CN103496743B - Preparation method of spherical strontium chromate powder controllable in micron-sized crystal growth morphology - Google Patents
Preparation method of spherical strontium chromate powder controllable in micron-sized crystal growth morphology Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 49
- NVKTUNLPFJHLCG-UHFFFAOYSA-N strontium chromate Chemical compound [Sr+2].[O-][Cr]([O-])(=O)=O NVKTUNLPFJHLCG-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000013078 crystal Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 31
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000005119 centrifugation Methods 0.000 claims description 13
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 8
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical class [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- UKAUYVFTDYCKQA-UHFFFAOYSA-N homoserine Chemical compound OC(=O)C(N)CCO UKAUYVFTDYCKQA-UHFFFAOYSA-N 0.000 claims description 6
- 229910001631 strontium chloride Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 3
- 229910052804 chromium Inorganic materials 0.000 claims 3
- 239000011651 chromium Substances 0.000 claims 3
- 229910052708 sodium Inorganic materials 0.000 claims 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims 2
- 239000003755 preservative agent Substances 0.000 claims 1
- 230000002335 preservative effect Effects 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 10
- PXLIDIMHPNPGMH-UHFFFAOYSA-N sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 239000000919 ceramic Substances 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 9
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 6
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 4
- 229940013553 strontium chloride Drugs 0.000 description 4
- 229940047908 strontium chloride hexahydrate Drugs 0.000 description 4
- AMGRXJSJSONEEG-UHFFFAOYSA-L strontium dichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Sr]Cl AMGRXJSJSONEEG-UHFFFAOYSA-L 0.000 description 4
- 239000013543 active substance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- IGFJNGLVIGYVQM-UHFFFAOYSA-N [Cr].[Sr] Chemical compound [Cr].[Sr] IGFJNGLVIGYVQM-UHFFFAOYSA-N 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- -1 alkaline earth metal strontium chromate Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
一种微米级晶体生长形貌可控的球形铬酸锶粉体的制备方法，涉及一种无机非金属粉体材料的制备方法。本发明是要解决现有方法制备铬酸锶粉体的工艺方法复杂，在不加活性添加剂的条件下生长形貌多为线状或棒状，无法得到生长形貌为微米级球形的铬酸锶粉体的技术问题。本发明的方法为：一、配制铬酸钠溶液；二、制备混合溶液A；三、制备混合溶液B；四、制备微米级晶体生长形貌可控的球形铬酸锶粉体。本发明只需在室温下进行，条件温和易控，成本低，制备方法简单，易大量生产；且制备的铬酸锶陶瓷粉体，颗粒形貌大小可控，性能良好并能实现大规模批量生产。本发明应用于无机非金属粉体材料的制备领域。
The invention discloses a preparation method of spherical strontium chromate powder with controllable micron-scale crystal growth morphology, and relates to a preparation method of an inorganic non-metallic powder material. The present invention is to solve the complex process of preparing strontium chromate powder in the existing method, and the growth morphology is mostly linear or rod-shaped without adding active additives, and it is impossible to obtain strontium chromate whose growth morphology is micron-scale spherical Powder technical problems. The method of the invention comprises: 1. preparing sodium chromate solution; 2. preparing mixed solution A; 3. preparing mixed solution B; 4. preparing spherical strontium chromate powder with controllable micron crystal growth morphology. The invention only needs to be carried out at room temperature, the conditions are mild and easy to control, the cost is low, the preparation method is simple, and it is easy to produce in large quantities; and the prepared strontium chromate ceramic powder has controllable particle shape and size, good performance and can realize large-scale batch production Production. The invention is applied to the field of preparation of inorganic non-metallic powder materials.
Description
技术领域technical field
本发明涉及一种无机非金属粉体材料的制备方法。The invention relates to a preparation method of an inorganic non-metallic powder material.
