CN108766859B - Preparation method of mixed salt solution for coprecipitation synthesis of aluminate electron emission materials - Google Patents
Preparation method of mixed salt solution for coprecipitation synthesis of aluminate electron emission materials Download PDFInfo
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- 150000004645 aluminates Chemical class 0.000 title claims abstract description 33
- 238000000975 co-precipitation Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 title claims abstract description 18
- 239000012266 salt solution Substances 0.000 title claims abstract description 18
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 15
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims abstract description 114
- 239000000243 solution Substances 0.000 claims abstract description 90
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims abstract description 66
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 33
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 32
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000292 calcium oxide Substances 0.000 claims abstract description 25
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000005303 weighing Methods 0.000 claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract 5
- 238000002156 mixing Methods 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000004876 x-ray fluorescence Methods 0.000 claims description 5
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 claims 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 2
- 238000001228 spectrum Methods 0.000 claims 1
- WMTSAHAFZXEJBV-UHFFFAOYSA-N [Ba].[W] Chemical compound [Ba].[W] WMTSAHAFZXEJBV-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 1
- ZHJGWYRLJUCMRT-UHFFFAOYSA-N 5-[6-[(4-methylpiperazin-1-yl)methyl]benzimidazol-1-yl]-3-[1-[2-(trifluoromethyl)phenyl]ethoxy]thiophene-2-carboxamide Chemical compound C=1C=CC=C(C(F)(F)F)C=1C(C)OC(=C(S1)C(N)=O)C=C1N(C1=C2)C=NC1=CC=C2CN1CCN(C)CC1 ZHJGWYRLJUCMRT-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
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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
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Luminescent Compositions (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
本发明提供一种铝酸盐电子发射材料共沉淀合成用混合盐溶液的制备方法，包括如下步骤：(1)精确称量硝酸钡、硝酸钙与硝酸铝溶液，经烘干、煅烧后精确称量所得煅烧硝酸钡、氧化钙与氧化铝的质量；(2)精确测定煅烧硝酸钡、氧化钙与氧化铝中硝酸钡、氧化钙与氧化铝的纯度；(3)计算100克硝酸钡溶液、100克硝酸钙溶液以及100克硝酸铝溶液经烘干、煅烧后所得纯硝酸钡、氧化钙与氧化铝的质量；(4)根据所要制备铝酸盐的化学组成和重量，计算所需硝酸钡、硝酸钙与硝酸铝溶液的重量；(5)按计算结果精确称量硝酸钡、硝酸钙与硝酸铝溶液，混合后得到本发明的铝酸盐电子发射材料共沉淀合成用混合盐溶液。本发明提供的制备方法，工艺设计合理、简单易于操作。The present invention provides a method for preparing a mixed salt solution for co-precipitation synthesis of aluminate electron emission materials, comprising the following steps: (1) accurately weighing solutions of barium nitrate, calcium nitrate and aluminum nitrate, drying and calcining, and then accurately weighing them. (2) Accurately measure the purity of barium nitrate, calcium oxide and alumina in calcined barium nitrate, calcium oxide and alumina; (3) Calculate 100 grams of barium nitrate solution, 100 grams of calcium nitrate solutions and 100 grams of aluminum nitrate solutions are the quality of the obtained pure barium nitrate, calcium oxide and alumina after drying and calcining; (4) according to the chemical composition and weight of the aluminate to be prepared, calculate the required barium nitrate , the weight of calcium nitrate and aluminum nitrate solution; (5) accurately weigh barium nitrate, calcium nitrate and aluminum nitrate solution according to the calculation result, obtain the mixed salt solution for coprecipitation synthesis of aluminate electron emission material of the present invention after mixing. The preparation method provided by the invention has reasonable process design, simple and easy operation.
Description
技术领域technical field
本发明属于微波电真空器件制造领域，具体涉及一种铝酸盐电子发射材料共沉淀合成用混合盐溶液的制备方法。The invention belongs to the field of microwave electric vacuum device manufacturing, and in particular relates to a preparation method of a mixed salt solution for co-precipitation synthesis of aluminate electron emission materials.
