CN115450041A - 一种具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料及其制备方法 - Google Patents
一种具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料及其制备方法 Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 91
- 239000004744 fabric Substances 0.000 title claims abstract description 89
- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 60
- 239000011029 spinel Substances 0.000 title claims abstract description 60
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 7
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 6
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 5
- -1 transition metal salt compounds Chemical class 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 238000005406 washing Methods 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 239000011651 chromium Substances 0.000 description 10
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 8
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 239000011572 manganese Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 4
- 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 description 3
- 229910021555 Chromium Chloride Inorganic materials 0.000 description 3
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 3
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 description 3
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 235000002867 manganese chloride Nutrition 0.000 description 3
- 239000011565 manganese chloride Substances 0.000 description 3
- 229940099607 manganese chloride Drugs 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910001428 transition metal ion Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料及其制备方法,该方法包括:碳布酸洗处理;选用Cr、Mn、Fe、Co、Ni、Cu、Zn和Al过渡金属盐类化合物中的五种按照金属离子摩尔比为1:1:1:1:1的比例配制成水溶液,然后按照过渡金属离子:尿素:氟化铵摩尔比为1:5:7的比例往金属离子水溶液中加入尿素和氟化铵得到混合溶液;将处理后的碳布与混合溶液置入水热反应釜中,封闭于180℃反应8h;冷却后取出清洗、干燥待用;将碳布置入马弗炉升温至400℃热处理2h,冷却得到具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料;本发明提高尖晶石远红外发射材料分散性能,增加发射比表面积,提高单位质量远红外发射率,且制备方法简单、生产能耗低。
Description
技术领域
