. Therefore, there is a problem that electrospinning is not smoothly performed.
특히, DMF(Dimethylformamide)에 PAN(polyacrylonitrile) 및 Fe2O3 나노입자를 혼합한 후 Fe2O3 나노입자의 분산성을 향상시키기 위해 70℃에서 800rpm으로 6시간동안 교반하여 방사용액을 제조하는 것이 좋다. In particular, after mixing PAN (polyacrylonitrile) and Fe 2 O 3 nanoparticles in DMF (Dimethylformamide), to improve the dispersibility of Fe 2 O 3 nanoparticles, the mixture was stirred for 6 hours at 70°C at 800 rpm to prepare a spinning solution. It is good.
그리고 상기 전기방사단계는 상기 방사용액을 전기방사시켜 자성복합 나노웹을 얻는 단계이다. And the electrospinning step is a step of obtaining a magnetic composite nanoweb by electrospinning the spinning solution.
이때 상기 전기방사단계에서 사용하는 전기방사장치는 통상의 장치를 사용할 수 있으며, 방사조건인 방사량, 유량, 전압차, 팁과 콜렉터와의 거리(Tip to Collector Distance, TCD) 등의 변수를 적절하게 조절하여 사용할 수 있다.At this time, the electrospinning device used in the electrospinning step may use a conventional device, and appropriately parameters such as radiation conditions, radiation amount, flow rate, voltage difference, and tip to collector distance (TCD). It can be adjusted and used.
특히, 전기방사시 인가전압은 15kV, 팁과 콜렉터와의 거리는 124mm가 바람직하다.In particular, the applied voltage during electrospinning is preferably 15 kV, and the distance between the tip and the collector is 124 mm.
다음으로 상기 안정화단계는 상기 전기방사단계에서 전기방사된 자성복합 나노웹을 안정화시키는 단계로서, PAN의 고분자 구조를 선형에서 사다리구조로 안정화시킬 수 있다Next, the stabilization step is a step of stabilizing the magnetic composite nanoweb electrospinned in the electrospinning step, and can stabilize the polymer structure of PAN from a linear to a ladder structure.
특히, 상기 자성복합 나노웹을 대기와 함께 280℃에서 2시간동안 가열하여 안정화하는 것이 바람직하다.In particular, it is preferable to stabilize the magnetic composite nanoweb by heating at 280° C. for 2 hours with the atmosphere.
그리고 상기 탄화단계는 상기 안정화된 자성복합 나노웹을 탄화시켜 자기성능이 우수한 PAN-Fe2O3 자성복합체를 얻는 단계이다.In addition, the carbonization step is a step of carbonizing the stabilized magnetic composite nanoweb to obtain a PAN-Fe 2 O 3 magnetic composite having excellent magnetic performance.
상기 안정화된 자성복합 나노웹을 파열시키지 않고 안정적으로 탄화된 자성복합체를 얻기 위해 비활성 분위기 내에서 750℃에서 1시간 동안 탄화시키는 것이 바람직하다.It is preferable to carbonize at 750° C. for 1 hour in an inert atmosphere in order to obtain a stable carbonized magnetic composite without rupturing the stabilized magnetic composite nanoweb.
다음으로, 본 발명의 PAN-Fe2O3 자성복합체의 제조방법을 실시예를 들어 상세히 설명하면 다음과 같고, 본 발명의 권리범위는 하기의 실시예에 한정되는 것은 아니다.Next, the method of manufacturing the PAN-Fe 2 O 3 magnetic composite of the present invention will be described in detail with reference to examples, and the scope of the present invention is not limited to the following examples.
[실시예][Example]
N,N-Dimethylmethanamide용매 83wt%, PAN 11wt% 및 30~40㎚크기의 Fe2O3 나노입자 6wt%를 혼합한 후 70℃에서 6시간 동안 800rpm으로 교반시켜 방사용액을 제조하였다.After mixing 83 wt% of N,N-Dimethylmethanamide solvent, 11 wt% of PAN, and 6 wt% of Fe 2 O 3 nanoparticles having a size of 30 to 40 nm, the mixture was stirred at 800°C for 6 hours at 800 rpm to prepare a spinning solution.
그리고 방사용액을 전기방사기를 이용하여 전기방사시켜 도 1의 자성복합 나노웹을 얻었다. 이때 전압은 15kv로 유지하였고, 방사용액의 주입속도는 27.3℃에서 2.1㎖/h로 유지하였으며, 챔버의 습도는 40%로 유지하였고, 팁과 콜렉터와의 거리는 124mm를 유지하였다.Then, the spinning solution was electrospun using an electrospinner to obtain the magnetic composite nanoweb of FIG. 1. At this time, the voltage was maintained at 15 kv, and the injection rate of the spinning solution was maintained at 2.1 ml/h at 27.3° C., the humidity of the chamber was maintained at 40%, and the distance between the tip and the collector was maintained at 124 mm.
그 다음 자성복합 나노웹을 tubular furnace에서 대기와 함께 280℃에서 2시간동안 가열하여 안정화시켜, 도 2의 안정화된 자성복합 나노웹을 얻었다. 이때 온두의 증가속도는 1℃/min으로 유지되었다.Then, the magnetic composite nanoweb was stabilized by heating for 2 hours at 280° C. with air in a tubular furnace to obtain a stabilized magnetic composite nanoweb of FIG. 2. At this time, the increase rate of ondu was maintained at 1°C/min.
