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Method for preparing standard sample for testing content of hard-alloy components and method for testing content of hard-alloy components

A technology of cemented carbide and standard samples, which is applied in the field of X-ray fluorescence spectroscopic analysis, can solve the problems of difficult uniformity of high-purity oxides, high operation requirements, and long grinding time, so as to remove the limitation of cemented carbide detection methods and shorten the Process and time, avoiding the effect of cumbersome valuation

Active Publication Date: 2012-07-04
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] ① Since most elements of tungsten-based cemented carbide are extremely difficult to dissolve, it is necessary to use highly corrosive hydrofluoric acid and it is extremely difficult to digest at room temperature, and adding unnecessary impurity elements to the standard solution will introduce unnecessary impurity elements, and it must be dried to test sample, high operating requirements
[0007] ②Chemical methods must be used to determine the value after the artificial standard samples are prepared according to the same process as the production method, and the workload is relatively large
[0008] ③The method of directly weighing high-purity oxides to prepare standard samples, the sample size is too small, resulting in large errors; but if the sample size is increased for preparation, it is necessary to grind the high-purity oxides to uniformity, and the high-purity Oxide is not uniform, takes too long to grind and stains easily
[0009] So far, the existing standard sample preparation technology still cannot solve the above problems

Method used

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  • Method for preparing standard sample for testing content of hard-alloy components and method for testing content of hard-alloy components
  • Method for preparing standard sample for testing content of hard-alloy components and method for testing content of hard-alloy components
  • Method for preparing standard sample for testing content of hard-alloy components and method for testing content of hard-alloy components

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preparation example Construction

[0022] According to one aspect of the present invention, the preparation method of the standard sample for determining the composition of cemented carbide by X-ray fluorescence spectrometry includes the following steps.

[0023] Step 1: Weigh a certain mass of single oxide, add flux according to the dilution ratio of 1:10~1:100, add flux 0.1~1 times the mass of flux and 0.1~2g release agent at the same time, mix well Then put it into a muffle furnace or a high-frequency automatic melting machine, heat it to 700 ° C ~ 1200 ° C for 5 ~ 40 minutes, and then place it to cool and automatically demould to obtain a single oxide glass fusion sheet, and prepare a variety of single oxide glass fusion sheets as required. piece. Preferably, the mixture of a single oxide, a flux, a co-solvent, and a release agent is melted at a temperature of 1150° C. for 25 minutes. If it is heated in a muffle furnace, it needs to be taken out and shaken once during the period; if it is heated in a high-...

Embodiment 1

[0039] Preparation of single oxide tantalum trioxide glass fusing powder

[0040] Taking the single oxide tantalum trioxide as an example to illustrate the preparation process and advantages of the single oxide glass frit powder in the standard sample preparation method of the present invention.

[0041] A. Weigh 0.2000g of high-purity tantalum trioxide, add 4.000g of lithium tetraborate at a dilution ratio of 1:20, and add 0.400g of lithium carbonate 0.1 times the mass of lithium tetraborate flux as a flux and 0.5g of lithium tetraborate at the same time. Ammonium iodide was used as a mold release agent, mixed evenly, put into a muffle furnace, heated to 1150°C and melted for 25 minutes, taken out and shaken once during the period, and then left to cool and automatically released from the mold to obtain a tantalum trioxide glass frit. Weigh the tantalum trioxide glass frit, calculate the mass of tantalum trioxide contained in the tantalum trioxide glass frit per unit mass, an...

Embodiment 2

[0050] Preparation of standard samples

[0051] Prepare two grades of tungsten-based cemented carbide standard samples to illustrate the preparation steps in the standard sample preparation method of the present invention.

[0052] Weigh 0.2000g of a single oxide, add 4.000g of lithium tetraborate at a dilution ratio of 1:20, and simultaneously add 0.400g of lithium carbonate that is 0.1 times the mass of lithium tetraborate flux as a flux and 0.5g of ammonium iodide as a flux. Release agent, mixed evenly, put into muffle furnace, heated to 1150°C and melted for 25 minutes, took out and shaked once during the period, then left to cool and automatically released from the mold to obtain a single oxide glass frit. In this example, cobalt trioxide glass frits, nickel sesquioxide glass frits, ferric oxide glass frits, chromium oxide glass frits, tantalum pentoxide glass frits, pentoxide glass frits, Niobium glass frit, tungsten trioxide glass frit.

[0053] Weigh each of the abov...

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Abstract

The invention discloses a method for preparing a standard sample for testing the content of hard-alloy components by adopting the X-ray fluorescence spectrometry and a method for testing the content of hard-alloy components by adopting the X-ray fluorescence spectrometry. The method for preparing the standard sample comprises the following steps: preparing a variety of high-purity single oxide glass fuse pieces under the same condition of preparing glass fuse pieces of the sample under test; grinding the high-purity single oxide glass fuse pieces into powder and filling the powder into bottles respectively; weighting the powder of the high-purity single oxide glass fuse pieces, which comprises a variety of elements under test in the sample under test, to prepare the standard sample, wherein the range of the content of a variety of elements of the standard sample covers the range of the content of a variety of elements of the sample under test; and finally preparing the glass fuse pieces of the standard sample according to the method. A working curve is made by using the glass fuse pieces of the standard sample, and then the content of a variety of elements of the hard alloy sample under test are tested by adopting the X-ray fluorescence spectrometry. Due to the adoption of the standard sample prepared by using the method of the invention, the limit to the detection method of the hard alloy, which is caused by the standard sample, can be eliminated, the accuracy of the result can be improved, and the application range of the X-ray fluorescence spectrometry can be expanded.

Description

technical field [0001] The invention belongs to the technical field of X-ray fluorescence spectrometry analysis, in particular, it relates to a method for measuring samples by X-ray fluorescence spectrometry and a method for preparing standard samples used therein, and more specifically, relates to a method for measuring X-ray fluorescence spectrometry Methods of cemented carbide compositions and the preparation of standard samples for their use. Background technique [0002] There are many grades of cemented carbide, and the range of element content of various product grades varies greatly, and the content of each component directly affects the performance of the finished cemented carbide. Therefore, it is necessary to quickly and accurately determine The content of each metal element in the pre-sintering mixture of cemented carbide and cemented carbide products is particularly important. X-ray fluorescence spectrometry is widely used because of its fast analysis speed, hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N23/223
Inventor 彭慧仙成勇
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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