背景技术Background technique
阴极是微波电真空电子器件的“心脏”，对大功率微波器件的功率输出和寿命等性能起着至关重要的作用。浸渍型钡钨阴极是由多孔钨基体与浸渍在其中的铝酸盐电子发射材料所组成，具有发射电流密度大、抗中毒性能优异等特性，在中、大功率的微波电真空电子器件中使用最为广泛。浸渍型钡钨阴极性能的优劣主要取决于铝酸盐电子发射材料化学组成以及各元素组成分布的均匀性。研究人员发现采用共沉淀技术能够提高合成铝酸盐化学成分的均匀性、降低铝酸盐的颗粒度；但是，在如何提高铝酸盐化学组成的准确性和一致性上却没有有效的措施。申请号为201110284836.5的中国专利公开了一种多注阴极用活性物质制备方法，以九水硝酸铝、四水硝酸钙、硝酸钡和碳酸铵为原料，采用共沉淀方法制备铝酸盐。该专利与多数文献报道一样，将市售硝酸盐直接称量后配制成共沉淀反应用混合盐溶液。由于市售硝酸盐中含有微量杂质、吸附水以及结晶水，通过直接称量几乎不可能得到各元素组分配比精确控制的共沉淀反应用混合盐溶液，这必将导致合成出的铝酸盐化学组成无法与设计成分保持一致；而且，当原料批次或者厂家更换时，合成铝酸盐组成及其性能的一致性也无法得到保证。The cathode is the "heart" of microwave electro-vacuum electronic devices, and plays a crucial role in the performance of high-power microwave devices such as power output and life. Impregnated barium tungsten cathode is composed of porous tungsten matrix and 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. the most extensive. 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. The researchers found that the use of co-precipitation technology can improve the uniformity of the chemical composition of synthetic aluminate and reduce the particle size of aluminate; however, there is no effective measure on how to improve the accuracy and consistency of the chemical composition of aluminate. The Chinese patent with the application number of 201110284836.5 discloses a method for preparing active materials for multi-injection cathodes, using aluminum nitrate nonahydrate, calcium nitrate tetrahydrate, barium nitrate and ammonium carbonate as raw materials, and using a coprecipitation method to prepare aluminate. This patent, like most literature reports, directly weighs commercially available nitrates and prepares a mixed salt solution for co-precipitation reaction. Since commercially available nitrates contain trace impurities, adsorbed water and crystal water, it is almost impossible to obtain a mixed salt solution for co-precipitation reaction with precise control of the distribution ratio of each element component by direct weighing, which will inevitably lead to the synthesis of aluminates. The chemical composition cannot be consistent with the design composition; moreover, when the raw material batch or manufacturer is changed, the consistency of the synthetic aluminate composition and its performance cannot be guaranteed.
发明内容SUMMARY OF THE INVENTION
本发明的目的是克服现有技术的不足，提供一种铝酸盐电子发射材料共沉淀合成用混合盐溶液的制备方法。The purpose of the present invention is to overcome the deficiencies of the prior art, and to provide a preparation method of a mixed salt solution for co-precipitation synthesis of aluminate electron emission materials.
