Attachment 3 Ge Recycyling Specifications for Ingots.pdf

Attachment 3

Specifications for Germanium Ingots and Packaging of Germanium Ingots1

I. Description This specification establishes the requirements and tests for zone refined polycrystalline intrinsic germanium metal that can be used to produce optical grade germanium metal that can be fabricated into optical elements.

II. Requirements

A. The germanium metal must be zone refined and must be capable of being converted into optical grade germanium metal for use over the spectral range from 2.5 microns to 14 microns.

B. Unless otherwise specified, the germanium metal must meet the performance requirements at an ambient temperature of 19o to 26o C.

C. Each production lot must consist of homogeneous germanium metal.

Every ingot in every production lot will be inspected to determine compliance with the specification requirements. Any lot that fails to comply with any specification requirement will be rejected.

D. The optical transmission will be measured from 2.5 through 16 micron wavelength range.

E. The optical transmission will be measured through an uncoated 10±1 mm thick sample polished planes parallel. The recorded transmission values must equal the transmission values on the curve in Figure 1. A +2% transmission tolerance on the transmission value will be permitted.

Figure 1 - Transmission through 10mm Sample

1. In part, National Defense Stockpile Purchase Specification, published by Department of Commerce, approved by Federal Emergency Management Agency, Intrinsic Germanium Metal, P-114-R, Washington, D.C., 16 December, 1986.

F. The germanium metal must have an electrical resistivity with a minimum numerical value of 50 ohm - centimeter at 20+0.5 C (40 ohm-centimeter at 25+0.5 C) over the entire ingot-length.

G. The electrical conductivity type must be N-Type over the entire ingot length.

H. The germanium metal must be supplied in the form of a uniform trapezoidal ingot. The minimum length of the ingot must be 43 centimeters and the maximum length must be 56 centimeters. The minimum diagonal cross section of the ingot must be 25 millimeters and the maximum diagonal cross section must be 63.5 millimeters. The tail end (the end last to freeze) of the ingot must be cut perpendicular to the length-wise axis of the ingot.

I. The ingot must be free of holes, inclusions, cracks, and chips.

J. The ingot must be permanently marked in the middle of the top surface with the product name or chemical symbol, the ingot serial number, and the name of the producer. The producer name may be abbreviated.

K. After marking, the ingot must be chemically etched. The ingot must be clean and of uniform color and quality.

III. Inspection, Sampling, Testing The contractor must inspect every ingot for compliance with the dimensional requirements of the specification. The government reserves the right to sample each production lot of ingots and test each sample for compliance with specifications.

The contractor must use the following test methods for ingot testing.

A. The transmission of the spectrographic sample (a 10+1 millimeter thick spectrographic sample will be removed from each sample ingot) must be measured from 2.5 through 16 microns using an infrared spectrophotometer.

The instrument 0% and 100% (Io) lines must be recorded on the same graph as the sample transmission curve.

B. The electrical resistivity must be measured using SEMI MF43-0316 – Test Method for Resistivity of Semiconductor Materials. The contractor must measure the resistivity on the clean bottom surface over the entire length of each sample ingot at one-centimeter intervals. The contractor must report these measurements in the CoA along with the temperature at which they performed the resistivity measurements.

C. The contractor must measure the electrical conductivity of each sample ingot using SEMI MF42-0316 – Test Method for Conductivity Type of Extrinsic Semiconducting Materials. The contractor must measure the conductivity on the clean bottom surface over the entire length of each sample ingot at one-centimeter intervals. The Contractor must report these results in the CoA.

D. Each ingot in each lot will undergo a visual examination by the contractor to determine compliance with quality marking requirements.

E. The contractor must weigh each ingot of each lot, using a balance capable of weighing to at least the nearest gram. The contractor must weigh each ingot after it has been marked, etched, and after removal of spectrographic sample (if applicable), but before being placed in the polyethylene bag.

