Solvent and Curing Effects on Diffusion at Polyimide Interfaces

1989 ◽  
Vol 153 ◽  
Author(s):  
S. F. Tead ◽  
E. J. Kramer ◽  
T. P. Russell ◽  
W. Volksen

AbstractInterdiffusion at interfaces between deuterated polyamic acid (d-PAA) and polyimide (PI) films was investigated with forward recoil spectrometry, an ion beam analysis technique. The PI films were prepared by spin - coating a solution of PAA on a silicon substrate, followed by an anneal at a temperature Ti, which produced partial or complete conversion of the PAA to PI. An overlayer of d-PAA was added in one set of samples by spin - coating from solution and in another set by transferring (in the absence of solvents) a dry d-PAA film onto the PI surface. The bilayer samples were then either annealed at a temperature Td or allowed to stand at room temperature. Bilayers prepared by spin - coating d-PAA from solution directly on partially cured PI films had interdiffusion distances w that decreased with increasing values of Ti to immeasurable levels by Ti = 200 °C. The decrease in w with increasing Ti is thought to be caused by a positive Flory parameter between PAA and PI which increases with the imide fraction in the PI film; the result is an increasing immiscibility between the swollen polymer layers. No interdiffusion occurred in the solventless - transfer samples for any combination of temperatures Ti or Td from room temperature up to 400 °C. Post - annealing of spin - coated bilayers at a temperature Td up to 400 °C was ineffective in producing any additional interdiffusion. Both of these results indicate that thermally activated interdiffusion (even for initially unimidized samples) does not exist in the absence of solvents, an effect attributed to the rapid increase of the glass transition temperature of the polymer with imidization.

1989 ◽  
Vol 154 ◽  
Author(s):  
S. F. Tead ◽  
E. J. Kramer ◽  
T. P. Russell ◽  
W. Volksen

AbstractInterdiffusion at interfaces between deuterated polyamic acid (d-PAA) and polyimide (PI) films was investigated with forward recoil spectrometry, an ion beam analysis technique. The PI films were prepared by spin – coating a solution of PAA on a silicon substrate, followed by an anneal at a temperature Ti, which produced partial or complete conversion of the PAA to PI. An overlayer of d-PAA was added in one set of samples by spin – coating from solution and in another set by transferring (in the absence of solvents) a dry d- PAA film onto the PI surface. The bilayer samples were then either annealed at a temperature Td or allowed to stand at room temperature. Bilayers prepared by spin – coating d-PAA from solution directly on partially cured PI films had interdiffusion distances w that decreased with increasing values of Ti to immeasurable levels by Ti = 200 °C. The decrease in w with increasing Ti is thought to be caused by a positive Flory parameter between PAA and PI which increases with the imide fraction in the PI film; the result is an increasing immiscibility between the swollen polymer layers. No interdiffusion occurred in the solventless – transfer samples for any combination of temperatures Ti or Td from room temperature up to 400 °C. Post – annealing of spin – coated bilayers at a temperature Td up to 400 °C was ineffective in producing any additional interdiffusion. Both of these results indicate that thermally activated interdiffusion (even for initially unimidized samples) does not exist in the absence of solvents, an effect attributed to the rapid increase of the glass transition temperature of the polymer with imidization.


2002 ◽  
Author(s):  
Shinji Nagata ◽  
Bun Tsuchiya ◽  
K. Toh ◽  
N. Ohtsu ◽  
Tsunemi Kakuta ◽  
...  

1997 ◽  
Vol 476 ◽  
Author(s):  
P. H. Townsend ◽  
S. J. Martin ◽  
J. Godschalx ◽  
D. R. Romer ◽  
D. W. Smith ◽  
...  

AbstractA novel polymer has been developed for use as a thin film dielectric in the interconnect structure of high density integrated circuits. The coating is applied to the substrate as an oligomeric solution, SiLK*, using conventional spin coating equipment and produces highly uniform films after curing at 400 °C to 450 °C. The oligomeric solution, with a viscosity of ca. 30 cPs, is readily handled on standard thin film coating equipment. Polymerization does not require a catalyst. There is no water evolved during the polymerization. The resulting polymer network is an aromatic hydrocarbon with an isotropie structure and contains no fluorine.The properties of the cured films are designed to permit integration with current ILD processes. In particular, the rate of weight-loss during isothermal exposures at 450 °C is ca. 0.7 wt.%/hour. The dielectric constant of cured SiLK has been measured at 2.65. The refractive index in both the in-plane and out-of-plane directions is 1.63. The flow characteristics of SiLK lead to broad topographic planarization and permit the filling of gaps at least as narrow as 0.1 μm. The glass transition temperature for the fully cured film is greater than 490 °C. The coefficient of thermal expansivity is 66 ppm/°C below the glass transition temperature. The stress in fully cured films on Si wafers is ca. 60 MPa at room temperature. The fracture toughness measured on thin films is 0.62 MPa m ½. Thin coatings absorb less than 0.25 wt.% water when exposed to 80% relative humidity at room temperature.


