CN111363181A - 一种导热硅胶片用离型膜及其制备方法 - Google Patents
一种导热硅胶片用离型膜及其制备方法 Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000000741 silica gel Substances 0.000 title claims abstract description 38
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 37
- 229920002545 silicone oil Polymers 0.000 claims abstract description 28
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 22
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012990 dithiocarbamate Substances 0.000 claims abstract description 14
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 10
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 10
- 230000001737 promoting effect Effects 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 39
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 27
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 27
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 14
- 229920001296 polysiloxane Polymers 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 claims description 9
- 239000005054 phenyltrichlorosilane Substances 0.000 claims description 8
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 claims description 8
- 239000003377 acid catalyst Substances 0.000 claims description 3
- 229920002379 silicone rubber Polymers 0.000 claims description 3
- 239000004945 silicone rubber Substances 0.000 claims description 2
- GWESVXSMPKAFAS-UHFFFAOYSA-N Isopropylcyclohexane Natural products CC(C)C1CCCCC1 GWESVXSMPKAFAS-UHFFFAOYSA-N 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 15
- 238000007254 oxidation reaction Methods 0.000 abstract description 15
- 229920000139 polyethylene terephthalate Polymers 0.000 description 22
- 239000005020 polyethylene terephthalate Substances 0.000 description 22
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 16
- 238000012360 testing method Methods 0.000 description 12
- -1 BOPET Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 229910052697 platinum Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 238000010891 electric arc Methods 0.000 description 7