背景技术Background technique
近年来，铬酸盐在高温固体润滑剂、光导介电材料、发光材料、催化剂和工业颜料等领域有着广泛的应用前景，而铬酸盐的晶体生长形貌、粒径和晶体结构对其性能有较大影响，因此如何制备出不同形貌的粉体对其后续的性能研究至关重要。目前制备铬酸锶陶瓷粉体的主要方法有模板法、水热法等，其制备方法较复杂。在不加任何活性添加剂的条件下，模板法和水热法等制备所得的铬酸锶粉体的晶体形貌都是微纳米线状或棒状产物，无法得到微纳米级球形的铬酸锶粉体。采用本发明方法通过添加EDTA活性剂和无水乙醇，制备得到的碱土金属铬酸锶粉体材料的物相单一，结晶性好，纯度高，生长形貌呈球形，可适用于大规模球形铬酸锶粉体生长和工业应用。In recent years, chromate has broad application prospects in the fields of high-temperature solid lubricants, photoconductive dielectric materials, luminescent materials, catalysts, and industrial pigments, and the crystal growth morphology, particle size, and crystal structure of chromate have great influence on its performance. Therefore, how to prepare powders with different morphologies is very important for its subsequent performance research. At present, the main methods for preparing strontium chromate ceramic powder include template method, hydrothermal method, etc., and the preparation method is relatively complicated. Without any active additives, the crystal morphology of strontium chromate powder prepared by template method and hydrothermal method is micro-nano wire or rod-shaped product, and it is impossible to obtain micro-nano spherical strontium chromate powder body. The alkaline earth metal strontium chromate powder material prepared by the method of the present invention by adding EDTA active agent and absolute ethanol has a single phase, good crystallinity, high purity, spherical growth shape, and can be applied to large-scale spherical chromium Strontium acid powder growth and industrial application.
发明内容Contents of the invention
本发明是要解决现有方法制备铬酸锶粉体的工艺方法复杂，在不加活性添加剂的条件下生长形貌多为线状或棒状，无法得到生长形貌为微米级球形的铬酸锶粉体的技术问题，从而提供了一种微米级晶体生长形貌可控的球形铬酸锶粉体的制备方法。The present invention is to solve the complex process of preparing strontium chromate powder in the existing method, and the growth morphology is mostly linear or rod-shaped without adding active additives, and it is impossible to obtain strontium chromate whose growth morphology is micron-scale spherical In order to solve the technical problems of the powder, a method for preparing spherical strontium chromate powder with controllable micron crystal growth morphology is provided.
本发明提供的一种微米级晶体生长形貌可控的球形铬酸锶粉体的制备方法是按以下步骤进行：The preparation method of spherical strontium chromate powder with controllable micron crystal growth morphology provided by the present invention is carried out according to the following steps:
一、称取2.34g～23.4g的四水铬酸钠(Na2CrO4.4H2O)溶解于蒸馏水中，配制成浓度为0.1mol/L～1mol/L的铬酸钠溶液；1. Weigh 2.34g~23.4g of sodium chromate tetrahydrate (Na 2 CrO 4 .4H 2 O) and dissolve it in distilled water to prepare a sodium chromate solution with a concentration of 0.1mol/L~1mol/L;
二、称取2.67g～26.7g的六水氯化锶(SrCl2.6H2O)溶解于蒸馏水中，配制成浓度为0.1mol/L～1mol/L的氯化锶溶液，然后向其中加入2g～8g的EDTA二钠，再用氨水调节溶液pH值为9～10，随后再用稀盐酸调节溶液pH值为6～8，得到混合溶液A；2. Weigh 2.67g-26.7g of strontium chloride hexahydrate (SrCl 2 .6H 2 O) and dissolve it in distilled water to prepare a strontium chloride solution with a concentration of 0.1mol/L-1mol/L, and then add 2g to 8g of disodium EDTA, and then use ammonia water to adjust the pH of the solution to 9 to 10, and then use dilute hydrochloric acid to adjust the pH of the solution to 6 to 8 to obtain a mixed solution A;
三、将步骤二得到的混合溶液A，加入30mL～50mL的无水乙醇，室温下开始搅拌，并滴入步骤一得到的铬酸钠溶液至混合溶液A为黄色，搅拌30min～50min后，用保鲜膜封闭烧杯口，在室温下静置12h～24h，得到混合溶液B；3. Add 30mL to 50mL of absolute ethanol to the mixed solution A obtained in step 2, start stirring at room temperature, and drop in the sodium chromate solution obtained in step 1 until the mixed solution A turns yellow. After stirring for 30min to 50min, use Seal the mouth of the beaker with plastic wrap, and let it stand at room temperature for 12h to 24h to obtain the mixed solution B;
四、将步骤三得到的混合溶液B离心分离，先用无水乙醇洗涤3～5次，然后再用去离子水洗涤3～5次，洗涤后放入烘箱中，在温度为60℃～160℃下干燥10h～24h，得到微米级晶体生长形貌可控的球形铬酸锶粉体；其中，离心分离的转速为5000rpm～15000rpm，离心分离的时间为1min～10min。4. Centrifuge the mixed solution B obtained in step 3, wash it with absolute ethanol for 3 to 5 times, then wash it with deionized water for 3 to 5 times, put it in an oven after washing, and put it in an oven at a temperature of 60°C to 160°C. Dry at ℃ for 10h-24h to obtain spherical strontium chromate powder with controllable micron-sized crystal growth morphology; wherein, the rotational speed of centrifugation is 5000rpm-15000rpm, and the time of centrifugation is 1min-10min.
