张航工程师的塞贝克量热计组装调试报告
2018-09-15 17:11:10   来源:冷聚变世界   评论:0 点击:

为了进行载氢金属异常放热的测量,设计组装了一台塞贝克量热计,该量热计设计参照Dennis G Letts & Dennis J Cravens的量热器构造形式,用塞贝克元件对实验装置进行六面体表面全覆盖,用电加热线圈来标定量热计,并进行了初步的氘气氛围下镍钯金属辉光放电异常放热现象。


塞贝克量热计的组装调试
Assembly and commissioning of Seebeck calorimeter



 
联系人:张航  Hang Zhang
秋然实验室 Qiuran Laboratory
Email: 715469127@qq.com


  为了进行载氢金属异常放热的测量,设计组装了一台塞贝克量热计,该量热计设计参照Dennis G. Letts & Dennis J. Cravens [1]的量热器构造形式,用塞贝克元件对实验装置进行六面体表面全覆盖,使用了40 mm ´ 40 mm塞贝克元件96片,每片元件由127对热电偶组成,合计12192对热电偶来测量热量,塞贝克元件外贴附水冷片,冷却循环水供水温度25°C,控制精度± 0.01 °C。用电加热线圈来标定量热计,并进行了初步的氘气氛围下镍钯金属辉光放电异常放热现象的观察。

  In order to measure the anomalous heat release of hydrogen-carrying metals, a Seebeck calorimeter was designed and assembled. The calorimeter was designed according to the structure of the calorimeter of Dennis G. Letts & Dennis J. Cravens [1] The hexahedron surface of the experimental device was carried out with Seebeck element. A total of 96 pieces of 40 mm ´ 40 mm Seebeck elements are used. Each piece consists of 127 pairs of thermocouples. A total of 12192 pairs of thermocouples are used to measure the heat. The Seebeck element is attached with water cooling sheets. The cooling water supply temperature is 25 ± 0.01 °C. The quantitative calorimeter was calibrated with an electric heating coil and the anomalous heat release of Ni-Pd glow discharge in deuterium atmosphere was observed.
 
关键词:塞贝克效应;量热计;温度
Keywords: Seebeck effect; calorimeter; temperature
 

  1 前言  Introduction

  为了测量载氢金属异常放热现象,设计制作了多个量热计:有温差法量热计、空气流量式量热计、水流量式量热计,均有不同问题:
  
  1. 温差法量热计可以直观快速观察到异常放热的产生,但不能直接测量出发热量;

  2. 空气流量式量热计可以直接测量出热量,受环境温度影响,计量误差较大;

  3. 水流量式量热计,液体流量计量和控制不准确,计量误差较大。

  In order to measure the abnormal exothermic phenomenon of hydrogen-carrying metals, several calorimeters were designed and manufactured, including thermometer, air flow calorimeter and water flow calorimeter.

  (1) Temperature difference calorimeter can directly and quickly observe the abnormal exothermic production, can not directly measure the starting heat.

  (2) the air flow calorimeter can directly measure the heat, which is influenced by the ambient temperature.

  (3) water flow calorimeter, liquid flow measurement and control is not accurate, the measurement error is large.
 

  2. 量热计组装 Calorimeter assembly

  参照Dennis G. Letts & Dennis J. Cravens的塞贝克量热器[1],将铜块改成了铝方管内衬保温棉,这样可以降低塞贝克原件的工作温度,并将空气散热器更换为水冷散热器,水冷散热器散热效果好于空气散热器。

  Referring to Dennis G. Letts Dennis J. Cravens USA's Selbeck calorimeter, the copper block is replaced with aluminium square tube lined insulation cotton, which can reduce the working temperature of the original Selbeck and replace the air radiator with water-cooled radiator. The water-cooled radiator is better than the air radiator.



图1. Dennis G. Letts & Dennis J. Cravens的塞贝克量热计
Fig. 1. Dennis G. Letts Dennis J. Cravens USA Seebeck calorimeter
 
  图2是塞贝克量热器剖面结构图,用一个铝合金方管作为内层,铝管尺寸80 mm ´ 80 mm ´ 450 mm,方管内衬保温棉,中心安装电加热器和反应容器,方管外贴塞贝克元件,塞贝克元件外安装水冷块,水冷块外安装保温材料。

  Fig. 2 is the sectional structure of the Seebeck calorimeter. An aluminum alloy square tube is used as the inner layer. The aluminum tube is 80 mm ´ 80 mm ´ 450 mm. Insulation cotton is installed in the square tube. Electric heater and reactor are installed in the center. The Seebeck element is pasted outside the square tube. Water-cooled block is installed outside the Seebeck element. Insulation material is installed outside the water-cooled block.