本发明解决技术问题采用的技术方案是：铝酸盐电子发射材料共沉淀合成用混合盐溶液的制备方法，其具体步骤如下：The technical scheme adopted by the present invention to solve the technical problem is: a preparation method of a mixed salt solution for co-precipitation synthesis of aluminate electron emission materials, and its specific steps are as follows:
(1)将硝酸钡与去离子水配制成一定浓度的硝酸钡溶液，称取一定重量后倒入重量为Wg1克、已煅烧至恒重的坩埚，称量溶液连同坩埚的准确质量Wbg1克，将坩埚首先放入烘箱中烘干，再置于电炉中在200～500℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量Wbg2克，得到煅烧硝酸钡的重量为(Wbg2-Wg1)克；将硝酸钙与去离子水配制成一定浓度的硝酸钙溶液，称取一定重量后倒入重量为Wg2克、已煅烧至恒重的坩埚，称量溶液连同坩埚的准确质量Wcg1克，将坩埚首先放入烘箱中烘干，再置于电炉中在800～1250℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量Wcg2克，得到煅烧氧化钙的重量为(Wcg2-Wg2)克；将硝酸铝与去离子水配制成一定浓度的硝酸铝溶液，称取一定重量后倒入重量为Wg3克、已煅烧至恒重的坩埚，称量溶液连同坩埚的准确质量Wag1克，将坩埚首先放入烘箱中烘干，再置于电炉中在800～1250℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量Wag2克，得到煅烧氧化铝的重量为(Wag2-Wg3)克；(1) barium nitrate and deionized water are mixed into a certain concentration of barium nitrate solution, after weighing a certain weight, pour into a crucible with a weight of W g1 gram, calcined to constant weight, weigh the solution together with the accurate mass of the crucible W bg1 gram, put the crucible into the oven at first to dry, then place it in the electric furnace and calcine to constant weight at 200～500 ℃, weigh the calcined product together with the accurate weight of the crucible W bg 2 grams, the weight that obtains calcined barium nitrate is (W bg . -W g1 ) gram; calcium nitrate and deionized water are mixed into a certain concentration of calcium nitrate solution, after weighing a certain weight, pour into the crucible with a weight of W g2 gram, calcined to constant weight, weigh the solution together with the accurate crucible of the crucible The mass is W cg1 g, the crucible is first put into an oven to dry, and then placed in an electric furnace at 800-1250 ° C to be calcined to a constant weight, the calcined product is weighed together with the accurate weight of the crucible W cg 2 g, the obtained weight of the calcined calcium oxide is: (W cg 2 -W g 2 ) gram; aluminum nitrate and deionized water are mixed into a certain concentration of aluminum nitrate solution, after weighing a certain weight, pour it into a crucible with a weight of W g 3 gram, calcined to constant weight, weigh the solution together with The exact mass of the crucible is W ag 1 g, the crucible is first put into an oven to dry, and then placed in an electric furnace at 800-1250 ° C to calcine to a constant weight, and the calcined product together with the accurate weight of the crucible W ag 2 g is weighed to obtain calcined alumina. The weight of (W ag2 -W g3 ) grams;
(2)采用X射线荧光光谱分析仪精确测定步骤(1)中制备的煅烧硝酸钡、煅烧氧化钙和煅烧氧化铝中硝酸钡的纯度Cb0、氧化钙的纯度Cc0和氧化铝的纯度Ca0；(2) Using an X-ray fluorescence spectrometer to accurately measure the purity C b0 of barium nitrate, the purity C c0 of calcium oxide and the purity C of alumina in the calcined barium nitrate, calcined calcium oxide and calcined alumina prepared in step (1) a0 ;