本发明属于远红外发射材料技术领域,具体涉及一种具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料及其制备方法。
背景技术
远红外发射材料能够在室温下具有较高的光热转化效益,发射的远红外线能够促进人体血液循环,减缓疲劳,治疗和增强人体免疫力,同时具有保温抗菌等功效,在日用生活用品和医疗保健领域中具有广阔的应用前景。
近年来,尖晶石铁氧体材料由于具有高的远红外发射率而被广泛研究,往往通过掺杂不同价态和价健结构的离子,在局部形成杂质能级的,从而达到提高发射率的目的。研究发现:在局部形成杂质能级,增强自由载流子由价带到导带跃迁的可能性,促进价带中的自由载流子(电子、空穴等)浓度的增加及带隙间的跃迁,从而提高近红外发射率,同时晶格的不对称性(晶格畸变)减少载流子中电子与空穴的复合频率,提高光子发射几率。因此,杂质能级和晶格畸变是导致高远红外发射率的主要原因。而高熵尖晶石陶瓷具有新奇的“高熵效应”,是稳定的杂质能级和晶格畸变集合体。因此,高熵尖晶石陶瓷材料具有较高远红外发射率。中国发明专利CN113429213A公开了一种具有尖晶石结构的高发射率红外节能高熵材料的制备方法,所述方法为高温固相法。固相法制备过程中,氧化物原料反应难度大,合成温度高,颗粒易团聚,单位质量红外发射率低。
发明内容
针对现有技术存在的不足,本发明的目的在于提供一种具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料及其制备方法,提高尖晶石远红外发射材料的分散性能,增加发射比表面积,提高单位质量远红外发射率,且制备方法简单、生产能耗低。
为了实现上述目的,本发明采用以下技术方案予以实现:
一种具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料的制备方法,包括以下步骤:
步骤一、将碳布分别用浓硝酸、乙醇和去离子水超声清洗三次,干燥后待用;
步骤二、选用Cr、Mn、Fe、Co、Ni、Cu、Zn和Al过渡金属盐类化合物中的五种按照金属离子摩尔比为1:1:1:1:1的比例配制成水溶液,其金属离子总摩尔浓度为0.1mol/L,然后按照过渡金属离子:尿素:氟化铵摩尔比为1:5:7的比例往金属离子水溶液中分别加入尿素和氟化铵,搅拌溶解后得到混合溶液;
步骤三、将步骤一处理后的碳布与步骤二所得的混合溶液置入水热反应釜中,使碳布完全浸渍在混合溶液中,将充填封闭后的反应釜置于180℃反应8h;冷却至室温后取出碳布,清洗、干燥待用;
步骤四、将步骤三所得的干燥碳布置于马弗炉中,以5℃/min升温速率升温至400℃热处理2h,冷却至室温后取出,得到具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料。
优选的,步骤一中所述的浓硝酸浓度不低于70%。
优选的,步骤二中所述的过渡金属盐类化合物为Cr、Mn、Fe、Co、Ni、Cu、Zn、Al的可溶性硝酸盐、氯化盐或硫酸盐。
优选的,步骤一和步骤三中所述的干燥均为60℃干燥12h。
优选的,步骤三中所述的反应釜的填充比为60%。
优选的,步骤三中所述的清洗为分别用无水乙醇和去离子水清洗三次。
本发明还保护一种具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料,采用如上所述的方法制得。
优选的,该材料中的尖晶石为A3O4,A为Cr、Mn、Fe、Co、Ni、Cu、Zn、Al原子中的五种,且摩尔比为1:1:1:1:1;所述的尖晶石微观形貌为纳米针状。
优选的,该材料的远红外发射率≥0.95。
本发明与现有技术相比,具有如下技术效果:
本发明在制备过程中,实现了过渡金属离子液相均质混合,有利于提高高熵尖晶石的“高熵效应”,碳布上原位生成纳米针状尖晶石,尖晶石合成温度低,形貌可控,降低了生产能耗;
本发明制备的具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料具有尖晶石(A3O4)结构,尖晶石组分中五种过渡金属离子相互掺杂,形成较多的杂质能级和晶格畸变,从而提高远红外发射率,且结构中纳米针状尖晶石分散性好,比表面积大,单位质量远红外发射率高,与碳布结合牢固,具有稳定发射远红外线的功能。
附图说明
图1为实施列1制备的具有高远红外发射率的碳布负载(CuNiCrMnFe)3O4高熵尖晶石陶瓷材料的X射线衍射图谱;
图2为实施列1制备的具有高远红外发射率的碳布负载(CuNiCrMnFe)3O4高熵尖晶石陶瓷材料的SEM照片;
图3为实施列1制备的具有高远红外发射率的碳布负载(CuNiCrMnFe)3O4高熵尖晶石陶瓷材料的SEM照片。
