CN116136067A - 一种碳陶刹车盘的制备方法 - Google Patents
一种碳陶刹车盘的制备方法 Download PDFInfo
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Abstract
本发明公开了一种碳陶刹车盘的制备方法,涉及刹车制动材料技术领域。该碳陶刹车盘以4‑苯基‑3‑氨基硫脲改性的短切碳纤维作为混合浆料成分,通过注塑成型工艺制备刹车盘坯体,再经炭化、粗加工、陶瓷化制得的碳陶刹车盘具有良好的体积密度、力学性能、导热性能及耐摩擦性能;本发明还采用5‑叔丁基‑2‑甲氧基苯胺改性树脂,然后再用于碳陶刹车盘的制备,使得碳陶刹车盘具有更优的体积密度、力学性能、导热性能及耐摩擦性能。
Description
技术领域
本发明属于刹车制动材料技术领域,具体涉及一种碳陶刹车盘的制备方法。
背景技术
目前汽车刹车盘以灰铸铁材料为主,与传统铸铁相比,碳陶复合材料刹车盘具有明显的性能优势:1)减重性能佳:碳陶制动盘比铸铁制动盘的质量降低了50%左右,例如在保时捷911Turbo跑车上,碳陶制动盘的直径比传统制动盘直径大2cm,但4个车轮的制动器总质量却减少了16kg;2)摩擦效果好:碳陶制动盘的摩擦因数远高于铸铁制动盘,大大提高了制动效率;3)耐高温:铸铁制动盘在连续高速制动后会因为温度过高而变形,制动盘表面会形成波纹,导致制动时车轮发生抖动,降低制动效率,在高温下,碳陶材料由于其较高的热稳定性值(碳陶为1350℃,铸铁为700℃)而更能抵抗变形或翘曲;4)寿命长:碳陶制动盘的表面硬度高,制动磨损小。测试结果表明,碳陶制动盘的使用寿命能够超过30万km。
目前碳陶制动盘依据碳纤维状态可以分为两大类,分别是短纤盘和长纤盘。长纤盘的制备首先是将连续碳纤维用针刺法做成碳纤维预制件,然后用化学气相渗透法增碳做成碳碳多孔体,再通过熔融渗硅进行陶瓷化做成碳陶复合材料,最后经机加工成碳陶制动盘;该工艺的优点是所制备出来的碳陶制动盘综合性能很好,但缺点是材料制备周期比较长,整个工艺周期大约2个月,成本较高;短纤盘采用短切碳纤维为原料,与酚醛树脂、碳粉等添加剂先干混,然后模压成型-固化、碳化、渗硅-陶瓷化、加工产品,该工艺路线制备周期短,成本低,但缺点也比较明显,即短切碳纤维分散困难,预混料成分不均匀,流动性差,模压时填料不均匀,最终导致材料强度比较低,韧性比较差,在使用过程中容易出现掉块、崩边和断裂的风险。
本发明通过制备短碳纤维均匀分散的浆料,再通过注塑成型工艺制备刹车盘坯体,解决目前短纤维混料-温压工艺面临的混料不均匀,填料不均匀、材料强度低、耐磨性差的问题。
发明内容
本发明的目的在于提供一种碳陶刹车盘的制备方法,该碳陶刹车盘具有良好的体积密度、力学性能、导热性能及耐摩擦性能。
本发明为实现上述目的所采取的技术方案为:
一种改性短切碳纤维,上述改性短切碳纤维包含短切碳纤维及其表面修饰基团;上述表面修饰基团包含硫脲基团、芳香环;上述短切碳纤维为PAN碳纤维;上述短切碳纤维长度为5-30mm。
优选地,上述改性短切碳纤维由4-苯基-3-氨基硫脲改性短切碳纤维制得。
本发明还公开了一种改性短切碳纤维的制备方法,包括:将短切碳纤维进行氧化处理,再进行酰氯化处理,然后与4-苯基-3-氨基硫脲进行接枝反应,制得改性短切碳纤维。
