Measuring the Particle Retention of Liquid Filters below 100 Nanometers

UF even withstands episodic increase of particle numbers in the feed (e.g., caused by conditioning of ion-exchange resins) without negative effects for water quality and service lifetime. Such a particle challenge typically involves high concentrations of ~10-nanometer (nm) particles. On the other hand, current on-line particle counters approach their lower detection limit at about 10nm. Large numbers of particles nearby and below this limit remain undetected. Hence, the integrity of a UF membrane is essential to keep these small particles under control; it can hardly be evaluated by comparing particle counts upstream and downstream. Therefore, better test methods are needed to identify membrane damages, and to decide on service life and replacement of UF membranes.

This presentation was given as part of the Ultrapure Micro 2021 annual conference. It was given as part of the ultrapure water strand.

This presentation was given as part of the Ultrapure Micro 2021 annual conference. It was given as part of the ultra high purity chemicals strand.

This presentation was given as part of the Ultrapure Micro 2021 annual conference. It was given as part of the ultrapure water strand.

The complexity of integrated circuit (IC) manufacturing for advanced nodes, paired with the growing demand for higher yields and lower defectivity, requires close alignment among industry stakeholders. New systematic improvements of system design, material choice and quality assurance methodologies are needed to minimise every possible source of contamination and variation in the manufacturing process. An extensive collaborative effort between SEMI Standards Task Forces and IRDS roadmap teams, representing the IC manufacturing supply chain, is focused on developing industry best practices to enable proactive yield management. As a result, relevant SEMI Standards are being revised to focus on the quality of UPW and liquid chemicals, design and operation of related systems, qualification of polymer assemblies and process critical materials and components. This article was originally published in the Ultrapure Micro Journal in March 2019.

Ultrapure water (UPW) is one of the main materials for electronics fabrication and therefore, it needs to be monitored for critical parameters such as nanoparticles (NP). The state-of-the-art online measurement techniques are challenged by particles at the killer particle sizes smaller than 10 nm. Due to the uncertainties in NP detection, the identification of NP sources and sinks in UPW system is limited nowadays. This review article aims to give an overview on the current developments and perspectives in metrologies for detection and control. The following topics will be discussed: transferability of general definition of NP to UPW, state-of-the-art particle analytics, sources and sinks of NP in UPW systems as well as dominant particle interactions responsible for NP contamination. This article was originally published in the Ultrapure Micro Journal in November 2017.

This article provides an overview of the biggest challenge of UPW technology – particle control. The latest semiconductor technologies require near particle-free water, where the “killer” particle size is far below the size that UPW metrology can effectively detect. Also, current advanced treatment methods cannot guarantee reliable removal of killer-sized particles. The quality of the high-purity materials used downstream of the final filters has not typically been tested for shedding of the “killer” particles. Consequently, the semiconductor industry requires a comprehensive approach for the particle control. A new approach should include mitigating particle occurrence and continuously improving the technologies used in UPW polish and distribution systems. Such an approach should also include extensive use of SEMI standards to improve the quality of the materials used; a new way to engineer solutions related to system-configuration and system design; improved process control; and a careful review of critical operational decisions. Collaboration throughout the industry via IRDS and SEMI Standards is key to enabling such systematic improvement, and overcoming the metrology and other constraints. This article was originally published in the Ultrapure Micro Journal in November 2017.

Particles in ultrapure water (UPW), used during the manufacture of microcircuits on semiconductor wafers, can deposit onto the wafer surface thereby causing decreased yield and reliability of the microcircuits. As microcircuit future sizes continue to decrease, understanding the ability of a filter to capture and retain these particles becomes increasingly important and challenging. In 2013, SEMI C79-0113, “Guide to Evaluate the Efficacy of Sub-15 nm Filters used in Ultrapure Water (UPW) Distribution System” was published. This document provides a SEMI recommended method for evaluating the efficacy of filter elements used to remove particles in UPW fluid streams. Since the release of this guide, the method has been enhanced to allow quantification of particle retention over a broad size range. This was accomplished by adding larger silica particles to the Ludox® SM30 silica specified by SEMI C79 resulting in a poly-dispersed silica challenge. A particle size distribution (PSD) slope of -2 (log-log) was selected so the challenge would more closely mimic a PSD typically found in UPW, yet still have sufficient large particles to measure a log retention value of 2 or 99% retention. This silica challenge has been designated as an “area-weighted challenge”. The use of this enhanced method has resulted in some interesting observations including indication of a most penetrating particle size similar to what is observed in gas filtration. The presence of a most penetrating particle size would indicate that retention mechanisms other than sieving are active, particularly for particles smaller than 30 nm. This paper will review the enhancements made to the test method, review the retention data from a number of filter types and manufacturers, and discuss the implications for filters used in UPW. This article was originally published in the Ultrapure Micro Journal in November 2017.

This article deliberates how it has become possible to test any microfine filter in real time, and in its actual conditions of use. For such testing to be possible it is vital to be able to obtain two particle-counting instruments matched for particle detection over a range of particle sizes. This attribute of matched detection appears to be possible with the acoustic method of detecting particles, and not commonly available with optical particle counters. This article was originally published in the Ultrapure Micro Journal in November 2017.

Nanoparticle contamination of ultrapure water (UPW) for microelectronics fabrication is expected to significantly decrease the yield and reliability of semiconductor devices. Tight nanoparticles control poses a technical and analytical challenge, especially in the particle size range down to a few nanometres. Most state-of-the-art online particle counters do not address the needs of advanced microelectronics manufacturing with critical particle sizes below 20 nm. Therefore, understanding of sources of nanoparticle contamination and strategies for control is limited. This study aims to profile nanoparticles ≥10 nm in a full-scale UPW polishing system after each process step using two novel particle measurement systems: an optical particle counter and an acoustic particle counter. For the first time, the performance of a whole UPW polishing system, including a Reverse Osmosis (RO) unit in terms of particle rejection, was investigated. Both particle counter instruments were evaluated with positive results. A statistical analysis was carried out to compare the significance of the particle counts achieved by the two different detection principles. Profiling throughout the UPW polishing system revealed that both instruments measure particle concentrations in the same range. The data is consistent and shows a clear trend: ion exchange mixed bed, Reverse Osmosis (RO) and ultrafiltration remove particles and represent sinks for nanoparticles ≥20 nm. The removal of nanoparticles between 10 nm and 20 nm is limited in this case however, especially for the final ultrafiltration. Scanning electron microscopy (SEM) with elemental analysis demonstrated that the particle chemistry was diverse. This indicates that different particle chemistries and particle properties might have influenced the particle counts. The results contribute to the advanced understanding of nanoparticle behaviour in UPW and provides more confidence in terms of monitoring at the lower particle range. This article was originally published in the Ultrapure Micro Journal in March 2019.