Method for testing thickness of oxide layer on surface of micro-nano aluminum ball

A technology of surface oxidation and testing methods, applied in measuring devices, material analysis using radiation diffraction, instruments, etc., can solve the problem of reducing the size of aluminum balls, and achieve accurate characterization and strong operability

Active Publication Date: 2019-10-01
XI'AN PETROLEUM UNIVERSITY
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  • Abstract
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  • Application Information

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Problems solved by technology

At present, the aluminum powder in TATB-based aluminum-containing explosives is mainly composed of aluminum spheres with diameters on the order of micronano, and with the gradual increase in the demand for energy parameters of energetic materials in practical applications, the size of aluminum spheres gradually decreases, which is a quantitative Characterizing the Thickness of the Oxide Layer on Aluminum Balls Presents Challenges

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  • Method for testing thickness of oxide layer on surface of micro-nano aluminum ball
  • Method for testing thickness of oxide layer on surface of micro-nano aluminum ball
  • Method for testing thickness of oxide layer on surface of micro-nano aluminum ball

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Embodiment 1

[0060] Such as figure 2 As shown, 2g of aluminum powder is dispersed on the surface of the conductive adhesive, put into the vacuum chamber of the focused ion beam system, and the air pressure is pumped to 10 -4 Pa; under the electronic imaging system of focused ion beam, choose such as image 3 Individual aluminum spheres around 10 μm in diameter are shown. Deposit a Pt protective layer on the surface of the aluminum ball to be processed through a gas injection system, and the current density of the ion beam during the deposition process is 4pA / μm 2 , with a deposition time of 2 minutes, we get Figure 4 The Pt protective layer with a thickness of about 1 μm on the surface of the aluminum ball shown; Figure 5 with Image 6 As shown, the Ga ion beam is used to cut the target area, the ion beam current is 3nA, and the aluminum ball matrix is ​​removed along both sides of the Pt protective layer to obtain a thin slice sample with a thickness of 2 μm; Figure 7 shown by 2p...

Embodiment 2

[0062] Disperse 3g of aluminum powder on the surface of the conductive adhesive, put it into the vacuum chamber of the focused ion beam system, and pump the air pressure to 10 - 4 Pa; a single aluminum sphere with a diameter of around 5 μm was selected under an electron imaging system with a focused ion beam. Deposit a Pt protective layer on the surface of the aluminum ball to be processed through a gas injection system, and the current density of the ion beam during the deposition process is 2pA / μm 2 , the deposition time was 1min, and a Pt protective layer with a thickness of about 1.3 μm on the surface of the aluminum ball was obtained; the Ga ion beam was used to cut the target area, the ion beam current was 2nA, and the aluminum ball matrix was removed along both sides of the Pt protective layer, and the thickness was obtained 2μm flake samples; pass 2pA / μm 2 The Pt ion beam deposition connects the nano-manipulator probe to the sheet by welding, and the sheet can be mov...

Embodiment 3

[0064] Disperse 5g of aluminum powder on the surface of the conductive adhesive, put it into the vacuum chamber of the focused ion beam system, and pump the air pressure to 10 - 4 Pa; a single aluminum sphere with a diameter of around 3 μm was selected under an electron imaging system with a focused ion beam. Deposit a Pt protective layer on the surface of the aluminum ball to be processed through a gas injection system, and the current density of the ion beam during the deposition process is 2pA / μm 2 , the deposition time was 1min, and a Pt protective layer with a thickness of about 1.5 μm on the surface of the aluminum ball was obtained; the Ga ion beam was used to cut the target area, and the ion beam current was 3nA, and the aluminum ball matrix was removed along both sides of the Pt protective layer, and the thickness was obtained. 1μm flake sample; pass 2pA / μm 2 The Pt ion beam deposition connects the nano-manipulator probe to the sheet by welding, and the sheet can be...

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Abstract

The invention discloses a method for testing the thickness of an oxide layer on the surface of a micro-nano aluminum ball. According to the method, micro-nano aluminum balls are subjected to micro-nano processing by adopting a double-beam focused ion beam system; through metal protection layer deposition and ion beam cutting, on the premise that the oxide layer on the surface of an aluminum ball is not damaged, the aluminum balls are processed into a final slice sample with the thickness capable of being represented by a high-resolution transmission electron microscope, and scanning and analyzing of the distribution rule of each element in the interface region of the aluminum ball and a protection layer are carried out by adopting an energy spectrum line of a transmission electron microscope, so that the thickness of the oxide layer on the surface is obtained; and the method is simple and effective, high in operability and capable of accurately representing the thickness of the oxide layer on the surface of the micro-nano aluminum ball.

Description

【Technical field】 [0001] The invention belongs to the technical field of micro-nano processing and characterization of materials, and in particular relates to a method for testing the thickness of an oxide layer on the surface of a micro-nano aluminum sphere. 【Background technique】 [0002] Triaminotrinitrobenzene (TATB)-based aluminum-containing explosives is one of the energetic materials widely used in missile warheads. However, the presence of chlorine residues in the synthesis process of TATB explosives will easily lead to oxidation on the surface of aluminum powder, thereby reducing the activity of aluminum powder and the key energy parameters of TATB. How to characterize the degree of oxidation on the surface of aluminum powder plays an important role in evaluating the activity of aluminum powder and the service life of TATB. At present, the activity of aluminum powder is mainly evaluated by indirect experimental means. For example, the elemental aluminum content me...

Claims

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Application Information

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IPC IPC(8): G01B15/02G01N23/04G01N23/20
CPCG01B15/02G01N23/04G01N23/20
Inventor 刘帅陈捷睢贺良
Owner XI'AN PETROLEUM UNIVERSITY
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