IV. Packaging and Marking

A. Each ingot must be individually wrapped in a new, clean, transparent polyethylene bag, which must be a minimum of 0.004 inch thick. The bag must be closed after heat sealing. After wrapping, the ingot must be packaged in a manner that will prevent damage to the ingot during shipment.

B. Each packaged ingot must be tightly packed in a new wooden box with sufficient protective material to prevent damage to the ingot during shipment and storage. The ingots, packing material, and box together must not exceed 25 kilograms.

C. The new wooden box with cleated ends must be equal to the requirements of ASTM D6880 – Standard Specifications for Wood Boxes, latest revision.

D. The contractor must affix durable tags/labels to the top and side of each wood box with the following information in English.

1. Material name

2. Material grade, type, or form

3. Country of origin

4. Producer name

5. Gross weight in pounds and kilograms. Kilograms must be in parentheses.

6. Net weight in pounds and kilograms. Kilograms must be in parentheses.

7. Lot number

8. Box serial number (S/N). The serial number is the individual box number out of the total number in the lot, e.g., “S/N 6 of 33”.

9. Government contract number

E. The contractor must secure the boxes of ingots to 48 inch by 48 inch pallets for loading, unloading, and transportation.

F. Identifying documents must accompany each box during shipment.

G. If the material is considered hazardous as defined by OSHA 29 CFR

1910.1200 and/or United Nations GHS, a label must be prepared and affixed to each drum in accordance with those requirements.

H. In accordance with the Hazard Communication Standard (HCS) (29 CFR 1910.1200(g)), the material safety data sheet must contain the chemical name and concentration or concentration range of all ingredients that are classified as health hazards and are present above their cut-off/concentration limits, or which present a health risk below the cut-off/concentration limits. The HCS and the material safety data sheet must be in English.

V. Palletizing Requirements:

A. Boxes must be placed onto new, undamaged pallets meeting the specifications listed below and be banded/shrink wrapped together to prevent box movement during handling, transportation, or other operations where boxes and/or personnel could be damaged and/or injured if the boxes shift. The contractor must not use recycled, repaired, used, remanufactured, and/or refurbished pallets.

B. A pallet, loaded with the boxes in which the Ge ingots are packaged, must not exceed the overall dimensions of a 48 inch cube.

C. Pallet design.

1. All pallets must be approximately 48 inches deep (front to back) and 48 inches wide (side to side) in size.

2. All pallets must contain four full length, solid stringers. One stringer must be located at each edge (side) and two stringers must be located in the interior of all pallets. Interior stringers must be spaced 18.5 inches (on center) from the outside of each edge (side). Stringers must be 1 5/8 inches in width and 3.5 inches in height. Segmented, composite, and/or clock stringers will not be acceptable.

3. All pallets must have flush sides (e.g., no wings).

4. All pallets must contain “top decking” and “bottom decking” boards.

Decking boards must be six inches in width for the lead boards and 3.5 inches in width for the interior boards. All decking boards must be ¾ inches in thickness and be solid.

5. All pallets must be of a “two way entry” configuration.

6. Pallets may be reversible in design.

7. All pallets must have a minimum rated load capacity of greater than 1,000 pounds per square foot.

D. Pallet construction.

1. All pallets must satisfy the requirements listed in ASTM D6199-18a

2. All pallets must be constructed entirely (except fasteners) of high density hardwood meeting the requirement of paragraph 6 of ASTM D6199-18a.

Only high density hardwood species categorized in “Group IV” of ASTM D6199-18a are acceptable for pallet construction. The only acceptable high density hardwood species used for pallet construction are beech, birch, hackberry, hard maple, hickory, oak (eastern), pecan, rock elm, American elm, white oak, and green oak. Pallets may be constructed by mixing together or using different high density hardwood species listed above interchangeably.

3. All pallets must satisfy the requirements listed in INSPM-15 (International Standards for Phytosanitary Measures Number 15) (e.g. heat treated etc.).

4. Only driven nails that are “helically” threaded, “annularly” threaded, or “fluted” will be acceptable for use in pallet construction. The fastener length must be sufficient to provide a minimum penetration of 1 1/4 inches into the stringer.