Features of SUMIKAEXCEL PES Powder

Powder grades of SUMIKAEXCEL PES are suitable for the following applications:

• Adhesives and paint and coating compounds in solvent solutions
• Hollow fiber membranes and cast films (flat films) in solvent solutions
• Compounds and epoxy reinforcing applications

The following powder grades are available.

Table 7-1 SUMIKAEXCEL PES Powder Grades

Powder Grade	RV (reduced viscosity)*	Main applications
3600P	0.36	Compound
4100P	0.41	Paints and coating agents, and adhesives
4800P	0.48	Hollow fiber membranes and adhesives
5003PS	0.50	Paints and coating agents, adhesives, and epoxy strengthening agents
5200P	0.52	Hollow fiber membranes
5900P	0.59	Hollow fiber membranes
7600P	0.76	Hollow fiber membranes

The reduced viscosity is measured in a 1% solution of dimethylformamide (DMF).

Table 7-2 Grade Lineup for SUMIKAEXCEL PES

Reduced viscosity		0.36	0.41	0.48	0.52	0.59	0.76
Powder		3600P	4100P	4800P	5200P	5900P	7600P
		5003PS*
Pellet	Unreinforced	3600G	4100G	4800G
	Glass fiber reinforced	3601GL20	4101GL20
		3601GL30	4101GL30

* End OH containing grade

Physical Properties of SUMIKAEXCEL Powder Grades

Properties of SUMIKAEXCEL 3600P, 4100P, and 4800P

To obtain the physical properties for the following grades: 3600P, 4100P, and 4800P, please refer to the physical properties for pellet-type grades: 3600G, 4100G, 4800G.

Table 7-3 Physical Properties of 3600G, 4100G and 4800G

		Test method	Unit	3600G/4100G/4800G
General Physical Properties	Density	ISO 1183	g/cm3	1.37
	Mold shrinkage (MD)	Internal	%	0.60
	Mold shrinkage (TD)	Internal	%	0.60
	Water absorption (23°C, 24hr)	ISO 62	%	1.0
Mechanical properties	Tensile strength	ISO 527-1,2	MPa	85
	Tensile yield strain	ISO 527-1,2	%	6.5
	Flexural strength	ISO 178	MPa	130
	Flexural modulus	ISO 178	MPa	2,600
	Izod impact strength (unnotched)	ISO 180/1U	kJ/m2	Does not break
	Izod impact strength (notched)	ISO 180/1A	kJ/m2	8
	Rockwell hardness (M scale)	ISO 2039-2	-	95
Thermal properties	Deflection temperature under load (0.45MPa)	ISO 75	°C	214
	Deflection temperature under load (1.80MPa)	ISO 75	°C	205
	Coefficient of linear thermal expansion (MD)	ISO 11359-1,2	10-5/K	5.5
	Coefficient of linear thermal expansion (TD)	ISO 11359-1,2	10-5/K	5.5
Electrical properties	Relative dielectric constant (dry:100Hz)	IEC 62631-2-1	-	3.5
	Relative dielectric constant (dry:1MHz)	IEC 62631-2-1	-	3.4
	Relative dielectric constant (dry:1GHz)	IEC 60250	-	3.4
	Dielectric dissipation factor (dry:100Hz)	IEC 62631-2-1	-	0.002
	Dielectric dissipation factor (dry:1MHz)	IEC 62631-2-1	-	0.004
	Dielectric dissipation factor (dry:1GHz)	IEC 60250	-	0.004
	Volume resistivity	IEC 62631-3-1	Ω·m	>1013
	Dielectric strength (1mm)	IEC 60243-1	kV/mm	43
	Tracking resistance	IEC 60112	V	150
Flammability	Flame retardant rank	IEC 60695-11-10	-	V-0
	Limiting oxygen index (1.6mm)	ASTM D2863	%	38

Properties of SUMIKAEXCEL 5003P and 5003PS

• SUMIKAEXCEL 5003P/5003PS is an amorphous resin that has a glass transition temperature of 230°C.
• Possesses excellent adhesive properties due to the large number of terminal hydroxyl groups, which range from 0.6 to 1.4 per 100 polymer repeating units.
• All other properties are similar to those of other grades of SUMIKAEXCEL PES.

Paint and Coating Applications

SUMIKAEXCEL 4100P and 5003PS grades are utilized as paints and coating agents. The following characteristics have been specially enhanced in the 5003PS grade: hardness after heating, chemical resistance, and adhesion toward metals.
This section describes the paints and coating agents that use SUMIKAEXCEL 5003PS.