1981 ◽  
Vol 4 ◽  
Author(s):  
P. S. Peercy ◽  
D. M. Follstaedt ◽  
S. T. Picraux ◽  
W. R. Wampler

ABSTRACTLattice defects and precipitates induced in unimplanted and Sb-implanted <110> single crystal Al by single pulse irradiation with a Q-switched ruby laser were studied using ion beam analysis and electron microscopy. The absorbed laser energy during irradiation is directly measured in these studies to allow precise numerical modeling of the melt times and temperature profiles. For unimplanted Al, slip deformation gives rise to increased channeled yields throughout the analyzed depth and occurs for energies well below the melt threshold energy of 3.5 J/cm2. Slip deformation is also observed for irradiation energies above the melt threshold energy, and melting is accompanied by a discontinuous increase in the minimum channeling yield, X min- Implanted Sb (to ∼2 at.% peak concentrations) is found to impede epitaxial regrowth and result in polycrystalline Al formation for laser energies such that the melt front is believed not to penetrate through the Sb-containing region. For deeper melt depths, a metastable alloy is formed with up to 35% of the Sb located in substitutional sites. AlSb precipitate formation in the melt was not observed for room temperature irradiations; however, randomly oriented AlSb precipitates are observed for irradiation at substrate temperatures of 100 and 200 °C These measurements yield an estimated time for nucleation of AlSb precipitates in molten Al of 5 nsec < tnuc < 25 nsec.


2020 ◽  
Vol 229 ◽  
pp. 03004
Author(s):  
Sandile Jongile ◽  
Ntombizonke Kheswa ◽  
Paul Papka ◽  
Olivier Sorlin ◽  
Antoine Lemasson ◽  
...  

A new method was developed to produce enriched Sulfur targets with minimum loss of material. This was made possible by inserting Sulfur in-between two 0.5 μm Mylar foils (C10H8O4). The initial aim was to ensure that the Sulfur targets reduce by no more than 50% of the initial thickness within 24 hours under the equivalent of 10 J/cm2 of integrated energy deposition by an energetic (Eb > 50 MeV) proton beam. There is no loss of enriched material while making the target, as all the material is deposited within the surface area to be exposed to the beam. During beam irradiation, the targets were frequently swivelled in order to expose each part of the target to the beam and achieve homogeneous irradiation. Targets of 0.4 mg/cm2 thickness were produced and characterised using ion beam analysis technique with a 3 MeV proton beam.


1989 ◽  
Vol 68 (9) ◽  
pp. 1313-1315 ◽  
Author(s):  
C.W. Fairhurst ◽  
D.T. Hashinger ◽  
S.W. Twiggs

Porcelain-fused-to-metal restorations are fired several hundred degrees above the glass-transition temperature and cooled rapidly through the glass-transition temperature range. Thermal expansion data from room temperature to above the glass-transition temperature range are important for the thermal expansion of the porcelain to be matched to the alloy. The effect of heating rate during measurement of thermal expansion was determined for NBS SRM 710 glass and four commercial opaque and body porcelain products. Thermal expansion data were obtained at heating rates of from 3 to 30°C/min after the porcelain was cooled at the same rate. By use of the Moynihan equation (where Tg systematically increases in temperature with an increase in cooling/heating rate), the glass-transition temperatures (Tg) derived from these data were shown to be related to the heating rate.


2018 ◽  
Vol 29 (10) ◽  
pp. 2164-2176 ◽  
Author(s):  
R Abishera ◽  
R Velmurugan ◽  
KV Nagendra Gopal

Thermally activated shape memory polymers are typically programmed by initially heating the material above the glass transition temperature ( Tg), deforming to the desired shape, cooling below Tg, and unloading to fix the temporary shape. This process of deforming at high temperatures becomes a time-, labor-, and energy-expensive process while applying to large structures. Alternatively, materials with reversible plasticity shape memory property can be programmed at temperatures well below the glass transition temperature which offers several advantages over conventional programming. Here, the free, partial, and fully constrained recovery analysis of cold-programmed multi-walled carbon nanotube–reinforced epoxy nanocomposites is presented. The free recovery analysis involves heating the temporary shape above Tg without any constraints (zero stress), and for fully constrained recovery analysis, the temporary shape is held constant while heating. The partially constrained recovery behavior is studied by applying a constant stress of 10%, 25%, and 50% of the maximum recovery stress obtained from the completely constrained recovery analysis. The samples are also characterized for their thermal, morphological, and mechanical properties. A non-contact optical strain measurement method is used to measure the strains during cold-programming and shape recovery. The different recovery behaviors are analyzed by using a thermo-viscoelastic–viscoplastic model, and the predictions are compared with the experimental results.


RSC Advances ◽  
2016 ◽  
Vol 6 (25) ◽  
pp. 21271-21276 ◽  
Author(s):  
Yung-Chi Chu ◽  
Ming-Hsiao Weng ◽  
Wen-Yi Lin ◽  
Hsin-Jung Tsai ◽  
Wen-Kuang Hsu

Composites made from fibers and epoxy display a low viscous drag and are rarely used as mechanical dampers at room temperature.


HortScience ◽  
1995 ◽  
Vol 30 (4) ◽  
pp. 874D-874
Author(s):  
L.E. Towill

Cryopreservation using vitrification has been reported for several plant species. Shoot tips and vitrification solution were placed in semen straws and immersed in liquid nitrogen (LN). Cracking of the external glass occurred, but may be avoided by annealing slightly below the glass transition temperature before immersion. A varying percentage still cracked with some vitrification solutions. Rapid warming also can cause cracking. There is concern that cracking may reduce viability. Shoot tips from Mentha species were used to examine this problem. Glass cracking during either cooling or warming did not produce visible damage to shoot tips. Viability of shoot tips from tubes that cracked during cooling was not different from those that did not crack; however, shoot formation was slightly reduced. Cracking upon warming did not reduce viability nor shoot formation. Very slow warming reduced viability, but warming in either water or air (room temperature) gave higher levels of survival.


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