CN108766859B - Preparation method of mixed salt solution for coprecipitation synthesis of aluminate electron emission material - Google Patents
Preparation method of mixed salt solution for coprecipitation synthesis of aluminate electron emission material Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/13—Solid thermionic cathodes
- H01J1/14—Solid thermionic cathodes characterised by the material
- H01J1/144—Solid thermionic cathodes characterised by the material with other metal oxides as an emissive material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/04—Manufacture of electrodes or electrode systems of thermionic cathodes
Abstract
The invention provides a preparation method of a mixed salt solution for coprecipitation synthesis of an aluminate electron emission material, which comprises the following steps: (1) accurately weighing barium nitrate, calcium nitrate and aluminum nitrate solution, drying and calcining, and accurately weighing the mass of the obtained calcined barium nitrate, calcium oxide and aluminum oxide; (2) accurately measuring the purity of barium nitrate, calcium oxide and aluminum oxide in the calcined barium nitrate, calcium oxide and aluminum oxide; (3) calculating the mass of pure barium nitrate, calcium oxide and aluminum oxide obtained by drying and calcining 100 g of barium nitrate solution, 100 g of calcium nitrate solution and 100 g of aluminum nitrate solution; (4) calculating the weight of barium nitrate, calcium nitrate and aluminum nitrate solution according to the chemical composition and weight of aluminate to be prepared; (5) and accurately weighing barium nitrate, calcium nitrate and aluminum nitrate solution according to the calculation result, and mixing to obtain the mixed salt solution for coprecipitation synthesis of the aluminate electron emission material. The preparation method provided by the invention has reasonable process design, is simple and is easy to operate.
Description
Technical Field
The invention belongs to the field of microwave electro-vacuum device manufacturing, and particularly relates to a preparation method of a mixed salt solution for coprecipitation synthesis of an aluminate electron emission material.
Background
The cathode is the heart of the microwave electric vacuum electronic device and plays an important role in the performance of the high-power microwave device, such as power output, service life and the like. The dipping barium tungsten cathode is composed of a porous tungsten matrix and an aluminate electron emission material dipped in the porous tungsten matrix, has the characteristics of large emission current density, excellent anti-poisoning performance and the like, and is most widely used in microwave electric vacuum electronic devices with medium and high power. The performance of the dipping barium-tungsten cathode is mainly determined by the chemical composition of the aluminate electron emission material and the uniformity of the composition distribution of each element. Researchers find that the uniformity of chemical components of the synthesized aluminate can be improved and the granularity of the aluminate can be reduced by adopting a coprecipitation technology; however, there is no effective measure on how to improve the accuracy and consistency of aluminate chemistry. Chinese patent No. 201110284836.5 discloses a method for preparing an active material for a multi-injection cathode, which uses aluminum nitrate nonahydrate, calcium nitrate tetrahydrate, barium nitrate and ammonium carbonate as raw materials to prepare aluminate by a coprecipitation method. In the patent, as reported in many documents, commercially available nitrates are directly weighed and then prepared into a mixed salt solution for coprecipitation reaction. As the nitrate sold in the market contains trace impurities, adsorption water and crystal water, the mixed salt solution for coprecipitation reaction with accurately controlled component ratios of each element can hardly be obtained by directly weighing, which inevitably causes that the chemical composition of the synthesized aluminate can not be kept consistent with the designed components; moreover, when the raw material batches or manufacturers are changed, the consistency of the composition and the performance of the synthesized aluminate cannot be ensured.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a mixed salt solution for coprecipitation synthesis of an aluminate electron emission material.
