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In-situ temperature measuring thermocouple on diamond anvil cell and preparation method thereof

A diamond-to-anvil, in-situ temperature technology, which is applied in the direction of measuring heat, thermometers, measuring devices, etc., can solve the problems of inaccurate measurement, large temperature measurement error, and in-situ temperature measurement problems that have not been well solved.

Inactive Publication Date: 2011-09-28
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the pressure calibration technology under extreme conditions has been very mature, but because the DAC sample cavity is only on the order of hundreds of microns, it is difficult to use ordinary thermocouples in it, so the problem of in-situ temperature measurement in the DAC has not been solved. good solution
The above three methods have their own disadvantages that limit their use: the first method leads to inaccurate measurement because the measurement point cannot directly contact the sample; It is easy to be oxidized and damaged, which limits the use of this temperature measurement method; in the third method, since the sample belongs to a gray body, the temperature measurement error using the black body radiation spectrum is very large
This method is limited to use at temperatures above 2000K. Optical temperature measurement below 2000K is affected by factors such as changes in emissivity, transmission loss, and reflection of ambient rays.

Method used

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  • In-situ temperature measuring thermocouple on diamond anvil cell and preparation method thereof
  • In-situ temperature measuring thermocouple on diamond anvil cell and preparation method thereof
  • In-situ temperature measuring thermocouple on diamond anvil cell and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 combined figure 1 , 2 Explain the structure of the present invention

[0035] exist figure 1 , 2 Among them, 1 is a diamond anvil, 2 is an aluminum oxide film, 3 is a tungsten film, 4 is a tantalum film, 5 is a conductive silver paste, 6 is a copper wire, 7 is a sample cavity, and 8 is a metal gasket.

[0036] figure 1 A schematic diagram of the assembled DAC device with a W-Ta thermocouple is given, in which the diamond anvil has two diamond anvils up and down, and the upper diamond anvil 1 is prepared with a W-Ta thermoelectric device by magnetron sputtering. Even; between the anvil surface of two diamond anvils up and down and the hole that has on metal spacer 8 forms sample chamber 7, is used for placing measured sample; Through each deposition layer (aluminum oxide film 2, tungsten film 3, The profile of the tantalum film 4) can clearly show the positional relationship of each deposited layer, wherein the aluminum oxide film 2 of the inner layer depo...

Embodiment 2

[0038] Example 2 combined image 3 Illustrate the preparation process of W-Ta thermocouple of the present invention

[0039] The present invention is accomplished through following technological process [whole process is as image 3 (a)-(f)]:

[0040] Step 1: Use conventional methods to remove stains on the surface of the diamond anvil 1. You can soak the diamond anvil in a mixture of acetone and alcohol for 20 minutes to remove surface stains. After taking it out, rinse it with deionized water. Such as image 3 (a) shown.

[0041] The second step: after drying, put it into the vacuum chamber of the magnetron sputtering device, and use the magnetron sputtering method to deposit the aluminum oxide film 2 on the surface of the diamond as the heat insulation between the sample chamber 7 and the diamond anvil 1 layer. Such as image 3 (b) shown.

[0042] In the sputtering process, metal aluminum is used as the target material, oxygen and argon with a flow ratio of 30:2.0~3....

Embodiment 3

[0059] Proofreading of W-Ta thermocouple under embodiment 3 normal pressure

[0060] A standard K-type thermocouple (NiSi-NiCr) is used to calibrate the variation relationship of the thermoelectric potential of the W-Ta thermocouple of the present invention with temperature, and the calibrated temperature range is 26-350°C. In the experiment, a copper wire with a diameter of 100 μm was selected as the compensation wire, and the connection between the copper wire 6 and the W film 3 and Ta film 4 on the side of the diamond anvil 1 was connected by conductive silver paste 5 leads. The advantage of this method is that it is easy to operate, the contact resistance is small, and the repeatability of the experiment is good.

[0061] From Figure 4 It can be seen from the figure that as the temperature increases, the thermoelectric potential of the W-Ta thermocouple increases gradually, and the temperature T and the thermoelectric potential V show a good linear relationship. When th...

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Abstract

The invention discloses an in-situ temperature measuring thermocouple on a diamond anvil cell and a preparation method thereof, belonging to the technical field of in-situ temperature measuring devices under extreme conditions. A W-Ta thermocouple in the invention has a structure that an alumina barrier (2) is deposited on the surface of a diamond anvil (1); a tungsten film (3) and a tantalum film (4) which are smaller than half of the surface area of the anvil in area are respectively deposited on the alumina barrier (2) to be used as conductors of the thermocouple and are spaced by the alumina barrier (2); the tungsten film (3) and the tantalum film (4) are in overlapped contact at the centre of the anvil surface and used as thermocouple contacts. The W-Ta thermocouple is manufactured on the surface of the diamond anvil (1) through a film manufacturing technology and a photoetching technology. The countercurrent heat transfer change between the W-Ta thermocouple disclosed by the invention and a detected surface is extremely small, the W-Ta thermocouple has extreme little interference to heat conduction on the surface, and is faster to respond to the temperature; moreover, the measured result reflects actual temperature of the measured surface and in-situ temperature measurement under the high temperature and high pressure conditions is realized.

Description

technical field [0001] The invention belongs to the technical field of devices for in-situ temperature measurement under extreme conditions, and in particular relates to a thermocouple for temperature measurement made on a diamond counter-anvil and a preparation method for the thermocouple. Background technique [0002] Diamond Counter Anvil (DAC) is currently the only scientific device capable of generating a static pressure of one million atmospheres, and is the most important scientific instrument in the field of high-pressure science and technology research. Using DAC, people can observe changes in the structure and physical properties of substances in ultra-high pressure environments, especially in the laboratory simulation of the pressure and temperature environment of the deep earth. The laboratory simulates the pressure and temperature environment in the deep part of the earth to study the static physical and chemical properties of related substances in various layer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01K7/02
Inventor 高春晓刘才龙韩永昊任万彬李明王月刘鲍胡廷静李岩张洪林
Owner JILIN UNIV
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