- 238000005096 rolling process Methods 0.000 description 7
- 239000003921 oil Substances 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
本发明提供一种导热硅胶片用离型膜的制备方法,包括:(1)将硅油和溶剂加入容器中搅拌均匀;(2)于容器中加入乙烯基三乙氧基硅烷、催化剂、附着力促进树脂和二烷基二硫代氨基甲酸盐;(3)于容器中加入改性烷基苯酚甲醛树脂,搅拌后加入异构十三醇聚氧乙烯醚并加热温度至40‑60度,得到离型液;(4)将离型液涂布在基材表面,经烘烤固化,制得导热硅胶片用离型膜。该制备方法中,借助乙烯基三乙氧基硅烷提高二烷基二硫代氨基甲酸盐和硅油的复合,利用二烷基二硫代氨基甲酸盐防止离型膜的硅油层未固化部分氧化,避免氧化黑点出现。引入改性烷基苯酚甲醛树脂提高离型膜的硅油层中固化部分与未充分固化部分之间的粘附,防止未充分固化部分出现脱落。
Description
技术领域
本发明涉及离型膜技术领域,尤其涉及一种导热硅胶片用离型膜及其制备方法。
背景技术
导热硅胶片又称为导热硅胶垫、导热矽胶片、软性导热垫,包括离型膜层、导热硅胶层、离型膜层。其利用离型膜为载体,将导热硅胶复合液体涂覆在离型膜上,再经过高温烘箱热固化形成。导热硅胶片能够填充缝隙,完成发热部位与散热部位间的热传递,同时还起到绝缘、减震、密封等作用,能够满足设备小型化及超薄化的设计要求,是极具工艺性和使用性的导热填充材料。
在导热硅胶片固化成型后,剥离离型膜贴合在电子产品上,要求离型膜具有良好的剥离性能,因而将导热硅胶片用离型膜涂布很厚(厚度2-4Um),过厚的涂布不可避免出现离型膜中硅油层的中间部分的硅油存在未固化的情况,导致硅油层的力学性能下降,局部硅油层脱落,且未固化部分的硅油容易出现氧化的现象,产生氧化黑点。
因此,如何提高离型膜中硅油层未固化部分之间的力学性能,让未固化部分的硅油粘附力更强,避免硅油层脱落,且阻止硅油层未固化部分氧化是离型膜行业一直探索的方向。针对上述存在的问题,本发明研发了一种防止硅油层脱落及抗硅油氧化的导热硅胶片用离型膜。
发明内容
本发明的目的之一是提供一种导热硅胶片用离型膜的制备方法,制备的导热硅胶片用离型膜,具有良好的防脱落及抗氧化性,避免硅油层脱落和氧化黑点的出现。
本发明的目的之二是提供一种采用上述制备方法制得的导热硅胶片用离型膜。
为了实现上述目的,本发明提供了一种导热硅胶片用离型膜的制备方法,其步骤包括:
(1)将8-15份的硅油和70-88份溶剂加入容器中搅拌均匀,搅拌速度为900-1500r/min;
(2)于容器中加入2-4份乙烯基三乙氧基硅烷、0.5-2份催化剂、1-1.5份附着力促进树脂和4-8份二烷基二硫代氨基甲酸盐,搅拌均匀;
(3)于容器中加入5-10份改性烷基苯酚甲醛树脂,搅拌均匀后加入1.5-3份异构十三醇聚氧乙烯醚并加热温度至40-60度,得到离型液;
(4)将所述离型液涂布在基材表面,经过烘烤固化,制得导热硅胶片用离型膜。
与现有技术相比,本发明导热硅胶片用离型膜的制备方法中,通过每个步骤的衔接降低离型膜的硅油层未固化部分,尤其是催化剂的加入可有效地提高反应速度,降低硅油层未固化部分。同时借助乙烯基三乙氧基硅烷提高二烷基二硫代氨基甲酸盐和硅油的复合,并利用二烷基二硫代氨基甲酸盐防止离型膜的硅油层未固化部分氧化,避免氧化黑点出现。引入改性烷基苯酚甲醛树脂提高离型膜的硅油层中固化部分与未充分固化部分之间的粘附,有效防止未充分固化部分出现脱落。
较佳者,所述硅油选自苯基三氯硅烷或道康宁硅油中的至少一种。
较佳者,所述溶剂选自甲苯、乙酸乙酯、异丙醇、环己烷、丙酮中的至少一种。
较佳者,所述溶剂选自甲苯、乙酸乙酯、异丙醇、环己烷、丙酮的混合物,且所述环己烷的用量等于其余各溶剂的用量之和,所述甲苯、乙酸乙酯、异丙醇、环己烷、丙酮的用量比为1:1:1:4:1。
较佳者,所述催化剂选自铂碳催化剂和氯铂酸催化剂中的至少一种。
进一步,铂碳催化剂的平均粒径(μm)为40-70μm,铂含量为1%-3%。
较佳者,所述基材表面经过电弧处理,形成2-4um厚度的粗糙层,进一步增加附着力,防止硅油脱落。
较佳者,所述基材选自PET、BOPET、PE或PVC中的至少一种。
较佳者,所述烘烤温度为120-130℃。
本发明还提供了一种采用上述的导热硅胶片用离型膜的制备方法制得的导热硅胶片用离型膜。
具体实施方式
下面通过具体实施方式来进一步说明本发明的技术方案,但不构成对本发明的任何限制。
实施例1
本实施例导热硅胶片用离型膜的制备方法,其步骤包括:
