Pretreatment method for silicon carbide powder sample to be tested by using laser ablation inductively coupled plasma mass spectrometry

A silicon carbide powder and laser ablation technology, applied in the field of analytical chemistry, can solve problems such as poor viscosity, detection of elements affecting the content and distribution, etc., and achieve the effect of good application prospects.

Active Publication Date: 2015-05-13
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, some samples (such as silicon carbide) have poor viscosity. When preparing them into block samples, it is often necessary to add certain binders, such as boric acid, polyvinyl alcohol (PVA), methyl cellulose, etc.
Adding a binder is helpful to the shape of the sample, but it is easy to introduce impurities, and the uniformity of mixing the binder with the sample affects the detection of the content and distribution of elements in the sample

Method used

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  • Pretreatment method for silicon carbide powder sample to be tested by using laser ablation inductively coupled plasma mass spectrometry
  • Pretreatment method for silicon carbide powder sample to be tested by using laser ablation inductively coupled plasma mass spectrometry
  • Pretreatment method for silicon carbide powder sample to be tested by using laser ablation inductively coupled plasma mass spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Weigh 1.0 g of silicon carbide (micron particle size), grind and sieve (200 mesh). Use manual tablet press, holding time 30s, pressure is 10Mpa, it is prepared into of small discs. The prepared silicon carbide wafer was sintered in a muffle furnace at a temperature of 1000°C, and the temperature was programmed to rise from room temperature to 500°C after 1.5 hours; then, the temperature was raised from 500°C to 500°C after 1.5 hours. to 1000°C; keep at 1000°C for 2 hours; then cool down from 1000°C to 500°C in 1.5 hours; finally cool down from 500°C to room temperature in 1.5 hours. After sintering, it was measured by laser ablation inductively coupled plasma mass spectrometry.

Embodiment 2

[0039] Weigh 1.0 g of silicon carbide (nanoscale particle size), grind and sieve (200 mesh). Use manual tablet press, holding time 30s, pressure is 10Mpa, it is prepared into of small discs. The prepared silicon carbide wafer was sintered in a muffle furnace at a temperature of 1000°C, and the temperature was programmed to rise from room temperature to 500°C after 1.5 hours; then, the temperature was raised from 500°C to 500°C after 1.5 hours. to 1000°C; keep at 1000°C for 2 hours; then cool down from 1000°C to 500°C in 1.5 hours; finally cool down from 500°C to room temperature in 1.5 hours. After sintering, it was measured by laser ablation inductively coupled plasma mass spectrometry.

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Abstract

The invention relates to a pretreatment method for a silicon carbide powder sample to be tested by using a laser ablation inductively coupled plasma mass spectrometry. The silicon carbide powder sample is produced into a blocky sample which is suitable for being tested by using the laser ablation inductively coupled plasma mass spectrometry through using the pretreatment method. The pretreatment methods comprises the steps: (1) grinding and sieving silicon carbide powder; (2) directly pressing the sieved silicon carbide powder into wafers by using a manual tablet press, wherein the pressure is 8-12Mpa, and the pressure maintaining time lasts for 30-50 seconds; (3) carrying out temperature programming on the wafers to 1000 DEG C, and preserving heat and sintering for 2 hours; (4) carrying out programmed cooling to room temperature.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a pretreatment method for a silicon carbide powder sample suitable for analysis and determination by laser ablation inductively coupled plasma mass spectrometry. Background technique [0002] Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) uses a high-energy laser to melt, sputter and evaporate the sample surface, and the vapor and fine particles generated are directly brought into the plasma by the carrier gas for absorption, dissociation and ionized, and then filtered by a mass spectrometer system to detect the analyte. LA-ICP-MS is a solid sampling analysis technique, which requires the sample to be a block solid with a certain strength. For chip, granular and powdery samples, in order to avoid the carrier gas from blowing the powder into ICP-MS and generating non-ablative signals, it needs to be processed into bulk solids. [0003] However, some samp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28
Inventor 汪正周慧朱燕李青
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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