CN105967749A - 一种亚稳态Bi2SiO5多孔材料的制备方法 - Google Patents
一种亚稳态Bi2SiO5多孔材料的制备方法 Download PDFInfo
- Publication number
- CN105967749A CN105967749A CN201610292951.XA CN201610292951A CN105967749A CN 105967749 A CN105967749 A CN 105967749A CN 201610292951 A CN201610292951 A CN 201610292951A CN 105967749 A CN105967749 A CN 105967749A
- Authority
- CN
- China
- Prior art keywords
- solution
- citric acid
- sio
- acid
- porous material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011148 porous material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 108
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 14
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 8
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 7
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 7
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000011975 tartaric acid Substances 0.000 claims abstract description 7
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- BDZGJPFBTVYBOA-UHFFFAOYSA-N ethene Chemical group C=C.C=C.C=C.C=C.C=C BDZGJPFBTVYBOA-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000908 ammonium hydroxide Substances 0.000 abstract 2
- 238000000465 moulding Methods 0.000 abstract 2
- 229960001484 edetic acid Drugs 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 229940057838 polyethylene glycol 4000 Drugs 0.000 description 2
- 229940093429 polyethylene glycol 6000 Drugs 0.000 description 2
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001451 bismuth ion Inorganic materials 0.000 description 1
- 238000009933 burial Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon ions Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/624—Sol-gel processing
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63488—Polyethers, e.g. alkylphenol polyglycolether, polyethylene glycol [PEG], polyethylene oxide [PEO]
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0051—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
- C04B38/0058—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity open porosity
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/549—Particle size related information the particle size being expressed by crystallite size or primary particle size
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
本发明公开了一种亚稳态Bi2SiO5多孔材料的制备方法，首先配制柠檬酸的氨水溶液，将氧化铋溶于硝酸中，再分别将氧化铋溶液和正硅酸乙酯溶于柠檬酸的氨水溶液中，加入一定量的乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇等分散剂，经凝胶化获得适合于直接压制成型的干凝胶粉体，经压制成型和热处理即可获得亚稳态Bi2SiO5多孔材料；该方法工艺设备简单、周期短、成本低。
Description
技术领域
本发明属于材料技术领域，特别涉及一种亚稳态Bi2SiO5多孔材料的制备方法。
背景技术
