固体熱物性クラブ第2回研究会

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1 Low-Temperature Interferometric Dilatometer using a Cryogenic refrigerator Schematic diagram of measurement system Rh-Fe resistance thermometer Clamping to compresser Cryogenic refrigerator Vacuum bellows to vacuum pomp Probe beam spots Performances: holder Heater on Cold head 4K-GM refrigerator (cryostat) - Controllable temperature range form 1 K to 3 K Double-path type laser interferometer - y an Optical heterodyne method - Fringe determination : < 1 nm Vacuum jacket Radiation shield cell Thermometer Optical table Rh-Fe resistance thermometer + Resistance bridge - Temperature determination : 6 mk Measurement results by this instrument: LTEC /1-6 K 3 1 Single crystal of Silicon Fit curve our data U(LTEC) CODATA Deviation /1-6 K /1-6 K L/L /% ULE1 ULE Zerodur CCZ-LS CCZ-HS Figure. LTEC of some low-ltec glasses ULE1 ULE Zerodur CCZ-LS CCZ-HS Figure 1. LTEC of FZ silicon (single crystal) Figure 3. L/L of some low-ltec glasses

Measurement system for linear thermal expansivity of solids by an absolute measurement method in NMIJ / AIST Schematic diagram of measurement system PC Data acquisition system L Lock-in amplifier -

2 Measurement system for linear thermal expansivity of solids by an absolute measurement method in NMIJ / AIST Schematic diagram of measurement system PC Data acquisition system L Lock-in amplifier - Our measurement system has achieved CTE measurement with high precision by a laser interferometer. Temp. control and Temp.measurement Interference signal Temperature controller / reader K Reference sigmnal At high temperature range High temperature furnace Elemental thermocouple (Au-Pt TC) at T <1 Radiation thermometer at T > 1 At room temperature range Thermal bath by using thermo-electric device Pt resisntance r.t. At cryogenic temperature Cryostat by using cryogenic refrigerator Rh-Fe (or Pt) resistance thermometer at K < T < 3 K Key technique: Displacement measurement by a laser interferometer Arrangement of a laser interferometer for dilatometry using an optical heterodyne method with a double-path Photodetector (for a reference signal) Retroreflector Polarized cube beam splitter modulated by 79.9 MHz modulated by 8. MHz Cryostat Photodetector (for a displacement signal) Quarter-Wave plates Features: Frequency stabilized laser beam (=63.8 nm) Half-wave plate Acoustooptic modulator Retroreflector PS 4 plate -Optical heterodyne method with high resolution -Acousto-optic modulators to generate probe beams AOMs Photo detector To specimen -Auto-cancellation of the effect of specimen tilt on displacement measurement

Development of New Reference Material for Thermal Expansion Measurements at Cryogenic Temperature We developed a new certified reference material (CRM; NMIJ CRM 583) for thermal expansion

This CRM can be used to calibrate a pushrod dilatometer and a thermo-mechanical analyzer, to estimate the measurement uncertainty, and to confirm the validity of measurement methods.

3 Development of New Reference Material for Thermal Expansion Measurements at Cryogenic Temperature We developed a new certified reference material (CRM; NMIJ CRM 583) for thermal expansion measurements in solid materials at cryogenic temperature. This CRM can be used to calibrate a pushrod dilatometer and a thermo-mechanical analyzer, to estimate the measurement uncertainty, and to confirm the validity of measurement methods. It was made from a single crystal of silicon and can be available in the temperature range from K to 3 K. Procedure of making CRM: 1) Preparation of a silicon ingot ) Sampling of specimens for calibration 3) CTE Calibration by the laser-interferometoric dilatometer 4) Evaluation of the uncertainty in the calibration values 5) Evaluation of homogeneity and long-term stability on CTE value 6) Determination of the certified value and its uncertainty 3) The specimens were measured by using a laserinterferometric dilatometer for cryogenic temperature. The CTE values of the specimens were measured by absolute measurement method using a laser interferometer. Size 1: mm 3 Size : mm 3 Photo 1 CRM; NMIJ CRM 583-a 1), ) The material of CRM is the single crystal of silicon which was made by a floating zone method. The purity of the silicon ingot is more than %. Some specimens were sampled from the ingot to calibrate CTE value. Photo. FZ-silicon ingot ( 5 inchx13 mm) LTEC /1-6 K Probe beam spots holder Rh-Fe resistance thermometer Clamping to compresser Heater on Cold head Cryogenic refrigerator Optical table Vacuum bellows to vacuum pomp Vacuum jacket Radiation shield cell Thermometer Figure 1. Schematic diagram of Laser-interferometric dilatometer 3 1 Single crystal of Silicon Fit curve U(LTEC) CODATA Deviation /1-6 K 4)- 6) The certified value were determined by a weighted least square method as functions of temperature and it is in good agreement with the recommended value of CODATA. The uncertainty of the certified value is also much smaller than that of previous reference materials. 4) The measurement uncertainty of each obtained value was evaluated respectively. The uniformity of thermal expansivity in the ingot was also estimated by analysis of variance. Conditions: L /m =.685 /1-6 K = T AVE /K =.174 Data file name 7716p T /K = 1.87 Step No. 4 Factor of uncertainty Uncertainty Detail (x i) u (x i) Unit u i( ) Type u ( ) = 1.E-5 1.3E Resolution of phase detection Fringe detamination u ( ) = 1.E-5 1.3E rad ( 1 and ) u ( ) =.3E-.9E-9 Reproducebility of phase change u ( ) =.3E-.9E-9 A Optical arraiment ( ) Inclination of optical axis u ( ) = 3.3E E3 Wave length of laser souce u ( ) = 1.6E5.5E Stability of wave length m ( 1 and ) u ( ) = 1.6E5.5E Refrective index Change of refractive index of themal u (n 1) =.8E-9.8E 1 A (n 1 and n ) exchange gas u (n ) =.8E-9.8E Resolution of linear gauge.5e-6 1.7E Determination of L Calibration of liniar gauge 8.1E-8 5.7E u (L ) = m (L ) Temperature of specimen at 7.8E-8 5.5E measurement Detection of temperature u ( T ) =.5E-3 3.5E Determination of Correction of temperature difference u ( T ) = 9.4E-3 temperature between specimen and termometer K 1.3E-9 ( T, T and T D) Stability of temperature control u ( T ) = 6.4E-5 9.1E A Calibration of thremometer u (T D) = 1.E- 1.7E A Combined standard uncertaity/k : u c( )= 4.3E-9 Expanded uncertaity/k (Converage factor; k =): U =ku c( )= 8.6E-9 Relative expanded uncertaity: (U )=.61% Table. Error budget sheet of LTEC measurement Certified value and uncertainty T (K) (1-6 K ) U(1-6 K )

