3M Zeta Plus 40Q User Manual

Zeta Plus™ 40Q Puriﬁer Cartridges

Superior Removal of Trace Metals From High Purity Chemicals

Zeta Plus 40Q purifier cartridges are high capacity purifiers designed to remove metallic ion contaminants from high purity chemicals such as resins, photoresists, and solvents in a single pass. The purifier contains ion exchange groups that have been bonded within a porous depth media structure. This construction enhances surface area for the ion exchange groups assuring metallic contaminant removal to single digit ppb levels.

Zeta Plus 40Q Puriﬁer Cartridge Vs Ion Exchange Columns

Ion exchange columns, a process step commonly used to remove trace metal ions from high purity chemicals are often the limiting factor in reducing the manufacturing cycle. Ion exchange columns are comprised of resin beads, which typically have a particle size distribution ranging between 0.3 mm and 1.2 mm in diameter, and are packed into a column. When the resin beads are packed into the column they cause a high differential pressure as the highly viscous fluid flows down through the column. Because a finite space exists between ion exchange resin beads, void or interstitial volume is formed. When a high purity chemical is introduced to the ion exchange column, the fluid will take the path of least resistance through the column, which is commonly referred to as “channeling”. To minimize the channeling effect, the ion exchange column is operated at a very low flow rate which in turn increases the contact or “residence time” with the fluid. Residence is described as the period of time when the fluid and functional sites of the ion exchange resin are in contact. Even with low flow rates and long residence times, ion exchange columns typically cannot reduce the

Features & Beneﬁts

Zeta Plus 40Q Metal Ion Removal Media

n Removes trace metals to single digit ppb levels n Superior metal removal capacity, lower cost-of-ownership

Graded Density Construction

n Large surface area increases contact time between the ﬂuid and reactive sites of the puriﬁer n Increased Puriﬁer lifetime

High Flow Rates

n Increased throughputs as compared to ion exchange columns

Wide Range of Conﬁgurations

n Allows for the same puriﬁcation media to be used during laboratory, pilot and full production

scale-up

n Low hold-up volume disk ﬁlters allow material suppliers to perform testing in a rapid and cost-

effective manner

n Puriﬁcation media can be customized to the speciﬁc application

Low Cartridge Extractables

n No leaching of contaminants into the process ﬂuid

Quality Manufacturing

n ISO 9001:2008 Registered Quality Management System. n Repeatable and reliable performance

Applications

Resins

Solvents

Recirculation Baths

I Line Photoresists

G Line Photoresists

Ancillary Chemicals

Acetone

DI Water

IPA

Plating Solutions

Post CMP Clean

Water Reclaim

Table 1: Single Pass Metals Removal from PGMEA/PGME (30/70 Mixture)

Metal

Ca 0.2 15 < D.L.

Cr 0.2 10 < D.L.

Cu 0.2 9 < D.L.

Fe 0.2 9 < D.L.

Mg 0.2 8 < D.L.

Mn 0.2 11 < D.L.

Na 0.2 9 1.6

Pb 0.2 10 < D.L.

Zn 0.2 7 < D.L.

* Detection Limit

Detection

Limit (ppb)

Al 0.2 10 < D.L.*

K 0.2 8 < D.L.

Ni 0.2 8 < D.L.

Influent

Level (ppb)

Effluent

Level (ppb)

Table 2: Single Pass Metals Removal from PGMEA

Metal

Ca < 10 1160 < D.L.

Fe < 10 838 < D.L.

Na < 10 902 < D.L.

Detection

Limit (ppb)

Influent

Level (ppb)

Effluent

Level (ppb)

Table 3: Single Pass Metals Removal from ECA

Metal

Ca < 10 590 < D.L.

Fe < 10 230 < D.L.

Na < 10 850 < D.L.

Detection

Limit (ppb)

Influent

Level (ppb)

Effluent

Level (ppb)

Table 4: Extractable Metals Content of Zeta Plus 40Q Purifier Cartridge in PGMEA

Metal

Ca 4.0 < D.L.

Cr 2.0 < D.L.

Cu 1.0 < D.L.

Fe 5.0 < D.L.

K 1.0 < D.L.

Na 5.0 < D.L.

Detection Limit

(ppb)

Effluent Level

(ppb)

trace metal content to the required specification levels in a single pass. One reason for this is that the ion exchange resin beads have a relatively low surface area to volume ratio and another reason is that a large void volume exists between each resin bead. When these two factors are combined the process fluid is not able to fully access the ion exchange sites thereby resulting in a less efficient means of purification. For this reason, it is often necessary to run the ion exchange column in re-circulation mode until the required parts-per-billion levels for trace metals is achieved. This is particularly true with high viscosity chemicals. While this technology is effective at reducing trace metal and ionic contaminants it lacks the throughput that material suppliers require.

