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CN107697886B - Preparation method of metal hydride thin sheet - Google Patents

Preparation method of metal hydride thin sheet Download PDF

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Publication number
CN107697886B
CN107697886B CN201711103823.7A CN201711103823A CN107697886B CN 107697886 B CN107697886 B CN 107697886B CN 201711103823 A CN201711103823 A CN 201711103823A CN 107697886 B CN107697886 B CN 107697886B
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metal hydride
sheet
vapor deposition
polymer film
thickness
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CN107697886A (en
Inventor
李启寿
程亮
叶林森
李强
雷洪波
张佳佳
何林
谢东华
谢金华
杨勇
单东伟
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Institute of Materials of CAEP
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B6/00Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
    • C01B6/04Hydrides of alkali metals, alkaline earth metals, beryllium or magnesium; Addition complexes thereof

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses a preparation method of a metal hydride sheet, and aims to solve the problems that light metal hydride is easy to chemically react with water in an atmospheric environment, and hydrolysis products are generated on the surface of the metal hydride sheet prepared by a conventional sand paper polishing method, so that terahertz characteristic wave distortion is caused, and the nondestructive detection effect of internal defects of related materials is influenced. The invention discloses a preparation method of a metal hydride sheet for extracting terahertz characteristic waves, which aims to obtain an accurate nondestructive detection result of metal hydride internal defects. The method comprises the steps of firstly forming a layer of compact waterproof polymer film on the surface of a metal hydride wafer by using a Chemical Vapor Deposition (CVD) technology, then placing a test piece in a metallographic sample making machine for processing, and finally carrying out chemical vapor deposition on a new polished surface of a sheet to obtain the metal hydride sheet for extracting the terahertz characteristic wave. Through actual measurement, the method can effectively solve the problems and ensure the accuracy and reliability of the measurement result.