Bi2SiO5是Bi2O3-SiO2系统中摩尔比为1∶1的亚稳定相化合物，Bi2SiO5属正交晶系的Cmc21空间群，其结构可以看作是由[Bi2O2]2+层分隔开的孤立的[SiO3]2-链所构成,因此结构式也可写成Bi4[O4][Si2O6]。正因为Bi2SiO5具有以上结构，其主要具有介电、热电以及非线性光学等性质,其非中心对称的晶体结构还使其有可能具有铁电性质。多孔陶瓷由于其多孔的结构，当孔隙小而分布均匀时，可使多孔陶瓷的比表面积大大增大，活性增强。相比于多孔纳米粉体材料，由于纳米粉体材料的表面断键数较多，比表面积增大，使纳米颗粒间易相互团聚，纳米颗粒越小，则表面活性越大，团聚越严重。如果多孔材料中的细孔分布均匀，则可解决这个问题，且保持了较高的比表面积和表面活性。
发明内容
为了克服上述现有技术的缺点，本发明的目的在于提供一种亚稳态Bi2SiO5多孔材料的制备方法，具有生产工艺简单、设备要求简单、周期短的特点。
为了实现上述目的，本发明采用的技术方案是：
一种亚稳态Bi2SiO5多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水中得到柠檬酸溶液A，将氧化铋溶于硝酸中反应形成溶液B；
(2)量取1/3的柠檬酸溶液A，将正硅酸乙酯溶于其中形成溶液C；将溶液B溶于剩余柠檬酸溶液A中形成溶液D；
(3)将分散剂加入溶液D中，再加入溶液C和无水乙醇搅拌溶解，之后调节pH值至1～3即获得溶胶E；
(4)将溶胶E于80～85℃下水浴1～3h至凝胶化，再在140～160℃下干燥形成干凝胶，室温下自然晾干后进行研磨过筛得到干凝胶粉体；
(5)将过筛后的干粉直接干压成型，形成块状坯体材料，最后将块状坯体材料进行热处理得到亚稳态Bi2SiO5多孔材料。
所述步骤(1)中，氨水的量以能溶解柠檬酸为准，硝酸的量以能完全溶解氧化铋为准。
所述正硅酸乙酯和氧化铋的用量满足Bi与Si的摩尔比为(1：2)～(1：5)，且Si离子与Bi离子之和与步骤(1)中柠檬酸的摩尔比为1：(0.5～1.0)。
所述步骤(2)中，所述分散剂由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇和聚乙二醇组成。
所述分散剂加入溶液D后，分散剂各组份的浓度范围均为0～1.0mol/L。
所述步骤(2)中，无水乙醇的体积是氨水体积的1/3～1/2。
所述步骤(4)中，所述热处理是在ZnO粉体中进行埋烧，温度为600℃～700℃。
与现有技术相比，本发明的有益效果是：本发明提供的亚稳态Bi2SiO5多孔材料的制备方法中，以乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇(如聚乙二醇400、聚乙二醇4000、聚乙二醇6000)等作为分散剂直接进行络合发泡的凝胶化过程，通过控制各物质的浓度，特别是各分散剂的用量，干燥后所形成的中间粉体物质可直接成型成块状材料，在这个制备方法中，不仅利用分散剂使铋离子和硅离子均匀地存在于体系中，使亚稳态Bi2SiO5多孔材料的结晶和复合过程更加均匀，而且减少造粒、陈腐的过程，使结晶过程与烧结一步完成，这都使制备周期缩短，成本降低。结合埋烧的热处理过程，利用有机物的发泡和分解燃烧过程形成亚稳态Bi2SiO5多孔材料，可获得开孔的亚稳态Bi2SiO5多孔材料。
具体实施方式
下面结合实施例详细说明本发明的实施方式。
实施例1
一种亚稳态Bi2SiO5多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水中形成柠檬酸溶液A，氨水的量以能溶解柠檬酸为准；将氧化铋溶于硝酸中反应形成溶液B，硝酸以能完全溶解氧化铋为准。
(3)量取1/3的溶液A，将正硅酸乙酯溶于其中形成溶液C；将溶液B溶于剩余柠檬酸溶液中形成溶液D，其中，Bi：Si(摩尔比)＝1：2，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：0.5。
(3)称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成，其中聚乙二醇又包括聚乙二醇400、聚乙二醇4000和聚乙二醇6000。)加入溶液D中，分散剂各组份的浓度控制在1.0mol/L，加入溶液C和无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的1/3)，之后调节pH值至1～3即获得溶胶E。
(4)将溶胶E于80℃下水浴1～3h至凝胶化，然后在140℃下干燥形成干凝胶，室温下自然晾干后将粉体进行研磨过筛。
(5)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中进行埋烧即获得亚稳态Bi2SiO5多孔材料，热处理温度为600℃。所得亚稳态Bi2SiO5多孔材料中为开孔结构，晶粒尺寸约为150nm～500nm，间隙尺寸为80nm～200nm。
实施例2
一种亚稳态Bi2SiO5多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水中形成柠檬酸溶液A，氨水的量以能溶解柠檬酸为准；将氧化铋溶于硝酸中反应形成溶液B，硝酸以能完全溶解氧化铋为准。
(3)量取1/3的溶液A，将正硅酸乙酯溶于其中形成溶液C；将溶液B溶于剩余柠檬酸溶液中形成溶液D，其中，Bi：Si(摩尔比)＝1：5的比例，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：1。
(3)称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成。)加入溶液D中，分散剂各组份的浓度控制在1.0mol/L，加入溶液C和无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的1/2)，之后调节pH值至1～3即获得溶胶E。
(4)将溶胶E于85℃下水浴1～3h至凝胶化，然后在140℃下干燥形成干凝胶，室温下自然晾干后将粉体进行研磨过筛。
(5)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中进行埋烧即获得亚稳态Bi2SiO5多孔材料，热处理温度为700℃。所得亚稳态Bi2SiO5多孔材料中为开孔结构，晶粒尺寸约为150nm～500nm，间隙尺寸为80nm～200nm。
实施例3
一种亚稳态Bi2SiO5多孔材料的制备方法，包括如下步骤：