안정화된 자성복합 나노웹을 질소분위기 내에서 750℃로 1시간 동안 탄화시켜 PAN-Fe2O3 자성복합체를 완성하였고, 완성된 PAN-Fe2O3 자성복합체를 도 3으로 나타냈다. 이때 온도의 증가속도는 5℃/min으로 유지되었다.The stabilized magnetic composite nanoweb was carbonized in a nitrogen atmosphere at 750° C. for 1 hour to complete the PAN-Fe 2 O 3 magnetic composite, and the completed PAN-Fe 2 O 3 magnetic composite was shown in FIG. 3. At this time, the rate of increase in temperature was maintained at 5°C/min.
그리고 도 1의 자성복합 나노웹에 대해 PAN나노섬유에 Fe2O3 나노입자가 함친된 상태를 확인하기 위해 SEM사진을 촬영하였고, SEM사진은 도 4로 나타냈다.In addition, for the magnetic composite nanoweb of FIG. 1, an SEM photograph was taken to confirm a state in which Fe 2 O 3 nanoparticles are impregnated in PAN nanofibers, and the SEM photograph is shown in FIG. 4.
SEM 이미지는 0.44와 0.8 μm 사이의 섬유를 보여주는 것으로서, Fe2O3 나노 입자가 PAN 섬유에 잘 매립되어 있음을 확인할 수 있다.The SEM image shows fibers between 0.44 and 0.8 μm, and it can be confirmed that Fe2O3 nanoparticles are well embedded in PAN fibers.
다음으로, 도 2의 안정화된 자성복합 나노웹의 SEM사진을 촬영하였고, SEM사진은 도 5로 나타냈다. 도 5에서 확인되는 바와 같이 안정화된 자성복합 나노웹의 섬유 직경은 안정화 공정 중에 안정적이었다. 안정화 동안 크기 변화가 관찰되지 않았다. 또한 Fe2O3 나노 입자는 손상되지 않고 그대로 유지되었으며 이 단계에서 왜곡되지 않았다. 입자가 섬유에 묻혀있는 위치에서 두드러진 입자임을 알 수 있다. 섬유의 뒤틀림이나 섬유 입자의 붕괴와 같은 결함은 보이지 않았다.Next, a SEM photograph of the stabilized magnetic composite nanoweb of FIG. 2 was taken, and the SEM photograph is shown in FIG. 5. As can be seen in Figure 5, the fiber diameter of the stabilized magnetic composite nanoweb was stable during the stabilization process. No size change was observed during stabilization. In addition, the Fe2O3 nanoparticles remained intact and did not distort at this stage. It can be seen that the particles are prominent particles at the location where they are buried in the fiber. There were no defects such as fiber warping or fiber particle collapse.
그리고 도 3의 탄화되어 완성된 PAN-Fe2O3 자성복합체의 SEM사진을 촬영하였고, 도 6으로 나타냈다. 도 6과 같이 PAN-Fe2O3 자성복합체에서는 탄소 섬유의 수축을 포함하여 약간의 변화가 관찰되었다. 섬유의 크기는 줄어들었고 약 0.36 ㎛인 것으로 밝혀졌다. 또한 Fe2O3 나노입자가 응집된 탄소섬유에는 네킹 현상이 관찰되었다.And the SEM photograph of the PAN-Fe 2 O 3 magnetic composite completed by carbonization of FIG. 3 was taken, and shown in FIG. As shown in FIG. 6, slight changes were observed in the PAN-Fe 2 O 3 magnetic composite including shrinkage of carbon fibers. The size of the fibers was reduced and found to be about 0.36 μm. In addition, a necking phenomenon was observed in the carbon fibers in which Fe 2 O 3 nanoparticles were aggregated.
Claims (6)
b) 상기 방사용액을 전기방사시켜 자성복합 나노웹을 얻는 단계와;
c) 상기 자성복합 나노웹을 대기와 함께 1℃/min으로 승온시켜 280℃에서 2시간동안 가열하여 안정화시키는 안정화 단계와;
d) 상기 안정화된 자성복합 나노웹을 비활성 분위기 내에서 5℃/min으로 승온시켜 750℃에서 1시간 동안 탄화시키는 탄화 단계를 포함하는 것을 특징으로 하는 PAN-Fe2O3 자성복합체의 제조방법.
a) mixing 12 to 15 parts by weight of PAN and 5 to 9 parts by weight of Fe 2 O 3 nanoparticles of 30 to 40 nm in size, and stirring for 6 hours at 800°C at 800 rpm to prepare a spinning solution; ;
b) obtaining a magnetic composite nanoweb by electrospinning the spinning solution;
c) a stabilization step of heating the magnetic composite nanoweb with air to 1°C/min and stabilizing by heating at 280°C for 2 hours;
d) A method of manufacturing a PAN-Fe 2 O 3 magnetic composite comprising the step of carbonizing the stabilized magnetic composite nanoweb at 5° C./min in an inert atmosphere and carbonizing at 750° C. for 1 hour.
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