Background Statement for SEMI Draft Document 4795 (Yellow Ballot) NEW STANDARD: SPECIFICATIONS FOR NITRIC ACID, USED IN PHOTOVOLTAIC APPLICATIONS

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1 Background Statement for SEMI Draft Document 4795 (Yellow Ballot) NEW STANDARD: SPECIFICATIONS FOR NITRIC ACID, USED IN PHOTOVOLTAIC APPLICATIONS Note: This background statement is not part of the balloted item. It is provided solely to assist the recipient in reaching an informed decision based on the rationale of the activity that preceded the creation of this document. Note: Recipients of this document are invited to submit, with their comments, notification of any relevant patented technology or copyrighted items of which they are aware and to provide supporting documentation. In this context, patented technology is defined as technology for which a patent has been issued or a patent application has been submitted. In the latter case, only publicly available information on the contents of the patent application is to be provided. Background The rapidly expanding PhotoVoltaic industry, in most cases, needs a different set of gas and chemical standards than existing semiconductor documents offer. Therefore the PV Gas and Liquid Chemical Purity TaskForce was formed to begin developing those needed standards. The ultimate intent being to: 1) Remove the ambiguity in what is being produced and provided... the customer gets what is truly needed and the supplier knows what to produce. 2) Provide a level playing field by preventing low bid possibilities where suppliers might meet the nomenclatural intent of the material but not the actual customer's need. 3) Avoid customer/supplier discussions about rejected material not performing as expected. 4) Give the end-user the ability to improve the process by adjusting the level of needed purity if deemed advantageous. Note: 1) This document refers to an as supplied product; not point of use. The results of this ballot will be reviewed by PV Gas and Liquid Chemicals Purity TF and adjudicated by NA PV Committee during their meetings at NA Spring Standards Meetings, March 29-30, 2011 at SEMI HQ in San Jose, CA. Please check for the latest update. If you have any questions on this ballot, please contact Marty Burkhart at martyburkhart@hipuretech.com or Tom Hackett at THackett@kmgchemicals.com or SEMI Staff, Kevin Nguyen at knguyen@semi.org.

2 SEMI Draft Document 4795 NEW STANDARD: SPECIFICATIONS FOR NITRIC ACID, USED IN PHOTOVOLTAIC APPLICATIONS 1 Purpose 1.1 This document standardizes requirements for nitric acid used in the photovoltaic industry and testing procedures to support those standards. Test methods have been shown to give statistically valid results. 2 Scope 2.1 The scope of this document is grades of nitric acid used in the photovoltaic industry. NOTICE: SEMI standards and Safety Guidelines do not purport to address all safety issues associated with their use. It is the responsibility of the user of this document to establish appropriate safety and health guides and determine the applicability of regulatory or other limitations prior to use. 3 Limitations 3.1 None 4 Referenced Standards and Documents 4.1 SEMI Standards SEMI C1 Guide for the Analysis of Liquid Chemicals SEMI C35 Specifications and Guideline for Nitric Acid 4.2 ASTM Standard 1 ASTM D5127 Standard Guide for Ultra Pure Water Used in the Electronics and Semiconductor Industry NOTICE: Unless otherwise indicated, all documents cited shall be the latest published versions. 5 Terminology 5.1 None 6 Properties of Nitric Acid Table 1 Properties of Nitric Acid (for information only) Chemical Formula HNO 3 CAS No Density at 25 C 1.42 g/ml Assay 65.0% 70.0% 7 Requirements 7.1 The requirements for nitric acid for PV Grades 1 and 2 are listed in Table 2. 1 American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, Pennsylvania , USA. Telephone: ; Fax: ; Page 1 Doc SEMI

