CN108203301A - 一种氮化铝粉末的表面疏水改性方法 - Google Patents
一种氮化铝粉末的表面疏水改性方法 Download PDFInfo
- Publication number
- CN108203301A CN108203301A CN201810020072.0A CN201810020072A CN108203301A CN 108203301 A CN108203301 A CN 108203301A CN 201810020072 A CN201810020072 A CN 201810020072A CN 108203301 A CN108203301 A CN 108203301A
- Authority
- CN
- China
- Prior art keywords
- nitride powder
- aluminium nitride
- silicone oil
- aluminum nitride
- hydroxyl silicone
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 79
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title abstract description 13
- 230000002209 hydrophobic effect Effects 0.000 title abstract description 8
- 238000002715 modification method Methods 0.000 title abstract description 3
- 229920002545 silicone oil Polymers 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 51
- 229910017083 AlN Inorganic materials 0.000 claims description 50
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 26
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- IXAWXWACDBWEJF-UHFFFAOYSA-L C(CCCCCCC)[Sn+2]CCCCCCCC.C(CCCCCCCCCCC)(=O)[O-].C(CCCCCCCCCCC)(=O)[O-].[Sn+4] Chemical compound C(CCCCCCC)[Sn+2]CCCCCCCC.C(CCCCCCCCCCC)(=O)[O-].C(CCCCCCCCCCC)(=O)[O-].[Sn+4] IXAWXWACDBWEJF-UHFFFAOYSA-L 0.000 claims description 2
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000012986 modification Methods 0.000 abstract description 16
- 230000004048 modification Effects 0.000 abstract description 16
- 239000002131 composite material Substances 0.000 abstract description 11
- 239000003607 modifier Substances 0.000 abstract description 8
- 229920000642 polymer Polymers 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 230000005661 hydrophobic surface Effects 0.000 abstract description 2
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 2
- 230000002045 lasting effect Effects 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 230000008859 change Effects 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000004411 aluminium Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 238000003825 pressing Methods 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 4
- 239000012456 homogeneous solution Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 238000007385 chemical modification Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 229920002943 EPDM rubber Polymers 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- -1 aluminium nitride powder;Modified aluminium nitride Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 239000002345 surface coating layer Substances 0.000 description 1
