1、Designation: C 1076 97 (Reapproved 2004)Standard Specification forNuclear Grade Hafnium Oxide Pellets1This standard is issued under the fixed designation C 1076; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revi
2、sion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This specification applies to pellets of stabilized cubichafnium oxide used in nuclear reactors.1.2 The values stated in SI un
3、its are to be regarded as thestandard. The values given in parentheses are for informationonly.2. Referenced Documents2.1 ASTM Standards:2C 559 Test Method for Bulk Density by Physical Measure-ments of Manufactured Carbon and Graphite ArticlesC 859 Terminology Relating to Nuclear MaterialsC 1098 Spe
4、cification for Nuclear Grade Hafnium OxidePowderE 105 Practice for Probability Sampling of Materials2.2 ANSI Standard:ANSI/ASME NQA-1 Quality Assurance Program Require-ments for Nuclear Facility Applications32.3 U.S. Government Document:Code of Federal Regulations, Title 10, Part 50Energy(10CFR 50)
5、Domestic Licensing of Production and Utili-zation Facilities43. Terminology3.1 DefinitionsTerms shall be defined in accordance withTerminology C 859 except for the following:3.1.1 buyerorganization issuing the purchase order.3.1.2 pelletfabricated geometric shape of stabilized cubichafnium oxide hav
6、ing a chemical composition as described inSection 4.3.1.3 pellet lotthe pellets produced from one hafniumoxide powder lot using one set of process parameters. Pellet lotsize shall be agreed upon between the seller and the buyer.3.1.4 phase transformationrearrangement of the atomicordering of a cryst
7、alline lattice as a material is cycled througha critical transformation or inversion temperature. The changefrom one crystalline phase to another may be accompanied bya volume change that could lead to cracks or defects in articlesfabricated from such materials.5 ,63.1.5 powder lota specified quanti
8、ty of hafnium oxidepowder with stabilizing additive, blended together such thatsamples taken in accordance with Section 7 can be consideredas representative of the entire quantity.3.1.6 sellerhafnium oxide pellet supplier.3.1.7 stabilizing additivea material which, when presentin sufficient concentr
9、ation in the subject material exhibiting thephase transformation, produces a stabilized crystalline phasethat does not undergo a transformation or inversion at anytemperature within the expected fabrication or usage regime ofthe manufactured pellet. The potentially deleterious volumechange is theref
10、ore avoided.4. Chemical Composition4.1 The starting hafnium oxide powder shall be in accor-dance with Specification C 1098.4.2 A stabilizing additive shall be utilized with the hafniumoxide. The recommended stabilizing additive is yttrium oxide(Y2O3). The typical concentration range is 7 to 10 weigh
11、t %Y2O3in the finished product. References to other stabilizingadditives (such as calcium oxide (CaO) and magnesium oxide(MgO) may be found in the literature and these additives maybe used if agreed upon by the buyer and seller. It is cautioned,however, that the buyer should be aware of potential de
12、stabi-lization during thermal cycling when MgO or CaO is used.4.3 Use analytical chemistry methods as agreed upon be-tween the buyer and the seller.4.4 The hafnium concentration, in grams of hafnium perunit volume or grams of hafnium per unit length, may bespecified by the buyer. In specifying the a
13、llowable range inhafnium concentration, the buyer should consider the follow-ing:1This specification is under the jurisdiction of ASTM Committee C-26 onNuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.03 onNeutron Absorber Materials Specifications.Current edition approved May
14、10, 1997. Published May 1998. Originallypublished as C 1076 87. Last previous edition C 1076 87.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Sevice at serviceastm.org. For Annual Book of ASTMStandardsvolume information, refer to the standards Document
15、 Summary page onthe ASTM website.3Available from American National Standards Institute, 11 W. 42nd St., 13thFloor, New York, NY 10036.4Available from Superintendent of Documents, U.S. Government PrintingOffice, Washington, DC 20402.5Curtis, C. E., Doney, L. M., and Johnson, J. R., “Some Properties o
16、fHafnium-Oxide, Hafnium-Silicate, Calcium-Hafnate, and Hafnium-Carbide,” Jour-nal of American Ceramics Society, Vol 37, 1954, pp. 458465.6Brown, L. M., and Madiyasni, K. S., “Characterization of Alkoxy-DerivedYttria-Stabilized Hafnia,” Journal of American Ceramics Society, Vol 53, 1970, pp.590594.1C
17、opyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.4.1 Variations in chemical composition,4.4.2 Pellet bulk density,4.4.3 Type and concentration of stabilizing additive, and4.4.4 Pellet dimensions and dimensional tolerances.4.5 The impu
18、rity concentration, excluding zirconia and thestabilizing additive, shall not exceed 0.5 weight %. Individualelement limits are specified in Table 1. The buyer may specifyadditional limits for any other elements not listed in Table 1.4.6 The zirconium concentration shall not exceed 4.5weight % on th
19、e basis of Zr/(Zr + Hf).4.7 The moisture concentration limit is included in the totalhydrogen limit (see Table 1).5. Physical Requirements5.1 Physical Dimensions:5.1.1 Dimensional requirements shall be in accordance withapplicable drawings and purchase order documents.5.1.2 Pellet dimensions shall b
20、e measured to ensure com-pliance with the buyers requirements. Sampling plans to meetthe acceptance criteria shall be agreed upon between the buyerand the seller to ensure that the pellets represented by thesample are within the required tolerance.5.2 Density:5.2.1 Pellet density limits shall be spe