(3)计算每100克硝酸钡溶液煅烧后所能得到纯硝酸钡的准确质量Mb0，Mb0＝100×(Wbg2-Wg1)/(Wbg1-Wg1)×Cb0；计算每100克硝酸钙溶液煅烧后所能得到纯氧化钙的准确质量Mc0，Mc0＝100×(Wcg2-Wg2)/(Wcg1-Wg2)×Cc0；计算每100克硝酸铝溶液煅烧后所能得到纯氧化铝的准确质量Ma0，Ma0＝100×(Wag2-Wg3)/(Wag1-Wg3)×Ca0；(3) Calculate the exact mass M b0 of pure barium nitrate that can be obtained after calcining every 100 grams of barium nitrate solution, M b0 =100×(W bg2 -W g1 )/(W bg1 -W g1 )×C b0 ; The exact mass M c0 of pure calcium oxide that can be obtained after calcining 100 grams of calcium nitrate solution, M c0 =100×(W cg2 -W g2 )/(W cg1 -W g2 )×C c0 ; Calculate every 100 grams of aluminum nitrate solution The exact mass M a0 of pure alumina that can be obtained after calcination, M a0 =100×(W ag2 -W g3 )/(W ag1 -W g3 )×C a0 ;
(4)计算制备化学组成为xBaO·yCaO·zAl2O3的铝酸盐L克所需硝酸钡溶液重量Wb1＝(L×26134×x)/(153.33x+56.08y+101.96z)/Mb0，所需硝酸钙溶液重量Wc1＝(5608×y×L)/(153.33x+56.08y+101.96z)/Mc0，所需硝酸铝溶液重量Wa1＝(10196×z×L)/(153.33x+56.08y+101.96z)/Ma0；(4) Calculate the weight of barium nitrate solution W b1 =(L×26134×x)/(153.33x + 56.08y+ 101.96z )/ M b0 , the required weight of calcium nitrate solution W c1 =(5608×y×L)/(153.33x+56.08y+101.96z)/M c0 , the required weight of aluminum nitrate solution W a1 =(10196×z×L) /(153.33x+56.08y+101.96z)/M a0 ;
(5)准确称量硝酸钡溶液Wb1克、硝酸钙溶液Wc1克和硝酸铝溶液Wa1克，混合搅拌均匀后制备得到铝酸盐电子发射材料共沉淀合成用混合盐溶液。(5) Accurately weigh the barium nitrate solution W b1 g, the calcium nitrate solution W c1 g and the aluminum nitrate solution W a1 g, mix and stir uniformly to prepare a mixed salt solution for coprecipitation synthesis of aluminate electron emission materials.
优选步骤1中坩埚材质为氧化铝，其质量含量大于99％，在1300～1400℃的电炉中煅烧至恒重。Preferably, in step 1, the material of the crucible is alumina, the mass content of which is greater than 99%, and is calcined in an electric furnace at 1300-1400° C. to a constant weight.
优选步骤1中硝酸钡、硝酸钙与硝酸铝原料的纯度规格至少为化学纯；所配制硝酸钡溶液的质量浓度为4～12％，硝酸钙溶液的质量浓度为20～45％，硝酸铝溶液的质量浓度为15～25％。Preferably, the purity specifications of the raw materials of barium nitrate, calcium nitrate and aluminum nitrate in step 1 are at least chemically pure; 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 aluminum nitrate solution is The mass concentration of 15 to 25%.
有益效果：Beneficial effects:
(1)本发明所述的铝酸盐电子发射材料共沉淀合成用混合盐溶液制备方法，工艺设计合理、简单易于操作。(1) The method for preparing a mixed salt solution for co-precipitation synthesis of aluminate electron emission materials according to the present invention is reasonable in process design, simple and easy to operate.
(2)本发明所述铝酸盐电子发射材料共沉淀合成用混合盐溶液制备方法，可以精确控制所制备混合盐溶液中的化学组成，以其为原料采用共沉淀方法制备的铝酸盐电子发射材料的化学组成的准确性高，发射电流密度大，性能一致性、重复性和稳定性好。(2) The preparation method of the mixed salt solution for co-precipitation synthesis of the aluminate electron emission material according to the present invention can precisely control the chemical composition in the prepared mixed salt solution, and the aluminate electron prepared by the co-precipitation method is prepared by using it as a raw material. The chemical composition of the emission material has high accuracy, high emission current density, and good performance consistency, repeatability and stability.
具体实施方式Detailed ways
以下是本发明的具体实施案例，注意这些案例仅用于说明本发明而不用于限制本发明的范围。The following are specific implementation examples of the present invention, and it should be noted that these examples are only used to illustrate the present invention and not to limit the scope of the present invention.