图2. 塞贝克量热计的剖面图(图中Seeback为Seebeck)
Fig. 2. profile of Seebeck calorimeter



图3. 塞贝克元件
Fig. 3. Seebeck element



图4. 塞贝克元件安装到内壳上
Fig. 4. Seebeck element is mounted on the inner shell.



图5.塞贝克元件表面贴导热硅胶
Fig. 5. Surface conductive silicone adhesive on Seebeck component



图6. 塞贝克元件上安装水冷板
Fig. 6. Installation of water-cooled plate on Seebeck element



图7. 水冷板管路连接
Fig. 7. Water cooled plate pipe connection




图8. 水冷板管路连接完成
Fig. 8. Connection of water-cooled plate pipe connection



图9. 端部塞贝克元件和水冷板安装
Fig. 9. Installation of Seebeck component and water cooling plate at the end





图10.量热器内部组件通水调试
Fig. 10. Commissioning of internal components of calorimeter



图11.量热器内部组件安装到箱体内并充填保温材
Fig. 11. Internal components of calorimeter are installed in the tank and filled with insulation materials.



图12. 量热器外壳端部的塞贝克元件和水冷板安装
Fig. 12. Seebeck element and water cooling plate installation at the end of calorimeter housing





图13. 实验系统照片
Fig. 13. Photo of experimental system

 
 
  3. 冷却水系统 Water Cooling system
   

  塞贝克量热器需要提供恒温循环冷却水,温度波动小于± 0.01 °C,经过反复试验,最终使用三个恒温水浴,使温度控制到25± 0.01 °C,系统如下:

  Seebeck calorimeter need to provide thermostatic circulating cooling water with temperature fluctuations of less than ± 0.01 °C. After repeated testing, the final use of three thermostatic water bath, temperature control to 25 ± 0.01 °C, the system is as follows:



 
图14.恒温循环水系统图

 

  4. 空白实验  Blank Experiment

  给加热器输入恒定功率,维持6小时,这时塞贝克输出电压稳定,数据复现性较好。

  The heater input constant power, maintain 6 hours, then Seebeck output voltage stability, data reproducibility is better.

表1.塞贝克量热计空白实验数据
Table 1. blank experimental data of Seebeck calorimeter
 
Input power Seebeck
voltage
Calculated
 power
error Percentage
 error[l1]
10.67 0.94 10.7179642 0.047964
0.449523899
21.45 1.84
21.3699412
-0.08006
-0.373234499
31.29 2.68
31.2789004
-0.0111
-0.035473314
40.32 3.45
40.33421975
0.01422
0.035267237
50.57 4.33
50.65048615
0.080486
0.1591579
60.4 5.16
60.3486668
-0.05133
-0.084988742
70.69 6.04
70.5972172
-0.09278
-0.131253077
80.57 6.88
80.3474164
-0.22258
-0.276261139
90.47 7.73
90.18136815
-0.28863
-0.319035979
100.43 8.58
99.9828074
-0.44719
-0.445277905
110.46 9.47
110.2106474
-0.24935
-0.225740223
120.94 10.37
120.5171594
-0.42284
-0.349628452
130.87 11.25
130.5593938
-0.31061
-0.237339535
140.05 12.04
139.5448972
-0.5051
-0.360658908
150.51 12.95
149.8604798
-0.64952
-0.431546243
160.53 13.81
159.5750226
-0.95498
-0.594890332
170.29 14.7
169.593401
-0.6966
-0.409066299
180.1 15.59
179.576135
-0.52387
-0.290874542
190.34 16.51
189.8578986
-0.4821
-0.25328436
200.45 17.41
199.8792906
-0.57071
-0.284714118
Calculated power = - 0.44635 + 11.89808 V - 0.0225V2    
 

 
图15.塞贝克电压和计算功率拟合图
Fig. 14. Fitting diagram of Seebeck voltage and calculated power
 
 

  5. 量热计的测试 Measurement of calorimeter

  该实验为氘钯辉光放电异常放热实验,容器由不锈钢制作内衬镍皮,容器中间是钯丝电极,辉光放电时,容器外壳是正极,钯丝电极是负极。

  The experiment is a deuterium-palladium glow discharge Abnormal exothermic experiment, the container is made of stainless steel lined with nickel skin, the middle of the container is a palladium wire electrode, glow discharge, the container shell is the positive, palladium wire electrode is the cathode.

