Cleanliness Validation of Parts & Sub-Assemblies

Transcription

1 Cleanliness Validation of Parts & Sub-Assemblies Pieter de Bokx Philips Innovation Services MiPlaza TMA bbb

2 Contents Introduction Philips Innovation Services & MiPlaza Cleanliness Validation for Gaseous Environments Cleanliness Validation for Aqueous Environments Cleanliness Validation for Vacuum Environments

3 We live in a world where technology increasingly touches every aspect of our daily lives and where innovation is to bring new sustainable solutions to formidable challenges. MiPlaza s mission is to help our customers to unleash their full innovation potential.

4 We are committed to Open Innovation Customer benefits: Leverage complementary technology Co-create opportunities Share cost and risk Accelerate time-to-market

5 MiPlaza (part of Philips Innovation Services) MiPlaza is an R&D Shared Service Center providing access to High Tech Campus infrastructure and generic expertise to several hundred valued customers.

6 Thin Film Clean room Electronic Measurement Lab Device Processing Facilities Electronic Prototyping Systems Engineering Photonics Facility Measurement & instrumentation Materials Analysis Life Science facility Experience lab Reliability lab With 14,000 m 2 of facilities and 400 specialists MiPlaza is (one of) the largest commercial facilities in Europe. MiPlaza is located at the High Tech Campus Eindhoven, a Technology Hotspot with: 90 companies 50 nationalities 8,000 residents and growing

7 MiPlaza Materials Analysis Expertise broad spectrum of analytical techniques and product knowledge actively involved in R&D, manufacturing and troubleshooting solution oriented, together with customers Analysis areas chemical analysis process analysis molecular analysis surface analysis

8 The MiPlaza Value Network Lead innovator customers and suppliers Global companies Small medium enterprises & High tech start-ups Universities & Research institutes Tech Suppliers

9 Cleanliness Validation for Gaseous Environments bbb

10 Why Cleanliness Validation Control of contamination in advanced semiconductor processing is critical Out-gassed (or leached) contaminants can adversely affect many processes resulting in yield loss, shortened tool life and reduced long-term device reliability Requirements on permissible contamination levels are very strict

11 Chemical Background 1/1,000 mm Thermal and photo-chemical decomposition of adsorbed contaminant species solid deposition and diffusion Shorter wavelengths (1980 s: 365nm; 2007/8: EUV: 13.5nm) more photo-chemical pathways

12 Contamination Control A.Definition phase: level of cleanliness required with respect to total organic contamination (TOC), is defined by end-user. Resulting specifications for each individual sub-assembly of the end-product are described in product specification sheets B.Realization phase: sub-assemblies are built and cleaned by customer according to the specification sheets C.Validation phase: before shipping the cleaned sub-assemblies to end-user for installation in end-product, a test is required to determine if the actual level of contamination is within specifications

13 Definitions Total Organic Contamination (TOC) is total carbon in organic compounds a.k.a. C x H y. Methane specified separately. TOC is subdivided in TOC nv and TOC v. TOC nv are non-volatile (condensable) organic compounds: boiling point >150 C or a molecular weight >120 g/mole. TOC v indicates the complementary fraction: a boiling point < 150 C and a molecular weight <120 g/mole.

14 Definitions Especially deleterious are so-called refractories, organics containing: Sulphur (S) Phosphorus (P) Boron (B) Silicon (Si) Chlorine (Cl) Iodine (I) Bromine (Br) Any metal atom

15 Concentration Ranges

16 Typical Specifications TARGET SPECIES De-gassing rate (pmole/min) Gas phase concentration TOC v 1 0.5ppb TOC nv ppt refractories ppt

17 Validation: Where? Sampling and measurement in Class 1,000 (Federal Standard 209 E) clean room Equipped with additional charcoal filters to ensure low-environmental TOC High quality gas % (N2 5.5N) available

18 Validation: How? Method recommended is based on several NIOSH, OSHA and EPA standard methods Flush unit with very clean N 2 -gas flow over a Tenax absorption tube TOC s from unit are trapped on Tenax mass flow controller pure nitrogen gas handling device flow meter tenax tube