(1)将柠檬酸溶于氨水中形成柠檬酸溶液A，氨水的量以能溶解柠檬酸为准；将氧化铋溶于硝酸中反应形成溶液B，硝酸以能完全溶解氧化铋为准。
(3)量取1/3的溶液A，将正硅酸乙酯溶于其中形成溶液C；将溶液B溶于剩余柠檬酸溶液中形成溶液D，其中，Bi：Si(摩尔比)＝1：3的比例，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：0.8。
(3)称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成。)加入溶液D中，分散剂各组份的浓度控制在0.01、0.1、0.1、0.5、0.5、1.0mol/L，加入溶液C和无水乙醇搅拌溶解(无水乙醇的体积是氨水体积的1/2)，之后调节pH值至1～3即获得溶胶E。
(4)将溶胶E于80℃～85℃下水浴1～3h至凝胶化，然后在140℃～160℃下干燥形成干凝胶，室温下自然晾干后将粉体进行研磨过筛。
(5)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中进行埋烧即获得亚稳态Bi2SiO5多孔材料，热处理温度为600℃。所得亚稳态Bi2SiO5多孔材料中为开孔结构，晶粒尺寸约为150nm～500nm，间隙尺寸为80nm～200nm。
Claims (7)
1.一种亚稳态Bi2SiO5多孔材料的制备方法，其特征在于，包括如下步骤：
(1)将柠檬酸溶于氨水中得到柠檬酸溶液A，将氧化铋溶于硝酸中反应形成溶液B；
(2)量取1/3的柠檬酸溶液A，将正硅酸乙酯溶于其中形成溶液C；将溶液B溶于剩余柠檬酸溶液A中形成溶液D；
(3)将分散剂加入溶液D中，再加入溶液C和无水乙醇搅拌溶解，之后调节pH值至1～3即获得溶胶E；
(4)将溶胶E于80～85℃下水浴1～3h至凝胶化，再在140～160℃下干燥形成干凝胶，室温下自然晾干后进行研磨过筛得到干凝胶粉体；
(5)将过筛后的干粉直接干压成型，形成块状坯体材料，最后将块状坯体材料进行热处理得到亚稳态Bi2SiO5多孔材料。
2.根据权利要求1所述亚稳态Bi2SiO5多孔材料的制备方法，其特征在于，所述步骤(1)中，氨水的量以能溶解柠檬酸为准，硝酸的量以能完全溶解氧化铋为准。
3.根据权利要求1所述亚稳态Bi2SiO5多孔材料的制备方法，其特征在于，所述正硅酸乙酯和氧化铋的用量满足Bi与Si的摩尔比为(1：2)～(1：5)，且Si离子与Bi离子之和与步骤(1)中柠檬酸的摩尔比为1：(0.5～1.0)。
4.根据权利要求1所述亚稳态Bi2SiO5多孔材料的制备方法，其特征在于，所述步骤(2)中，所述分散剂由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇和聚乙二醇组成。
5.根据权利要求4所述亚稳态Bi2SiO5多孔材料的制备方法，其特征在于，所述分散剂加入溶液D后，分散剂各组份的浓度范围均为0～1.0mol/L。
6.根据权利要求4所述亚稳态Bi2SiO5多孔材料的制备方法，其特征在于，所述步骤(2)中，无水乙醇的体积是氨水体积的1/3～1/2。
7.根据权利要求1所述亚稳态Bi2SiO5多孔材料的制备方法，其特征在于，所述步骤(4)中，所述热处理是在ZnO粉体中进行埋烧，温度为600℃～700℃。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610292951.XA CN105967749A (zh) | 2016-05-05 | 2016-05-05 | 一种亚稳态Bi2SiO5多孔材料的制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610292951.XA CN105967749A (zh) | 2016-05-05 | 2016-05-05 | 一种亚稳态Bi2SiO5多孔材料的制备方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105967749A true CN105967749A (zh) | 2016-09-28 |
Family
ID=56991930
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610292951.XA Pending CN105967749A (zh) | 2016-05-05 | 2016-05-05 | 一种亚稳态Bi2SiO5多孔材料的制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105967749A (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110252341A (zh) * | 2019-06-18 | 2019-09-20 | 陕西科技大学 | 一种Bi2O2SiO3/Bi2O3/BiOBr异质复合光材料的制备方法 |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57196718A (en) * | 1981-05-26 | 1982-12-02 | Res Assoc Petroleum Alternat Dev<Rapad> | Novel crystalline silicate and its manufacture |
| CN1796552A (zh) * | 2004-12-29 | 2006-07-05 | 华东理工大学 | 一种用于生物酶载体的块状多孔材料的制备方法 |
| CN101362085A (zh) * | 2008-09-18 | 2009-02-11 | 武汉理工大学 | 可见光催化剂Bi2WO6纳米粉体的制备方法 |
| CN101367539A (zh) * | 2008-09-19 | 2009-02-18 | 沈阳化工学院 | 溶胶凝胶法制备纳米发光粉体 |
| CN101724395A (zh) * | 2009-11-24 | 2010-06-09 | 沈阳化工学院 | 一种溶胶凝胶法制备纳米SrHfO3:Ce3+发光粉体的方法 |