实施例1：Example 1:
将购于西陇化工股份有限公司的化学纯硝酸钡与去离子水配制成质量浓度为4％的硝酸钡溶液，称取一定重量后倒入在1300℃煅烧至恒重、重量为255.15克的坩埚(氧化铝含量为99.3％)，称量溶液连同坩埚的准确质量411.15克，将坩埚首先放入100℃烘箱中烘24小时，再置于电炉中在200℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量261.39克，得到煅烧硝酸钡的重量为6.24克。将购于西陇化工股份有限公司的化学纯硝酸钙与去离子水配制成质量浓度为20％的硝酸钙溶液，称取一定重量后倒入在1300℃煅烧至恒重、重量为263.02克的坩埚(氧化铝含量为99.3％)，称量溶液连同坩埚的准确质量419.76克，将坩埚首先放入150℃烘箱中烘12小时，再置于电炉中在800℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量273.73克，得到煅烧氧化钙的重量为10.71克。将购于西陇化工股份有限公司的化学纯硝酸铝与去离子水配制成质量浓度为15％的硝酸铝溶液，称取一定重量后倒入在1300℃煅烧至恒重、重量为263.57克的坩埚(氧化铝含量为99.3％)，称量溶液连同坩埚的准确质量419.82克，将坩埚首先放入120℃烘箱中烘18小时，再置于电炉中在800℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量269.18克，得到煅烧氧化铝的重量为5.61克。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%. Crucible (with alumina content of 99.3%), weigh the solution together with the exact mass of the crucible 411.15 grams, put the crucible into a 100°C oven for 24 hours, and then place it in an electric furnace at 200°C to calcine to constant weight, weigh and calcine The exact weight of the product along with the crucible was 261.39 grams, giving 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%. Crucible (with alumina content of 99.3%), weigh the solution together with the exact mass of the crucible 419.76 grams, put the crucible into a 150°C oven for 12 hours, and then place it in an electric furnace at 800°C to calcine to a constant weight, weigh and calcine The exact weight of the product together with the crucible was 273.73 grams, giving a weight of 10.71 grams of calcined calcium oxide. The chemically pure aluminum nitrate purchased from Xilong Chemical Co., Ltd. and deionized water were prepared into an aluminum nitrate solution with a mass concentration of 15%. Crucible (with alumina content of 99.3%), weigh the solution together with the exact mass of the crucible 419.82 grams, put the crucible into a 120°C oven for 18 hours, and then place it in an electric furnace at 800°C to calcine to constant weight, weigh and calcine The exact weight of the product along with the crucible was 269.18 grams, giving a weight of 5.61 grams of calcined alumina.
采用X射线荧光光谱分析仪(ARL ADVANT'XP)精确测定煅烧硝酸钡、煅烧氧化钙和煅烧氧化铝中硝酸钡的纯度为99.32％、氧化钙的纯度为99.45％和氧化铝的纯度为99.38％。The calcined barium nitrate, calcined calcium oxide and calcined alumina were accurately determined by X-ray fluorescence spectrometer (ARL ADVANT'XP) to be 99.32% pure barium nitrate, 99.45% pure calcium oxide and 99.38% pure alumina .
计算每100克硝酸钡溶液煅烧后所能得到纯硝酸钡的准确质量为3.9728克；计算每100克硝酸钙溶液煅烧后所能得到纯氧化钙的准确质量为6.7954克；计算每100克硝酸铝溶液煅烧后所能得到纯氧化铝的准确质量为3.5681克。Calculate the accurate mass of pure barium nitrate that can be obtained after calcination per 100 grams of barium nitrate solution is 3.9728 grams; calculate the accurate mass of pure calcium oxide that can be obtained per 100 grams of calcium nitrate solution calcined to be 6.7954 grams; Calculate per 100 grams of aluminum nitrate The exact mass of pure alumina that can be obtained after solution calcination is 3.5681 grams.
计算制备化学组成为6BaO·CaO·2Al2O3的铝酸盐1000克所需硝酸钡溶液重量为33449.20克，所需硝酸钙溶液重量699.39克，所需硝酸铝溶液重量4843.32克。The weight of barium nitrate solution required to prepare 1000 grams of aluminate with chemical composition 6BaO·CaO·2Al 2 O 3 is calculated to be 33449.20 grams, the required weight of calcium nitrate solution is 699.39 grams, and the required weight of aluminum nitrate solution is 4843.32 grams.
