Method for preparing polycrystalline materials by aid of high-throughput hybridization microwave synthesis processes
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A polycrystalline material and microwave synthesis technology, applied in the magnetic field, can solve the problems of slow heating rate and achieve the effects of high heating efficiency, high heating rate and shortened synthesis time
Inactive Publication Date: 2016-12-07
SHANGHAI UNIV
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[0010] R TiO 3 Polycrystalline has been prepared by traditional solid-state reaction method before, because trivalent titanate is easy to generate derivatives of other components when heated to around 300 °C
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Embodiment 1
[0052] In this example, see Figure 1~3 , a high-throughput hybrid microwave synthesis method R TiO 3 A method for a polycrystalline material, comprising the steps of:
[0053] (1) Preparation of initial raw materials and preforming process:
[0054] The purity is 99.8% Ti respectively 2 o 3 and Nd with a purity of 99.9% 2 o 3 、Sm 2 o 3 and La 2 o 3 As the starting material, the Sm 2 o 3 、Nd 2 o 3 and La 2 o 3 respectively with Ti 2 o 3 After weighing according to the molar ratio of 1:1, the Sm 2 o 3 、Nd 2 o 3 and La 2 o 3 respectively with Ti 2 o 3 Fully mixed, in a hand box under an inert gas environment, grind and fully mix 3 kinds of reaction raw materials with different proportions with an agate mortar to obtain 3 kinds of mixed raw material powders;
[0055] (2) Blank forming:
[0056] The mixed raw material powders fully mixed in the step (1) were put into the mold respectively, and then isostatically pressed under a pressure of 10 MPa to prep...
Embodiment 2
[0062] This embodiment is basically the same as Embodiment 1, especially in that:
[0063] In this example, a high-throughput hybrid microwave synthesis method was used to prepare Na x WO 3 A method for a polycrystalline material, comprising the steps of:
[0064] ① Preparation of initial raw materials and preforming process:
[0065] Using pure WO 3 、Na 2 WO 4 2H 2 O and W powder are used as initial reaction raw materials, according to the following reaction equation:
[0066] Na 2 WO 4 + WO3+ W=Na x WO 3
[0067] The ratio of the reactants participating in the chemical reaction is matched, and the ratio of 0x x WO 3 Prepare a series of initial reaction raw material mixtures for each component point, and then use an agate mortar to grind and fully mix the reaction raw material mixtures with different proportions in a hand box under an inert gas environment to obtain a mixed raw material powder;
[0068] ② Blank forming:
[0069] The mixed raw material powd...
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Abstract
The invention discloses a method for preparing polycrystalline materials by the aid of high-throughput hybridization microwave synthesis processes. The method includes weighing high-purity substance powder in glove boxes according to molar ratios; sufficiently grinding and mixing the high-purity substance powder and manufacturing wafer biscuits by the aid of tablet presses; arranging reactants in cylindrical aluminum oxide crucibles; heating the reactants in microwave ovens by the aid of SiC which is used as a heat conduction material. The method has the advantages that a plurality of samples or different composition points of the same sample can be simultaneously prepared in a high-throughput manner; the samples can be heated by the aid of microwave, the SiC is used as the heat conduction material, accordingly, the temperatures of the samples can reach required reaction temperatures within extremely short time, and the polycrystalline materials can be quickly and economically synthesized in a high-throughput manner; the polycrystalline materials can be prepared in the high-throughput manner by the aid of the method, the shortcoming of limitation on the reaction temperature and the reaction time in existing sample preparation procedures can be overcome, and the polycrystalline materials can be efficiently synthesized; synthesized tungsten bronze series AxWO3 (A=Na, Ca and B) and rare earth titanium compounds RTiO3 (R represents rare earth elements) which are prepared by the aid of the method are crystals, and accordingly the method can be widely applied to the field of technologies for preparing magnetic, superconducting and relevant materials.
Description
technical field [0001] The invention relates to a method for preparing polycrystalline materials, in particular to a method for preparing polycrystalline materials by a high-temperature solid-state reaction method, which is applied in the technical fields of magnetism, superconductivity and related material preparation. Background technique [0002] "Materials high-throughput experiment" is to complete the preparation and characterization of a large number of samples in a short time. Its core idea is to change the sequential iterative method used in traditional materials research to parallel processing, and to cause qualitative changes in the efficiency of materials research with quantitative changes. [0003] In 1970, Hanak first proposed the concept of "multi-sample experiment" and applied it to the study of binary and ternary superconducting materials in thin film form. sample array. In 2011, U.S. President Barack Obama signed the "Materials Genome Initiative (MGI)" tec...
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