Description

Preparation method of metal hydride thin sheet
Technical Field
The invention relates to the field of chemistry, in particular to a preparation method of a metal hydride sheet. More specifically, the invention provides a preparation method of a metal hydride sheet for extracting terahertz characteristic waves, and the prepared sheet can reflect a real characteristic spectrum and ensure the accuracy and reliability of a detection result.
Background
The light metal hydride has high hydrogen density and low mass density, has strong chemical potential for water, is easy to carry out hydrolysis reaction in atmospheric environment, has unique physical and chemical properties, and generally comprises sodium hydride, magnesium hydride, calcium hydride, lithium hydride and the like. The light metal hydride is used as a popular candidate material for ultra-light structural parts and hydrogen fuel sources, and has important significance for the research thereof.
The terahertz technology can be used for carrying out nondestructive detection on the internal defects of the metal hydride. The terahertz technology is used for representing the metal hydride sheets in different states, obtaining the characteristic spectrum of the metal hydride, discriminating the characteristic curve of the flawless hydride product, and providing reliable data support for the optimization of the production process of the light metal hydride product and the control of the product quality. When the light metal hydride terahertz characteristic wave is extracted, strict requirements are imposed on the thickness of a sample, and the thickness is generally required to be less than 1 mm. However, light metal hydride has strong affinity to water and can generate chemical reaction under the condition of low water partial pressure, and when the metal hydride sheet is prepared by adopting the conventional mould pressing and sand paper polishing method, because the sample of a target material is not protected in real time, the surface of the metal hydride sheet can generate chemical reaction during the preparation, the real characteristic spectrum of the metal hydride sheet cannot be reflected, and the reliability of a nondestructive detection result is influenced.
Therefore, a new method is urgently needed to solve the above problems.
Disclosure of Invention
The invention aims to: the preparation method of the metal hydride sheet is provided for solving the problems that the light metal hydride is easy to chemically react with water in the atmospheric environment, and the metal hydride sheet prepared by the conventional unprotected measure sand paper polishing method generates hydrolysis products on the surface of the metal hydride sheet, so that terahertz characteristic waves are distorted, and the nondestructive detection effect of internal defects of related materials is influenced. The invention discloses a preparation method of a metal hydride sheet for extracting terahertz characteristic waves, which aims to obtain an accurate nondestructive detection result of metal hydride internal defects. The method comprises the steps of firstly forming a layer of compact waterproof polymer film on the surface of a metal hydride wafer by using a Chemical Vapor Deposition (CVD) technology, then placing a test piece in a metallographic sample making machine for processing, and finally carrying out chemical vapor deposition on a new polished surface of a sheet to obtain the metal hydride sheet for extracting the terahertz characteristic wave. Through practical measurement, the method can effectively solve the problems, ensure the accuracy and reliability of the measurement result, and has important application value for obtaining the characteristic spectrum of the metal hydride.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a metal hydride thin sheet is provided, wherein the diameter of the metal hydride thin sheet is 10mm-20mm, and the thickness of the metal hydride thin sheet is 0.5mm-1 mm.
The method comprises the following steps:
(1) depositing a layer of compact waterproof polymer film on the surface of the metal hydride sheet to obtain a first sheet;
(2) placing the first sheet in a metallographic sample making machine for processing, and polishing to a set thickness to obtain a second sheet;
(3) and (3) carrying out chemical vapor deposition on the newly ground surface of the second sheet to obtain the metal hydride sheet for extracting the terahertz characteristic wave.
In the step (1), the metal hydride sheet is cleaned and then placed in a deposition chamber for vapor deposition, so that a layer of compact waterproof polymer film is deposited on the surface of the metal hydride sheet;
the deposition conditions were as follows: the temperature is 640-660 ℃, and the vacuum is 4.0-6.2 Pa;
initial metal hydride sheet size: the diameter is 10mm-20mm, and the thickness is 2mm-4 mm.
In step 1, the metal hydride sheet is circular.
In the step (2), the first sheet coated with the waterproof polymer film is placed on a metallographic sample making machine disc, the first sheet is fixed by using an air pressure transmission pressure rod equipped with the first sheet, and is ground by using a volatile solvent as a medium, wherein the grinding conditions are as follows: the pressure is 10N-30N, and the time is 40sec-2 min; grinding to a target size, and immediately putting the glass powder into a glass container filled with a volatile solvent; the volatile solvent is a solvent that does not react with the metal hydride.
In the step (2), the sand paper adopted in the grinding process is 500# -1000 #.
In the step (3), after cleaning the newly ground surface of the second sheet, placing the second sheet in a deposition chamber with the second sheet facing upwards for vapor deposition, wherein the deposition conditions are as follows: the temperature is 640-660 ℃, and the vacuum is 4.0-6.2 Pa.
In the steps (1) and (3), the cleaning treatment is ultrasonic cleaning, the ultrasonic frequency is 120Hz, the ultrasonic time is 3min-5min, and the cleaning medium is a volatile solvent which does not react with the metal hydride.
The waterproof polymer film in the steps (1) and (3) is composed of p-xylene ring dimer, and the film thickness is 0.02mm-0.05 mm.