准确称量硝酸钡溶液33449.20克、硝酸钙溶液699.39克和硝酸铝溶液4843.32克，混合搅拌均匀后制备得到铝酸盐电子发射材料共沉淀合成用混合盐溶液。Accurately weigh 33449.20 g of barium nitrate solution, 699.39 g of calcium nitrate solution and 4843.32 g of aluminum nitrate solution, mix and stir evenly to prepare a mixed salt solution for co-precipitation synthesis of aluminate electron emission materials.
实施例2Example 2
将购于国药集团化学试剂有限公司的化学纯硝酸钡与去离子水配制成质量浓度为12％的硝酸钡溶液，称取一定重量后倒入在1400℃煅烧至恒重、重量为269.39克的坩埚(氧化铝含量为99.5％)，称量溶液连同坩埚的准确质量421.45克，将坩埚首先放入150℃烘箱中烘12小时，再置于电炉中在500℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量287.64克，得到煅烧硝酸钡的重量为18.25克。将购于国药集团化学试剂有限公司的化学纯硝酸钙与去离子水配制成质量浓度为45％的硝酸钙溶液，称取一定重量后倒入在1400℃煅烧至恒重、重量为272.15克的坩埚(氧化铝含量为99.5％)，称量溶液连同坩埚的准确质量432.50克，将坩埚首先放入120℃烘箱中烘18小时，再置于电炉中在1250℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量296.81克，得到煅烧氧化钙的重量为24.66克。将购于国药集团化学试剂有限公司的化学纯硝酸铝与去离子水配制成质量浓度为25％的硝酸铝溶液，称取一定重量后倒入在1400℃煅烧至恒重、重量为270.57克的坩埚(氧化铝含量为99.5％)，称量溶液连同坩埚的准确质量433.79克，将坩埚首先放入100℃烘箱中烘24小时，再置于电炉中在1250℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量280.34克，得到煅烧氧化铝的重量为9.77克。The chemically pure barium nitrate purchased from Sinopharm Chemical Reagent Co., Ltd. and deionized water were prepared into a barium nitrate solution with a mass concentration of 12%. Crucible (with alumina content of 99.5%), weigh the solution together with the exact mass of the crucible 421.45 grams, put the crucible into a 150 ℃ oven for 12 hours, and then place it in an electric furnace at 500 ℃ to calcine to constant weight, weigh and calcine The exact weight of the product along with the crucible was 287.64 grams, giving a weight of 18.25 grams of calcined barium nitrate. The chemically pure calcium nitrate purchased from Sinopharm Chemical Reagent Co., Ltd. and deionized water were prepared into a calcium nitrate solution with a mass concentration of 45%. Crucible (with alumina content of 99.5%), weigh the solution together with the exact mass of the crucible 432.50 grams, put the crucible into a 120 ℃ oven for 18 hours, and then place it in an electric furnace at 1250 ℃ to calcine to constant weight, weigh and calcine The exact weight of the product along with the crucible was 296.81 grams, giving a weight of 24.66 grams of calcined calcium oxide. The chemically pure aluminum nitrate purchased from Sinopharm Chemical Reagent Co., Ltd. and deionized water were prepared into an aluminum nitrate solution with a mass concentration of 25%. Crucible (with alumina content of 99.5%), weigh the solution together with the exact mass of the crucible 433.79 grams, put the crucible into a 100 ℃ oven for 24 hours, and then place it in an electric furnace at 1250 ℃ to calcine to constant weight, weigh and calcine The exact weight of the product along with the crucible was 280.34 grams, giving a weight of 9.77 grams of calcined alumina.
采用X射线荧光光谱分析仪(ARL ADVANT'XP)精确测定煅烧硝酸钡、煅烧氧化钙和煅烧氧化铝中硝酸钡的纯度为99.49％、氧化钙的纯度为99.54％和氧化铝的纯度为99.21％。The calcined barium nitrate, calcined calcium oxide and calcined alumina were accurately determined by X-ray fluorescence spectrometer (ARL ADVANT'XP) to be 99.49% pure barium nitrate, 99.54% pure calcium oxide and 99.21% pure alumina .