During the manufacturing process, molecules carrying a positive charge are chemically bonded to the filter matrix permanently forming an interconnected filtration structure with positively charged electrokinetic capture sites. The resulting porous depth filter is a tortuous network of charge-enhanced flow channels capable of removing bacteria, particulate, cellular debris and submicronic contaminants to a level which mechanical screening alone cannot achieve.

3M Purification has developed a chemically modified purifier that is capable of removing metallic or ionic contaminants from photoresists, resins, solvents, and ancillary chemicals while improving flow and throughput. This is accomplished by maximizing purification surface area, which reduces the potential for channeling and increases the contact time between the chemical and reactive sites of the purifier. This increase in purification surface area is achieved by using the Zeta Plus 40Q purifier cartridge metal ion removal media.

Superior Metals Removal Capacity Provided by Zeta Plus 40Q Puriﬁer Cartridge

Zeta Plus 40Q purifier cartridges contain multiple ion exchange groups that reduce trace metals such as Na, Fe, K, and Ca to single digit parts per billion levels in single pass or recirculation mode applications. Unlike competitive purifiers that only contain ion exchange technologies on the surface of the media, Zeta Plus 40Q purifier cartridges are able to purify ionic contaminants throughout the entire depth of the media. This design provides a more efficient means of purification per surface area while increasing flow and lifetime. Tables 1, 2, and 3 show the metal removal performance of Zeta Plus 40Q purifier cartridge in propylene glycol monomethyl ether acetate (PGMEA), propylene glycol monomethyl ether (PGME), and ethyl cellosolve acetate (ECA). Metals removal was quantified using a graphite furnace atomic absorption spectrometer.

Zeta Plus 40Q Puriﬁer Cartridge Extractables

The purifier’s clean materials of construction ensure that ionic, organic, and metallic contaminants are not being added back into the process chemical. Ionic, organic, and metallic contaminants can extract from other filter materials, which may change the photo-speed, viscosity, or molecular weight of the chemical. A static soak test was performed to determine the amount of contaminants extracted from the solvent PGMEA. After a 24-hour static soak, extractables were quantified using a graphite furnace atomic absorption spectrometer (Table 4).

Zeta Plus 40Q Puriﬁer Cartridge Puriﬁer Scale-Up

For laboratory and pilot scale testing, 3M Purification offers low hold-up volume Zeta Plus 40Q purifier disks (47mm, 90mm, 142mm) and housings to allow end users to assess parameters such as material compatibility, photo-speed, and trace metals removal in a rapid and cost effective manner. The compact size allows for easy replacement and installation of purification media while reducing the waste of expensive chemicals.

Zeta Plus 40Q purifier cartridge disks contain the same filter media as full size Zeta Plus 40Q purifier cartridges, ensuring repeatable and reliable performance throughout laboratory, pilot, and full production testing. This makes the scale-up process simple, linear, and predictable.

In full scale production, Zeta Plus 40Q purifier cartridge is offered in cartridge diameter sizes of 8”, 12”, and 16” providing up to 34.7 ft2 (3.2 m2) of surface area in a single cartridge. Zeta Plus Housings can vertically accommodate 1, 2, 3, or 4 Zeta Plus 40Q purifier cartridges, allowing the end user to tailor the filtration system to their required flow rate.

Zeta Plus 40Q Puriﬁer Cartridge Lifetime

The lifetime of the purifier will vary based on the ionic contamination loading in the fluid, the batch or bath size, and the desired metal effluent specification. As a result, the purifier should be sized based on the desired flow rate for the application. 3M Purifica-

tion recommends ≤0.25 gpm (0.95 lpm) flow rate per 1 ft2 (0.09 m2) of Zeta Plus 40Q purifier cartridge media for a 1cps fluid and ≤0.1 gpm (0.38 lpm) flow rate per 1 ft2

(0.09m2) of Zeta Plus 40Q purifier cartridge media for 10 to 100 cps fluids. For fluids

greater than 100 cps, consult the factory. Table 5 provides the recommended f low rate

for each Zeta Plus 40Q purifier cartridge available.