In view of the foregoing problems, the present invention provides a method for preparing a metal hydride sheet. The method comprises the following 3 steps: the method comprises the steps of firstly depositing a layer of compact waterproof polymer film on the surface of a metal hydride wafer by using a Chemical Vapor Deposition (CVD) technology, then polishing the metal hydride wafer to a target thickness by using a metallographic sample preparation machine by using a volatile solvent as a medium, and finally depositing the waterproof film on a newly-polished surface of the metal hydride wafer by using vapor deposition to obtain the metal hydride wafer for extracting the terahertz characteristic wave.
The invention effectively solves the technical problems that the metal hydride with strong water chemical potential is easy to generate hydrolysis products under the atmospheric environment, so that the terahertz characteristic wave is distorted, and the nondestructive detection effect of the internal defects of the related materials is influenced. The invention combines the characteristics of a vapor deposition technology and a metallographic sample making machine, has good process repeatability, can control the thickness of the metal hydride sheet within the range of 0.5mm-1mm, can be used for extracting the terahertz characteristic wave of the metal hydride, lays a foundation for the terahertz nondestructive detection technology research of the internal defects of the metal hydride product, and has obvious improvement significance.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
Example 1
1) Performing ultrasonic cleaning treatment on a calcium hydride wafer (with the diameter of 15mm and the thickness of 3 mm) by using carbon disulfide as a medium, wherein the ultrasonic frequency is 120Hz, and the ultrasonic time is 3min-5 min.
2) Placing the calcium hydride wafer cleaned in the step 1) in a deposition chamber, and carrying out vapor deposition by taking the p-xylene ring dimer as a raw material, wherein the deposition process conditions are as follows: the temperature is 650 ℃, and the vacuum is 4.0Pa, thus obtaining the calcium oxide wafer coated with the protective film.
3) The calcium hydride wafer coated with the protective film is placed on a disc of a metallographic sample making machine, a sample is fixed by using an air pressure transmission compression bar equipped with the disc, and the disc is ground by using carbon disulfide as a medium, wherein the grinding process conditions are as follows: the abrasive paper is 500#, the pressure is 10N, and the time is 2 min; immediately after milling was completed, it was placed in a glass container containing carbon disulfide to provide a second sheet.
4) Ultrasonically cleaning a newly-ground surface of a second sheet by taking carbon disulfide as a medium, then placing the second sheet upwards in a deposition chamber for vapor deposition of a layer of waterproof protective film, wherein the deposition process conditions are as follows: and (3) obtaining the calcium hydride slice for extracting the terahertz characteristic wave at the temperature of 650 ℃ and under the vacuum of 4.0 Pa.
The calcium hydride flakes produced in this example were measured to have a thickness of 0.8mm and a surface water-repellent film thickness of 0.03mm, and the sample did not react with water.
Example 2
1) Performing ultrasonic cleaning treatment on a calcium hydride wafer (with the diameter of 10mm and the thickness of 3 mm) by using carbon disulfide as a medium, wherein the ultrasonic frequency is 120Hz, and the ultrasonic time is 3min-5 min.
2) Placing the calcium hydride wafer cleaned in the step 1) in a deposition chamber, and carrying out vapor deposition by taking the p-xylene ring dimer as a raw material, wherein the deposition process conditions are as follows: the temperature is 660 ℃, and the vacuum is 6.2Pa, so that the calcium oxide wafer coated with the protective film is obtained.
3) The calcium hydride wafer coated with the protective film is placed on a disc of a metallographic sample making machine, a sample is fixed by using an air pressure transmission compression bar equipped with the disc, and the disc is ground by using carbon disulfide as a medium, wherein the grinding process conditions are as follows: the abrasive paper is 1000#, the pressure is 30N, and the time is 1 min; immediately after milling was complete, it was placed in a glass container containing carbon disulfide.
4) Ultrasonically cleaning the newly ground surface of the calcium hydride wafer prepared in the step 3) by taking carbon disulfide as a medium, then placing the wafer upwards in a deposition chamber for vapor deposition of a layer of waterproof protective film, wherein the deposition process conditions are as follows: and (3) obtaining the calcium hydride slice for extracting the terahertz characteristic wave at the temperature of 660 ℃ and under the vacuum of 6.2 Pa.
The calcium hydride flakes produced in this example were measured to have a thickness of 0.5mm and a surface water-repellent film thickness of 0.02mm, and the samples were not reacted with water.
Example 3
1) Performing ultrasonic cleaning treatment on a calcium hydride wafer (with the diameter of 20mm and the thickness of 3 mm) by using carbon disulfide as a medium, wherein the ultrasonic frequency is 120Hz, and the ultrasonic time is 3min-5 min.
2) Placing the calcium hydride wafer cleaned in the step 1) in a deposition chamber, and carrying out vapor deposition by taking a p-xylene ring dimer as a raw material to obtain a calcium oxide wafer coated with a protective film; the deposition process conditions were as follows: the temperature is 640 ℃, and the vacuum is 5.0 Pa.
3) The calcium hydride wafer coated with the protective film is placed on a disc of a metallographic sample making machine, a sample is fixed by using an air pressure transmission compression bar equipped with the disc, and the disc is ground by using carbon disulfide as a medium, wherein the grinding process conditions are as follows: the abrasive paper is 700#, the pressure is 20N, and the time is 40 sec; immediately after milling was complete, it was placed in a glass container containing carbon disulfide.
4) Ultrasonically cleaning the newly ground surface of the calcium hydride wafer prepared in the step 3) by taking carbon disulfide as a medium, then placing the wafer upwards in a deposition chamber for vapor deposition of a layer of waterproof protective film, wherein the deposition process conditions are as follows: and (3) obtaining the calcium hydride slice for extracting the terahertz characteristic wave at the temperature of 640 ℃ and under the vacuum of 5.0 Pa.
The calcium hydride flakes produced in this example were measured to have a thickness of 1.0mm, a surface waterproofing membrane thickness of 0.05mm, and the sample was not reacted with water.
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.

