GB/T 21183-2017Zirconium and zirconium alloy sheet, strip and foil (English PDF)

3.1 Product Classification

3.1.1 Product nameplate, variety, supply status and specification

Product nameplate shall comply with the stipulations in Table 1. Product variety, supply status and specification shall comply with the stipulations in Table 2.

3.1.2 Product designation

Product designation shall be expressed in accordance with the sequence: product name, standard serial No., nameplate, supply status and specification. Please see designation examples as follows:

Example 1: Zr-0 manufactured, cold processing status of foil, thickness: 0.05 mm, width: 100 mm and length: L mm, shall be marked as: foil GB/T 21183-2017 Zr-0 Y 0.05 x 100 x L.

Example 2: Zr-2 manufactured, annealing status of strip, thickness: 1.0 mm, width: 100 mm and length: L mm, shall be marked as: strip GB/T 21183-2017 Zr-2 M 1.0 x 100 x L.

NOTE: when the demand-side indicates in the contract (or order sheet), stress-relieving annealing status (m) of products may be provided.

Example 3: Zr-4 manufactured, thermal processing status of sheet, thickness: 10 mm, width: 600 mm and length: L mm, shall be marked as: sheet GB/T 21183-2017 Zr-4 R 10.0 x 600 x L.

3.2 Chemical Composition

Product's chemical composition shall comply with the requirements in GB/T 26314.

3.3 Dimensions and Allowable Deviation

3.3.1 Dimensions and allowable deviation for sheet, strip and foil are shown in Table 3, Table 4 and Table 5, or, they shall be negotiated and determined by the demand-side and the supply-side.

NOTE 2: length allowable deviation is merely applicable to sheet, strip and foil products which are delivered in slices. Strip and foil products which are delivered in coils shall implement requirements in the contract (or order sheet).

3.3.2 Sheet and strip products shall be flat and straight. After the shearing, finished products' side curvature shall be not more than 3 mm/m. Foil products which are under annealing status allow to have slight waves.

3.3.3 Unevenness of products delivered in slices shall comply with the stipulations in Table 6.

3.3.4 Through shearing, the edges of sheet, strip and foil products shall be evenly trimmed. There shall be no cracks, edge curls or stratification. It is allowed to have slight burrs. Foil products may be delivered in the untrimmed status. All angles of sheet products shall be sheared into right angle.

3.4 Mechanical Properties

Mechanical properties of sheet and strip products shall comply with the stipulations in Table 7. The requirements of mechanical properties for foil products; sheet products whose thickness is more than 10 mm; products in other delivery status shall be negotiated and determined by the demand-side and the supply-side.

3.5 Corrosion Performance

Sheet and strip products for the purposes of nuclear industry shall receive corrosion performance test. Place sample at (400 ± 3) °C, (10.3 ± 0.7) MPa water vapor; conduct 72-h or 336-h of corrosion. After the corrosion test, the surface of the sample shall have a black and compact oxide film with uniform gloss. After 72-h of corrosion, the weight gain of the sample shall be not more than 22 mg/dm². When the 72-h test result is unqualified, a corrosion test with 336-h of accumulative time (or re-take a double size of the sample) may be continued; the weight gain of the sample shall be not more than 38 mg/dm².

3.6 Ultrasonic Examination

Sheet products for the purposes of nuclear industry shall receive ultrasonic examination. Requirements of the acceptance check shall be negotiated and determined by the demand-side and the supply-side.

3.7 Grain Size

In terms of recrystallized and annealed status of sheet and strip products for the purposes of nuclear industry, thickness not more than 4.8 mm, the average grain size shall be not lower than Level-7, which is stipulated in GB/T 6394. The grain size of other products shall be negotiated by the demand-side and the supply-side, and indicated in the contract.

3.8 Appearance Quality

3.8.1 The surface of products shall be smooth and clean. There shall be no macroscopic defects, such as oil stains, oxidization, acid spots, contamination, cracks, peeling, folding, metallic or non-metallic pressing.