本发明提供了一种改性短切碳纤维的制备方法,将4-苯基-3-氨基硫脲以化学接枝的方法连接到短切碳纤维表面,制得的改性短切碳纤维用于碳陶刹车盘的制备,使得碳陶刹车盘具有良好的体积密度、力学性能、导热性能及耐摩擦性能;原因可能是由于4-苯基-3-氨基硫脲对短切碳纤维的改性作用,增强了碳纤维表面的粗糙程度,有利于界面处的物理锁合作用增强,使得碳纤维与树脂结合的更加紧密。且氮元素的掺杂还可以增强碳材料的导电性,促进离子的快速迁移;另外,可能由于硫元素的存在影响了改性短切碳纤维在炭化过程中的生长,进一步增强了其韧性,改善其力学性能。
具体地,上述改性短切碳纤维的制备方法,包括以下步骤:
1)氧化处理:将短切碳纤维置于索氏提取器中,回流抽提70-80h,在75-85℃下真空干燥10-12h;然后将干燥后的短切碳纤维浸入过硫酸钾/硝酸银混合溶液中(混合溶液中过硫酸钾的浓度为0.1-0.15mol/L,硝酸银的浓度为0.01-0.015mol/L),在68-75℃反应1.5-2h,去离子水洗涤3-5次,乙醇抽提后,在85-90℃真空干燥4-6h,制得氧化短切碳纤维;
2)酰氯化处理:将氧化短切碳纤维浸入氯化亚砜/N,N-二甲基甲酰胺混合溶液(氯化亚砜与N,N-二甲基甲酰胺的体积比为1:0.045-0.055)中,在75-83℃条件下,反应45-52h,减压蒸馏,制得酰氯化短切碳纤维;
3)接枝处理:将酰氯化短切碳纤维浸入到浓度为3-5g/L的4-苯基-3-氨基硫脲甲醇溶液中,在8-9MPa,255-270℃条件下反应23-30min,然后冷却至室温,去离子水洗涤3-5次,甲醇洗涤3-5次,真空干燥20-30h,制得改性短切碳纤维。
优选地,上述短切碳纤维与过硫酸钾/硝酸银混合溶液的质量体积比为1g:20-30mL;氧化短切碳纤维与氯化亚砜/N,N-二甲基甲酰胺混合溶液的质量体积比为1g:20-30mL;酰氯化短切碳纤维与4-苯基-3-氨基硫脲甲醇溶液的质量体积比为1g:20-30mL。
本发明还公开了一种碳陶刹车盘,包含上述改性短切碳纤维制备的混合浆料,通过注塑成型工艺得到碳纤维增强复合材料坯体,再经炭化、粗加工、陶瓷化制得碳陶刹车盘。
优选地,上述混合浆料还包含树脂、添加剂。
优选地,上述混合浆料中,按重量份计,改性短切碳纤维的用量为20-30份;树脂的用量为50-60份;添加剂的用量为10-20份。
优选地,上述树脂包含酚醛树脂、呋喃树脂中的至少一种。
优选地,上述树脂室温粘度≤500mpas。
优选地,上述添加剂包含鳞片石墨、石墨烯、二硫化钼、二硫化钨中的至少一种。
具体地,上述碳陶刹车盘的制备方法,包括以下步骤:
1)原料混合:将改性短切碳纤维、树脂、添加剂充分混合,混合温度50-80℃,转速100-500r/min,时间0.5-2h,制得混合浆料;
2)注塑成型:将混合浆料投入注塑机的料筒中,保持料温50-80℃,然后注入注塑模具的型腔中并保压,压力为100-130Mpa;
3)升温固化:将注塑模具加热至150-250℃,并保持10-30min;
4)开模取料:取出注塑模具,放入20-25℃的冷却水中冷却后开模,得到碳纤维增强复合材料坯体;