The technical scheme adopted by the invention for solving the technical problem is as follows: the preparation method of the mixed salt solution for coprecipitation synthesis of the aluminate electron emission material comprises the following specific steps:
(1) barium nitrate and deionized water are prepared into barium nitrate solution with certain concentration, and a certain weight is weighed and poured into the solution with the weight of Wg1G, crucible calcined to constant weight, weighing the exact mass W of the solution together with the cruciblebg1G, firstly putting the crucible into an oven for drying, then putting the crucible into an electric furnace for calcining at 200-500 ℃ to constant weight, and weighing the accurate weight W of the calcined product and the cruciblebg2G, weight of the obtained calcined barium nitrate is (W)bg2-Wg1) G; preparing calcium nitrate solution with certain concentration by calcium nitrate and deionized water, weighing a certain weight, and pouring the weighed solution Wg2G, crucible calcined to constant weight, weighing the exact mass W of the solution together with the cruciblecg1G, firstly putting the crucible into an oven for drying, then putting the crucible into an electric furnace for calcining at 800-1250 ℃ to constant weight, and weighing the accurate weight W of the calcined product and the cruciblecg2G, weight of the obtained calcined calcium oxide is (W)cg2-Wg2) G; preparing aluminum nitrate and deionized water into an aluminum nitrate solution with a certain concentration, weighing a certain weight, and pouring the weighed solution into a container with a weight of Wg3G, crucible calcined to constant weight, weighing the exact mass W of the solution together with the crucibleag1G, firstly putting the crucible into an oven for drying, then putting the crucible into an electric furnace for calcining at 800-1250 ℃ to constant weight, and weighing the accurate weight W of the calcined product and the crucibleag2G, weight of calcined alumina obtained is (W)ag2-Wg3) G;
(2) accurately measuring the purity C of the barium nitrate in the calcined barium nitrate, the calcined calcium oxide and the calcined aluminum oxide prepared in the step (1) by adopting an X-ray fluorescence spectrum analyzerb0Purity of calcium oxide Cc0And purity C of aluminaa0；
(3) Calculating the accurate mass M of the pure barium nitrate obtained after each 100 g of barium nitrate solution is calcinedb0，Mb0＝100×(Wbg2-Wg1)/(Wbg1-Wg1)×Cb0(ii) a Calculating the accurate mass M of the pure calcium oxide obtained after each 100 g of calcium nitrate solution is calcinedc0，Mc0＝100×(Wcg2-Wg2)/(Wcg1-Wg2)×Cc0(ii) a Calculating the accurate mass M of the pure aluminum oxide obtained after each 100 g of aluminum nitrate solution is calcineda0，Ma0＝100×(Wag2-Wg3)/(Wag1-Wg3)×Ca0；
(4) The chemical composition of the calculation preparation is xBaO, yCaO and zAl2O3L g of aluminate required weight W of barium nitrate solutionb1＝(L×26134×x)/(153.33x+56.08y+101.96z)/Mb0Weight W of calcium nitrate solution requiredc1＝(5608×y×L)/(153.33x+56.08y+101.96z)/Mc0Weight W of aluminum nitrate solution requireda1＝(10196×z×L)/(153.33x+56.08y+101.96z)/Ma0；
(5) Accurately weighing barium nitrate solution Wb1G, calcium nitrate solution Wc1G and aluminium nitrate solution Wa1And g, uniformly mixing and stirring to prepare a mixed salt solution for coprecipitation synthesis of the aluminate electron emission material.
Preferably, in the step 1, the crucible is made of alumina, the mass content of the alumina is more than 99%, and the alumina is calcined in an electric furnace at 1300-1400 ℃ to constant weight.
Preferably, the purity specification of the raw materials of barium nitrate, calcium nitrate and aluminum nitrate in the step 1 is at least chemical purity; the mass concentration of the prepared barium nitrate solution is 4-12%, the mass concentration of the calcium nitrate solution is 20-45%, and the mass concentration of the aluminum nitrate solution is 15-25%.
Has the advantages that:
(1) the preparation method of the mixed salt solution for coprecipitation synthesis of the aluminate electron emission material has reasonable process design, is simple and is easy to operate.
(2) The preparation method of the mixed salt solution for coprecipitation synthesis of the aluminate electron emission material can accurately control the chemical composition in the prepared mixed salt solution, and the aluminate electron emission material prepared by taking the mixed salt solution as a raw material and adopting the coprecipitation method has the advantages of high accuracy of the chemical composition, large emission current density, and good performance consistency, repeatability and stability.
Detailed Description
The following are specific embodiments of the present invention, and it should be noted that these embodiments are only used for illustrating the present invention and are not used to limit the scope of the present invention.
