Method for making sample of chemical deposited nickel fixed alloy powder for transmission electron microscope observing

A technology for chemical deposition of nickel and chemical deposition, which is applied in the field of sample preparation for transmission electron microscopy experiments, can solve the problems of low success rate, high cost, complicated electroplating method and process flow, etc., and achieves the effect of high sample preparation success rate.

Inactive Publication Date: 2003-05-28
UNIV OF SCI & TECH BEIJING
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Problems solved by technology

[0003] The invention solves the problems of complex process flow, low success rate and high cost of the electroplating method

Method used

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  • Method for making sample of chemical deposited nickel fixed alloy powder for transmission electron microscope observing
  • Method for making sample of chemical deposited nickel fixed alloy powder for transmission electron microscope observing
  • Method for making sample of chemical deposited nickel fixed alloy powder for transmission electron microscope observing

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Experimental program
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Embodiment Construction

[0027] 1. Determination of chemical deposition ratio and experimental conditions

[0028] Pre-test chemical nickel plating deposition solution formula and experimental conditions are as follows:

[0029] Deposition solution: nickel sulfate (25g / l) + sodium hypophosphite (22.5g / l) + anhydrous sodium acetate (15g / l) + citric acid (2g / l) + lead acetate (5 drops / l);

[0030] PH value of deposition solution: 4.6;

[0031] Experimental temperature: 88°C.

[0032] Substrate and powder: wash with 5% hydrochloric acid alcohol solution (30 minutes), and then evenly distribute nickel-based powder superalloy (FGH95) powder particles (Φ50-150μm) on the activated copper block

[0033] In order to determine the optimal ratio of deposition solution and find out the influence rules of various factors, the influence of nickel sulfate content, sodium hypophosphite content, sodium acetate content and citric acid content on the deposition rate was done by using mathematical statistics orthogonal...

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Abstract

A process for preparing the specimen of chemically deposited nickel fixed alloy powder in order to observe it by transmission electron microscope includes preparing deposition solution in beaker, slowly putting the copper block coated with powder on an insulating plate in said solution, putting the beaker in water bath at 83-92 deg.C, chemical depositing for 4-6 hr, tearing the deposited film from the copper block, sticking it to frosted glass, abrasing to 30-50 microns by abrasive paper, punching to become small circular film with 3 mm of diameter, and ion thinning. Its advantages are easy control and high successful rate.

Description

Technical field: [0001] The invention belongs to the technical field of transmission electron microscope (TEM) experimental sample preparation. Background technique: [0002] In the preparation of alloys by powder metallurgy, the solidification structure characteristics and phase composition of the basic powder particles of the alloy will directly affect the microstructure of the powder solidified (cold, hot isostatic pressing, etc.), which ultimately affects the mechanical properties of the material. performance. In order to optimize the milling process and select subsequent processing parameters, it is usually necessary to systematically study the solidification structure characteristics of the original powder particles. Due to the fine powder particles (between tens of microns and hundreds of microns), it is suitable for transmission electron microscope (TEM) observation. The sample preparation is very difficult, which has troubled most of the material structure research...

Claims

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Application Information

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IPC IPC(8): G01N1/28
Inventor 胡本芙李慧英陈焕铭宋铎
Owner UNIV OF SCI & TECH BEIJING
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