5)炭化:在氮气氛围下,将碳纤维增强复合材料坯体炭化处理,炭化温度700-900℃,时间30-50h,得到多孔碳纤维复合材料坯体;
6)粗加工:将多孔碳纤维复合材料坯体按照设计形状进行粗加工;
7)陶瓷化:将粗加工后的多孔碳纤维复合材料坯体置于石墨坩埚中,坩埚底铺上硅粉(硅粉与粗加工后的多孔碳纤维复合材料坯体的质量比为1:1-1.5),然后放入真空渗硅炉中,抽真空至1000Pa以下,升温至1400-1700℃,保温1-4h,自然降温至150℃以下出炉,再经精加工,即可制备出碳陶刹车盘。
优选地,上述碳陶刹车盘的体积密度为2.0-2.3g/cm3。
优选地,上述碳陶刹车盘的抗弯强度为60-140MPa。
优选地,上述碳陶刹车盘的摩擦系数为0.35-0.45。
优选地,上述碳陶刹车盘的导热系数为20-70Wm-1k-1。
为进一步提升碳陶刹车盘的性能,本发明还对酚醛树脂进行改性处理。
本发明还公开了一种改性酚醛树脂的制备方法,包括:采用苯酚、5-叔丁基-2-甲氧基苯胺、甲醛,经加成反应、缩聚反应后,制得改性酚醛树脂。
本发明提供了一种改性酚醛树脂的制备方法,采用苯酚、5-叔丁基-2-甲氧基苯胺、甲醛经加成反应、缩聚反应,制得的改性酚醛树脂用于碳陶刹车盘的制备,使得碳陶刹车盘具有更优的体积密度、力学性能、导热性能及耐摩擦性能;原因可能是由于5-叔丁基-2-甲氧基苯胺与甲醛的反应,增加了酚醛树脂的交联程度,树脂分子之间结合的程度较未改性的酚醛树脂更加紧密;且5-叔丁基-2-甲氧基苯胺属于芳香族化合物,固化后形成三维网状结构,使得酚醛树脂交联网络结构分布更加均匀,与短切碳纤维的接触面积变大,粘结强度提高。
具体地,上述改性酚醛树脂的制备方法,包括以下步骤:
在苯酚中加入氢氧化钡、甲醛,在60-65℃反应1.5-2h,在73-80℃反应1.5-2h,在85-88℃反应25-35min,加入5-叔丁基-2-甲氧基苯胺,升温至90-93℃,反应至溶液出现浑浊后,再反应25-30min停止反应,旋蒸,待无蒸出物后停止旋蒸,干燥,制得改性酚醛树脂。
优选地,上述苯酚与甲醛的摩尔比为1:1.2-1.6;苯酚与5-叔丁基-2-甲氧基苯胺的摩尔比为1:0.25-0.4;苯酚与氢氧化钡的质量比为1:0.05-0.07。
本发明还公开了上述制备方法得到的改性酚醛树脂在制备碳陶刹车盘中的用途。
本发明的有益效果包括:
本发明获得了一种碳陶刹车盘的制备方法,该碳陶刹车盘以4-苯基-3-氨基硫脲改性的短切碳纤维、树脂、添加剂组成的混合浆料通过注塑成型工艺制备刹车盘坯体,再经炭化、粗加工、陶瓷化制得的碳陶刹车盘具有良好的体积密度、力学性能、导热性能及耐摩擦性能;本发明还采用5-叔丁基-2-甲氧基苯胺对树脂进行改性处理,然后用于碳陶刹车盘的制备,使得碳陶刹车盘具有更优的体积密度、力学性能、导热性能及耐摩擦性能;本发明提供了一种强度高、耐磨性好而且制备周期短、成本低的碳陶刹车盘材料。
因此,本发明提供了一种碳陶刹车盘的制备方法,该碳陶刹车盘具有良好的体积密度、力学性能、导热性能及耐摩擦性能。
附图说明
图1为碳陶刹车盘示意图;
图2为实施例3制备的改性短切碳纤维及短切碳纤维的红外光谱图测试结果;
图3为实施例4制备的改性酚醛树脂及酚醛树脂的红外光谱图测试结果。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明确,以下结合具体实施方式对本发明的技术方案作进一步详细描述:
实施例1:
一种碳陶刹车盘的制备方法,包括以下步骤:
1)原料混合:将T700级PAN短切碳纤维、酚醛树脂(室温粘度为370mpas)、添加剂(添加剂包含鳞片石墨、石墨烯、二硫化钼、二硫化钨,鳞片石墨、石墨烯、二硫化钼、二硫化钨的质量比为1:1:1:1)充分混合,混合温度50℃,转速100r/min,时间2h,制得混合浆料;
2)注塑成型:将混合浆料投入注塑机的料筒中,保持料温50℃,然后注入注塑模具的型腔中并保压,压力为130Mpa;
3)升温固化:将注塑模具加热至250℃,并保持10min;
4)开模取料:取出注塑模具,放入20℃的冷却水中冷却后开模,得到碳纤维增强复合材料坯体;
5)炭化:在氮气氛围下,将碳纤维增强复合材料坯体炭化处理,炭化温度700℃,时间50h,得到多孔碳纤维复合材料坯体;
6)粗加工:将多孔碳纤维复合材料坯体按照设计形状进行粗加工;
7)陶瓷化:将粗加工后的多孔碳纤维复合材料坯体置于石墨坩埚中,坩埚底铺上硅粉(硅粉与粗加工后的多孔碳纤维复合材料坯体的质量比为1:1),然后放入真空渗硅炉中,抽真空至1000Pa以下,升温至1400℃,保温4h,自然降温至150℃以下出炉,再按照图1所示的图纸进行精加工,即可制备出碳陶刹车盘;
其中,混合浆料中,按重量份计,短切碳纤维的用量为20份;酚醛树脂的用量为50份;添加剂的用量为10份。
实施例2:
一种碳陶刹车盘的制备方法与实施例1的区别:采用呋喃树脂替代酚醛树脂。
实施例3:
一种碳陶刹车盘的制备方法与实施例1的区别:采用改性短切碳纤维替代短切碳纤维。
改性短切碳纤维的制备方法,包括以下步骤:
1)氧化处理:将短切碳纤维置于索氏提取器中,回流抽提70h,在75℃下真空干燥12h;然后将干燥后的短切碳纤维浸入过硫酸钾/硝酸银混合溶液中(混合溶液中过硫酸钾的浓度为0.1mol/L,硝酸银的浓度为0.01mol/L),在68℃反应1.5h,去离子水洗涤3次,乙醇抽提后,在85℃真空干燥4h,制得氧化短切碳纤维;
2)酰氯化处理:将氧化短切碳纤维浸入氯化亚砜/N,N-二甲基甲酰胺混合溶液(氯化亚砜与N,N-二甲基甲酰胺的体积比为1:0.045)中,在75℃条件下,反应45h,减压蒸馏,制得酰氯化短切碳纤维;
3)接枝处理:将酰氯化短切碳纤维浸入到浓度为3g/L的4-苯基-3-氨基硫脲甲醇溶液中,在8MPa,255℃条件下反应23min,然后冷却至室温,去离子水洗涤3次,甲醇洗涤3次,真空干燥20h,制得改性短切碳纤维;
其中,短切碳纤维与过硫酸钾/硝酸银混合溶液的质量体积比为1g:20mL;氧化短切碳纤维与氯化亚砜/N,N-二甲基甲酰胺混合溶液的质量体积比为1g:20mL;酰氯化短切碳纤维与4-苯基-3-氨基硫脲甲醇溶液的质量体积比为1g:20mL。
实施例4:
一种碳陶刹车盘的制备方法与实施例1的区别:采用改性酚醛树脂替代酚醛树脂。
改性酚醛树脂的制备方法,包括以下步骤:
在苯酚中加入氢氧化钡、甲醛,在60℃反应1.5h,在73℃反应2h,在85℃反应25min,加入5-叔丁基-2-甲氧基苯胺,升温至90℃,反应至溶液出现浑浊后,再反应25min停止反应,旋蒸,待无蒸出物后停止旋蒸,干燥,制得改性酚醛树脂。