本发明包括以下有益效果：The present invention comprises following beneficial effect:
1、本发明通过直接沉淀法制备微米级球状的铬酸锶粉体，只需在室温下进行，条件温和易控，成本低，制备方法简单，且易大量生产；1. The present invention prepares micron-sized spherical strontium chromate powder by direct precipitation method, which only needs to be carried out at room temperature, the conditions are mild and easy to control, the cost is low, the preparation method is simple, and it is easy to produce in large quantities;
2、本发明制备的微米级球状的铬酸锶粉体，颗粒形貌大小可控，性能良好并能实现大规模批量生产。2. The micron-sized spherical strontium chromate powder prepared by the present invention has controllable particle shape and size, good performance and can realize large-scale batch production.
附图说明Description of drawings
图1为试验一制备的微米级球状的铬酸锶粉体的XRD图；Fig. 1 is the XRD pattern of the micron-sized spherical strontium chromate powder that test one prepares;
图2为试验三制备的微米级球状的铬酸锶粉体的SEM形貌；Fig. 2 is the SEM morphology of the micron-sized spherical strontium chromate powder prepared in test three;
图3为试验六制备的微米级球状的铬酸锶粉体的SEM形貌。Fig. 3 is the SEM morphology of the micron-sized spherical strontium chromate powder prepared in Experiment 6.
具体实施方式Detailed ways
具体实施方式一：本实施方式的一种微米级晶体生长形貌可控的球形铬酸锶粉体的制备方法是按以下步骤进行：Embodiment 1: The preparation method of a spherical strontium chromate powder with controllable micron-scale crystal growth morphology in this embodiment is carried out according to the following steps:
一、称取2.34g～23.4g的四水铬酸钠(Na2CrO4.4H2O)溶解于蒸馏水中，配制成浓度为0.1mol/L～1mol/L的铬酸钠溶液；1. Weigh 2.34g~23.4g of sodium chromate tetrahydrate (Na 2 CrO 4 .4H 2 O) and dissolve it in distilled water to prepare a sodium chromate solution with a concentration of 0.1mol/L~1mol/L;
二、称取2.67g～26.7g的六水氯化锶(SrCl2.6H2O)溶解于蒸馏水中，配制成浓度为0.1mol/L～1mol/L的氯化锶溶液，然后向其中加入2g～8g的EDTA二钠，再用氨水调节溶液pH值为9～10，随后再用稀盐酸调节溶液pH值为6～8，得到混合溶液A；2. Weigh 2.67g-26.7g of strontium chloride hexahydrate (SrCl 2 .6H 2 O) and dissolve it in distilled water to prepare a strontium chloride solution with a concentration of 0.1mol/L-1mol/L, and then add 2g to 8g of disodium EDTA, and then use ammonia water to adjust the pH of the solution to 9 to 10, and then use dilute hydrochloric acid to adjust the pH of the solution to 6 to 8 to obtain a mixed solution A;
三、将步骤二得到的混合溶液A，加入30mL～50mL的无水乙醇，室温下开始搅拌，并滴入步骤一得到的铬酸钠溶液至混合溶液A为黄色，搅拌30min～50min后，用保鲜膜封闭烧杯口，在室温下静置12h～24h，得到混合溶液B；3. Add 30mL to 50mL of absolute ethanol to the mixed solution A obtained in step 2, start stirring at room temperature, and drop in the sodium chromate solution obtained in step 1 until the mixed solution A turns yellow. After stirring for 30min to 50min, use Seal the mouth of the beaker with plastic wrap, and let it stand at room temperature for 12h to 24h to obtain the mixed solution B;
