Photoresist key substances-photoacid generator (PAG)-CAD Detector Application Note
trifluorobutyl sulfonate

1, Preface

Lithography is the integrated circuit (IC) is a key process in manufacturing, occupying the chip manufacturing process 40%–50% time course. In the photolithography process, not only a photolithography machine is needed, but also a key material - photoresist. Photoresist is one of the most critical materials in the semiconductor industry. In the entire integrated circuit manufacturing process, the photolithography process accounts for approximately 35% of the entire chip manufacturing cost, is the core process in semiconductor manufacturing.

Photoresist is a complex mixture, mainly composed of organic solvents, polymer resins,photoacid generator (PAG)(PAG), additive composition. Among them photoacid generator (PAG) It is a key component of photoresist and plays a decisive role in the sensitivity and resolution of photoresist.photoacid generator (PAG) The purity and impurity control have an important impact on the yield of photoresist and entire semiconductor products. photoacid generator (PAG) The common components are the cationic part of triphenylsulfide and the anionic part of polyfluorosulfonate, and the anionic part has basically no UV absorption.Charged Aerosol Detector (CAD) Does not rely on compounds to be optically active and can be used as a control photoacid generator (PAG) Ideal detector for quality.

This application should be based on trifluorobutyl sulfonate For example, explore CAD Yes photoacid generator (PAG) feasibility of quality control.

Charged Aerosol Detector (CAD)(charged aerosol detector,CAD) is a new general-purpose detector developed in recent years. Its detection has nothing to do with the molecular structure of the substance being measured, and the substance being measured does not need to be ionized. It can be used as long as the substance being measured is a semi-volatile or non-volatile compound.CAD detection. At the same time,CAD It is a mass-sensitive detector. The response value of the measured substance is determined by the absolute mass of the sample being tested. As long as the absolute mass of the sample being tested is consistent, the measured response value will basically be the same, and a lower detection limit and higher sensitivity can be obtained.

Charged Aerosol Detector (CAD) Yes INSTRUMAX The R&D team has achieved major scientific and technological achievements after years of painstaking research and repeated experiments. The detector uses advanced electricity and atomization technology to achieve high-sensitivity and high-precision detection of trace samples.

2, instruments and materials

Instruments:Agilent1200 liquid chromatograph+Charged Aerosol Detector (CAD)(INSTRUMAX, Model: CADetector a1)

Reagents: pure water (Watson's distilled water), acetonitrile (chromatography grade), formic acid (analytical grade)

Sample: triphenylsulfonium trifluorobutanesulfonate.

3, methods and results

3.1 Chromatographic conditions

Column: InfinityLab Poroshell 120 EC-C18 Column temperature:55℃

Flow rate:0.4mL/min Injection volume:5μL

Mobile phase A: 0.2%Formic acid aqueous solution mobile phase B: acetonitrile

Gradient elution

CAD Conditions:

Instrument model:INSTRUMAX CADetector a1

Drift tube temperature:40℃

Atomized air flow:3L/min

Polarization current:1μA

Polarized airflow:1L/min

3.2 Sample preparation

Thinner: methanol, methanol-water (1:1)

Preparation of triphenylsulfonium trifluorobutanesulfonate mother liquor 2000 µg/mL, dissolved in pure methanol solution.

Use methanol-water (1:1) The solution is diluted step by step to prepare the mother liquor with concentrations of 1,2,5,10,100 and 1000 µg/mL series of solutions.

3.3 Experimental results

3.3.1 Method applicability

Under the conditions of this method, the retention time of anions and cations is suitable, and the resolution, peak shape and peak response are all good.

3.3.2 method sensitivity

1 µg/mL sample, injection 5μL; Triphenyl sulfide responds well, with a signal-to-noise ratio of 1097.4(ASTM law);trifluorobutyl sulfonate Good response, signal-to-noise ratio 122.9(ASTM law)

3.3.3 Repeatability

continuous 6 Needle Repeatability, Triphenyl Sulfide Peak Area RSD% is 0.880;trifluorobutyl sulfonate Peak area RSD% is 1.222%, all less than 2.0%, indicating that the method has good repeatability.

3.3.4 Linear

1~1000 µg/mL concentration, the triphenyl sulfide correlation coefficient R is 0.99995;trifluorobutyl sulfonate The correlation coefficient R is 0.99976, good linearity and wide linear range.

4, experimental conclusion

This article adopts HPLC-CAD method pair photoacid generator (PAG) Analyze the anions in the sample. This solution has high sensitivity, good ion separation and repeatability, and wide linear range. It can be used as photoacid generator (PAG) evaluation method.

HPLC-CAD The method is simple to operate, highly specific and highly sensitive, and can be used as photoacid generator (PAG) Quality control and method evaluation.