- 230000010148 water-pollination Effects 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
-
- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
-
- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
- C04B35/6264—Mixing media, e.g. organic solvents
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)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
一种氮化铝粉末的表面疏水改性方法:将端羟基硅油溶液30~100份加入氮化铝粉末100份中,再添加去离子水0.1~1份,超声分散8~15min,然后添加催化剂0.1~2份,继续超声分散10~20min,得到均匀的溶液,将所得溶液烘干,即完成氮化铝粉末的表面疏水改性;本发明通过控制合适的表面改性剂的分子链长度,一方面做到与氮化铝粉体有效结合,形成疏水表面,另一方面又在表面保留合适的分子链长度,从而形成由氮化铝粉体连接而成的聚合物网络;改性后的氮化铝粉末疏水性能好,稳定性持久,能够有效解决氮化铝粉末在复合材料中的分散性和相容性问题,提高了复合材料的性能;本发明制备工艺简单易行,成本低廉。
Description
(一)技术领域
本发明涉及一种氮化铝粉末的表面处理方法,具体涉及一种氮化铝粉末的表面疏水改性方法。
(二)背景技术
氮化铝陶瓷是目前应用最为广泛的陶瓷材料之一,其所用原料为氮化铝陶瓷粉体,由于该粉体具有高热导、耐高温、耐腐蚀以及耐磨损等优异性能而被广泛应用于和金属材料、高分子材料的复合。在与非极性基体混合过程中,由于氮化铝陶瓷粉体具有较强的亲水性,因此,复合过程中与非极性基体材料润湿性较差,复合均匀度和填充量都受到限制,复合材料的性能远达不到理论指标。为改善界面的润湿性,使复合材料的组织变得更加均匀,从而改善复合材料的性能,氮化铝粉末的改性受到国内外材料工作者的广泛关注,尤其是其改性方法的研究。氮化铝粉末改性的方法很多,综合国内外的研究方法,可归纳如下:
一、包覆改性法:粉体的表面包覆改性是指在原来单一组分的基元物质表面上,均匀地引入一种或者是多种其它组分的物质,以改变原来基元的基本性质的方法。氮化铝粉体包覆改性的方法主要有表面吸附、液相包覆、机械力化学法包覆改性。在2010年第5期第38卷的《硅酸盐学报》上公开的文章《表面涂覆氮化铝粉末的抗水化性》中研究了表面涂覆硬脂酸和吐温80对氮化铝粉末抗水化性能的影响。通过表面改性工艺在氮化铝粉末表面包裹一层有机化合物,能有效地抑制氮化铝与水的反应,阻碍水分子向氮化铝粉末表面侵蚀。在2014年第2期第35卷的《青岛科技大学学报》上公开的文章《改性氮化铝/三元乙丙橡胶复合材料导热性能和力学性能的研究》中通过酚醛树脂(PF)对氮化铝进行表面改性处理,增加了其在橡胶基体中的分散性。
二、表面化学改性:表面化学改性通过表面改性剂与粉体表面进行化学反应或化学吸附的方式完成。常用的表面改性剂有偶联剂、高级脂肪酸及其盐、不饱和有机酸和有机硅等。在2006年第5期的《电子元件与材料》上公开的文章《纳米氮化铝粉末表面修饰的研究》中研究了偶联剂-苯乙烯接枝改性剂对纳米AlN粉末进行表面改性,经表面修饰后的粉末对水呈现较强的非浸润性。在2005年第2期第28卷的《兵器材料科学与工程》上公开的文章《氮化铝颗粒表面镀铜及其增强铜基复合材料》中采用化学镀的方式在AIN颗粒表面包覆铜,增加了AIN颗粒与铜基体之间的界面结合强度,使复合材料在相对密度、硬度、屈服强度、导电性能及摩擦磨损性能等方面均有不同程度的提高。
从上面可以看出,目前的改性方法主要集中在偶联剂、有机酸等几个途径,然而,这些方法都没有考虑到改性后氮化铝粉体表面的状态,比如改性剂的分子链长度及其应用状态。偶联剂是最常用的表面改性剂,然而,其为单分子结构,过短的分子链使得形成单分子层非常困难,很难保证硅氧烷基团全部反应掉。当有剩余硅氧烷基团存在时,则仍然会有保留亲水性。另外,对于全部是非极性基团的单分子层包覆的氮化铝粉体来说,其与聚合物基体的结合又受到影响。而采用有机羧酸类包覆的话,有机长链又影响其高温的应用。
(三)发明内容
针对现有技术中存在的不足,本发明提出采用有机硅长链分子作为表面改性剂,通过控制合适的表面改性剂的分子链长度,一方面做到与氮化铝粉体有效结合,形成疏水表面,另一方面又在表面保留合适的分子链长度,从而形成由氮化铝粉体连接而成的聚合物网络,这样,可以使得在复合过程中,聚合物基体有效地贯穿于该复合网络中间,形成更加均匀的复合体。
本发明的技术方案如下:
一种氮化铝粉末的表面疏水改性方法,所述方法为:
将端羟基硅油溶液30~100份(优选50~80份)加入氮化铝粉末100份中,再添加去离子水0.1~1份(优选0.3~0.8份),超声分散8~15min(超声功率为50W,下同),然后添加催化剂0.1~2份(优选0.8~1.5份),继续超声分散10~20min,得到均匀的溶液,将所得溶液烘干,即完成氮化铝粉末的表面疏水改性。
