CN115135606A - 一种制备四方相钛酸钡纳米颗粒的方法 - Google Patents
一种制备四方相钛酸钡纳米颗粒的方法 Download PDFInfo
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- CN115135606A CN115135606A CN202080093960.0A CN202080093960A CN115135606A CN 115135606 A CN115135606 A CN 115135606A CN 202080093960 A CN202080093960 A CN 202080093960A CN 115135606 A CN115135606 A CN 115135606A
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- barium
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- water
- barium titanate
- soluble salt
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- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 77
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 48
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 title claims abstract description 37
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000010936 titanium Substances 0.000 claims abstract description 52
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 52
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 51
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229960000583 acetic acid Drugs 0.000 claims abstract description 43
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims abstract description 43
- 150000003839 salts Chemical class 0.000 claims abstract description 41
- 229910052788 barium Inorganic materials 0.000 claims abstract description 30
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000002844 melting Methods 0.000 claims abstract description 27
- 230000008018 melting Effects 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 238000001354 calcination Methods 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 25
- 108010025899 gelatin film Proteins 0.000 claims abstract description 9
- 150000001553 barium compounds Chemical class 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 55
- 235000011151 potassium sulphates Nutrition 0.000 claims description 55
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical group [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 54
- 235000002639 sodium chloride Nutrition 0.000 claims description 42
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 239000001103 potassium chloride Substances 0.000 claims description 5
- 235000011164 potassium chloride Nutrition 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims description 5
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 3
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 3
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 3
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000003985 ceramic capacitor Substances 0.000 abstract 1
- 230000009466 transformation Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 83
- 239000000843 powder Substances 0.000 description 41
- 238000004062 sedimentation Methods 0.000 description 18
- 239000012071 phase Substances 0.000 description 14
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000009388 chemical precipitation Methods 0.000 description 4
- 238000003837 high-temperature calcination Methods 0.000 description 4
- 238000002955 isolation Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- -1 various sensors Substances 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical class CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
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- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
提供一种高分散四方相钛酸钡纳米颗粒的制备方法，包括：1）将钛酸四丁酯溶于有机溶剂中，得到溶液A；将钡化合物加入冰乙酸中，溶解或反应后，得到溶液B；将溶液A和B混合配制出含有钛和钡的有机溶胶；2）用该溶胶与水溶性盐混合，静置或离心，使水溶性盐沉降，去除上部多余的有机溶胶，得到溶胶与水溶性盐的混合物；3）保温，发生溶胶凝胶转变，凝胶干燥后在水溶性盐颗粒表面包覆干凝胶膜；4）在600℃以上和盐熔点以下煅烧，干凝胶膜转变为钛酸钡纳米颗粒，形成煅烧产物；5）水洗、干燥，得到四方相钛酸钡纳米颗粒。该方法可以快速批量制备出高分散四方相钛酸钡纳米颗粒，可用于制备超薄层多层陶瓷电容器等基础电子元件。
Description
PCT国内申请，说明书已公开。
Claims (4)
- PCT国内申请，权利要求书已公开。
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| JP (1) | JP7487971B2 (zh) |
| CN (1) | CN115135606B (zh) |
| WO (1) | WO2021168736A1 (zh) |
Cited By (1)
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|---|---|---|---|---|
| CN115403068A (zh) * | 2022-10-14 | 2022-11-29 | 西南交通大学 | 一种钛酸钡纳米立方块材料及其制备方法和应用 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115483383A (zh) * | 2022-09-30 | 2022-12-16 | 陕西科技大学 | 一种钛酸钡包覆三元正极材料及其制备方法和应用 |
| CN115744993B (zh) * | 2022-11-04 | 2024-06-07 | 济南大学 | 一种大批量合成超小Mn3O4纳米酶的方法 |
| CN118005072B (zh) * | 2024-04-10 | 2024-06-18 | 杭州兴容科技有限公司 | 一种钛酸钡的水热合成方法 |
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2020
- 2020-02-27 WO PCT/CN2020/076963 patent/WO2021168736A1/zh active Application Filing
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Cited By (2)
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|---|---|---|---|---|
| CN115403068A (zh) * | 2022-10-14 | 2022-11-29 | 西南交通大学 | 一种钛酸钡纳米立方块材料及其制备方法和应用 |
| CN115403068B (zh) * | 2022-10-14 | 2023-11-21 | 西南交通大学 | 一种钛酸钡纳米立方块材料及其制备方法和应用 |
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| Publication number | Publication date |
|---|---|
| JP7487971B2 (ja) | 2024-05-21 |
| WO2021168736A1 (zh) | 2021-09-02 |
| JP2023532164A (ja) | 2023-07-27 |
| CN115135606B (zh) | 2024-07-16 |
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