(1)将15份的苯基三氯硅烷、11份的甲苯、11份的乙酸乙酯、11份的异丙醇、44份的环己烷、11份的丙酮加入容器中搅拌均匀,搅拌速度为1500r/min;
(2)于容器中加入2份乙烯基三乙氧基硅烷、2份铂碳催化剂(铂含量为3wt%)、1份附着力促进树脂和4份二烷基二硫代氨基甲酸盐,搅拌均匀;
(3)于容器中加入5份改性烷基苯酚甲醛树脂,搅拌均匀后加入1.5份异构十三醇聚氧乙烯醚并加热温度至40度,得到离型液;
(4)将PET基材表面经过电弧处理,形成4um厚度的粗糙层,采用微凹辊将离型液涂布在PET基材表面,经过烘箱进行烘烤固化,烘箱温度为130℃,烘箱风速为1.3m/min,再经过冷却收卷,制得导热硅胶片用离型膜。
实施例2
本实施例导热硅胶片用离型膜的制备方法,其步骤包括:
(1)将10份的道康宁硅油、9份的甲苯、18份的乙酸乙酯、10份的异丙醇、24份的环己烷、20份的丙酮加入容器中搅拌均匀,搅拌速度为1200r/min;
(2)于容器中加入4份乙烯基三乙氧基硅烷、1份氯铂酸催化剂(铂含量为3wt%)、1.5份附着力促进树脂和8份二烷基二硫代氨基甲酸盐,搅拌均匀;
(3)于容器中加入10份改性烷基苯酚甲醛树脂,搅拌均匀后加入3份异构十三醇聚氧乙烯醚并加热温度至60度,得到离型液;
(4)将PET基材表面经过电弧处理,形成3um厚度的粗糙层,采用微凹辊将离型液涂布在PET基材表面,经过烘箱进行烘烤固化,烘箱温度为120℃,烘箱风速为1.0m/min,再经过冷却收卷,制得导热硅胶片用离型膜。
实施例3
本实施例导热硅胶片用离型膜的制备方法,其步骤包括:
(1)将15份的苯基三氯硅烷、15份的甲苯、15份的乙酸乙酯、30份的异丙醇、8份的环己烷、20份的丙酮加入容器中搅拌均匀,搅拌速度为1500r/min;
(2)于容器中加入2份乙烯基三乙氧基硅烷、2份铂碳催化剂(铂含量为3wt%)、1份附着力促进树脂和4份二烷基二硫代氨基甲酸盐,搅拌均匀;
(3)于容器中加入5份改性烷基苯酚甲醛树脂,搅拌均匀后加入1.5份异构十三醇聚氧乙烯醚并加热温度至40度,得到离型液;
(4)将PET基材表面经过电弧处理,形成4um厚度的粗糙层,采用微凹辊将离型液涂布在PET基材表面,经过烘箱进行烘烤固化,烘箱温度为130℃,烘箱风速为1.3m/min,再经过冷却收卷,制得导热硅胶片用离型膜。
实施例4
本实施例导热硅胶片用离型膜的制备方法,其步骤包括:
(1)将15份的苯基三氯硅烷、11份的甲苯、20份的乙酸乙酯、17份的异丙醇、40份的丙酮加入容器中搅拌均匀,搅拌速度为1500r/min;
(2)于容器中加入2份乙烯基三乙氧基硅烷、2份铂碳催化剂(铂含量为3wt%)、1份附着力促进树脂和4份二烷基二硫代氨基甲酸盐,搅拌均匀;
(3)于容器中加入5份改性烷基苯酚甲醛树脂,搅拌均匀后加入1.5份异构十三醇聚氧乙烯醚并加热温度至40度,得到离型液;
(4)将PET基材表面经过电弧处理,形成4um厚度的粗糙层,采用微凹辊将离型液涂布在PET基材表面,经过烘箱进行烘烤固化,烘箱温度为130℃,烘箱风速为1.3m/min,再经过冷却收卷,制得导热硅胶片用离型膜。
对比例1
本对比导热硅胶片用离型膜的制备方法,其步骤包括:
(1)将15份的苯基三氯硅烷、11份的甲苯、11份的乙酸乙酯、11份的异丙醇、44份的环己烷、11份的丙酮加入容器中搅拌均匀,搅拌速度为1500r/min;
(2)于容器中加入2份铂碳催化剂(铂含量为3wt%)、1份附着力促进树脂和4份二烷基二硫代氨基甲酸盐,搅拌均匀;
(3)于容器中加入5份改性烷基苯酚甲醛树脂,搅拌均匀后加入1.5份异构十三醇聚氧乙烯醚并加热温度至40度,得到离型液;
(4)将PET基材表面经过电弧处理,形成4um厚度的粗糙层,采用微凹辊将离型液涂布在PET基材表面,经过烘箱进行烘烤固化,烘箱温度为130℃,烘箱风速为1.3m/min,再经过冷却收卷,制得导热硅胶片用离型膜。
对比例2
本对比本实施例导热硅胶片用离型膜的制备方法,其步骤包括:
(1)将15份的苯基三氯硅烷、11份的甲苯、11份的乙酸乙酯、11份的异丙醇、44份的环己烷、11份的丙酮加入容器中搅拌均匀,搅拌速度为1500r/min;
(2)于容器中加入2份乙烯基三乙氧基硅烷、2份铂碳催化剂(铂含量为3wt%)、1份附着力促进树脂,搅拌均匀;
(3)于容器中加入5份改性烷基苯酚甲醛树脂,搅拌均匀后加入1.5份异构十三醇聚氧乙烯醚并加热温度至40度,得到离型液;
(4)将PET基材表面经过电弧处理,形成4um厚度的粗糙层,采用微凹辊将离型液涂布在PET基材表面,经过烘箱进行烘烤固化,烘箱温度为130℃,烘箱风速为1.3m/min,再经过冷却收卷,制得导热硅胶片用离型膜。
对比例3
本对比例本实施例导热硅胶片用离型膜的制备方法,其步骤包括:
(1)将15份的苯基三氯硅烷、11份的甲苯、11份的乙酸乙酯、11份的异丙醇、44份的环己烷、11份的丙酮加入容器中搅拌均匀,搅拌速度为1500r/min;
(2)于容器中加入2份乙烯基三乙氧基硅烷、2份铂碳催化剂(铂含量为3wt%)、1份附着力促进树脂和4份二烷基二硫代氨基甲酸盐,搅拌均匀;
(3)于容器中加入1.5份异构十三醇聚氧乙烯醚并加热温度至40度,得到离型液;
(4)将PET基材表面经过电弧处理,形成4um厚度的粗糙层,采用微凹辊将离型液涂布在PET基材表面,经过烘箱进行烘烤固化,烘箱温度为130℃,烘箱风速为1.3m/min,再经过冷却收卷,制得导热硅胶片用离型膜。
对实施例1-4和对比例1-3获得的导热硅胶片用离型膜进行脱落性能测试和抗氧化性能测试。脱落性能测试结果见表1,抗氧化性能测试结果见表2。
脱落性能测试方法:
(1)取实施例1-4和对比例1-3制备的离型膜作为测试对象,尺寸为A4大小,测试各离型膜的初始离型力L;
(2)然后将上述各离型膜放置在平整干净的玻璃面板上,用右手的食指与中指合并用力搓各离型膜的离型面,同一个区域搓2次,待搓完后,测试被搓部位的离型力M;计算离型力变化率S=(M-L)/(L)×100%。,离型力变化率越大,说明抗脱落性能越差。
抗氧化性能测试方法:
(1)取实施例1-4和对比例1-3制备的离型膜作为测试对象,尺寸为A4大小,测试各离型膜的初始离型力L;
(2)然后将上述各离型膜放置在氧化烘箱中烘烤,烘箱温度为70度,氧气浓度为40%,静置24H、48H后,分别观察离型膜是否有氧化变黑的情况,氧化黑点的数量,同时测试其氧化后的离型力M。离型膜氧化会影响其离型力和薄膜的外观,导致离型膜无法正常使用,故需要杜绝离型膜的氧化黑化的现象。
表1脱落性能测试结果
表2抗氧化性能测试结果
从表1-2的数据可知,通过本申请导热硅胶片用离型膜的制备方法制得的离型膜具有良好的防脱落及抗氧化性。这是由于本申请的制备方法中,通过每个步骤的衔接降低离型膜的硅油层未固化部分,尤其是催化剂的加入可有效地提高反应速度,降低硅油层未固化部分。同时借助乙烯基三乙氧基硅烷提高二烷基二硫代氨基甲酸盐和硅油的复合以提高防脱落性,并利用二烷基二硫代氨基甲酸盐防止离型膜的硅油层未固化部分氧化,避免氧化黑点出现。引入改性烷基苯酚甲醛树脂提高离型膜的硅油层中固化部分与未充分固化部分之间的粘附,有效防止未充分固化部分出现脱落。
最后所应当说明的是,以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制,尽管参照最佳实施例对本发明做了详细的说明,但本发明并不局限于以上揭示的实施例,而应当涵盖各种根据本发明的本质进行的修改、等效组合。
Claims (9)
1.一种导热硅胶片用离型膜的制备方法,其特征在于,其步骤包括:
(1)将8-15份的硅油和70-88份溶剂加入容器中搅拌均匀,搅拌速度为900-1500r/min;
(2)于容器中加入2-4份乙烯基三乙氧基硅烷、0.5-2份催化剂、1-1.5份附着力促进树脂和4-8份二烷基二硫代氨基甲酸盐,搅拌均匀;
(3)于容器中加入5-10份改性烷基苯酚甲醛树脂,搅拌均匀后加入1.5-3份异构十三醇聚氧乙烯醚并加热温度至40-60度,得到离型液;
(4)将所述离型液涂布在基材表面,经过烘烤固化,制得导热硅胶片用离型膜。
2.如权利要求1所述的导热硅胶片用离型膜的制备方法,其特征在于,所述硅油选自苯基三氯硅烷或道康宁硅油中的至少一种。
3.如权利要求1所述的导热硅胶片用离型膜的制备方法,其特征在于,所述溶剂选自甲苯、乙酸乙酯、异丙醇、环己烷、丙酮中的至少一种。
4.如权利要求1所述的导热硅胶片用离型膜的制备方法,其特征在于,所述溶剂选自甲苯、乙酸乙酯、异丙醇、环己烷、丙酮的混合物,且所述环己烷的用量等于其余各溶剂的用量之和,所述甲苯、乙酸乙酯、异丙醇、环己烷、丙酮的用量比为1:1:1:4:1。
5.如权利要求1所述的导热硅胶片用离型膜的制备方法,其特征在于,所述催化剂选自铂碳催化剂和氯铂酸催化剂中的至少一种。
6.如权利要求1所述的导热硅胶片用离型膜的制备方法,其特征在于,所述基材表面经过电弧处理,形成2-4um厚度的粗糙层。
7.如权利要求1所述的导热硅胶片用离型膜的制备方法,其特征在于,所述基材选自PET、BOPET、PE或PVC中的至少一种。
8.如权利要求1所述的导热硅胶片用离型膜的制备方法,其特征在于,所述烘烤温度为120-130℃。
9.一种导热硅胶片用离型膜,其特征在于,所述导热硅胶片用离型膜采用如权利要求1-8任一项所述的导热硅胶片用离型膜的制备方法制得。
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