3.8.2 The surface roughness Ra of sheet products shall be not more than 3.2 µm. The surface roughness Ra of strip and foil products shall be not more than 1.25 µm.

3.8.3 Products shall not have stratification or inclusion.

3.8.4 The surface of foil products shall be flat and smooth; slight waves may be allowed. However, when foil products are coiled on a coiling block whose diameter is 50 mm ~ 60 mm, the waves shall be able to be eliminated.

4.1 Chemical Composition

Products' chemical composition analysis shall comply with the stipulations in GB/T 13747, or methods negotiated and determined by the demand-side and the supply-side.

4.2 Dimensions and Allowable Deviation

The inspection of dimensions and allowable deviation shall be conducted through a measuring instrument of corresponding precision. Thickness shall be measured at a distance of not less than 9.5 mm from the edges of the product.

4.3 Mechanical Properties

4.3.1 Room-temperature tensile test shall be conducted in accordance with GB/T 228.1-2010. In terms of products whose thickness is 0.1 mm ~ < 3 mm, take P5 sample; in terms of products whose thickness is 3 mm ~ 10 mm, take P12 sample; in terms of products whose thickness is over 10 mm, take R7 sample.

4.3.2 High-temperature tensile test shall be conducted in accordance with GB/T 228.2.

4.4 Corrosion Performance

The inspection of corrosion performance shall be conducted in accordance with Appendix A.

4.5 Ultrasonic Examination

The method for ultrasonic examination shall be negotiated and determined by the demand-side and the supply-side.

4.6 Grain Size

The rating of grain size shall comply with GB/T 6394.

4.7 Appearance Quality

The inspection of surface roughness shall be conducted in accordance with the requirements in GB/T 10610. Other items shall receive visual inspection.

5.1 Inspection and Acceptance Check

5.1.1 Products shall be inspected by the supply-side, which shall guarantee that product quality complies with the stipulations in this Standard or the contract (or order sheet). In addition, a product quality certificate shall be filled out.

5.1.2 The demand-side shall inspect the received products in accordance with the stipulations in this Standard. When the inspection result does not comply with the stipulations in this Standard, the demand-side shall propose this to the supply-side within 3 months since the date of receiving the products. This shall be solved by the demand-side and the supply-side through negotiation. If arbitration is needed, arbitration sampling shall be jointly conducted by the demand-side and the supply-side.

5.2 Group Batch

Products shall be submitted for acceptance check in batches. Each batch shall be constituted of products of the same nameplate, the same furnace No., the same specification, the same manufacturing method, the same status and the same thermal processing furnace (batch).

5.3 Inspection Items and Sampling

Requirements towards inspection items and sampling are shown in Table 8.

In terms of nitrogen, hydrogen and oxygen content, take 1 sample from finished products. In terms of other elements, the supply-side may submit in the original ingot analysis result. The demand-side shall take samples from finished products.

5.4 Determination of Inspection Result

5.4.1 When chemical composition is unqualified, re-take a double size of sample from this batch of products for a re-inspection. If the re-inspection result still shows that some elements are unqualified, then, this batch of products shall be determined as unqualified.

5.4.2 When dimensions and allowable deviation, or appearance quality are unqualified, then, the individual PCS (coil) shall be determined as unqualified.

5.4.3 In mechanical properties, corrosion performance and grain size test, if the inspection result is unqualified, then, re-take a double size of sample from this batch of products (including the previous products being inspected) for a re-inspection of the unqualified items. If the re-inspection result is still unqualified, then, this batch of products shall be determined as unqualified.

5.4.4 When the ultrasonic examination result is unqualified, then, the individual PCS of product shall be determined as unqualified.

6.1 Product Marking

6.1.1 Each batch of qualified products shall have a label or a sign, which indicates: product nameplate, specification, status, batch No. and quantity.

6.1.2 In terms of strip and foil products, an identical sign shall be put onto the external side of the marking. In terms of sheet products, a sign shall be put onto individual PCS on a single side or both sides.

