Preparation method of mixed salt solution for co-precipitation synthesis of aluminate electron emission materials

An electron emission material and aluminate technology, which is applied in thermionic cathode manufacturing, discharge tube/lamp parts, circuits, etc., can solve the problem that the chemical composition of aluminate cannot be kept consistent in design, and the composition and performance of synthetic aluminate Consistency can not be guaranteed and other problems, to achieve the effect of high accuracy, good repeatability and stability, and reasonable process design

Active Publication Date: 2020-02-21
NANJING TECH UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

Since commercially available nitrates contain trace impurities, adsorbed water, and crystallized water, it is almost impossible to obtain a mixed salt solution for coprecipitation reaction with precise control of the proportion of each element component by direct weighing, which will inevitably lead to the synthesis of aluminate The chemical composition cannot be consistent with the design composition; moreover, when raw material batches or manufacturers are replaced, the consistency of the synthetic aluminate composition and its performance cannot be guaranteed

Method used

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  • Preparation method of mixed salt solution for co-precipitation synthesis of aluminate electron emission materials
  • Preparation method of mixed salt solution for co-precipitation synthesis of aluminate electron emission materials

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Effect test

Embodiment 1

[0017] The chemically pure barium nitrate purchased from Xilong Chemical Co., Ltd. and deionized water were prepared into a barium nitrate solution with a mass concentration of 4%. After a certain weight was weighed, it was poured into a 255.15-gram barium nitrate solution calcined at 1300°C to a constant weight. Crucible (alumina content is 99.3%), weigh the solution and the accurate mass of the crucible is 411.15 grams, first put the crucible in an oven at 100°C for 24 hours, then place it in an electric furnace and calcinate at 200°C to constant weight, weigh and calcinate The exact weight of the product, together with the crucible, was 261.39 grams, resulting in a weight of 6.24 grams of calcined barium nitrate. The chemically pure calcium nitrate purchased from Xilong Chemical Co., Ltd. and deionized water were prepared into a calcium nitrate solution with a mass concentration of 20%. After a certain weight was weighed, it was poured into calcination at 1300°C to constant ...

Embodiment 2

[0023]The chemically pure barium nitrate and deionized water purchased from Sinopharm Group Chemical Reagent Co., Ltd. were prepared into a barium nitrate solution with a mass concentration of 12%. After a certain weight was weighed, it was poured into a 269.39 g barium nitrate solution calcined at 1400°C to a constant weight. Crucible (alumina content is 99.5%), weigh the solution and the accurate mass of the crucible is 421.45 grams, first put the crucible in an oven at 150 ° C for 12 hours, then place it in an electric furnace and calcined at 500 ° C to constant weight, weigh and calcined The exact weight of the product, together with the crucible, was 287.64 grams, resulting in a weight of 18.25 grams of calcined barium nitrate. The chemically pure calcium nitrate purchased from Sinopharm Group Chemical Reagent Co., Ltd. and deionized water were prepared into a calcium nitrate solution with a mass concentration of 45%. After a certain weight was weighed, it was poured into ...

Embodiment 3

[0029] The chemically pure barium nitrate purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. and deionized water were prepared into a barium nitrate solution with a mass concentration of 8%, weighed a certain weight, poured it into calcination at 1400°C to constant weight, and the weight was 258.35 gram of crucible (aluminum oxide content is 99.7%), weigh the solution and the accurate mass of the crucible is 410.28 grams, first put the crucible in a 120°C oven and bake it for 18 hours, then place it in an electric furnace and calcinate it to constant weight at 400°C, weigh Measure the calcined product together with the accurate weight of the crucible of 270.50 grams to obtain a weight of 12.15 grams of calcined barium nitrate. The chemically pure calcium nitrate purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. and deionized water were prepared into a calcium nitrate solution with a mass concentration of 30%. Weighed a certain weight and poured it i...

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Abstract

The invention provides a preparation method of a mixed salt solution for coprecipitation synthesis of an aluminate electron emissive material. The method comprises the following steps that (1) bariumnitrate, calcium nitrate and aluminum nitrate solutions are weighed accurately, and dried, sintered and weighed accurately to obtain the weights of barium nitrate, calcium nitrate and aluminum nitrate; (1) the purity of the barium nitrate, calcium nitrate and aluminum nitrate in the sintered barium nitrate, calcium nitrate and aluminum nitrate is measured accurately; (3) the weights of barium nitrate, calcium nitrate and aluminum nitrate after drying and sintering of a 100g of barium nitrate solution, a 100g of calcium nitrate solution and a 100g of aluminum nitrate solution are calculated respectively; (4) the needed weights of the barium nitrate, calcium nitrate and aluminum nitrate solutions are calculated to the chemical composition and weight of an aluminate to be prepared; and (5) the barium nitrate, calcium nitrate and aluminum nitrate solutions are weighed accurately according to a calculation result, and mixed to obtain the mixed salt solution for coprecipitation synthesis ofthe aluminate electron emissive material. The preparation method is reasonable in technical design and easy to operation.

Description

technical field [0001] The invention belongs to the field of microwave electric vacuum device manufacture, in particular to a method for preparing a mixed salt solution for co-precipitation and synthesis of aluminate electron emission materials. Background technique [0002] The cathode is the "heart" of microwave vacuum electronic devices, and plays a vital role in the power output and life of high-power microwave devices. The impregnated barium tungsten cathode is composed of a porous tungsten matrix and an aluminate electron emission material impregnated in it. It has the characteristics of high emission current density and excellent anti-poisoning performance. It is used in medium and high-power microwave electric vacuum electronic devices. most widely. The performance of the impregnated barium tungsten cathode mainly depends on the chemical composition of the aluminate electron emission material and the uniformity of the composition distribution of each element. Resea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01J9/04H01J1/144
CPCH01J1/144H01J9/04
Inventor 魏建君李婧琳冯永宝
Owner NANJING TECH UNIV
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