3 Table 2 Impurity Limits and Other Requirements for Nitric Acid PV Grade 1 PV Grade 2 (Specifications) (Specification) Assay (HNO 3 ) 65% % 70.0% 69.0% % 70.0% Color (APHA) 10 max 10 max. Chloride (Cl) 500 ppb max. 80 ppb max Phosphate (PO 4 ) ppb max Sulfate (SO 4 ) 1000 ppb max. 500 ppb max Aluminum (Al) 50 ppb max 5 ppb max Antimony (Sb) 50 ppb max. 10 ppb max Arsenic (As) 50 ppb max. 10 ppb max Barium (Ba) ppb max Boron (B) 50 ppb max. 10 ppb max Cadmium (Cd) 10 ppb max 5 ppb max Calcium (Ca) 100 ppb max 10 ppb max Chromium (Cr) 50 ppb max 10 ppb max Copper (Cu) 20 ppb max 10 ppb max Iron (Fe) 300 ppb max 5 ppb max Lead (Pb) 50 ppb max 10 ppb max Lithium (Li) -- 5 ppb max Magnesium (Mg) 100 ppb max 10 ppb max Manganese (Mn) 100 ppb max 10 ppb max Nickel (Ni) 50 ppb max 10 ppb max Potassium (K) 100 ppb max 5 ppb max Sodium (Na) 300 ppb max 5 ppb max Tin (Sn) 50 ppb max 10 ppb max Titanium (Ti) 100 ppb max 10 ppb max Vanadium (V) ppb max Zinc (Zn) 50 ppb max 10 ppb max 8 PV Grade 1 Procedures NOTE 1: Each laboratory is responsible for verifying the validity of the method within its own operation. 8.1 Assay Accurately weigh a small glass-stoppered conical flask containing about 15 ml of water. Deliver from a pipet about 2 ml of the sample near the water surface, stopper immediately, cool, and reweigh. Dilute to about 50 ml with water, add 0.10 ml of methyl orange indicator solution, and titrate with standardized 1 N sodium hydroxide to a red to yellow color change. 8.2 Color Dilute 2.0 ml of platinum-cobalt stock solution (APHA No. 500, see SEMI C1) to 100 ml with water. Compare this standard (APHA No. 10) with 100 ml of sample in Nessler tubes. View vertically over a white background. The sample must be no darker than the standard. 8.3 Chloride Dilute 17 ml (24 g) of sample with 10 ml of water, add 1 ml of silver nitrate reagent solution [see SEMI C1], and evaporate to dryness on a steam bath in a hood. Dissolve the residue in 0.5 ml of ammonium (1) Page 2 Doc SEMI

4 hydroxide, dilute with 20 ml of water, and add 1.5 ml of nitric acid. Any turbidity produced should be no greater than that produced when 0.01 mg of chloride ion is treated as the sample. 8.4 Sulfate To 35 ml (50 g) of sample add 10 ml of sodium carbonate reagent solution [see SEMI Cl] and evaporate to dryness in a hood. Dissolve the residue in 10 ml of water and 1 ml of dilute hydrochloric acid (1 + 19); filter if necessary. Add 1 ml of barium chloride reagent solution [see SEMI Cl], mix, and allow to stand for 10 minutes. Any turbidity developed should be no greater than that produced when 0.05 mg of sulfate ion (SO 4 ) is treated as the sample. 8.5 Trace Metals Analysis The following method has given satisfactory results in determining metal ion impurities at the values specified for each of the following metals: aluminum (Al), antimony (Sb), arsenic (As), boron (B), cadmium (Cd), calcium (Ca), chromium (Cr), copper (Cu), iron (Fe), lead (Pb), magnesium (Mg), manganese (Mn), nickel (Ni), potassium (K), sodium (Na), tin (Sn), titanium (Ti), and zinc (Zn). Alternative methods may be used as long as appropriate method validation as per SEMI C1 has been demonstrated Special Reagents Nitric Acid, Ultra Pure Use nitric acid equivalent or better than SEMI Grade 3 (see SEMI C35) % Nitric Acid Solution Dilute 20 g of ultrapure nitric acid to 200 g using water meeting the criteria for Type E1.1 in ASTM D Water The water used for all the dilution, calibration and standards should meet at a minimum the criteria for Type E1.1 in ASTM D5127 in regard to cation analysis Indium Internal Standard Make up an indium internal standard solution to a concentration of 20 μg/ml (ppm) from a appropriate concentrated indium standard solution Sample Preparation In a clean environment, place 2.00 g of sample into a tared FEP bottle (30 ml), dilute with Type E1.1 water to a final weight of 20.0 g. Add 20 μl of the indium internal standard solution. Run a reagent blank Analysis Using the prepared solutions and blanks, analyze sodium, potassium, calcium and iron by graphite furnace atomic absorption (GFAA) and the remaining elements by inductively coupled plasma mass spectrometry (ICP/MS). For calibration, the standards are made up with the 7.0 % nitric acid solution and the indium internal standard such that the final concentration is 20 ng/g of indium. 9 PV Grade 2 Procedures NOTE 2: Each laboratory is responsible for verifying the validity of the method within its own operation. 9.1 Assay See Color See Chloride Dilute 84 ml (120 g) of sample with 10 ml of water, add 1 ml of silver nitrate reagent solution [SEMI C1], and evaporate to dryness on a steam bath in a hood. Dissolve the residue in 0.5 ml of ammonium hydroxide, dilute with 20 ml of water, and add 1.5 ml of nitric acid. Any turbidity produced should be no greater than that produced when 0.01 mg of chloride ion is treated as the sample. 9.4 Phosphate To 35 ml (50 g) of sample add 10 ml of sodium carbonate reagent solution [SEMI C1] and evaporate to dryness on a steam bath in a hood. Dissolve the residue in 25 ml of 0.5 N sulfuric acid. Add 1 ml of ammonium molybdate reagent solution [SEMI C1] and 1 ml of p-(methylamino)phenol sulfate reagent solution [SEMI C1]. Allow to stand at room temperature for 2 hours. Any blue color produced should be no greater than that produced when 0.01 mg of phosphate ion (PO 4 ) is treated as the sample. 9.5 Sulfate To 70 ml (100 g) of sample add 10 ml of sodium carbonate reagent solution [SEMI C1] and evaporate to dryness in a hood. Dissolve the residue in 10 ml of water and 1 ml of dilute hydrochloric acid (1 + 19); filter if necessary. Add 1 ml of barium chloride reagent solution [SEMI C1], mix, and allow to stand for 10 Page 3 Doc SEMI