四、将步骤三得到的混合溶液B离心分离，先用无水乙醇洗涤3～5次，然后再用去离子水洗涤3～5次，洗涤后放入烘箱中，在温度为60℃～160℃下干燥10h～24h，得到微米级晶体生长形貌可控的球形铬酸锶粉体；其中，离心分离的转速为5000rpm～15000rpm，离心分离的时间为1min～10min。4. Centrifuge the mixed solution B obtained in step 3, wash it with absolute ethanol for 3 to 5 times, then wash it with deionized water for 3 to 5 times, put it in an oven after washing, and put it in an oven at a temperature of 60°C to 160°C. Dry at ℃ for 10h-24h to obtain spherical strontium chromate powder with controllable micron-sized crystal growth morphology; wherein, the rotational speed of centrifugation is 5000rpm-15000rpm, and the time of centrifugation is 1min-10min.
本实施方式包括以下有益效果：This embodiment includes the following beneficial effects:
1、本实施方式通过直接沉淀法制备微米级球状的铬酸锶粉体，只需在室温下进行，反应条件温和易控，成本低，制备方法简单，且易大量生产；1. In this embodiment, the micron-sized spherical strontium chromate powder is prepared by the direct precipitation method, which only needs to be carried out at room temperature, the reaction conditions are mild and easy to control, the cost is low, the preparation method is simple, and it is easy to produce in large quantities;
2、本实施方式制备的微米级球状的铬酸锶粉体，晶体生长形貌、粒径大小可控，性能良好，并能实现大规模批量生产。2. The micron-sized spherical strontium chromate powder prepared in this embodiment has controllable crystal growth morphology and particle size, good performance, and can realize large-scale batch production.
具体实施方式二：本实施方式与具体实施方式一不同的是：步骤一中称取2.34g的四水铬酸钠(Na2CrO4.4H2O)溶解于蒸馏水中，配制成摩尔浓度为0.1mol/L的铬酸钠溶液。其它与具体实施方式一相同。Specific embodiment 2: The difference between this embodiment and specific embodiment 1 is that in step 1, 2.34 g of sodium chromate tetrahydrate (Na 2 CrO 4 .4H 2 O) was weighed and dissolved in distilled water, and the molar concentration was prepared to be 0.1mol/L sodium chromate solution. Others are the same as in the first embodiment.
具体实施方式三：本实施方式与具体实施方式一或二不同的是：步骤二中称取2.67g的六水氯化锶(SrCl2.6H2O)溶解于蒸馏水中，配制成摩尔浓度为0.1mol/L的氯化锶溶液。其它与具体实施方式一或二相同。Specific embodiment three: the difference between this embodiment and specific embodiment one or two is that in step two, 2.67g of strontium chloride hexahydrate (SrCl 2 .6H 2 O) is weighed and dissolved in distilled water, and the molar concentration is prepared to be 0.1mol/L strontium chloride solution. Others are the same as in the first or second embodiment.
具体实施方式四：本实施方式与具体实施方式一至三之一不同的是：步骤二中用氨水调节溶液pH值为9。其它与具体实施方式一至三之一相同。Embodiment 4: The difference between this embodiment and one of Embodiments 1 to 3 is that in step 2, ammonia water is used to adjust the pH of the solution to 9. Others are the same as those in the first to third specific embodiments.
具体实施方式五：本实施方式与具体实施方式一至四之一不同的是：步骤三中加入50mL的无水乙醇。其它与具体实施方式一至四之一相同。Embodiment 5: This embodiment is different from one of Embodiments 1 to 4 in that: 50 mL of absolute ethanol is added in Step 3. Others are the same as one of the specific embodiments 1 to 4.