21、cified by the buyer.The incorporation of a stabilizing additive will introduce achange in the theoretical density of the fabricated pellets andshould be taken into account. The method of establishing thetheoretical density value shall be mutually agreed upon be-tween the buyer and the seller.5.2.2 T
22、he method of density measurement shall be TestMethod C 559 or an alternative method submitted by the sellerfor approval by the buyer. Sampling plans to meet theacceptance criteria shall be agreed upon between the buyer andthe seller. The method of density measurement and the methodof compliance with
23、 5.2.1 shall be submitted by the seller to thebuyer for approval.5.3 Mechanical PropertiesRequired mechanical proper-ties and test methods shall be mutually agreed upon betweenthe buyer and the seller. It is recommended that the plan ofmechanical testing to verify pellet integrity include compres-si
24、ve testing at 69 MPa (10 000 psi).5.4 Phase StabilizationA crushed sample of the firedproduct shall be tested by powder X-ray diffraction. Thediffraction pattern must show that the required cubic crystallinephase has been developed in the product. The criteria forsatisfactory development of the cubi
25、c phace shall be mutuallyagreed upon between the buyer and the seller.5.5 Visual AppearanceVisual examination shall be con-ducted on finished pellets in accordance with Section 7 onSampling. The seller and the buyer shall agree on visualstandards as representing the requirements of 5.5.1, 5.5.2, and
26、5.5.3. These standards shall be used as acceptance standards forthe visual examination of the pellets. In the event of a dispute,the method of defect measurement shall be submitted by theseller for approval by the buyer. Maximum permissible defectsare defined as follows:5.5.1 End ChipsPellet-end sur
27、face shall not be chippedbeyond 10 % of the end-face surface area and no chip shallexceed 1.02 mm (0.040 in.) in depth.5.5.2 Circumferential ChipsPellet circumferential sur-faces shall not be chipped beyond 5 % of the circumferentialsurface area. No single chip shall exceed a depth of 1.02 mm(0.040
28、in.).5.5.3 CracksCracks not exceeding 90 of circumferencein length are acceptable provided the other requirements of thespecifications are met.5.5.4 Fissures and other defects shall be evaluated withrespect to the criteria of 5.5.1, 5.5.2, and 5.5.3.6. Cleanliness6.1 The finished pellets shall be ha
29、ndled in a manner toavoid contamination by grinding fluids and dust, cleaningagents, and organic materials such as plastics and paper used inpackaging. Cleaning solutions, if used, shall be free of halidesor non-volatile additives and shall be removed from the pelletsprior to sampling and packaging.
30、7. Sampling7.1 Sampling plans to meet the acceptance criteria andinspection and measurement procedures that describe themethod of compliance with this specification shall be approvedby the buyer. The degree of sampling varies with the applica-tion and for this reason should be specified on the purch
31、aseorder. Practice E 105 is referenced as a guide.7.2 Each powder and pellet sample taken shall be sufficientto perform the following in the event they are necessary ordesired by the buyer:7.2.1 Quality verification tests,7.2.2 Acceptance tests,7.2.3 Referee tests, in the event these become necessar
32、y, and7.2.4 Retention of archive sample by the seller.7.3 Archive samples shall be retained by the seller for aperiod of time specified by the buyer and delivered to the buyerupon request.8. Inspection and Certification8.1 The seller shall inspect the material covered by thisspecification and shall
33、furnish the buyer with certificates of testshowing the results of testing and inspection performed oneach pellet lot prior to shipment. The seller shall certify thateach pellet lot is in compliance with the provisions of thisspecification.TABLE 1 Impurity Concentration LimitsElementMaximumConcentrat
34、ionLimit (g/g Pellet)B 400C 1 000Gd 200Gd+Sm+Eu+Dy 500Co 100Si 2 000Th 400F3F+Cl+Br+I 100H (total hydrogen from all sources) 2C 1076 97 (2004)29. Rejection and Rehearing9.1 Unless the buyer and the seller agree otherwise, rejec-tion and acceptance shall be on a pellet lot basis.9.2 Pellet lots that
35、fail to conform to the requirements of thisspecification may be rejected by the buyer. The seller maypetition the buyer to waive selected requirements for identifiedout-of-specification lots. Decision to grant such waiver belongsto the buyer. The seller may also apply any remedy to bringrejected lot
36、s into specification providing the seller can demon-strate to the buyer that such remedy does not impair thefunction or preclude the certification of the rejected material.9.3 In the event of disagreement over the results of analysis,samples shall be submitted to a mutually selected referee forresol
37、ution.10. Packaging and Shipping10.1 The pellets shall be packaged in sealed containers toprevent loss or damage, or both, of material and contaminationfrom airborne or container materials. The exact size and type ofpackaging shall be as mutually agreed upon between the buyerand seller.10.2 Each con
38、tainer shall be clearly marked with the fol-lowing:10.2.1 Hafnium oxide pellets plus stabilizing additive,10.2.2 Purchase order number,10.2.3 Gross, tare, and net weight,10.2.4 Lot number, and10.2.5 Name of pellet manufacturer.11. Quality Assurance11.1 Quality assurance requirements shall be agreed
39、uponbetween the buyer and the seller when specified in the purchaseorder. Code of Federal Regulations, Title 10, Part 50 (Appen-dix B) and ANSI/ASME NQA-1 are referenced as guides.12. Keywords12.1 CaO; hafnium oxide; MgO; stabilizer; stabilizing;additive; thermal cycling test; Y2O3ASTM International
40、 takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their ow
41、n responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be ad
42、dressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, a
43、t the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).C 1076 97 (2004)3