本发明所述方法中,份数均指重量份。
所述氮化铝粉末为商业氮化铝粉,呈白色或灰白色粉状物,颗粒尺寸在0.5~10μm范围,可通过常规途径商购获得。
所述端羟基硅油溶液由端羟基硅油与有机溶剂按质量比0.1~1:100(优选0.5~0.8:100)混合而得;所述有机溶剂为正己烷、丙酮、甲苯、二甲苯或石油醚等;所述端羟基硅油为低粘度羟基硅油,粘度在5~40mm2/s之间;当粘度低于5mm2/s时,聚合度极低,由于氮化铝粉体的位阻效应,端羟基硅油的羟基难以完全反应掉,影响疏水性;当粘度过大时,硅油的分子链较长,相互之间会发生缠绕,引起氮化铝粉体团聚。
所述催化剂为二月桂酸二丁基锡或二月桂酸二辛基锡;催化剂的主要作用是促进端羟基硅油与氮化铝粉体的表面结合,如果催化剂用量过低,则结合不充分,如果催化剂用量过高,则催化剂会有剩余,不但增加成本,而且会作为杂质影响最后复合材料的性能。
所述添加0.1~1份去离子水,目的是使氮化铝表面适度水解。
限定第一次超声分散的时间为8~15min,第二次超声分散的时间为10~20min,是由于超声分散时间太短,则氮化铝粉体表面难以形成均匀的表面包覆层;超声分散时间过长,则影响制备效率。
所述烘干推荐在60~80℃真空干燥箱中烘干4~12h。
本发明的有益效果是:本发明通过控制合适的表面改性剂的分子链长度,一方面做到与氮化铝粉体有效结合,形成疏水表面,另一方面又在表面保留合适的分子链长度,从而形成由氮化铝粉体连接而成的聚合物网络;改性后的氮化铝粉末疏水性能好,稳定性持久,能够有效解决氮化铝粉末在复合材料中的分散性和相容性问题,提高了复合材料的性能;本发明制备工艺简单易行,成本低廉。
(四)附图说明
图1为本发明实施例1(左)和对比例1(右)所得的氮化铝粉末在水中充分搅拌并静置1h后的效果图;
图2为本发明实施例1(a)和对比例1(b)所得氮化铝粉末的SEM形貌图;
图3为本发明实施例1所得的氮化铝粉末干压成块体后的接触角实验效果图。
(五)具体实施方式
下面通过具体实施例对本发明作进一步的说明,但本发明的保护范围并不仅限于此。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
以下实施例中用到的端羟基硅油为商业化的低分子量羟基硅油产品(湖北四海化工股份有限公司,粘度15-40mm2/s);氮化铝粉末购自日本德山公司;其他试剂均可通过常规途径购买获得。
实施例1:
将0.5g端羟基硅油溶入100g丙酮中,搅拌混合均匀,得到含有端羟基硅油的有机溶液;将含有端羟基硅油的有机溶液60g,加入100g氮化铝粉末中,再添加0.3g去离子水,然后超声分散10min;在经超声分散后的粉体中加入0.8g二月桂酸二丁基锡,并继续超声分散10min成均匀溶液;将该溶液放在80℃的真空干燥箱中烘干6h,即得经过表面疏水改性的氮化铝粉末。
改性处理后的粉末干压成块,用水滴滴在表面,接触角为118°,结果如图3所示。
对比例1:
取氮化铝粉末不做任何处理,将粉末浸泡在水里充分搅拌后静置1h。同时,取实施例1所得经过表面疏水改性的氮化铝粉末浸泡在水里充分搅拌后静置1h。结果如图1所示。
实施例2:
将0.2g端羟基硅油溶入100g丙酮中,搅拌混合均匀,得到含有端羟基硅油的有机溶液;将含有端羟基硅油的有机溶液50g,加入100g氮化铝粉末中,再添加0.1g去离子水,然后超声分散8min;在经超声分散后的粉体中加入0.2g二月桂酸二丁基锡,并继续超声分散15min成均匀溶液;将该溶液放在80℃的真空干燥箱中烘干5h,即得经过表面疏水改性的氮化铝粉末。
改性处理后的粉末干压成块,用水滴滴在表面,接触角为116°。
实施例3:
将0.8g端羟基硅油溶入100g甲苯中,搅拌混合均匀,得到含有端羟基硅油的有机溶液;将含有端羟基硅油的有机溶液60g,加入100g氮化铝粉末中,再添加0.5g去离子水,然后超声分散15min;在经超声分散后的粉体中加入1g二月桂酸二辛基锡,并继续超声分散15min成均匀溶液;将该溶液放在70℃的真空干燥箱中烘干8h,即得经过表面疏水改性的氮化铝粉末。
改性处理后的粉末干压成块,用水滴滴在表面,接触角为120°。
实施例4:
将1g端羟基硅油溶入100g甲苯中,搅拌混合均匀,得到含有端羟基硅油的有机溶液;将含有端羟基硅油的有机溶液80g,加入100g氮化铝粉末中,再添加0.8g去离子水,然后超声分散15min;在经超声分散后的粉体中加入1.5g二月桂酸二辛基锡,并继续超声分散20min成均匀溶液;将该溶液放在80℃的真空干燥箱中烘干9h,即得经过表面疏水改性的氮化铝粉末。
改性处理后的粉末干压成块,用水滴滴在表面,接触角为121°。
通过附图1-3中相关数据结果可以看出:氮化铝粉末经过表面疏水改性处理后,具有了很强的疏水能力,且在一定的时间内疏水能力稳定性较好。经表面处理后,粉末表面形貌无明显变化,说明经过表面处理后,氮化铝粉末表面反应层较薄,没有改变粉末表面形貌,所采用的疏水处理方法是有效的。
Claims (6)
1.一种氮化铝粉末的表面疏水改性方法,其特征在于,所述方法为:
将端羟基硅油溶液30~100份加入氮化铝粉末100份中,再添加去离子水0.1~1份,超声分散8~15min,然后添加催化剂0.1~2份,继续超声分散10~20min,得到均匀的溶液,将所得溶液烘干,即完成氮化铝粉末的表面疏水改性;
其中份数均指重量份;
所述催化剂为二月桂酸二丁基锡或二月桂酸二辛基锡;