具体实施方式六：本实施方式与具体实施方式一至五之一不同的是：步骤三中在室温下静置24h。其它与具体实施方式一至五之一相同。Embodiment 6: The difference between this embodiment and one of Embodiments 1 to 5 is: in step 3, let stand at room temperature for 24 hours. Others are the same as one of the specific embodiments 1 to 5.
具体实施方式七：本实施方式与具体实施方式一至六之一不同的是：步骤四中在温度为80℃下干燥18h。其它与具体实施方式一至六之一相同。Embodiment 7: This embodiment is different from Embodiment 1 to Embodiment 6 in that: in step 4, the temperature is 80° C. for 18 hours. Others are the same as one of the specific embodiments 1 to 6.
具体实施方式八：本实施方式与具体实施方式一至七之一不同的是：步骤四中离心分离的转速为8000rpm，离心分离的时间为2min。其它与具体实施方式一至七之一相同。Embodiment 8: This embodiment differs from Embodiment 1 to Embodiment 7 in that: the speed of centrifugation in step 4 is 8000 rpm, and the time of centrifugation is 2 minutes. Others are the same as one of the specific embodiments 1 to 7.
通过以下试验验证本发明的有益效果：Prove the beneficial effect of the present invention by following test:
试验一：本试验的一种微米级球状的铬酸锶陶瓷粉体的制备方法是按以下步骤实现的：Test 1: The preparation method of a kind of micron-scale spherical strontium chromate ceramic powder in this test is realized according to the following steps:
一、称取2.34g的四水铬酸钠(Na2CrO4.4H2O)溶解于蒸馏水中，配制成摩尔浓度为0.1mol/L的铬酸钠溶液；1. Dissolve 2.34 g of sodium chromate tetrahydrate (Na 2 CrO 4 .4H 2 O) in distilled water to prepare a sodium chromate solution with a molar concentration of 0.1 mol/L;
二、称取2.67g的六水氯化锶(SrCl2.6H2O)溶解于蒸馏水中，配制成摩尔浓度为0.1mol/L的氯化锶溶液，然后向其中加入2g的EDTA二钠，再用氨水调节溶液pH值为9，随后再用稀盐酸调节溶液pH值为6，得到混合溶液A；2. Dissolve 2.67g of strontium chloride hexahydrate (SrCl 2 .6H 2 O) in distilled water to prepare a strontium chloride solution with a molar concentration of 0.1mol/L, then add 2g of disodium EDTA to it, The pH value of the solution was adjusted to 9 with ammonia water, and then the pH value of the solution was adjusted to 6 with dilute hydrochloric acid to obtain a mixed solution A;
三、将步骤二得到的混合溶液A，加入50mL的无水乙醇，室温下开始搅拌，并滴入步骤一得到的铬酸钠溶液至混合溶液A为黄色，搅拌30min后，用保鲜膜封闭烧杯口，在室温下静置24h，得到混合溶液B；3. Add 50mL of absolute ethanol to the mixed solution A obtained in step 2, start stirring at room temperature, and drop the sodium chromate solution obtained in step 1 until the mixed solution A turns yellow. After stirring for 30 minutes, seal the beaker with plastic wrap Mouth, stand at room temperature 24h, obtain mixed solution B;
四、将步骤三得到的混合溶液B离心分离，先用无水乙醇洗涤3次，然后再用去离子水洗涤3次，洗涤后放入烘箱中，在温度为80℃下干燥18h，得到微米数量级球状的铬酸锶陶瓷粉体；其中，离心分离的转速为8000rpm，离心分离的时间为2min。4. Centrifuge the mixed solution B obtained in step 3, wash it with absolute ethanol for 3 times, then wash it with deionized water for 3 times, put it in an oven after washing, and dry it at a temperature of 80°C for 18 hours to obtain micron Order of magnitude spherical strontium chromate ceramic powder; wherein, the rotational speed of centrifugation is 8000rpm, and the time of centrifugation is 2min.