 [l1]有效数字不会这么多




图16.加热器
Fig. 16. Heater



图17. 加热器与容器
Fig. 17. Heaters and Containers



图18. 容器放入加热器内
Figure 18. The container is placed in the heater


  5.1 加热实验测试  Heating experiment test

  正式实验加热器内放入装了燃料的实验容器,测试在加热状态下的异常放热,初步实验未观测到多余功率,数据与空白实验吻合。
 
  The formal experimental heater is placed in a fuel-filled experimental container, test the abnormal heat in the heating state, the initial experiment did not observe the excess power, the data and the blank experimental agreement.
 
表2. 20180907塞贝克量热计7号容器加热实验
Table 2. 20180907 heating test of the Seebeck calorimeter No. 7 container
 
Input power Seebeck voltage Calculated power error Percentage error
60.12 5.1 59.648633 -0.47137 -0.78404358
150.78 12.98 150.1999194 -0.58008 -0.384719857
Calculated power=11.89808V-0.0225V*V-0.44635    
 
  5.2 辉光放电实验测试 Glow Discharge Test

  给实验容器电极加载电压,在氘气状态下辉光放电,测量辉光放电状态下的异常放热,

  未观测到多余功率,测试数据比空白实验低,原因需分析。

  The electrode load voltage of the experimental vessel, glow discharge in the state of deuterium gas, and the abnormal heat emission under the condition of glow discharge are measured.No excess power is observed, the test data is lower than the blank experiment, the reason needs analysis.
 
表3. 20180907塞贝克量热计7号容器辉光放电实验
Table 3.20180907 glow discharge test of the Seebeck calorimeter 7 container
 
Input power Seebeck voltage Calculated power error Percentage error
40.26 3.32 38.8072716 -1.45273 -3.608366617
40.2 3.32 38.8072716 -1.39273 -3.464498507
40.26 3.35 39.15971175 -1.10029 -2.732956408
40.23 3.36 39.2771828 -0.95282 -2.368424559
Calculated power=11.89808V-0.0225V*V-0.44635    
 
 
  6. 思考 Discussion

  加热实验数据与空白实验吻合,这说明两个工况一致,无多余热量,复现性较好, 辉光放电实验数据与空白实验不吻合,误差较大,数据偏低,这是个问题。因为辉光放电实验与空白实验工况不同,辉光放电发热位置不均匀,使得计量产生误差,这个误差是负误差。

  塞贝克量热器,要测量准确,尽量保持每一个塞贝克元件温度一致,或保持温度场一致,见下图,这是Dr. Storms的塞贝克量热计[2],里面用风扇搅动空气,达到温度场均匀,计量精度高。
 
  The experimental data of heating is in agreement with the blank experiment, which shows that the two working conditions are consistent, no excess heat, and reproducibility is better. The experimental data of glow discharge does not coincide with the blank experiment, the error is large, the data is low, which is a problem.

  Because the glow discharge experiment is different from the blank experimental condition, the glow discharge heating position is uneven, which makes the metering error, which is a negative error.

  Seebeck calorimeter, to measure accurately, try to keep each Seebeck element temperature consistent, or maintain the same temperature field, see the following figure, which is Dr. Storms Seebeck calorimeter [2], the inside with the fan stirred air, to achieve uniform temperature field, high measurement accuracy.

 


 
图19.Dr. Storms的塞贝克量热器
Figure 19.Dr. Storms Seebeck calorimeter

 
致谢

  感谢中科院化学所张武寿博士的指导,感谢美国鲍勃希金斯博士的宝贵建议。

Thanks

  Thanks to Dr. Wu-Shou Zhang, Institute of chemistry, CAS, thanks to Dr. Bob Higgins for his valuable advice.
 
参考文献
References
[1] Dennis G. Letts Dennis J. Cravens USA Building & Testing a High Temperature Seebeck Calorimeter   
[2] Edmund Storms USA The enthalpy of formation of PdH as a function of H/Pd atom ratio and treatment


 
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2018年9月15日 

 





 

 

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