Example 1:
preparing a barium nitrate solution with the mass concentration of 4% by using chemically pure barium nitrate purchased from west longs chemical corporation and deionized water, weighing a certain weight, pouring the weighed solution into a crucible (the content of alumina is 99.3%) which is calcined to the constant weight of 255.15 g at 1300 ℃, weighing 411.15 g of the solution and the accurate weight of the crucible, firstly putting the crucible into a 100 ℃ oven to be dried for 24 hours, then putting the crucible into an electric furnace to be calcined to the constant weight at 200 ℃, weighing 261.39 g of the calcined product and the accurate weight of the crucible, and obtaining 6.24 g of the calcined barium nitrate. Preparing 20 mass percent calcium nitrate solution from chemically pure calcium nitrate and deionized water purchased from west Longchemistry GmbH, weighing a certain weight, pouring into a crucible (with the alumina content of 99.3%) which is calcined to constant weight at 1300 ℃ and has the weight of 263.02 g, weighing 419.76 g of the solution and the accurate weight of the crucible, firstly putting the crucible into a 150 ℃ oven to be dried for 12 hours, then putting the crucible into an electric furnace to be calcined to constant weight at 800 ℃, weighing 273.73 g of the calcined product and the accurate weight of the crucible, and obtaining the weight of the calcined calcium oxide of 10.71 g. Preparing a 15 mass percent aluminum nitrate solution from chemically pure aluminum nitrate and deionized water purchased from Xilonggaku chemical corporation, weighing a certain weight, pouring the weighed solution into a crucible (the content of aluminum oxide is 99.3 percent) which is calcined to be constant in weight at 1300 ℃ and is 263.57 grams, weighing 419.82 grams of the solution and the accurate mass of the crucible, firstly putting the crucible into a 120 ℃ oven to be dried for 18 hours, then putting the crucible into an electric furnace to be calcined to be constant in weight at 800 ℃, weighing 269.18 grams of the calcined product and the accurate weight of the crucible, and obtaining the weight of the calcined aluminum oxide to be 5.61 grams.
The purity of barium nitrate, the purity of calcium oxide and the purity of aluminum oxide in the calcined barium nitrate, calcined calcium oxide and calcined aluminum oxide were accurately measured by an X-ray fluorescence spectrometer (ARL ADVANT' XP) to be 99.32%, 99.45% and 99.38%.
Calculating the accurate mass of the pure barium nitrate obtained after each 100 g of barium nitrate solution is calcined to be 3.9728 g; the accurate mass of pure calcium oxide obtained after each 100 g of calcium nitrate solution is calculated to be 6.7954 g; the exact mass calculated to give pure alumina after calcination per 100 grams of aluminum nitrate solution was 3.5681 grams.
The chemical composition of the calculation preparation is 6BaO & CaO & 2Al2O3For 1000 g of aluminate, the weight of the required barium nitrate solution is 33449.20 g, the weight of the required calcium nitrate solution is 699.39 g, and the weight of the required aluminum nitrate solution is 4843.32 g.
33449.20 g of barium nitrate solution, 699.39 g of calcium nitrate solution and 4843.32 g of aluminum nitrate solution are accurately weighed, and mixed and stirred uniformly to prepare the mixed salt solution for coprecipitation synthesis of the aluminate electron-emitting material.
Example 2
Preparing a barium nitrate solution with the mass concentration of 12% by using chemically pure barium nitrate purchased from national medicine group chemical reagent limited company and deionized water, weighing a certain weight, pouring the weighed solution into a crucible (the content of alumina is 99.5%) which is calcined to the constant weight of 269.39 g at 1400 ℃, weighing 421.45 g of the solution and the accurate weight of the crucible, firstly putting the crucible into an oven with the temperature of 150 ℃ for drying for 12 hours, then putting the crucible into an electric furnace for calcining to the constant weight at the temperature of 500 ℃, weighing 287.64 g of the calcined product and the accurate weight of the crucible, and obtaining the weight of the calcined barium nitrate of 18.25 g. Preparing 45 mass percent calcium nitrate solution from chemically pure calcium nitrate and deionized water purchased from national medicine group chemical reagent limited company, weighing a certain weight, pouring into a crucible (the content of alumina is 99.5%) which is calcined to constant weight at 1400 ℃ and has the weight of 272.15 g, weighing 432.50 g of the solution and the accurate weight of the crucible, firstly putting the crucible into a 120 ℃ oven to be dried for 18 hours, then putting the crucible into an electric furnace to be calcined to constant weight at 1250 ℃, weighing 296.81 g of the calcined product and the accurate weight of the crucible to obtain 24.66 g of calcined calcium oxide. Preparing a 25 mass percent aluminum nitrate solution from chemically pure aluminum nitrate and deionized water purchased from national medicine group chemical reagent limited company, weighing a certain weight, pouring into a crucible (the content of aluminum oxide is 99.5%) which is calcined to constant weight at 1400 ℃ and has a weight of 270.57 g, weighing 433.79 g of the solution and the accurate weight of the crucible, firstly putting the crucible into a 100 ℃ oven to be dried for 24 hours, then putting the crucible into an electric furnace to be calcined to constant weight at 1250 ℃, weighing 280.34 g of the calcined product and the accurate weight of the crucible to obtain 9.77 g of calcined aluminum oxide.