Features of Paints and Coating Agents of SUMIKAEXCEL 5003PS

• Stable even after long periods of usage in the air at a temperature of 250°C, and when used under conditions of repetitive heating and cooling cycles (between 0°C and 250°C).
• Adhesive properties and bonding: Demonstrates outstanding adhesion to glass, ceramic, iron, stainless steel, aluminum, and aluminum alloys.
• Solvent resistance: Demonstrates the highest solvent resistance among most amorphous resins.
• Resistance to hydrolysis: Polyethersulfone resin itself has outstanding hydrolysis resistance, yet 5003PS possesses even greater resistance to hydrolysis.
• Film formation properties: Has superior film formation properties and provides effective protection for base materials.
• Flame retardancy: Has high flame retardancy without utilizing any flame retardant components.
• Transparency: Has excellent transparency and does not change the appearance of the base material, even after application.
• Hygienic properties: Does not contain additives, such as plasticizers, thus making it highly hygienic.

Coating Procedures for SUMIKAEXCEL 5003PS (Example of Solution Method)

• Remove all oil and grease from the base material. If necessary, sandblast or etch the surface.
• Dissolve 5003PS in a solvent solution.
• Apply this solution to the base material, using any of the following methods: immersion, brush application, or spraying. Allow to air dry for 20 minutes.
• Heat-treat the material in hot air at a temperature of 350 to 400°C for 30 minutes.

Gelation Prevention

The SUMIKAEXCEL PES solution may become a gel, and it is described as liquid crystal related to both PES molecules and the solvent.

(Features)

• The solution may become cloudy and the whole solution may solidify.
• If a gel is formed, it is difficult to dissolve again even if a solvent is added.
• The gel is the core of the gelation of the ungelatinized solution.
• By applying temperature, it melts and returns to the original solution.

(Gelation prevention)

• Do not apply excessive shear stress. Do not use a homogenizer.
• Do not leave PES in a highly concentrated state for a long period of time. Do not leave swollen PES in unstirred solvent.
• The use of mixed solvents is recommended.

Concentration-Viscosity Correlation

The following figure shows the concentration-viscosity correlation of NMP solutions of SUMIKAEXCEL 4100P and 5003PS.

Figure 7-1 Concentration-Viscosity Correlation of NMP Solutions of SUMIKAEXCEL 4100P and 5003PS

Heat Resistance of SUMIKAEXCEL 5003PS Coating on Aluminum Sheet (Example)

Table 7-4 Heat Resistance Under Continuous Service (in the Air at a Temperature of 250°C)

Evaluation items	Time (hr)
	0	115	235
Change in appearance	-	No change	No change
Cross-cut Adhesion Test*1	100/100	100/100	100/100
Corrosion Resistance Test*2	No corrosion	No corrosion	No corrosion

Table 7-5 Repetitive Heating and Cooling Cycle Test (2 minutes in ice water at 0°C 2 minutes in oven at 250°C)

Evaluation items	Number of cycles (times)
	0	25	50
Change in appearance	-	Almost no change	Slight occurrence of foam around edges
Cross-cut Adhesion Test*1	100/100	100/100	100/100
Corrosion Resistance Test*2	No corrosion	No corrosion	No corrosion

(*1)

The test procedure for cross-cut adhesion is as follows: Using a safety razor, create a mesh of intersecting cuts (the shape of lines on a checkerboard) into a base material that has been coated with SUMIKAEXCEL 5003PS. The cuts must be deep enough to reach the base material and should be spaced 1mm apart, to form a series of 1mm × 1mm squares, over an area of 100mm2. Place adhesive tape over the area of the cuts and apply pressure, then remove the tape. Check the squares to determine the number of squares that still contain the PES coating.

(*2)

The test procedure for corrosion resistance is as follows: Place several drops of a solution containing 15% (vol) nitric acid onto the test surface that has been coated with SUMIKAEXCEL 5003PS. Cover the surface with a glass plate and let it stand for 24 hours. Observe any changes in the surface appearance.

Applications as Impact Modifier for Epoxy Based Systems

SUMIKAEXCEL 5003PS is utilized in the creation of epoxy-based composite materials. The advantages of adding SUMIKAEXCEL 5003PS to epoxy-based composites are as follows:

• Improves the breaking strength of epoxy.
• Has a very high Tg.
• Has excellent mechanical properties.

Enhancing the Plasticity of Epoxy Resins

SUMIKAEXCEL 5003PS is essentially plastic in behavior, thus has both a high Tg and flexural modulus. Therefore, it has the ability to add plasticity to epoxy resins without degrading the overall performance of the composite itself. The table below indicates a large increase in breaking strength (GIC). It is also apparent that Tg does not decrease significantly.

Table 7-6 Effects When Blended with TGDDM / 4, 4'-DDS

Results of Comparing Epoxy Resin and As4CF at a Polymer Concentration of 30% (wt)

Table 7-7 Comparison between SUMIKAEXCEL PES and PEI

Application of SUMIKAEXCEL PES to Aircraft and Sporting Goods Fields

Epoxy thermosetting resins are utilized as the resin matrix in CFRPs (carbon fiber reinforced polymers).
Although epoxy resins possess excellent mechanical and thermal properties, it is more susceptible to fracture than thermoplastic resins. For applications in the area of aircraft and sporting equipment, it is mandatory that its fracture toughness (compression after impact [CAI] strength) is improved. If 5003P is added to epoxy resin, a reaction occurs, which increases the resin’s plasticity, toughening it against impact fractures that may cause delamination within the resin matrix.