具体实施方式
以下结合实施例对本发明的具体内容做进一步详细解释说明。
实施例1:
一种具有高远红外发射率的碳布负载(CuNiCrMnFe)3O4高熵尖晶石陶瓷材料及其制备方法,具体包括以下步骤:
步骤1:将碳布分别用浓硝酸、乙醇和去离子水超声清洗3次,于60℃干燥12h后待用;
步骤2:选用硝酸铜、硝酸镍、硝酸铬、硝酸锰和硝酸铁按照Cu:Ni:Cr:Mn:Fe摩尔比为1:1:1:1:1的比例配制成水溶液,其金属离子总摩尔浓度为0.1mol/L水溶液,然后按照金属离子、尿素、氟化铵摩尔比为1:5:7的比例往金属离子水溶液中分别加入尿素和氟化铵,搅拌溶解后得到混合溶液;
步骤3:将步骤1处理后的碳布与步骤2所得的混合溶液置入水热反应釜中,使碳布完全浸渍在混合溶液中,反应釜填充比为60%;将充填封闭后反应釜置于180℃反应8h;冷却至室温后取出碳布,分别用无水乙醇和去离子水清洗三次,于60℃干燥12h后待用;
步骤4:将步骤3所得的干燥碳布置于马弗炉中,以5℃/min升温速率升温至400℃热处理2h,冷却至室温后取出,得到具有高远红外发射率的碳布负载(CuNiCrMnFe)3O4高熵尖晶石陶瓷材料。
图1为实施列1制备的具有高远红外发射率的碳布负载(CuNiCrMnFe)3O4高熵尖晶石陶瓷材料的X射线衍射图谱;参照图1可知,本实施例制备的具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料的衍射峰位于五种单组分之间,五种组分相互共熔掺杂,属于尖晶石晶相,无其他杂质相,表明合成具有单一相的高熵材料(CuNiCrMnFe)3O4,同时衍射峰发生宽化,说明尖晶石晶粒细小,主要由于其针状结构造成。
图2和图3为实施列1制备的具有高远红外发射率的碳布负载(CuNiCrMnFe)3O4高熵尖晶石陶瓷材料的SEM照片;参照图2和图3可知,本实施例制备的具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料中的高熵尖晶石(CuNiCrMnFe)3O4微观形貌为纳米针状结构,具有好的分散性和比表面积,从而单位质量远红外发射率高。
实施例2:
一种具有高远红外发射率的碳布负载(CuCrMnFeCo)3O4高熵尖晶石陶瓷材料及其制备方法,具体包括以下步骤:
步骤1:将碳布分别用浓硝酸、乙醇和去离子水超声清洗3次,于60℃干燥12h后待用;
步骤2:将氯化铜、氯化铬、氯化锰、氯化铁和氯化钴按照Cu:Cr:Mn:Fe:Co摩尔比为1:1:1:1:1的比例配制成水溶液,其金属离子总摩尔浓度为0.1mol/L水溶液,然后按照金属离子、尿素、氟化铵摩尔比为1:5:7的比例往金属离子水溶液中分别加入尿素和氟化铵,搅拌溶解后得到混合溶液;
步骤3:将步骤1处理后的碳布与步骤2所得的混合溶液置入水热反应釜中,使碳布完全浸渍在混合溶液中,反应釜填充比为60%;将充填封闭后反应釜置于180℃反应8h;冷却至室温后取出碳布,分别用无水乙醇和去离子水清洗三次,于60℃干燥12h后待用;
步骤4:将步骤3所得的干燥碳布置于马弗炉中,以5℃/min升温速率升温至400℃热处理2h,冷却至室温后取出,得到具有高远红外发射率的碳布负载(CuCrMnFeCo)3O4高熵尖晶石陶瓷材料。
实施例3:
一种具有高远红外发射率的碳布负载(NiCrMnFeCo)3O4高熵尖晶石陶瓷材料及其制备方法,具体包括以下步骤:
步骤1:将碳布分别用浓硝酸、乙醇和去离子水超声清洗3次,于60℃干燥12h后待用;
步骤2:将氯化镍、氯化铬、氯化锰、氯化铁和氯化钴按照Ni:Cr:Mn:Fe:Co摩尔比为1:1:1:1:1的比例配制成水溶液,其金属离子总摩尔浓度为0.1mol/L水溶液,然后按照金属离子、尿素、氟化铵摩尔比为1:5:7的比例往金属离子水溶液中分别加入尿素和氟化铵,搅拌溶解后得到混合溶液;
步骤3:将步骤1处理后的碳布与步骤2所得的混合溶液置入水热反应釜中,使碳布完全浸渍在混合溶液中,反应釜填充比为60%;将充填封闭后反应釜置于180℃反应8h;冷却至室温后取出碳布,分别用无水乙醇和去离子水清洗三次,于60℃干燥12h后待用;
步骤4:将步骤3所得的干燥碳布置于马弗炉中,以5℃/min升温速率升温至400℃热处理2h,冷却至室温后取出,得到具有高红外发射率的碳布负载(NiCrMnFeCo)3O4高熵尖晶石陶瓷材料。
实施例4:
一种具有高远红外发射率的碳布负载(ZnCrMnFeCo)3O4高熵尖晶石陶瓷材料及其制备方法,具体包括以下步骤:
步骤1:将碳布分别用浓硝酸、乙醇和去离子水超声清洗3次,于60℃干燥12h后待用;