The purity of barium nitrate, the purity of calcium oxide and the purity of aluminum oxide in the calcined barium nitrate, calcined calcium oxide and calcined aluminum oxide were accurately measured by an X-ray fluorescence spectrometer (ARL ADVANT' XP) to be 99.49%, 99.54% and 99.21%.
Calculating the accurate mass of the pure barium nitrate obtained after each 100 g of barium nitrate solution is calcined to be 11.9406 g; the accurate mass of pure calcium oxide obtained after each 100 g of calcium nitrate solution is calculated to be 15.3081 g; the exact mass calculated to give pure alumina after calcination per 100 grams of aluminum nitrate solution was 5.9385 grams.
The chemical composition of the calculation preparation is 4BaO, CaO and Al2O3For 1000 g of aluminate, the weight of the required barium nitrate solution is 11349.62 g, the weight of the required calcium nitrate solution is 474.93 g, and the weight of the required aluminum nitrate solution is 2225.85 g.
11349.62 g of barium nitrate solution, 474.93 g of calcium nitrate solution and 2225.85 g of aluminum nitrate solution are accurately weighed, and mixed and stirred uniformly to prepare the mixed salt solution for coprecipitation synthesis of the aluminate electron-emitting material.
Example 3:
the method comprises the steps of preparing a barium nitrate solution with the mass concentration of 8% by using chemically pure barium nitrate and deionized water purchased from Shanghai Aladdin Biotechnology GmbH, weighing a certain weight, pouring the weighed solution into a crucible (the content of alumina is 99.7%) which is calcined to the constant weight of 258.35 g at 1400 ℃, weighing the solution and the accurate weight of the crucible of 410.28 g, firstly putting the crucible into a 120 ℃ oven to be dried for 18 hours, then putting the crucible into an electric furnace to be calcined to the constant weight at 400 ℃, weighing the calcined product and the accurate weight of the crucible of 270.50 g, and obtaining the weight of the calcined barium nitrate of 12.15 g. Preparing a 30% calcium nitrate solution from chemically pure calcium nitrate and deionized water purchased from Shanghai Allan Biotechnology corporation, weighing a certain weight, pouring into a crucible (the content of alumina is 99.7%) which is calcined to be constant in weight at 1400 ℃ and is 263.97 g, weighing 424.27 g of the solution and the accurate weight of the crucible, firstly putting the crucible into a 100 ℃ oven to be dried for 24 hours, then putting the crucible into an electric furnace to be calcined to be constant in weight at 1000 ℃, weighing 280.40 g of the calcined product and the accurate weight of the crucible to obtain 16.44 g of calcined calcium oxide. Preparing 20 mass percent aluminum nitrate solution from chemically pure aluminum nitrate and deionized water purchased from Shanghai Aladdin Biotechnology, Inc., weighing a certain weight, pouring into a crucible (the content of aluminum oxide is 99.7%) which is calcined to constant weight at 1400 ℃ and has the weight of 258.39 g, weighing 424.53 g of the solution and the accurate weight of the crucible, firstly putting the crucible into a 150 ℃ oven to be dried for 12 hours, then putting the crucible into an electric furnace to be calcined to constant weight at 1000 ℃, weighing 266.34 g of the calcined product and the accurate weight of the crucible, and obtaining the weight of the calcined aluminum oxide of 7.95 g.
The purity of barium nitrate, the purity of calcium oxide and the purity of aluminum oxide in the calcined barium nitrate, calcined calcium oxide and calcined aluminum oxide were accurately measured by an X-ray fluorescence spectrometer (ARL ADVANT' XP) to be 99.28%, 99.31% and 99.47%.
Calculating the accurate mass of the pure barium nitrate obtained after each 100 g of barium nitrate solution is calcined to be 7.9395 g; the accurate mass of pure calcium oxide obtained after each 100 g of calcium nitrate solution is calculated to be 10.1788 g; the exact mass calculated to give pure alumina after calcination per 100 grams of aluminum nitrate solution was 4.7598 grams.
Computational preparationThe chemical composition is 5 BaO.3CaO.2Al2O3For 1000 g of aluminate, the weight of the required barium nitrate solution is 14452.07 g, the weight of the required calcium nitrate solution is 1451.38 g, and the weight of the required aluminum nitrate solution is 3762.04 g.
14452.07 g of barium nitrate solution, 1451.38 g of calcium nitrate solution and 3762.04 g of aluminum nitrate solution are accurately weighed, and mixed and stirred uniformly to prepare the mixed salt solution for coprecipitation synthesis of the aluminate electron-emitting material.