5 minutes. Any turbidity developed should be no greater than that produced when 0.05 mg of sulfate ion (SO 4 ) is treated as the sample. 9.6 Trace Metals Analysis The following method has given satisfactory results in determining metal ion impurities at the values specified for each of the following metals: aluminum (Al), antimony (Sb), arsenic (As), barium (Ba), boron (B), cadmium (Cd), calcium (Ca), chromium (Cr), copper (Cu), iron (Fe), lead (Pb), lithium (Li), magnesium (Mg), manganese (Mn), nickel (Ni), potassium (K), sodium (Na), tin (Sn), titanium (Ti), vanadium (V), and zinc (Zn). Alternative methods may be used as long as appropriate method validation as per SEMI C1 has been demonstrated Special Reagents Nitric Acid, Ultra Pure Use nitric acid equivalent or better than SEMI Grade 3 (see SEMI C35) % Nitric Acid Solution Dilute 20 g of ultrapure nitric acid to 200 g using water meeting the criteria for Type E1.1 in ASTM D Water The water used for all the dilution, calibration and standards should meet at a minimum the criteria for Type E1.1 in ASTM D5127 in regard to cation analysis Indium Internal Standard Make up an indium internal standard solution to a concentration of 20 μg/ml (ppm) from a appropriate concentrated indium standard solution Sample Preparation In a clean environment, place 2.00 g of sample into a tared FEP bottle (30 ml), dilute with Type E1.1 water to a final weight of 20.0 g. Add 20 μl of the indium internal standard solution. Run a reagent blank Analysis Using the prepared solutions and blanks, analyze sodium, potassium, calcium and iron by graphite furnace atomic absorption (GFAA) and the remaining elements by inductively coupled plasma mass spectrometry (ICP/MS). For calibration, the standards are made up with the 7.0 % nitric acid solution and the indium internal standard such that the final concentration is 20 ng/g of indium. 10 PV Grade 3 Procedures 10.1 This section does not apply to this chemical. 11 PV Grade 4 Procedures 11.1 This section does not apply to this chemical. 12 PV Grade 5 Procedures 12.1 This section does not apply to this chemical. 13 PV Tier A Procedures 13.1 This section does not apply to this chemical. 14 PV Tier B Procedures 14.1 This section does not apply to this chemical. 15 PV Tier C Procedures 15.1 This section does not apply to this chemical. 16 PV Tier D Procedures 16.1 This section does not apply to this chemical. Page 4 Doc SEMI

6 NOTICE: SEMI makes no warranties or representations as to the suitability of the standards set forth herein for any particular application. The determination of the suitability of the standard is solely the responsibility of the user. Users are cautioned to refer to manufacturer's instructions, product labels, product data sheets, and other relevant literature, respecting any materials or equipment mentioned herein. These standards are subject to change without notice. By publication of this standard, Semiconductor Equipment and Materials International (SEMI) takes no position respecting the validity of any patent rights or copyrights asserted in connection with any items mentioned in this standard. Users of this standard are expressly advised that determination of any such patent rights or copyrights, and the risk of infringement of such rights are entirely their own responsibility. Page 5 Doc SEMI