其中,苯酚与甲醛的摩尔比为1:1.2;苯酚与5-叔丁基-2-甲氧基苯胺的摩尔比为1:0.25;苯酚与氢氧化钡的质量比为1:0.05。
实施例5:
一种碳陶刹车盘的制备方法与实施例3的区别:采用改性酚醛树脂替代酚醛树脂。
改性酚醛树脂的制备方法同实施例4。
试验例:
1.红外光谱测试
采用NICOLET 5700型红外光谱仪,以KBr压片法测试样品的FTIR图谱,分辨率为6cm-1,测试范围4000-400cm-1,每个样品扫描100次。
对实施例3制备的改性短切碳纤维及短切碳纤维进行上述测试,结果如图2所示。由图2可知,与短切碳纤维的红外谱图相比,改性短切碳纤维的红外谱图在1400-1600cm-1处存在苯环的红外特征吸收峰;在1468cm-1处存在C=S键的红外特征峰;说明4-苯基-3-氨基硫脲参与了改性短切碳纤维的生成反应。
对实施例4制备的改性酚醛树脂及酚醛树脂进行上述测试,结果如图3所示。由图3可知,与酚醛树脂的红外谱图相比,改性酚醛树脂的红外谱图在1050cm-1处存在C-N键的红外特征吸收峰,说明5-叔丁基-2-甲氧基苯胺参与了改性酚醛树脂的生成反应。
2.体积密度测试
采用体积-重量法对碳陶刹车盘样品的体积密度进行测试。
表1 体积密度测试结果
实验分组 | 体积密度/g·cm-3 |
实施例1 | 2.00 |
实施例2 | 2.05 |
实施例3 | 2.16 |
实施例4 | 2.12 |
实施例5 | 2.25 |
对实施例1-实施例5制备的碳陶刹车盘进行上述测试,结果如表1所示。由表1可知,实施例1-实施例5制备的碳陶刹车盘具有较低的体积密度,不到钢体积密度的四分之一,能满足不同车型的制动技术要求。且实施例3、实施例4、实施例5与实施例1相比体积密度均有所提升,但整体变化不大。
3.力学性能测试
采用DDL300型电子万能试验机测试抗拉强度。
表2 抗拉强度测试结果
实验分组 | 抗拉强度/MPa |
实施例1 | 90 |
实施例2 | 89 |
实施例3 | 112 |
实施例4 | 107 |
实施例5 | 130 |
对实施例1-实施例5制备的碳陶刹车盘进行上述测试,结果如表2所示。由表2可知,实施例3与实施例1、实施例5与实施例4相比,抗拉强度明显增强,说明4-苯基-3-氨基硫脲改性短切碳纤维后,将其用于碳陶刹车盘的制备,使得碳陶刹车盘具有良好的力学性能;实施例4与实施例1、实施例5与实施例3相比,抗拉强度也有所增强,说明5-叔丁基-2-甲氧基苯胺改性酚醛树脂后,将其用于碳陶刹车盘的制备,使得碳陶刹车盘也具有良好的力学性能。
4.导热系数的测试
采用TC-3000热常数测定仪,按GJB1201.1测试碳陶刹车盘样品的导热系数,其测试温度为800℃,试样尺寸为D10mm×3.1mm。
表3 导热系数测试结果
实验分组 | 导热系数/Wm-1k-1 |
实施例1 | 40 |
实施例2 | 41 |
实施例3 | 48 |
实施例4 | 52 |
实施例5 | 61 |
