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Polymer Phase Structure Analyzer PP-1000

PP-1000 analyzes the structure of polymers and film in-situ (on site) and in real time by using the small angle light scattering method. This analyzer is able to analyze larger structures (μm order) compared to analyzers that use x-rays and neutron beams because it uses visible light.

Evaluation of optical anisotropy and analysis of spherulite diameter of crystalline film can be carried out from Hv scattering which uses polarizers. Analysis of polymer blend correlation length can be carried out from Vv scattering.

 

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Product

Features
  • Measures scattering angle of 0.33 to 45 degrees in 10 msec at the fastest
  • Evaluates structures of submicron to several hundred micron size
  • Measures solution samples with specialized cells
  • Allows user to easily switch between Hv and Vv scattering with software
  • Can be set up in labs because it is a table-top type

 ※When not using HDR function

 

Measurement Items
  • Phase separation process of polymer blends
  • Crystallization process of polymers
  • Calculation of crystal size, crystallization growth rate
  • Orientation state
  • Aggregation process
  • Thermoset process
  • Structure change when temperature change occurs
  • Structure change caused by stretching
  • Curing process caused by ultraviolet light

 ※These items require separate consultation. Please feel free to contact us about details for these items.

 

Measurement Range (Theoretical Value)
  • Spherulite diameter 1.3~270μm
  • Correlation length 0.1~100μm

 

Specifications

Specifications
Measurement principle Small angle light scattering method
Light source Semiconductor laser
(wavelength 785nm)
Detector CMOS Camera
Measurement range
(Theoretical value)
Spherulite diameter 1.3~270μm
Correlation length 0.1~100μm
Dynamic range From 120db +(when using HDR function)
Measurement angle 0.33°~45°(dependent on camera length)
camera length
50mm
150mm
300mm
Angle range
2°~45°
0.67°~18.4°
0.33°~9.5°
Angular resolution
0.3°
0.1°
0.05°
Obtained pattern Hv scattering pattern,Vv scattering pattern
Measurement spot Approx. 1mm
Beam stopper φ3mm
Measurement time 10msec~
Power requirements AC100-240V 75VA
Size W350×D500×H760(mm)
Data processing unit Laptop PC(Windows10)

※When using HDR function 100msec~

■ HDR
  Abbrevation of `High Dynamic Range Imaging`
  Technology that combines multiple photographs of different exposure levels.

 about HDR

Principle

Optical system schematic drawing

Optical system schematic drawing

 

Hv Scattering

This measures in crossed-nicols (polarizer and analyzer are orthogonal).
A scattering pattern will appear if the scatterer is optically anisotropic (birefringent) which allows the user to evaluate the size, orderliness, and orientation of higher order structures of polymers.

(Measurement example) Analysis of the spherulite diameter of crystallization film

(Measurement example) Analysis of the spherulite diameter of crystallization film

A four-leaf clover shape Hv scattering pattern is obtained when the spherulitic structure of crystalline polymers are being formed.
The scattering intensity reaches a maximum at azimuth angle 45°, and the scattering vector (q) is plotted on the horizontal axis and the scattering intensity (Is) is plotted on the vertical axis.
With this, a scattering profile with the measurement angle θmax, which is the maximum scattering intensity, can be obtained. Using this θmax, the spherulite radius can be calculated from the following equation:
 

Spherulite radius

~Introduction of each scattering pattern~
Left:Spherulite structure,Right:Rod-like structure

 

Vv Scattering

Measures with parallel nicols (polarizer and analyzer are parallel).
・Evaluation of phase separation process of polymer blends
・Size of `sea-island` structure (correlation length)
・Evaluation of particle size ※etc

※ The volume fraction of the `island` portion of the `sea-island` structure is required

(Example of measurement) Analysis of correlation length of phase separation structure

(Example of measurement) Analysis of correlation length of phase separation structure

When it has a disordering structure such as a `sea-island` structure, a circular Vv scattering pattern can be obtained.
The correlation length ξ of a sample can be obtained using a Debye-Bueche plot (a graph plotting q2 on the horizontal axis and Is-1/2 on the vertical axis).
The analysis is based on the following equation. If the slope of the linearly approximated straight line is a and the intercept is b in the specified range, the correlation length ξ can be obtained from the following equation:
 

 correlation length

~Introduction of each scattering pattern~
Left:Ordering structure,Right:Disordering structure

 

Measured Data

Evaluating crystallization process of polyvinylidene diflouride film
(230℃→160℃)

Evaluating crystallization process of polyvinylidene diflouride film(230℃→160℃)

 

Methylcellulose solution phase separation process evaluation
(ambient temperature→60℃)

Methylcellulose solution phase separation process evaluation(ambient temperature→60℃)

【References】
 Motoki Shibata, Tsuyoshi Koga, Koji Nishida, Polymer 178, 121574 (2019)

 

Option

● Heating and cooling stage
● Sample stretching stage

※Other stage setups possible. Please feel free to contact us about details.

 

Related Information

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