• Procedures for SUMIKAEXCEL 5003P
  The 5003P is dissolved directly in the epoxy base resin and mixed until a homogeneous solution is obtained. Next, the hardener is mixed into the solution. As the epoxy mixture hardens, it reacts with the hydroxyl radicals in the 5003P, forming a special morphology that contains a "sea island structure" (matrix and discontinuous phase), thus providing improved impact resistance. Either of the two following procedures can be utilized in order to obtain a homogeneous solution of 5003P in epoxy base resin: the 5003P can be ground finely and dissolved directly in the epoxy base resin in an N₂ atmosphere at a temperature of approximately 150°C. Alternately, the 5003P can first be dissolved uniformly in a solvent, then the solvent is later removed. The epoxy base resin is then mixed into this remaining compound to obtain a homogeneous solution.
• Amounts of 5003P for Usage in Composites (Example)
  • Per unit of matrix range
    Epoxy base resin (100 phr) : Hardening agent (30 to 40 phr) : 5003P (30 phr)
  • Per unit of prepreg
    Up to 10wt%
• Usage in Aircraft Structural Composites
  In order to utilize 5003P in structural composites for aircraft, precisely-sized fine particles of 5003P (tough balls), are sprinkled onto the surface of CF prepreg, which has been produced according to the above section entitled "Procedures for SUMIKAEXCEL 5003P". Next, several dozen of these CF prepreg layers are laminated together. This process improves the impact resistance, due to the PES particles that are located on the boundaries of each surface.
  Furthermore, a variety of creative laminating methods have also been invented thus far.

  (Example : structural composite standards for Boeing aircraft)

  • CAI (compression after impact) value must be 310MPa or greater
  • CS (compressive strength under hot/wet conditions) value must be 1,100MPa (at 82°C) or greater.

Adhesive Applications

SUMIKAEXCEL PES can be utilized as a heat resistant adhesive. It possesses particularly outstanding adhesive strength toward metals.

Features

• Bonded surfaces possess high tensile adhesive shear strength and T-peel adhesive strength. Its characteristics are well balanced, as it also possesses both rigidity and flexibility.
• PES possesses the highest heat resistance of most commercial thermoplastic resin adhesives. It possesses an extremely high tensile fracture adhesion strength of 20MPa, even at a temperature of 200°C.
  As well, for short periods of time, it can be utilized repeatedly at temperatures of up to 250°C.
• PES has outstanding chemical resistant and heat resistant properties.
• PES does not contain any solvents or volatile components and demonstrates excellent adhesion toward a variety of materials, including unprimed metals such as aluminum, stainless steel, steel, and brass.

Adhesion Method

• Hot melt type adhesion method using SUMIKAEXCEL PES film
  • Cut the film to the size of the objects being bonded (adherends).
  • Roughen the adherend surfaces using sandpaper or a disc sander, then clean the surfaces with acetone or toluene.
  • Sandwich the film between the adherends, apply a small amount of pressure using a jig, then heat the joint for 10 to 30 minutes at a temperature of 300 to 360°C. An adequate level of pressure will be achieved if the melted resin just begins to ooze out from between the adherends, as flash.
  • A strong bond will be obtained if the joint is left to stand in cold conditions.
• Adhesion method using an adhesive solution
  Solvent Solutions for SUMIKAEXCEL 5003PS
  When 5003PS is dissolved in a single solvent, it is unstable and PES precipitates, so a mixed solvent system is usually used. (Solution stability is low in a single solvent, thus causing gelation.)

Table 7-8 Examples of Mixed Solvent Solutions for SUMIKAEXCEL 5003PS

Solvent	Solvent	Mixing ratio (volume ratio)
A	Dimethylformamide Cyclohexanone Methyl ethyl ketone	20 80 25
B	N-methyl-2-pyrrolidone Toluene or xylene	2 1
C	N-methyl-2-pyrrolidone Toluene or xylene Silicon flow modifier Methyl ethyl ketone	60 30 0.5-1 35
D	Sulfolane γ-butyrolactone	1 1
E	Sulfolane Acetone or methyl ethyl ketone	1 1

Adhesion Method
As the strength of PES adhesives will vary depending on the thermal treatment conditions, it is necessary to determine the appropriate conditions in accordance with each particular application.
(Condition 1) Dry for 2 hours at a temperature of 130°C
(Condition 2) Dry for 1 hour at a temperature of 100°C, then continue drying for 15 minutes at a temperature of 350°C

Properties of SUMIKAEXCEL 5003PS Adhesives

It has excellent adhesive strength at high temperatures. For example, Tables 7-9 and 7-10 show the changes in adhesive strength when the temperature increases to 220°C and the results for the adhesive strength retention rate for aging at 150°C when 18-8 stainless steel is bonded together using a SUMIKAEXCEL 5003PS adhesive.

Cartridge Filters Utilizing PES Membranes (Courtesy of Toyo Roshi)