1.3 Reversible shape memory polymers
1.3.3 Multi-time shape memory polymers
One time reversibility is still a one way transition, and a special application for triple shape memory effect. True reversibility requires the ability to change between two shapes for multiple times like actuators. Many researches have been devoted to introduce the two way actuation to the shape memory polymers. The recent focus on two way shape memory focused on actuation under constant non-zero external load100- 102. The sample undergoes crystalline induced elongation and melting induced contraction during cycles of cooling and heating. There are two factors contribute to the crystalline induced elongation effect, the rubber elasticity which decreases when the temperature decrease, leads to elongation with the load. In addition, the stress induced crystallization orientates along the loading axis and extends the bulk shape of the material. The drawback of this protocol is the lack of freedom as the presence of an external load is constantly required. Composite materials are developed to incorporate the external load into the system by using an additional elastic material to provide external force. However, the material is still not free to perform the reversible motion
and the programmability, which is the major advantage over the changing polymers, is significantly reduced. Our research will focus on new protocols to make multi-time reversible shape memory without any external load and free to program as conventional shape memory polymers.
1.3.4 Memory of crystalline physical network.
Most polymers are semi-crystalline which means the crystallinity is always less than 100%, there always amorphous segments remain in a crystallized polymer sample. So in a semi-crystalline shape memory polymer, the shape is not merely held by freezing of all chain movement as in the case of glass transition. The crystals also act as additional physical crosslinks in the network. A semi-crystalline shape memory can be described as a dual network systems with a chemical network formed at the initial state during synthesis, and a physical network formed at the programmed state during fixation.
In conventional shape memory researches, the memory is only preserved in the permanent chemical network which corresponds to initial shape. The only role for switching segment is to temporarily freeze the programmed shapes, no history or memory remains through transition. In our goal to create reversible shape memory behavior, we would like to ‘teach’ the physical network to retain the memory as well as the chemical network.
Thereare two types of primary nucleation: homogeneous andheterogeneous nucleation. Homogeneous nucleation can bedefined by spontaneous aggregation of polymer molecules toform a nucleus, which must be above a certaincritical size below
the melting point. Above this size, thenucleation occurs sporadically. In heterogeneous nucleation,nucleation sites pre-exist in a sample and are activated instantaneously and kinetically much faster than the homogeneous nucleation. When a polymer is only partially melted or even above the melting point, if the melt temperature or its holding time is insufficient, remnants of the previous structure (residual crystal) can act as predetermined nucleation sites upon subsequent cooling. This phenomenon is referred to as self-seeding effect and offers memory for the partially melted crystals103. Figure 1.7 demonstrate one scenario of the effect as crystals are partially melted, the
amorphous chains are confined by neighboring remaining crystals, and the structure and position of the previous crystals are conserved and its kinetically favorable for previous crystals to reform when the crystallization starts again.
Figure 1.7 Confinement effect and Self-seeding. When a crystal is partially molten the molten chains are kinetically confined in their crystalline position and highly likely to recrystallize into the same crystals before partial melting.
The independent network hypothesis was proposed to describe dual networks that crosslinks form under different shapes104,105. The networks formed at different strain can be treated separately and the overall response is the balance of the individual stresses for each network. As the stress is proportional to the density of the crosslinks, balance between the two states can be controlled by removing and adding temporary physical crosslinks, i.e. crystals.
We propose to create microscopically reversible change of crystals between partial melted and crystalline states, and according to independent network hypothesis, transfer the microscopic reversibility to macroscopic shape changes and demonstrate true reversible shape memory effect using semi-crystalline polymers. Our research will look into answers of the following questions:
Can polymer crystals be reversibly controlled through partial melting and crystallization?
Can new protocols be developed to transfer the microscopic reversibility to macroscopic shape change?
Can multiple cycles of reversible shape change be achieved using the new protocol?
What kind of shape changes and motions can be performed reversibly with the new protocol?
What are the effects on the reversibility of the material and how can we improve the reversibility by material designing and optimizing protocols?
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CHAPTER 2: PERFECT MIXING OF IMMISCIBLE MACROMOLECULES AT FLUID