6.2 Packaging, Transportation and Storage

6.2.1 Each sheet product shall be separated from each other through a soft paper, then, be packed in boxes.

6.2.2 Strip product needs to be properly wrapped with moisture-proof paper, then, placed in a dry box. Use filling materials to stuff the gap among the coils, so as to prevent the products from moving backward and forward.

6.2.3 A mandrel shall be added to foil products which are delivered in coils; use plastic cloth and plastic bag to tightly pack them, then, pack them in boxes.

6.2.4 The boxes shall be lined with moisture-proof paper; on the external side of the boxes, characters or signs like "keep away from moisture" and "handle with care" shall be indicated.

6.2.5 In transportation and storage, collision, moisture and corrosion of active chemicals shall be prevented.

6.3 Quality Certificate

Each batch of products shall be attached with a quality certificate, which indicates:

a) The supply-side's name;

b) Product name, nameplate, specification and status;

c) Product batch No. (or furnace No.), batch weight and quantity;

d) Analysis and test result; inspection department's stamp;

e) Serial No. of this Standard;

f) Date of packaging.

A.1 Terms

The following terms are applicable to this Appendix.

A.1.1 Standard

Standard refers to sample, which has already-known performance and is used to determine the test's validity.

A.1.2 Grade A water

Grade A water refers to pure water, whose electrical resistivity is not less than 1.0 Mohm-cm, and whose pH is 5.0 ~ 8.0.

A.1.3 Grade B water

Grade B water refers to deionized water or softened water, whose electrical resistivity is not less than 0.5 Mohm-cm.

A.2 Equipment and Instruments

A.2.1 High-pressure autoclave: high-pressure autoclave is pressure vessel made of 300 series of stainless steel or nickel-base alloy. High-pressure autoclave shall be equipped with pressure and temperature measuring and controlling device, safety device and air release valve. The pressure and temperature controlling system shall satisfy the requirements of this test. Sample fixture and other internal accessories shall be made of 300 series or 400 series of stainless steel or nickel-base alloy.

A.2.2 Pickling vessel: pickling tank made of polyethylene or polypropylene.

A.2.3 Measuring equipment: balance (division value shall be not less than 1 x 10^-4 g), micrometer and caliper.

A.3 Reagents

A.3.1 Grade A water, Grade B water.

A.3.2 Acetone and ethanol, nitric acid (chemically pure), hydrofluoric acid (chemically pure), sulfuric acid (chemically pure).

A.4 Sample and Standard

A.4.1 Generally speaking, sample's length x width shall be 30 mm x 20 mm. The surface shall be rinsed with water or be acid pickled.

A.4.2 Each batch of samples and standards shall be respectively marked.

A.5 Test Requirements

A.5.1 Water quality: water used in the corrosion test shall be Grade A water.

A.5.2 Quantity of samples: the total area of samples being placed into the high- pressure autoclave each time shall not exceed 0.1 m²/L.

A.5.3 Please see the test conditions as follows:

---Temperature: (400 ± 3) °C.

---Pressure: (10.3 ± 0.7) MPa.

---Time: under the stipulated temperature and pressure, the total corrosion time may prolong 8 h at the most, in comparison with the stipulated time. The time may be discontinuous.

A.6 Sample Preparation

A.6.1 Use acetone or ethanol to eliminate the grease.

A.6.2 Number the samples one by one.

A.6.3 Use 180#, 300#, 400# and 500# abrasive paper to grind the surface of the samples, from coarse to fine; eliminate the deformed layer.

A.6.4 Pickling:

a) If there is any requirement towards pickling, acid solution shall adopt the following recommended matching ratios, which may be adjusted in accordance with product requirements:

Pure zirconium and zirconium tin alloy acid solution matching ratio: (3 ± 1)% volume fraction of hydrofluoric acid, (39 ± 5)% volume fraction of nitric acid; the remaining is distilled water or softened water.