计算每100克硝酸钡溶液煅烧后所能得到纯硝酸钡的准确质量为11.9406克；计算每100克硝酸钙溶液煅烧后所能得到纯氧化钙的准确质量为15.3081克；计算每100克硝酸铝溶液煅烧后所能得到纯氧化铝的准确质量为5.9385克。Calculate the accurate mass of pure barium nitrate obtained after calcination per 100 grams of barium nitrate solution is 11.9406 grams; calculate the accurate mass of pure calcium oxide that can be obtained after calcination per 100 grams of calcium nitrate solution is 15.3081 grams; Calculate per 100 grams of aluminum nitrate The exact mass of pure alumina that can be obtained after solution calcination is 5.9385 grams.
计算制备化学组成为4BaO·CaO·Al2O3的铝酸盐1000克所需硝酸钡溶液重量为11349.62克，所需硝酸钙溶液重量474.93克，所需硝酸铝溶液重量2225.85克。The weight of barium nitrate solution required to prepare 1000 grams of aluminate with chemical composition 4BaO·CaO·Al 2 O 3 is 11349.62 grams, the weight of calcium nitrate solution is 474.93 grams, and the weight of aluminum nitrate solution is 2225.85 grams.
准确称量硝酸钡溶液11349.62克、硝酸钙溶液474.93克和硝酸铝溶液2225.85克，混合搅拌均匀后制备得到铝酸盐电子发射材料共沉淀合成用混合盐溶液。Accurately weigh 11349.62 grams of barium nitrate solution, 474.93 grams of calcium nitrate solution and 2225.85 grams of aluminum nitrate solution, mix and stir evenly to prepare a mixed salt solution for coprecipitation synthesis of aluminate electron emission materials.
实施例3：Example 3:
将购于上海阿拉丁生化科技股份有限公司的化学纯硝酸钡与去离子水配制成质量浓度为8％的硝酸钡溶液，称取一定重量后倒入在1400℃煅烧至恒重、重量为258.35克的坩埚(氧化铝含量为99.7％)，称量溶液连同坩埚的准确质量410.28克，将坩埚首先放入120℃烘箱中烘18小时，再置于电炉中在400℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量270.50克，得到煅烧硝酸钡的重量为12.15克。将购于上海阿拉丁生化科技股份有限公司的化学纯硝酸钙与去离子水配制成质量浓度为30％的硝酸钙溶液，称取一定重量后倒入在1400℃煅烧至恒重、重量为263.97克的坩埚(氧化铝含量为99.7％)，称量溶液连同坩埚的准确质量424.27克，将坩埚首先放入100℃烘箱中烘24小时，再置于电炉中在1000℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量280.40克，得到煅烧氧化钙的重量为16.44克。将购于上海阿拉丁生化科技股份有限公司的化学纯硝酸铝与去离子水配制成质量浓度为20％的硝酸铝溶液，称取一定重量后倒入在1400℃煅烧至恒重、重量为258.39克的坩埚(氧化铝含量为99.7％)，称量溶液连同坩埚的准确质量424.53克，将坩埚首先放入150℃烘箱中烘12小时，再置于电炉中在1000℃煅烧至恒重，称量煅烧产物连同坩埚的准确重量266.34克，得到煅烧氧化铝的重量为7.95克。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%. gram crucible (alumina content of 99.7%), weigh the solution together with the exact mass of the crucible 410.28 grams, put the crucible into a 120 ℃ oven to bake for 18 hours, and then place it in an electric furnace at 400 ℃ to calcine to constant weight, weigh The exact weight of the calcined product along with the crucible was 270.50 grams, resulting in 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%. After weighing a certain weight, pour it into a calcined at 1400 ° C to a constant weight and the weight is 263.97 gram crucible (with alumina content of 99.7%), weigh the solution together with the crucible's exact mass of 424.27 grams, put the crucible into a 100 ℃ oven for 24 hours, and then place it in an electric furnace at 1000 ℃ to calcine to a constant weight, weighed. The exact weight of the calcined product along with the crucible was 280.40 grams, resulting in a weight of 16.44 grams of calcined calcium oxide. The chemically pure aluminum nitrate purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. and deionized water were prepared into an aluminum nitrate solution with a mass concentration of 20%. After weighing a certain weight, pour it into calcined at 1400 ° C to a constant weight and the weight is 258.39 gram crucible (alumina content of 99.7%), weigh the solution together with the exact mass of the crucible 424.53 grams, put the crucible into a 150 ℃ oven for 12 hours, and then place it in an electric furnace at 1000 ℃ to calcine to constant weight, weigh The exact weight of the calcined product along with the crucible was 266.34 grams, resulting in a weight of 7.95 grams of calcined alumina.