对实施例1-实施例5制备的碳陶刹车盘进行上述测试,结果如表3所示。由表3可知,实施例3与实施例1、实施例5与实施例4相比,导热系数有所增强,说明4-苯基-3-氨基硫脲改性短切碳纤维后,并将其用于碳陶刹车盘的制备,使得碳陶刹车盘具有良好的导热性能;实施例4与实施例1、实施例5与实施例3相比,导热系数也明显增强,说明5-叔丁基-2-甲氧基苯胺改性酚醛树脂后,将其用于碳陶刹车盘的制备,使得碳陶刹车盘也具有良好的导热性能。
5.摩擦性能测试
采用MM-1000摩擦试验机对碳陶刹车盘样品的动摩擦系数及磨损率进行测试,其试环有效摩擦面外径D75mm/内径D55mm×10mm,比压为98N/cm2,惯量为3kgf·cm·s2,线速度为25m/s。
表4 摩擦系数测试结果
实验分组 | 摩擦系数 | 磨损率(μm/面·次) |
实施例1 | 0.41 | 0.72 |
实施例2 | 0.40 | 0.7 |
实施例3 | 0.42 | 0.65 |
实施例4 | 0.41 | 0.61 |
实施例5 | 0.43 | 0.53 |
对实施例1-实施例5制备的碳陶刹车盘进行上述测试,结果如表4所示。由表4可知,实施例1-实施例5均具有较小的摩擦系数,且相差不大;而实施例3与实施例1、实施例5与实施例4相比,磨损率有所下降,说明4-苯基-3-氨基硫脲改性短切碳纤维后,并将其用于碳陶刹车盘的制备,使得碳陶刹车盘具有良好的耐磨性能;实施例4与实施例1、实施例5与实施例3相比,磨损率也明显降低,说明5-叔丁基-2-甲氧基苯胺改性酚醛树脂后,将其用于碳陶刹车盘的制备,使得碳陶刹车盘也具有良好的耐磨性能。
上述实施例中的常规技术为本领域技术人员所知晓的现有技术,故在此不再详细赘述。
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应以所述权利要求的保护范围为准。
Claims (10)
1.一种改性短切碳纤维,其特征在于:所述改性短切碳纤维包含短切碳纤维及其表面修饰基团;所述表面修饰基团包含硫脲基团、芳香环;所述短切碳纤维为PAN碳纤维;所述短切碳纤维长度为5-30mm。
2.一种碳陶刹车盘,其特征在于:所述碳陶刹车盘由包含权利要求1所述的改性短切碳纤维的混合浆料,通过注塑成型工艺得到碳纤维增强复合材料坯体,再经炭化、粗加工、陶瓷化制得碳陶刹车盘。
3.根据权利要求2所述的一种碳陶刹车盘,其特征在于:所述混合浆料中,按重量份计,改性短切碳纤维的用量为20-30份。
4.根据权利要求2所述的一种碳陶刹车盘,其特征在于:所述碳陶刹车盘的导热系数为20-70Wm-1k-1。
5.根据权利要求2所述的一种碳陶刹车盘,其特征在于:所述碳陶刹车盘的抗弯强度为60-140MPa。
6.根据权利要求2所述的一种碳陶刹车盘,其特征在于:所述碳陶刹车盘的体积密度为2.0-2.3g/cm3。
7.根据权利要求2所述的一种碳陶刹车盘,其特征在于:所述混合浆料还包含树脂、添加剂。
8.根据权利要求7所述的一种碳陶刹车盘,其特征在于:所述混合浆料中,按重量份计,树脂的用量为50-60份;添加剂的用量为10-20份。
9.根据权利要求7所述的一种碳陶刹车盘,其特征在于:所述树脂包含酚醛树脂、呋喃树脂中的至少一种。
10.根据权利要求7所述的一种碳陶刹车盘,其特征在于:所述添加剂包含鳞片石墨、石墨烯、二硫化钼、二硫化钨中的至少一种。
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