Zirconium niobium alloy acid solution matching ratio: (9 ± 1)% volume fraction of hydrofluoric acid, (30 ± 5)% volume fraction of nitric acid, (30 ± 5)% volume fraction of sulfuric acid; the remaining is distilled water or deionized water.

b) The surface area of pickling samples pickled by each liter of pickling solution shall be not more than 4 dm². The temperature of acid solution shall be 32 °C ~ 45 °C. The amount of elimination by pickling shall be controlled between 0.01 mm ~ 0.1 mm. When the color of the acid solution manifests yellow, it shall be abandoned. Then, acid solution shall be re-prepared.

A.6.5 Use tap water to rinse it, then, use Grade B water, which is at room temperature, to rinse it.

A.6.6 Use Grade B water, which is not lower than 80 °C, to rinse it for around 10 min.

A.6.7 Place the samples into a drying box. At 60 °C ~ 80 °C, dry it for 0.5 h ~ 1 h. Take out the samples, then, cool it down at room temperature. Or, use hot wind to blow-dry the surface of the samples, then, cool it down at room temperature. The cooling time of the samples may be controlled at above 15 min. In the end, it shall be guaranteed that the samples are at the same temperature as the balance.

A.7 Operating Procedures

A.7.1 Sample inspection: the surface of corrosion test samples shall manifest no folding, cracks, bubbles, foreign substances, oxidization or acid spots.

A.7.2 Dimension measurement: measure the dimensions of each sample, accurate to 0.01 mm. After the calculation of the surface area, the result shall be rounded off to 1 x 10^-4 dm².

A.7.3 Weighing: use a balance to weigh the samples; the result shall at least be accurate to 1 x 10^-4 g. The balance shall receive zero-setting once after weighing every 5 samples.

A.7.4 Corrosion test of high-pressure autoclave:

a) Use Grade B water to rinse the internal wall of the high-pressure autoclave for not less than two times.

b) Place samples on a clean sample rack. Samples shall not touch with each other. Use Grade B water to rinse the samples and the sample rack.

c) Place the previously rinsed samples and the sample rack into the high-pressure autoclave. Add Grade A water, which occupies around 1/4 ~ 3/4 of the high-pressure autoclave in full water. Buckle up the king bolt and the compression bolt to seal it up, then, start to heat it up.

d) Air release: when the temperature is raised to 150 °C ~ 190 °C, start to release air. Release little air in multiple times, till the temperature and the pressure reach the stipulated value.

e) After the temperature reaches 400 °C, start thermal insulation. Maintain thermal insulation for 72 h or 336 h.

f) After the thermal insulation ends, put on clean gloves (or use clean tweezers) to take out the samples. Use Grade B water, or ethanol to rinse the samples, then, dry them in the air. Place the samples into the drying box, at 60 °C ~ 80 °C, start the drying for 0.5 h ~ 1 h. Then, take out the samples, cool them down at room temperature. Or, use hot wind to blow-dry the surface of the samples, then, cool it down at room temperature. The cooling time of the samples may be controlled at above 15 min. In the end, it shall be guaranteed that the samples are at the same temperature as the balance.

A.8 Corrosion Result

A.8.1 Calculation

Weight gain through corrosion shall be calculated in accordance with Formula (A.1):

Where,

DeltaW---weight gain through corrosion, expressed in (mg/dm2);

m2---sample mass after corrosion, expressed in (g);

m1---sample mass before corrosion, expressed in (g);

A---total surface area of sample, expressed in (dm2).

A.8.2 Surface observation

After the corrosion test, examine the color, gloss and uniformity of the surface of each sample. Record the result. Appearance inspection shall be conducted under bright environment.

A.9 Report

The content of test report includes, but shall not be limited to:

a) Name of laboratory;

b) Serial No. of this Standard;

c) Sample status;

d) Serial No. of high-pressure autoclave; test date;

e) Water's electrical resistivity before the test;

f) Test temperature, pressure and time;

g) Weight gain through corrosion;

h) Surface condition of sample.