步骤2:将氯化锌、氯化铬、氯化锰、氯化铁和氯化钴按照Zn:Cr:Mn:Fe:Co摩尔比为1:1:1:1:1的比例配制成水溶液,其金属离子总摩尔浓度为0.1mol/L水溶液,然后按照金属离子、尿素、氟化铵摩尔比为1:5:7的比例往金属离子水溶液中分别加入尿素和氟化铵,搅拌溶解后得到混合溶液;
步骤3:将步骤1处理后的碳布与步骤2所得的混合溶液置入水热反应釜中,使碳布完全浸渍在混合溶液中,反应釜填充比为60%;将充填封闭后反应釜置于180℃反应8h;冷却至室温后取出碳布,分别用无水乙醇和去离子水清洗三次,于60℃干燥12h后待用;
步骤4:将步骤3所得的干燥碳布置于马弗炉中,以5℃/min升温速率升温至400℃热处理2h,冷却至室温后取出,得到具有高远红外发射率的碳布负载(ZnCrMnFeCo)3O4高熵尖晶石陶瓷材料。
实施例5:
一种具有高远红外发射率的碳布负载(CuCrMnFeAl)3O4高熵尖晶石陶瓷材料及其制备方法,具体包括以下步骤:
步骤1:将碳布分别用浓硝酸、乙醇和去离子水超声清洗3次,于60℃干燥12h后待用;
步骤2:将硝酸铜、硝酸铬、硝酸锰、硝酸铁和硝酸铝按照Cu:Cr:Mn:Fe:Al摩尔比为1:1:1:1:1的比例配制成水溶液,其金属离子总摩尔浓度为0.1mol/L水溶液,然后按照金属离子、尿素、氟化铵摩尔比为1:5:7的比例往金属离子水溶液中分别加入尿素和氟化铵,搅拌溶解后得到混合溶液;
步骤3:将步骤1处理后的碳布与步骤2所得的混合溶液置入水热反应釜中,使碳布完全浸渍在混合溶液中,反应釜填充比为60%;将充填封闭后反应釜置于180℃反应8h;冷却至室温后取出碳布,分别用无水乙醇和去离子水清洗三次,于60℃干燥12h后待用;
步骤4:将步骤3所得的干燥碳布置于马弗炉中,以5℃/min升温速率升温至400℃热处理2h,冷却至室温后取出,得到具有远高红外发射率的碳布负载(CuCrMnFeAl)3O4高熵尖晶石陶瓷材料。
实施例6:
一种具有高远红外发射率的碳布负载(NiCrMnFeAl)3O4高熵尖晶石陶瓷材料及其制备方法,具体包括以下步骤:
步骤1:将碳布分别用浓硝酸、乙醇和去离子水超声清洗3次,于60℃干燥12h后待用;
步骤2:将硝酸镍、硝酸铬、硝酸锰、硝酸铁和硝酸铝按照Cu:Cr:Mn:Fe:Al摩尔比为1:1:1:1:1的比例配制成水溶液,其金属离子总摩尔浓度为0.1mol/L水溶液,然后按照金属离子、尿素、氟化铵摩尔比为1:5:7的比例往金属离子水溶液中分别加入尿素和氟化铵,搅拌溶解后得到混合溶液;
步骤3:将步骤1处理后的碳布与步骤2所得的混合溶液置入水热反应釜中,使碳布完全浸渍在混合溶液中,反应釜填充比为60%;将充填封闭后反应釜置于180℃反应8h;冷却至室温后取出碳布,分别用无水乙醇和去离子水清洗三次,于60℃干燥12h后待用;
步骤4:将步骤3所得的干燥后碳布置于马弗炉中,以5℃/min升温速率升温至400℃热处理2h,冷却至室温后取出,得到具有高远红外发射率的碳布负载(NiCrMnFeAl)3O4高熵尖晶石陶瓷材料。
实施例7:
一种具有高远红外发射率的碳布负载(ZnCrMnFeAl)3O4高熵尖晶石陶瓷材料及其制备方法,具体包括以下步骤:
步骤1:将碳布分别用浓硝酸、乙醇和去离子水超声清洗3次,于60℃干燥12h后待用;
步骤2:将硝酸锌、硝酸铬、硝酸锰、硝酸铁和硝酸铝按照Zn:Cr:Mn:Fe:Al摩尔比为1:1:1:1:1的比例配制成水溶液,其金属离子摩尔浓度为0.1mol/L水溶液,然后按照金属离子、尿素、氟化铵摩尔比为1:5:7的比例往金属离子水溶液中分别加入尿素和氟化铵,搅拌溶解后得到混合溶液;
步骤3:将步骤1处理后的碳布与步骤2所得的混合溶液置入水热反应釜中,使碳布完全浸渍在混合溶液中,反应釜填充比为60%;将充填封闭后反应釜置于180℃反应8h;冷却至室温后取出碳布,分别用无水乙醇和去离子水清洗三次,于60℃干燥12h后待用;
步骤4:将步骤3所得的干燥后碳布置于马弗炉中,以5℃/min升温速率升温至400℃热处理2h,冷却至室温后取出,得到具有高远红外发射率的碳布负载(ZnCrMnFeAl)3O4高熵尖晶石陶瓷材料;
性能检测
采用IR-2双波段发射率测量仪测试本发明实施例1-7制备的碳布负载高熵尖晶石陶瓷材料的远红外发射率结果如表1所示,其远红外发射率均≥0.95。
实施例 | 组成 | 8μm-14μm波段发射率 |
实施例1 | (CuNiCrMnFe)<sub>3</sub>O<sub>4</sub> | 0.97 |
实施例2 | (CuCrMnFeCo)<sub>3</sub>O<sub>4</sub> | 0.98 |
实施例3 | (NiCrMnFeCo)<sub>3</sub>O<sub>4</sub> | 0.97 |