4 平成 3 年度回固体熱物性クラブ全体会合 Jan.. 1 熱膨張率標準供給項目詳細 (1. 1 現在 ) 供給形態名称適用範囲等不確かさ等標準物質依頼試験標準物質名適用温度範囲参照値の不確かさ / 頒布形状単結晶シリコン相対拡張不確かさ : < 1. % (NMIJ RM 111-a) 93 K - 1 K 頒布形状 :4.5 角 L6 mm 3, 9. 角 L6 mm 3 ガラス状炭素 (NMIJ RM 11-a) ガラス状炭素 (NMIJ RM 114-a) 93 K - 11 K 93 K - 約 16 K 相対拡張不確かさ : < 3.3 % 頒布形状 :6. 角 L1 mm 3, 6. 角 L mm 3 相対拡張不確かさ :.91 %~1.7 % 頒布形状 :6. 角 L1 mm 3 単結晶シリコン拡張不確かさ : 6. 1 (NMIJ CRM 583-a) K -3 K -9 K ~ K 頒布形状 :1. 角 L3 mm 3, 1. 角 L6 mm 3 試験名校正温度範囲他校正測定能力 (k =) 単結晶シリコンもしくはガラス状炭素の熱膨張率校正固体ブロックの熱膨張率校正 ( 特殊 ) 短尺ブロックゲージの熱膨張率校正 5 5 t6 の単結晶シリコンもしくはガラス状炭素試験片校正温度範囲は 93 K K. 1-8 K t8 の固体ブロック校正温度範囲は 15 K-3 K K ~ K 呼び長 mm 以上かつ 1 mm 以下のブロックゲージもしくはこれと同等寸法精度形状の固体ブロック校正温度範囲は 5-35 A + C α 1 α T A = 4.3 +,.38,. = + = + 3 C L L L 尚 L <4 の場合は A=. とするまた入力量の単位は α が 1-6 K, L が mm, ΔT が K とする ;

5 平成 3 年度回固体熱物性クラブ全体会合 Jan.. 1 今後の整備予定 4 年度単結晶シリコン (RM111-a) ガラス状炭素 (RM11-a) 単結晶シリコン (RM113-a) RM114-a CRM 583-a 銅 (CRM585-a) (13 年度供給開始予定 ) 単結晶 Si, GC の熱膨張率校正 ( 一般 ) 短尺 G の熱膨張率校正 ( 一般 ) 固体ブロックの熱膨張率校正 ( 特殊 )

第 3 秋葉原 Feb 熱膨張率標準の整備状況 (8. 現在 ) 標準物質 :PR 式膨張計や MA のための参照試験片依頼試験 : レーザ干渉式膨張計群による器物の熱膨張率校正標準開発 / 供給の状況 : 3 年度単結晶シリ

第 3 秋葉原 Feb 熱膨張率標準の整備状況 (8. 現在 ) 標準物質 :PR 式膨張計や MA のための参照試験片依頼試験 : レーザ干渉式膨張計群による器物の熱膨張率校正標準開発 / 供給の状況 : 3 年度単結晶シリ第 3 回固体熱物性クラブ講演会 @ 秋葉原 Feb. 7. 8. 固体熱物性標準整備の現状と開発計画熱膨張率産業技術総合研究所山田修史熱膨張率標準の整備状況説明標準物質開発例の紹介第 3 回固体熱物性クラブ講演会 @ 秋葉原 Feb. 7. 8. 熱膨張率標準の整備状況 (8. 現在 ) 標準物質 :PR 式膨張計や MA のための参照試験片依頼試験 : レーザ干渉式膨張計群による器物の熱膨張率校正