所述端羟基硅油溶液由端羟基硅油与有机溶剂按质量比0.1~1:100混合而得;所述有机溶剂为正己烷、丙酮、甲苯、二甲苯或石油醚;所述端羟基硅油为低粘度羟基硅油,粘度在5~40mm2/s之间。
2.如权利要求1所述的氮化铝粉末的表面疏水改性方法,其特征在于,将端羟基硅油溶液50~80份加入氮化铝粉末100份中,再添加去离子水0.3~0.8份,超声分散8~15min,然后添加催化剂0.8~1.5份,继续超声分散10~20min,得到均匀的溶液,将所得溶液烘干,即完成氮化铝粉末的表面疏水改性。
3.如权利要求1所述的氮化铝粉末的表面疏水改性方法,其特征在于,所述端羟基硅油溶液由端羟基硅油与有机溶剂按质量比0.5~0.8:100混合而得。
4.如权利要求1~3任一项所述的氮化铝粉末的表面疏水改性方法,其特征在于,所述氮化铝粉末颗粒尺寸在0.5~10μm范围。
5.如权利要求1~3任一项所述的氮化铝粉末的表面疏水改性方法,其特征在于,所述超声的功率为50W。
6.如权利要求1~3任一项所述的氮化铝粉末的表面疏水改性方法,其特征在于,所述烘干为:在60~80℃真空干燥箱中烘干4~12h。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810020072.0A CN108203301A (zh) | 2018-01-09 | 2018-01-09 | 一种氮化铝粉末的表面疏水改性方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810020072.0A CN108203301A (zh) | 2018-01-09 | 2018-01-09 | 一种氮化铝粉末的表面疏水改性方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN108203301A true CN108203301A (zh) | 2018-06-26 |
Family
ID=62606261
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810020072.0A Pending CN108203301A (zh) | 2018-01-09 | 2018-01-09 | 一种氮化铝粉末的表面疏水改性方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108203301A (zh) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111320949A (zh) * | 2020-04-03 | 2020-06-23 | 深圳昌茂粘胶新材料有限公司 | 一种分散超好导热绝缘丙烯酸胶的制备方法 |
CN113024262A (zh) * | 2021-04-13 | 2021-06-25 | 福建华清电子材料科技有限公司 | 一种氮化铝微球的制备方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1872692A (zh) * | 2006-06-15 | 2006-12-06 | 南京工业大学 | 抗水化易分散的氮化铝粉末的制备方法 |
US20100206811A1 (en) * | 2007-09-10 | 2010-08-19 | National University Of Singapore | Polymeric membranes incorporating nanotubes |
CN102031025A (zh) * | 2010-10-20 | 2011-04-27 | 中科院广州化学有限公司 | 一种硅油表面改性氢氧化铝阻燃剂的制备方法 |
US20140174792A1 (en) * | 2012-12-24 | 2014-06-26 | Samsung Electro-Mechanics Co., Ltd. | Insulating film for printed circuit board having improved thermal conductivity, manufacturing method thereof, and printed circuit board using the same |
CN106847667A (zh) * | 2016-12-27 | 2017-06-13 | 苏州大学 | 一种表面改性的氮化物半导体及其制备方法 |
-
2018
- 2018-01-09 CN CN201810020072.0A patent/CN108203301A/zh active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1872692A (zh) * | 2006-06-15 | 2006-12-06 | 南京工业大学 | 抗水化易分散的氮化铝粉末的制备方法 |
US20100206811A1 (en) * | 2007-09-10 | 2010-08-19 | National University Of Singapore | Polymeric membranes incorporating nanotubes |
CN102031025A (zh) * | 2010-10-20 | 2011-04-27 | 中科院广州化学有限公司 | 一种硅油表面改性氢氧化铝阻燃剂的制备方法 |