Aluminate XRF test results are shown in Table 1
From the above table, it can be seen that: the difference between the oxide content of the aluminate and the theoretical value is less than 1 percent, while the difference between the oxide content of the aluminate obtained by the traditional weighing method and the theoretical value is in the range of 2 to 15 percent, namely, the content of the aluminate oxide prepared by the mixed salt solution of the embodiment 1 to 3 obtained by the technical scheme of the invention is closer to the theoretical value. Therefore, the technical scheme of the invention can ensure the accuracy of the proportioning of the obtained aluminate under the condition of simple and convenient operation.
Claims (3)
1. The preparation method of the mixed salt solution for coprecipitation synthesis of the aluminate electron emission material comprises the following specific steps:
(1) barium nitrate and deionized water are prepared into barium nitrate solution with certain concentration, and a certain weight is weighed and poured into the solution with the weight of Wg1G, crucible calcined to constant weight, weighing the exact mass W of the solution together with the cruciblebg1G, firstly putting the crucible into an oven for drying, then putting the crucible into an electric furnace for calcining at 200-500 ℃ to constant weight, and weighing the accurate weight W of the calcined product and the cruciblebg2G, weight of the obtained calcined barium nitrate is (W)bg2-Wg1) G; calcium nitrate and deionized water are prepared into calcium nitrate solution with certain concentrationWeighing a certain weight, and pouring into a container with a weight Wg2G, crucible calcined to constant weight, weighing the exact mass W of the solution together with the cruciblecg1G, firstly putting the crucible into an oven for drying, then putting the crucible into an electric furnace for calcining at 800-1250 ℃ to constant weight, and weighing the accurate weight W of the calcined product and the cruciblecg2G, weight of the obtained calcined calcium oxide is (W)cg2-Wg2) G; preparing aluminum nitrate and deionized water into an aluminum nitrate solution with a certain concentration, weighing a certain weight, and pouring the weighed solution into a container with a weight of Wg3G, crucible calcined to constant weight, weighing the exact mass W of the solution together with the crucibleag1G, firstly putting the crucible into an oven for drying, then putting the crucible into an electric furnace for calcining at 800-1250 ℃ to constant weight, and weighing the accurate weight W of the calcined product and the crucibleag2G, weight of calcined alumina obtained is (W)ag2-Wg3) G;
(2) accurately measuring the purity C of the barium nitrate in the calcined barium nitrate, the calcined calcium oxide and the calcined aluminum oxide prepared in the step (1) by adopting an X-ray fluorescence spectrum analyzerb0Purity of calcium oxide Cc0And purity C of aluminaa0；
(3) Calculating the accurate mass M of the pure barium nitrate obtained after each 100 g of barium nitrate solution is calcinedb0，Mb0＝100×(Wbg2-Wg1)/(Wbg1-Wg1)×Cb0(ii) a Calculating the accurate mass M of the pure calcium oxide obtained after each 100 g of calcium nitrate solution is calcinedc0，Mc0＝100×(Wcg2-Wg2)/(Wcg1-Wg2)×Cc0(ii) a Calculating the accurate mass M of the pure aluminum oxide obtained after each 100 g of aluminum nitrate solution is calcineda0，Ma0＝100×(Wag2-Wg3)/(Wag1-Wg3)×Ca0；
(4) The chemical composition of the calculation preparation is xBaO, yCaO and zAl2O3L g of aluminate required weight W of barium nitrate solutionb1＝(L×26134×x)/(153.33x+56.08y+101.96z)/Mb0Weight W of calcium nitrate solution requiredc1＝(5608×y×L)/(153.33x+56.08y+101.96z)/Mc0On demand, ofWeight W of aluminum nitrate solutiona1＝(10196×z×L)/(153.33x+56.08y+101.96z)/Ma0；
(5) Accurately weighing barium nitrate solution Wb1G, calcium nitrate solution Wc1G and aluminium nitrate solution Wa1And g, uniformly mixing and stirring to prepare a mixed salt solution for coprecipitation synthesis of the aluminate electron emission material.
2. The method of claim 1, wherein: in the step 1, the crucible is made of alumina, the mass content of the alumina is more than 99%, and the alumina is calcined in an electric furnace at 1300-1400 ℃ to constant weight.
3. The method of claim 1, wherein: in the step 1, the purity specification of the raw materials of barium nitrate, calcium nitrate and aluminum nitrate is at least chemical purity; the mass concentration of the prepared barium nitrate solution is 4-12%, the mass concentration of the calcium nitrate solution is 20-45%, and the mass concentration of the aluminum nitrate solution is 15-25%.
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