| CN101891206A (zh) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | 一种SiO2/TiO2复合微球的制备方法 |
| CN102275942A (zh) * | 2011-07-06 | 2011-12-14 | 陕西科技大学 | 一种硅酸铋纳米粉体的制备方法 |
-
2016
- 2016-05-05 CN CN201610292951.XA patent/CN105967749A/zh active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57196718A (en) * | 1981-05-26 | 1982-12-02 | Res Assoc Petroleum Alternat Dev<Rapad> | Novel crystalline silicate and its manufacture |
| CN1796552A (zh) * | 2004-12-29 | 2006-07-05 | 华东理工大学 | 一种用于生物酶载体的块状多孔材料的制备方法 |
| CN101362085A (zh) * | 2008-09-18 | 2009-02-11 | 武汉理工大学 | 可见光催化剂Bi2WO6纳米粉体的制备方法 |
| CN101367539A (zh) * | 2008-09-19 | 2009-02-18 | 沈阳化工学院 | 溶胶凝胶法制备纳米发光粉体 |
| CN101724395A (zh) * | 2009-11-24 | 2010-06-09 | 沈阳化工学院 | 一种溶胶凝胶法制备纳米SrHfO3:Ce3+发光粉体的方法 |
| CN101891206A (zh) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | 一种SiO2/TiO2复合微球的制备方法 |
| CN102275942A (zh) * | 2011-07-06 | 2011-12-14 | 陕西科技大学 | 一种硅酸铋纳米粉体的制备方法 |
Non-Patent Citations (2)
| Title |
|---|
| 米晓云等: "《Al2O3纳米粉体及透明陶瓷》", 31 March 2012, 吉林大学出版社 * |
| 衣宝廉: "《燃料电池-原理.技术.应用》", 31 August 2003, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110252341A (zh) * | 2019-06-18 | 2019-09-20 | 陕西科技大学 | 一种Bi2O2SiO3/Bi2O3/BiOBr异质复合光材料的制备方法 |
| CN110252341B (zh) * | 2019-06-18 | 2021-11-16 | 陕西科技大学 | 一种Bi2O2SiO3/Bi2O3/BiOBr异质复合光材料的制备方法 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108516818B (zh) | 一种基于改进的Isobam凝胶体系制备YAG透明陶瓷的方法 | |
| CN100548919C (zh) | 一种低温制备Bi3TiNbO9微纳米压电铁电粉体的方法 | |
| CN103086692A (zh) | 一种块状SiO2-Y2O3复合气凝胶的制备方法 | |
| CN105967723A (zh) | 一种二氧化硅多孔材料的制备方法 | |
| CN105330286A (zh) | 一种巨介电常数纳米钛酸铜钙陶瓷材料的制备方法 | |
| CN104445346A (zh) | 一种纳米氧化钇粉体的水热合成方法 | |
| CN105967749A (zh) | 一种亚稳态Bi2SiO5多孔材料的制备方法 | |
| CN104909747B (zh) | 一种高介电常数、低介电损耗CaCu3Ti4‑xZrxO12陶瓷的制备方法 | |
| CN105948809A (zh) | 一种多孔ZnO块体材料的制备方法 | |
| CN105967721A (zh) | 一种Bi2SiO5多孔材料的制备方法 | |
| CN105967747A (zh) | 一种稳态Bi4Si3O12多孔材料的制备方法 | |
| CN105964235B (zh) | 一种多孔二氧化钛-二氧化硅块材的制备方法 | |
| CN105948805A (zh) | 一种二氧化钛多孔材料的制备方法 | |
| CN105924144A (zh) | 一种多孔亚稳态Bi2SiO5块材的制备方法 | |
| CN104445343A (zh) | 一种纳米氧化钇粉体的合成方法 | |
| CN105218076B (zh) | 一种利用溶胶凝胶法制备SrMnO3陶瓷粉体的方法 | |
| CN105944705B (zh) | 一种TiO2-SiO2多孔材料的制备方法 | |
| CN105948118B (zh) | 一种多孔Bi4Si3O12块材的制备方法 | |
| CN105948808A (zh) | 一种稳态Bi12SiO20多孔材料的制备方法 | |
| CN107573069A (zh) | 一种中温烧结的中介电常数高q值微波介质材料 | |
| CN105948806A (zh) | 一种多孔稳态Bi4Si3O12块材的制备方法 | |
| CN105967745A (zh) | 一种多孔稳态Bi12SiO20块材的制备方法 | |
| CN105944706B (zh) | 一种SiO2-TiO2多孔材料的制备方法 | |
| CN105036201A (zh) | 锶和铝掺杂y型铁氧体复合吸波材料及其制备方法 | |
| CN105967724A (zh) | 一种氧化锌多孔材料的制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160928 |
|
| RJ01 | Rejection of invention patent application after publication |