US20140174792A1 (en) * | 2012-12-24 | 2014-06-26 | Samsung Electro-Mechanics Co., Ltd. | Insulating film for printed circuit board having improved thermal conductivity, manufacturing method thereof, and printed circuit board using the same |
CN106847667A (zh) * | 2016-12-27 | 2017-06-13 | 苏州大学 | 一种表面改性的氮化物半导体及其制备方法 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111320949A (zh) * | 2020-04-03 | 2020-06-23 | 深圳昌茂粘胶新材料有限公司 | 一种分散超好导热绝缘丙烯酸胶的制备方法 |
CN113024262A (zh) * | 2021-04-13 | 2021-06-25 | 福建华清电子材料科技有限公司 | 一种氮化铝微球的制备方法 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Hou et al. | Recent advances and future perspectives for graphene oxide reinforced epoxy resins | |
Mohammadkhani et al. | Designing a dual-functional epoxy composite system with self-healing/barrier anti-corrosion performance using graphene oxide nano-scale platforms decorated with zinc doped-conductive polypyrrole nanoparticles with great environmental stability and non-toxicity | |
Ahmadi et al. | Hybrid silane coating reinforced with silanized graphene oxide nanosheets with improved corrosion protective performance | |
CN103555016B (zh) | 一种耐高温耐磨石墨烯涂料及其制备方法 | |
Lin et al. | Surface functionalization of BaTiO 3 nanoparticles and improved electrical properties of BaTiO 3/polyvinylidene fluoride composite | |
CN104508056B (zh) | 可调的材料 | |
CN101899657B (zh) | 一种无铬钝化处理剂及其制备方法 | |
CN108178964A (zh) | 一种石墨烯无溶剂防腐涂料及制备技术 | |
CN108624195B (zh) | 一种g-C3N4-G/水性环氧复合涂料的制备方法 | |
WO2009035439A1 (en) | Thermally conductive composition | |
CN109796794A (zh) | 基于石墨烯的有机无机耐高温防腐涂料及其制备方法 | |
CN108997916A (zh) | 一种金属基材长效防腐中涂漆及其制备方法 | |
CN101824278A (zh) | 一种超疏水无机有机纳米复合高分子涂层材料及其制备方法 | |
CN107903755A (zh) | 一种氧化石墨烯改性水性丙烯酸防腐涂料的制备方法 | |
CN108203301A (zh) | 一种氮化铝粉末的表面疏水改性方法 | |
CN108659457B (zh) | 一种氮化硼包覆磺化石墨烯-环氧树脂复合材料及其制备方法 | |
CN106987164B (zh) | 一种氮化硼-氧化石墨烯复合防腐填料的制备方法 | |
CN113308139B (zh) | 一种二维纳米杂化复合防腐涂料填料及其制备方法和应用 | |
CN107987770A (zh) | 高导热绝缘胶粘剂组合物及其制备方法 | |
WO2021068506A1 (zh) | 一种基于氧化石墨烯的水基防腐涂料及其制备方法 | |
CN109097761B (zh) | 环保型纳米皮膜剂及其制备方法 | |
CN110183934A (zh) | 一种耐磨型双组分石墨烯防腐涂料 | |
Van et al. | Synthesis of silica/polypyrrole nanocomposites and application in corrosion protection of carbon steel | |
CN113493619A (zh) | 一种石墨烯表面包覆二氧化硅复合材料及其制备方法和应用 | |
Chen et al. | Chitosan functionalized hexagonal boron nitride nanomaterial to enhance the anticorrosive performance of epoxy resin |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180626 |