本试验制备的微米级球状的铬酸锶粉体的XRD图如图1所示，从图1可见，铬酸锶粉体为单斜相。对照标准卡片(JCPDS.card.no15-365)看出(110)、(011)、(021)、(200)、(120)、(210)以及(012)、(-202)、(-212)、(031)、(-131)、(212)、(-132)、(040)、(140)、(410)、(332)、(-124)和(-332)等晶面的特征衍射与标准卡片一致。衍射图谱中除了上述晶面的衍射峰以外，并未见其他衍射峰，证明本实验所得SrCrO4化合物无杂质，纯度高，结晶性良好。The XRD pattern of the micron-sized spherical strontium chromate powder prepared in this test is shown in Figure 1. From Figure 1, it can be seen that the strontium chromate powder is a monoclinic phase. Compared with the standard card (JCPDS.card.no15-365), it can be seen that (110), (011), (021), (200), (120), (210) and (012), (-202), (-212 ), (031), (-131), (212), (-132), (040), (140), (410), (332), (-124) and (-332) etc. Diffraction is consistent with standard cards. Except for the diffraction peaks of the above-mentioned crystal planes, no other diffraction peaks are seen in the diffraction pattern, which proves that the SrCrO compound obtained in this experiment has no impurities, high purity and good crystallinity.
试验二：本试验与试验一不同的是：步骤二中用稀盐酸调节溶液pH值为7。其它与试验一相同。Test 2: The difference between this test and Test 1 is that in Step 2, dilute hydrochloric acid is used to adjust the pH value of the solution to 7. Others are the same as experiment one.
试验三：本试验与试验一不同的是：步骤二中用稀盐酸调节溶液pH值为8。其它与试验一相同。Test 3: The difference between this test and Test 1 is that in Step 2, dilute hydrochloric acid is used to adjust the pH value of the solution to 8. Others are the same as experiment one.
本试验制备的微米级球状的铬酸锶粉体的SEM形貌如图2所示，从图2可见，通过同时添加EDTA活性剂和无水乙醇，采用直接化学沉淀法制备出生长形貌呈球形的铬酸锶粉体，粒径为微米级，粒径均匀、大小适中(平均粒径为2μm)，分散性好等优点，可广泛应用于微米级球状的铬酸锶粉体材料的制备。The SEM morphology of the micron-sized spherical strontium chromate powder prepared in this experiment is shown in Figure 2. It can be seen from Figure 2 that by adding EDTA active agent and absolute ethanol at the same time, the growth morphology was prepared by direct chemical precipitation method. Spherical strontium chromate powder, with micron particle size, uniform particle size, moderate size (average particle size 2μm), good dispersibility, etc., can be widely used in the preparation of micron spherical strontium chromate powder materials .
试验四：本试验与试验一不同的是：步骤二中加入4g的EDTA二钠。其它与试验一相同。Test 4: The difference between this test and test 1 is that 4 g of disodium EDTA is added in step 2. Others are the same as experiment one.
试验五：本试验与试验一不同的是：步骤二中加入6g的EDTA二钠。其它与试验一相同。Test five: the difference between this test and test one is that 6 g of disodium EDTA is added in step two. Others are the same as experiment one.
试验六：本试验与试验一不同的是：步骤二中加入8g的EDTA二钠。其它与试验一相同。Test 6: The difference between this test and test 1 is that 8 g of disodium EDTA is added in step 2. Others are the same as experiment one.
本试验制备的微米级球状的铬酸锶粉体的SEM形貌如图3所示，从图3可见，通过同时添加EDTA活性剂和无水乙醇，采用直接化学沉淀法制备出生长形貌呈球形的铬酸锶粉体，粒径为微米级，粒径均匀、大小适中(平均粒径为1μm)，分散性好等优点，可广泛应用于微米级球状的铬酸锶粉体材料的制备。The SEM morphology of the micron-sized spherical strontium chromate powder prepared in this experiment is shown in Figure 3. It can be seen from Figure 3 that by adding EDTA active agent and absolute ethanol at the same time, the growth morphology was prepared by direct chemical precipitation method. Spherical strontium chromate powder has the advantages of micron-scale particle size, uniform particle size, moderate size (average particle size is 1 μm), and good dispersion. It can be widely used in the preparation of micron-scale spherical strontium chromate powder materials .
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