采用X射线荧光光谱分析仪(ARL ADVANT'XP)精确测定煅烧硝酸钡、煅烧氧化钙和煅烧氧化铝中硝酸钡的纯度为99.28％、氧化钙的纯度为99.31％和氧化铝的纯度为99.47％。The calcined barium nitrate, calcined calcium oxide and calcined alumina were accurately determined by X-ray fluorescence spectrometer (ARL ADVANT'XP) to be 99.28% pure barium nitrate, 99.31% pure calcium oxide and 99.47% pure alumina .
计算每100克硝酸钡溶液煅烧后所能得到纯硝酸钡的准确质量为7.9395克；计算每100克硝酸钙溶液煅烧后所能得到纯氧化钙的准确质量为10.1788克；计算每100克硝酸铝溶液煅烧后所能得到纯氧化铝的准确质量为4.7598克。Calculate the accurate mass of pure barium nitrate that can be obtained after calcination per 100 grams of barium nitrate solution is 7.9395 grams; calculate the accurate mass of pure calcium oxide that can be obtained after calcination per 100 grams of calcium nitrate solution is 10.1788 grams; Calculate per 100 grams of aluminum nitrate The exact mass of pure alumina that can be obtained after solution calcination is 4.7598 grams.
计算制备化学组成为5BaO·3CaO·2Al2O3的铝酸盐1000克所需硝酸钡溶液重量为14452.07克，所需硝酸钙溶液重量1451.38克，所需硝酸铝溶液重量3762.04克。The weight of barium nitrate solution required to prepare 1000 grams of aluminate with chemical composition 5BaO·3CaO·2Al 2 O 3 is calculated to be 14452.07 grams, the required weight of calcium nitrate solution is 1451.38 grams, and the required weight of aluminum nitrate solution is 3762.04 grams.
准确称量硝酸钡溶液14452.07克、硝酸钙溶液1451.38克和硝酸铝溶液3762.04克，混合搅拌均匀后制备得到铝酸盐电子发射材料共沉淀合成用混合盐溶液。Accurately weigh 14452.07 g of barium nitrate solution, 1451.38 g of calcium nitrate solution and 3762.04 g of aluminum nitrate solution, mix and stir evenly to prepare a mixed salt solution for co-precipitation synthesis of aluminate electron emission materials.
铝酸盐XRF测试结果如表1The aluminate XRF test results are shown in Table 1
由上表可知：实施例铝酸盐的氧化物含量与理论值之间的差值小于1％，而采用传统的称量方法所得铝酸盐的氧化物含量与理论值之间的差值在2％-15％的范围内，即采用本发明的技术方案所得的实施例1-3的混合盐溶液制备的铝酸盐氧化物含量更接近理论值。因而本发明的技术方案可以在操作简便的情况下保证所得铝酸盐配比的准确性。It can be seen from the above table that the difference between the oxide content of the aluminate in the embodiment and the theoretical value is less than 1%, while the difference between the oxide content of the aluminate obtained by the traditional weighing method and the theoretical value is Within the range of 2%-15%, that is, the aluminate oxide content prepared by the mixed salt solutions of Examples 1-3 obtained by adopting the technical solution of the present invention is closer to the theoretical value. Therefore, the technical scheme of the present invention can ensure the accuracy of the obtained aluminate proportioning under the condition of easy operation.
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