Claims (8)

1. The preparation method of the metal hydride flake is characterized in that the diameter of the metal hydride flake is 10mm-20mm, and the thickness of the metal hydride flake is 0.5mm-1 mm;
the method comprises the following steps:
(1) depositing a layer of compact waterproof polymer film on the surface of the metal hydride sheet to obtain a first sheet;
(2) placing the first sheet in a metallographic sample making machine for processing, and polishing to a set thickness to obtain a second sheet;
(3) performing chemical vapor deposition on a newly ground surface of the second sheet to obtain a metal hydride sheet for extracting the terahertz characteristic wave;
the metal hydride is calcium hydride, and the waterproof polymer film takes a p-xylene ring dimer as a raw material.
2. The method for preparing a metal hydride sheet as claimed in claim 1, wherein in the step (1), the metal hydride sheet is cleaned and then placed in a deposition chamber for vapor deposition, thereby depositing a layer of dense waterproof polymer film on the surface of the metal hydride sheet;
the deposition conditions were as follows: the temperature is 640-660 ℃, and the vacuum is 4.0-6.2 Pa;
initial metal hydride sheet size: the diameter is 10mm-20mm, and the thickness is 2mm-4 mm.
3. The method for preparing a metal hydride sheet as claimed in claim 1, wherein in the step 1, the metal hydride sheet is circular.
4. The method for preparing a metal hydride foil as claimed in any one of claims 1 to 3, wherein in the step (2), the first sheet coated with the waterproof polymer film is placed on a disc of a metallographic sample preparation machine, the first sheet is fixed by a pneumatic transmission pressure rod provided with the disc, and grinding is performed by using a volatile solvent as a medium under the following grinding conditions: the pressure is 10N-30N, and the time is 40sec-2 min; grinding to a target size, and immediately putting the glass powder into a glass container filled with a volatile solvent; the volatile solvent is a solvent that does not react with the metal hydride.
5. The method for producing a metal hydride sheet as claimed in claim 4, wherein in the step (2), the sand paper used for the grinding is 500# -1000 #.
6. The method for producing a metal hydride sheet as claimed in claim 1, wherein in the step (3), after cleaning the freshly ground surface of the second sheet, the second sheet is placed in a deposition chamber facing upward for vapor deposition under the following conditions: the temperature is 640-660 ℃, and the vacuum is 4.0-6.2 Pa.
7. The method for producing a metal hydride sheet as claimed in any one of claims 2 and 6, wherein in the steps (1) and (3), the cleaning treatment is ultrasonic cleaning with an ultrasonic frequency of 120Hz for 3min to 5min, and the cleaning medium is a volatile solvent which does not react with the metal hydride.
8. The method for preparing a metal hydride foil as claimed in any one of claims 1, 2 and 6, wherein the waterproof polymer film in the steps (1) and (3) has a composition of p-xylene dimer, and the film thickness is 0.02mm to 0.05 mm.
CN201711103823.7A 2017-11-10 2017-11-10 Preparation method of metal hydride thin sheet Expired - Fee Related CN107697886B (en)

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CN110522129A (en) * 2019-09-29 2019-12-03 东莞市瑞翔新型材料科技有限公司 A kind of water-proof metal zipper and its manufacture craft
US11874223B1 (en) 2022-08-30 2024-01-16 The Goodyear Tire & Rubber Company Terahertz characterization of a multi-layered tire tread

Citations (8)

* Cited by examiner, † Cited by third party
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GB896038A (en) * 1959-04-29 1962-05-09 Eastwood Plastics Ltd Method of generating hydrogen by the interaction of water and lithium hydride and the like
WO2005008761A1 (en) * 2003-07-10 2005-01-27 Honeywell International Inc. Layered components, materials, methods of production and uses thereof
CN1636863A (en) * 2003-11-19 2005-07-13 气体产品与化学公司 Removal of sulfur-containing impurities from volatile metal hydrides
CN103728167A (en) * 2013-12-23 2014-04-16 四川材料与工艺研究所 Long-term preservation method and observation method of light metal hydride metallographic specimen
CN103979496A (en) * 2014-04-30 2014-08-13 北京理工大学 Antioxidation method of light rare earth metal hydride
CN107004843A (en) * 2014-12-10 2017-08-01 巴斯夫公司 metal hydride compositions and lithium ion battery
CN107021864A (en) * 2017-05-27 2017-08-08 河南纳宇滤材有限公司 A kind of metal hydride in-situ polymerization coats passivating method
CN107043907A (en) * 2016-02-06 2017-08-15 北京有色金属研究总院 A kind of metal hydride surface hydrogen permeation barrier and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB896038A (en) * 1959-04-29 1962-05-09 Eastwood Plastics Ltd Method of generating hydrogen by the interaction of water and lithium hydride and the like
WO2005008761A1 (en) * 2003-07-10 2005-01-27 Honeywell International Inc. Layered components, materials, methods of production and uses thereof
CN1636863A (en) * 2003-11-19 2005-07-13 气体产品与化学公司 Removal of sulfur-containing impurities from volatile metal hydrides
CN103728167A (en) * 2013-12-23 2014-04-16 四川材料与工艺研究所 Long-term preservation method and observation method of light metal hydride metallographic specimen
CN103979496A (en) * 2014-04-30 2014-08-13 北京理工大学 Antioxidation method of light rare earth metal hydride
CN107004843A (en) * 2014-12-10 2017-08-01 巴斯夫公司 metal hydride compositions and lithium ion battery
CN107043907A (en) * 2016-02-06 2017-08-15 北京有色金属研究总院 A kind of metal hydride surface hydrogen permeation barrier and preparation method thereof
CN107021864A (en) * 2017-05-27 2017-08-08 河南纳宇滤材有限公司 A kind of metal hydride in-situ polymerization coats passivating method

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