19 Sampling Device Mark III

20 Analysis of Process Gas Detection limit of method defined as: 3σ 0 LoD s with σ 0 the standard deviation of the blank and S the sensitivity Figure of Merit NH 3 SO 2 Sensitivity (ng/pptv) LoD (ppqv) (24h sampling at 30l/min)

21 Validation: How? Gas phase concentrations too low for direct measurement Solution: pre-concentration Tenax (2,6-diphenylene oxide polymer): thermally stable ( max. 350 o C) high affinity for C 5 and higher low affinity for C 2 -C 5 Glass tube Tenax Sample gas

22 Validation: How? Place Tenax tube in TCT Heat Tenax to 200 C under helium. TOC s are desorbed and trapped on a C trap. Injection on analytical column by heating cold trap to 200 C within 1 minute helium tenax tube thermal desorption Fast injection; little peak gas chromatograph broadening Separation of components on analytical column Detection: FID, MS or AED (Atomic Emission Detector) detector

23 Thermal Desorption - Cold Trap Injection (TCT) Tenax tube 200 C Detector Trap 125 C Analytical column

24 Validation: How? Chromatogram: detector signal as function of time Time (Min.) Every peak is a different organic compound Retention time typical for compound: measure of volatility Peak area is a measure of amount

25 Peak area Validation: Calibration Load Tenax tube with known amount of toluene Analyze in same way as samples Calibration factor: slope of calibration plot Calibration FID (Ultra trace GC) with Toluene Date E+06 3.E+06 3.E+06 2.E+06 y = 2E+06x E+06 1.E+06 5.E+05 0.E Nanogram toluene per Tenax-tube

26 Validation: Quantification Add peak areas involved, e.g., all peaks with RT>14 min. for TOC nv Correct for sample blank (mainly Tenax) Apply calibration factor Compare with spec Approve or reject

27 Detector respons FID (mv) Unit Contaminated with Loctite Adhesive Result: > 120 pmol/min Time (min)

28 Detector respons FID (mv) Contaminated Teflon Tubing 200 Result: 15 pmole/min Time (min)

29 GC-Atomic Emission Detector

30 Selective Detection of C, S and Si Si S C

31 Cleanliness Validation for Aqueous Environments bbb

32 Emission to Aqueous Phase (Leaching) TOCw measurements. High flow rates up to 10 l/min. Specifications < 0.2 (ng/l) contribution

33 Total Inorganic / Organic Carbon in Water (TIC / TOC) Sievers 900 Portable Sievers 500RL On-line

34 Determination of TOC in Water Inject sample Add acid Add oxidant Split sample Destruct organics by oxidation Measure CO 2 using membrane conductivity TOC=TC-TIC Typical TOC detection limit: 0.06ppb

35 Leaching of Metals (ICP-MS) excitation ionisation Me + recombination ICP-MS Me Me Me Me Me free atoms Excited state 2 Excited state 1 λ 3 λ 2 dissociation MeCl MeCl MeCl MeCl molecules λ 1 vaporize Ground state salt particles desolvating ca. 1 % to plasma / flame sample / solution nebulizer aerosol drops 1-10 µm

36 ICP-MS

37 Typical Limits of Detection ICP-AES and ICP-MS Element ICP-AES (ppb) ICP-MS (ppb) Li Be B Al Cr Mn Co Cu Zn Se 75 4 Sr Mo Ba Tl Pb

38 Cleanliness Validation for Vacuum Environments bbb

39 Typical Specifications TARGET SPECIES TOC v Maximum out-gassing in mbarl/s TOC nv S-compounds P-compounds Si-compounds

40 Emission to Vacuum Environment Cleanliness validation of parts for EUV currently done using Residual Gas Analysis (RGA), a mass-spectrometric technique Drawbacks: RGA does not involve sample pre-concentration. Specifications difficult to attain. RGA does not allow elemental discrimination necessary to determine out-gassing rates of compounds containing refractories

41 New Developments

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