实施例4 | (ZnCrMnFeCo)<sub>3</sub>O<sub>4</sub> | 0.96 |
实施例5 | (CuCrMnFeAl)<sub>3</sub>O<sub>4</sub> | 0.96 |
实施例6 | (NiCrMnFeAl)<sub>3</sub>O<sub>4</sub> | 0.96 |
实施例7 | (ZnCrMnFeAl)<sub>3</sub>O<sub>4</sub> | 0.95 |
以上内容是对本发明所作的进一步详细说明,不能认定本发明的具体实施方式仅限于此,对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干简单的推演或替换,都应当视为属于本发明由所提交的权利要求书确定保护范围。
Claims (9)
1.一种具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料的制备方法,其特征在于,包括以下步骤:
步骤一、将碳布分别用浓硝酸、乙醇和去离子水超声清洗三次,干燥后待用;
步骤二、选用Cr、Mn、Fe、Co、Ni、Cu、Zn和Al过渡金属盐类化合物中的五种按照金属离子摩尔比为1:1:1:1:1的比例配制成水溶液,其金属离子总摩尔浓度为0.1mol/L,然后按照过渡金属离子:尿素:氟化铵摩尔比为1:5:7的比例往金属离子水溶液中分别加入尿素和氟化铵,搅拌溶解后得到混合溶液;
步骤三、将步骤一处理后的碳布与步骤二所得的混合溶液置入水热反应釜中,使碳布完全浸渍在混合溶液中,将充填封闭后的反应釜置于180℃反应8h;冷却至室温后取出碳布,清洗、干燥待用;
步骤四、将步骤三所得的干燥碳布置于马弗炉中,以5℃/min升温速率升温至400℃热处理2h,冷却至室温后取出,得到具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料。
2.如权利要求1所述的具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料的制备方法,其特征在于,步骤一中所述的浓硝酸浓度不低于70%。
3.如权利要求1所述的具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料的制备方法,其特征在于,步骤二中所述的过渡金属盐类化合物为Cr、Mn、Fe、Co、Ni、Cu、Zn、Al的可溶性硝酸盐、氯化盐或硫酸盐。
4.如权利要求1所述的具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料的制备方法,其特征在于,步骤一和步骤三中所述的干燥均为60℃干燥12h。
5.如权利要求1所述的具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料的制备方法,其特征在于,步骤三中所述的反应釜的填充比为60%。
6.如权利要求1所述的具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料的制备方法,其特征在于,步骤三中所述的清洗为分别用无水乙醇和去离子水清洗三次。
7.一种具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料,其特征在于,采用如权利要求1至6中任一项所述的方法制得。
8.如权利要求7所述的具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料,其特征在于,该材料中的尖晶石为A3O4,A为Cr、Mn、Fe、Co、Ni、Cu、Zn、Al原子中的五种,且摩尔比为1:1:1:1:1;所述的尖晶石微观形貌为纳米针状。
9.如权利要求7所述的具有高远红外发射率的碳布负载高熵尖晶石陶瓷材料,其特征在于,该材料的远红外发射率≥0.95。
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CN114956802A (zh) * | 2022-06-01 | 2022-08-30 | 武汉科技大学 | 一种低导热红外发射材料及其制备方法与应用 |
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CN111161960A (zh) * | 2019-12-31 | 2020-05-15 | 华北水利水电大学 | 在碳布基底上生长的尖晶石型CuCo2O4高性能电极材料合成方法 |
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