Zeta Plus® 40Q Puriﬁer Cartridges

Superior Removal of Trace Metals From High Purity Chemicals

Table 5: Recommended Flow Rate per Cartridge Configuration

Maximum Flow Rate for

Catalog Number

1 cps fluids

GPM LPM GPM LPM

Z8F (8” - 2 cell) 0.20 0.76 0.08 0.30

45167 (8” - 7 cell) 0.75 2.85 0.30 1.14

45109 (8” - 8 cell) 0.85 3.23 0.34 1.29

45244-01 (12” - 9 cell) 2.3 8.5 0.9 3.4

45237-01 (12” - 12 cell) 3.0 11.3 1.2 4.5

45245-01 (12” - 16 cell) 4.0 15.1 1.6 6.1

Z16P (16” - 14 cell) 9.3 35.0 3.7 14.0

Maximum Flow Rate for

10 to 100 cps fluids

Table 6: Product Specifications

Catalog Number

Z8F

(8” - 2 cell)

45167

(8” - 7 cell)

45109

(8” - 8 cell)

45244-01

(12” - 9 cell)

45237-01

(12” - 12 cell)

45245-01

(12” - 16 cell)

Z16P

(16” - 14 cell)

Maximum Operating Temperature 176°F (80°C)

Maximum Differential Pressure 35 psid @ 176°F (2.4 bar @ 80°C)

Nominal Diameter Height Media Surface Area

Inches mm Inches mm Ft

8 203 3

8 203 6

8 203 6 9/

12 273 7

12 273 10

16 406 10

88 0.7 0.065

168 2.5 0.23

166 2.8 0.26

192 9.2 0.90

273 12.3 1.1

273 16.4 1.5

273 34.7 3.2

Various O-ring/Gasket Materials

Polypropylene End Caps

Zeta Plus 40Q Media

Polypropylene Cell

Separator

Polypropylene Edge Seal

Polypropylene Center Post

Figure 1: Zeta Plus 40Q Purifier Cartridge Construction

Zeta Plus 40Q Puriﬁer Cartridge Ordering Guide

Zeta Plus Conﬁguration 2-123 O-Ring

Packaging Grade

Material

Z8F (8” - 2 Cell)

SOE Cartridge

A2NP

A - Silicone B - Fluorocarbon C - EPR D - Nitrile K - PTFE Encapsulated Fluorocarbon

2 40Q

Conﬁguration 2-123 O-Ring Material Grade

45167 (8” - 7 cell)

SOE Cartridge

01 - Nitrile 02 -EPR 03 - Fluorocarbon 04 - Silicon 09 - PTFE Encapsulated Fluorocarbon

Conﬁguration DOE Gasket Material Grade

45109 (8” - 8 cell)

DOE Cartridge

11 - Nitrile 13 - Fluorocarbon 14 - EPR 22 - Silicone 23 - PTFE

40Q

Zeta Plus 40Q Puriﬁer Disk Ordering Guide

47 mm Disk B0204-40Q

90 mm Disk B0406-40Q

142 mm Disk B0611-40Q

Conﬁguration DOE Gasket Material Grade

45244-01 (12” - 9 cell)

45237-01 (12” -12 cell)

45245-01 (12” - 16 cell)

Conﬁguration DOE Gasket Material Grade

Z16P (16” - 14 cell)

A - Silicone B - Fluorocarbon C - EPR D - Nitrile E - PTFE

40Q

Important Notice: The information described in this literature is accurate to the best of our knowledge. A variety of factors, however, can affect the performance of the Product(s) in a particular application, some of which are uniquely within your knowledge and control. INFORMATION IS SUPPLIED UPON THE CONDITION THAT THE PERSONS RECEIVING THE SAME WILL MAKE THEIR OWN DETERMINATION AS TO ITS SUITABILITY FOR THEIR USE. IN NO EVENT WILL 3M PURIFICATION INC. BE RESPONSIBLE FOR DAMAGES OF ANY NATURE WHATSOEVER RESULTING FROM THE USE OF OR RELIANCE UPON INFORMATION.

It is your responsibility to determine if additional testing or information is required and if this product is ﬁt for a particular purpose and suitable in your speciﬁc application.

3M PURIFICATION INC. MAKES NO REPRESENTATIONS OR WARRANTIES, EITHER EXPRESS OR IMPLIED INCLUDING WITHOUT LIMITATION ANY WARRANTIES OF MERCHANTABILITY, FITNESS FOR A PARTICULAR PURPOSE OR OF ANY OTHER NATURE HEREUNDER WITH RESPECT TO INFORMATION OR THE PRODUCT TO WHICH INFORMATION REFERS

Limitation of Liability: 3M Puriﬁcation Inc. will not be liable for any loss or damage arising from the use of the Product(s), whether direct, indirect, special, incidental, or consequential, regardless

of the legal theory asserted, including warranty, contract, negligence or strict liability. Some states do not allow the exclusion or limitation of incidental or consequential damages, so the above limitation may not apply to you.

Your Local 3M Puriﬁcation Distributor:

3M Puriﬁcation Inc.

400 Research Parkway Meriden, CT 06450 U.S.A. (800) 243-6894 (203) 237-5541 Fax (203) 630-4530 www.3Mpuriﬁcation.com

3M Zeta Plus 40Q User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual