CN116790190A - 一种用于碳化硅精抛的抛光材料及其制备方法 - Google Patents
一种用于碳化硅精抛的抛光材料及其制备方法 Download PDFInfo
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 48
- 229920005749 polyurethane resin Polymers 0.000 claims abstract description 35
- 229920005862 polyol Polymers 0.000 claims abstract description 34
- 150000003077 polyols Chemical class 0.000 claims abstract description 34
- 239000002904 solvent Substances 0.000 claims abstract description 32
- 239000012948 isocyanate Substances 0.000 claims abstract description 26
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 26
- 239000011527 polyurethane coating Substances 0.000 claims abstract description 17
- 239000004970 Chain extender Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 7
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 7
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 7
- 150000002009 diols Chemical class 0.000 claims description 39
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- 238000003756 stirring Methods 0.000 claims description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
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- 125000003118 aryl group Chemical group 0.000 claims description 2
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 9
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- C09G1/00—Polishing compositions
- C09G1/06—Other polishing compositions
- C09G1/14—Other polishing compositions based on non-waxy substances
- C09G1/16—Other polishing compositions based on non-waxy substances on natural or synthetic resins
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Abstract
本申请涉及涉及一种抛光材料，具体公开了一种用于碳化硅精抛的抛光材料及其制备方法。一种用于碳化硅精抛的抛光材料，所述抛光材料的原料包括载体、聚氨酯涂层、聚对苯二甲酸乙二酯薄膜；所述聚氨酯涂层的原料包括如下重量份的组分：聚氨酯树脂80~120份、溶剂40~60份、表面活性剂1~20份；所述聚氨酯树脂的原料包括如下重量份的组分：多元醇组合物20~35份、扩链剂0.1~1份、异氰酸酯3~9份、溶剂60~70份、封端剂0.02~0.04份。本申请中的抛光材料抗氧化性能较好，具有较高的使用寿命。
Description
技术领域
本申请涉及一种抛光材料，尤其是涉及一种用于碳化硅精抛的抛光材料及其制备方法。
背景技术
碳化硅是由碳元素和硅元素组成的一种半导体材料，具有耐高温、耐高频、耐高压的特性。在集成电路以及电子设备制造中，需要将沉积在半导体晶片或晶圆表面的多层导电材料、半导体材料和介电材料去除，化学机械平面抛光是目前用于工件表面抛光最常用的技术。在利用抛光材料进行抛光时，需要利用抛光液进行抛光，抛光液中含有一些过氧化物，会使得抛光材料氧化，从而抛光材料的使用寿命较短。
发明内容
为了提高抛光材料的抗氧化性能，本申请提供一种用于碳化硅精抛的抛光材料及其制备方法。
第一方面，本申请提供的一种用于碳化硅精抛的抛光材料，采用如下的技术方案：一种用于碳化硅精抛的抛光材料，所述抛光材料的原料包括载体、聚氨酯涂层、聚对苯二甲酸乙二酯薄膜；所述聚氨酯涂层的原料包括如下重量份的组分：聚氨酯树脂80～120份、溶剂40～60份、表面活性剂1～20份；所述聚氨酯树脂的原料包括如下重量份的组分：多元醇组合物20～35份、扩链剂0.1～1份、异氰酸酯3～9份、溶剂60～70份、封端剂0.02～0.04份。
通过采用上述技术方案，利用载体和聚氨酯涂层形成的具有微孔结构的聚氨酯材料，可以对工件表面进行抛光；多元醇组合物、异氰酸酯合成的聚氨酯树脂，具有较强抗氧化性能，从而在进行抛光时，使得抛光材料不易被抛光液所氧化，从而提高了抛光材料的使用寿命。
在一个具体的可实施方案中，所述多元醇组合物包括聚四氢呋喃二醇和聚酯二元醇组成混合物。
在一个具体的可实施方案中，所述聚酯二元醇为二元酸和二元醇通过高温脱水缩聚而成的线性高分子聚合物，且分子链两端均为可与异氰酸酯反应的羟基；所述二元酸包括己二酸、丁二酸、分子量底于300的脂肪族或芳香族二元羧酸中的一种或多种；所述二元醇含有一个或多个侧链且有一个或多个侧链的碳链长度大于2。
在一个具体的可实施方案中，所述多元醇组合物还包括聚碳酸酯二元醇、聚己内酯二元醇、内酯共聚物、聚酯二元醇中的一种或多种。
在一个具体的可实施方案中，所述聚四氢呋喃二醇和所述聚酯二元醇在所述多元醇组合物中的质量分数为30％-100％。
通过采用上述技术方案，利用二元酸和二元醇通过高温脱水缩聚而成的聚酯二元醇和聚四氢呋喃二醇组成的多元醇组合物，且进一步限定了聚酯二元醇和聚四氢呋喃二醇的用量，使得制得的抛光材料具有较高的耐氧化性能。
在一个具体的可实施方案中，所述扩链剂包括乙二醇、1,4丁二醇、乙二胺中的一种或多种。
在一个具体的可实施方案中，所述聚氨酯树脂的原料还包括0.01～0.1重量份的助剂，所述助剂包括抗氧化剂、紫外光吸收剂、泡孔调节剂、改性硅油。
通过采用上述技术方案，抗氧化剂和紫外光吸收剂的加入，可以进一步提高制得抛光材料的抗氧化性能。
第二方面，本申请提供的一种用于碳化硅精抛的抛光材料的制备方法，采用如下的技术方案：
一种用于碳化硅精抛的抛光材料的制备方法，包括以下步骤：
聚酯二元醇的合成：将二元酸和二元醇投入反应釜中，在氮气的保护下，先在90-100℃下搅拌，然后在150-160℃下恒温反应1.5-2.5h，再升温至220-230℃，开启真空，至物料的羟值为54-58mgKOH/g且酸值为0.1-0.5mgKOH/g，停止真空，降温至120℃出料，得到聚酯二元醇；
聚氨酯树脂的合成：将部分溶剂和部分多元醇组合物加入反应釜中搅拌均匀，在25-35℃下,加入部分异氰酸酯，升高温度至65-75℃，加入部分溶剂、剩下的多元醇组合物、扩链剂，降温至45-55℃，搅拌均匀后加入剩下的异氰酸酯，在75-85℃下反应至反应物的粘度为150000cps/25℃，接着加入剩下的溶剂、封端剂，在70-80℃下搅拌反应0.5-1.5h，最后加入助剂继续搅拌反应0.5-1.5h，冷却出料，得到聚氨酯树脂；
复合：将聚氨酯树脂、溶剂、表面活性剂、色料搅拌混合均匀后过滤真空脱泡涂布在载体上，然后放入水中凝固、清洗、烘干、切片、打磨，在载体上形成聚氨酯涂层，得到聚氨酯材料；在聚对苯二甲酸乙二酯薄膜上涂布热熔胶，然后复合在聚氨酯材料上，得到抛光材料。
通过采用上述技术方案，先合成耐过氧化物的聚酯二元醇，接着在合成聚氨酯树脂时，先将部分含有聚酯二元醇的多元醇组合物和部分异氰酸酯溶解在部分溶剂中，进行一定程度的预聚，使得体系具有一定的粘度，然后再加入余下多元醇组合物和异氰酸酯以及小分子扩链剂进行二次聚合，从而提高了制得抛光材料的抗氧化性能。
综上所述，本申请包括以下至少一种有益技术效果：
1.本申请中利用载体和聚氨酯涂层形成的具有微孔结构的聚氨酯材料，可以对工件表面进行抛光；多元醇组合物、异氰酸酯合成的聚氨酯树脂，具有较强抗氧化性能，从而在进行抛光时，使得抛光材料不易被抛光液所氧化，从而提高了抛光材料的使用寿命；
2.本申请中利用多元醇组合物、异氰酸酯合成的聚氨酯树脂，具有较强抗氧化性能，从而使得形成的聚氨酯涂层不易被抛光液所氧化，且载体和聚氨酯涂层形成的具有微孔结构的聚氨酯材料，可以对工件表面进行抛光，从而提高了抛光材料的抛光效果；
3.本申请中的方法，先合成耐过氧化物的聚酯二元醇，接着在合成聚氨酯树脂时，先将部分含有聚酯二元醇的多元醇组合物和部分异氰酸酯溶解在部分溶剂中，进行一定程度的预聚，使得体系具有一定的粘度，然后再加入余下多元醇组合物和异氰酸酯以及小分子扩链剂进行二次聚合，从而提高了制得抛光材料的抗氧化性能。
附图说明
图1、2是本申请实施例中抛光材料的结构示意图。
具体实施方式
以下结合实施例对本申请作进一步详细说明。
实施例中所有原料均可通过市售获得。其中异氰酸酯为4,4-二苯基甲烷二异氰酸酯；抗氧化剂型号为1010；紫外光吸收剂型号为UV531；泡孔调节剂CAS号：63148-62-9；改性硅油CAS号：68937-55-3；载体为PE/PVC材料或玻璃板。
实施例
实施例1
实施例1提供了一种用于碳化硅精抛的抛光材料的制备方法，包括以下步骤：
聚酯二元醇的合成：将200份的二元酸和212.6份的二元醇投入反应釜中，在氮气的保护下，先在95℃下搅拌，然后在155℃下恒温反应2h，再升温至225℃，待出水量为二元酸重量的1/8时，开启真空，至物料的羟值为54-58mgKOH/g且酸值为0.1-0.5mgKOH/g，停止真空，降温至120℃出料，得到聚酯二元醇，且聚酯二元醇的羟值为56.3mgKOH/g，酸值为0.3mgKOH/g；其中二元酸为己二酸；二元醇为1,6-己二醇和2-甲基-1，3丙二醇组成的混合物，且己二酸、1,6-己二醇、2-甲基-1，3丙二醇的重量比为200：123：89.6；
聚氨酯树脂的合成：将部分溶剂和部分多元醇组合物加入反应釜中搅拌均匀，在30℃下,加入部分异氰酸酯，升高温度至70℃，反应粘度为80000cps/70℃时，加入部分溶剂、剩下的多元醇组合物、0.1kg扩链剂，降温至50℃，搅拌均匀后加入剩下的异氰酸酯，在80℃下反应至反应物的粘度为150000cps/25℃，接着加入剩下的溶剂、0.02kg封端剂，在75℃下搅拌反应1h，冷却出料，得到聚氨酯树脂；其中溶剂为N,N-二甲基甲酰胺，重量为60kg，且三次加入溶剂的重量比依次为2：2：1；多元醇组合物为聚四氢呋喃二醇和聚酯二元醇组成混合物，且聚四氢呋喃二醇和聚酯二元醇的重量比为1：1；多元醇组合物的重量为20kg，且两次加入多元醇组合物的重量比依次为7：3；异氰酸酯的重量为3kg，且两次加入异氰酸酯的重量比依次为1：4；扩链剂为乙二醇；封端剂为甲醇；
复合：将80kg聚氨酯树脂、40kg溶剂、1kg表面活性剂、3kg色料搅拌混合均匀后过滤真空脱泡涂布在载体上，然后放入水中凝固、清洗、烘干、切片、打磨，在载体上形成聚氨酯涂层，得到聚氨酯材料；在聚对苯二甲酸乙二酯薄膜上涂布热熔胶，然后复合在聚氨酯材料上，得到抛光材料，抛光材料的结构示意图如图1、2所示；其中溶剂为N,N-二甲基甲酰胺；表面活性剂为聚硅氧烷-聚氧化烯烃醚嵌段共聚物；色料根据所需颜色进行选择；载体为PE材料。
实施例2
实施例2与实施例1的区别在于，聚氨酯树脂的合成步骤中，将部分溶剂和部分多元醇组合物加入反应釜中搅拌均匀，在30℃下,加入部分异氰酸酯，升高温度至70℃，反应粘度为80000cps/70℃时，加入部分溶剂、剩下的多元醇组合物、0.1kg扩链剂，降温至50℃，搅拌均匀后加入剩下的异氰酸酯，在80℃下反应至反应物的粘度为150000cps/25℃，接着加入剩下的溶剂、0.02kg封端剂，在75℃下搅拌反应1h，再加入0.05助剂，继续搅拌1h，冷却出料，得到聚氨酯树脂；其中助剂为抗氧化剂、紫外光吸收剂、泡孔调节剂、改性硅油，且抗氧化剂、紫外光吸收剂、泡孔调节剂、改性硅油的重量比为1：1：1：1；其余步骤与实施例1相一致。
实施例3
实施例3与实施例2的区别在于，聚氨酯树脂的合成步骤中，多元醇组合物的重量为27kg，扩链剂的重量为0.5kg，异氰酸酯的重量为6kg，溶剂的重量为65kg，封端剂的重量为0.03kg；复合步骤中：将100kg聚氨酯树脂、50kg溶剂、10kg表面活性剂、6kg色料搅拌混合均匀后过滤真空脱泡涂布在载体上，然后放入水中凝固、清洗、烘干、切片、打磨，在载体上形成聚氨酯涂层，得到聚氨酯材料；其余步骤与实施例2相一致。
实施例4
实施例4与实施例2的区别在于，聚氨酯树脂的合成步骤中，多元醇组合物的重量为35kg，扩链剂的重量为1kg，异氰酸酯的重量为9kg，溶剂的重量为70kg，封端剂的重量为0.04kg；复合步骤中：将120kg聚氨酯树脂、60kg溶剂、20kg表面活性剂、10kg色料搅拌混合均匀后过滤真空脱泡涂布在载体上，然后放入水中凝固、清洗、烘干、切片、打磨，在载体上形成聚氨酯涂层，得到聚氨酯材料；其余步骤与实施例2相一致。
实施例5
实施例5与实施例3的区别在于，多元醇组合物为聚四氢呋喃二醇和聚碳酸酯二元醇组成混合物，且聚四氢呋喃二醇和聚碳酸酯二元醇的重量比为1：1；其余步骤与实施例3相一致。
实施例6
实施例6与实施例3的区别在于，多元醇组合物为聚己内酯二元醇和聚酯二元醇组成混合物，且聚己内酯二元醇和聚酯二元醇的重量比为1：1；其余步骤与实施例3相一致。
对比例
对比例1
对比例1提供了一种抛光材料的制备方法，包括以下步骤：
将80kg聚氨酯树脂、40kg溶剂、1kg表面活性剂、3kg色料搅拌混合均匀后过滤真空脱泡涂布在载体上，然后放入水中凝固、清洗、烘干、切片、打磨，在载体上形成聚氨酯涂层，得到聚氨酯材料；在聚对苯二甲酸乙二酯薄膜上涂布热熔胶，然后复合在聚氨酯材料上，得到抛光材料；其中聚氨酯树脂CAS号为9009-54-5；溶剂为N,N-二甲基甲酰胺；表面活性剂为聚硅氧烷-聚氧化烯烃醚嵌段共聚物；色料根据所需颜色进行选择；载体为PE材料。
性能检测试验
抗氧化性能：将各实施例和对比例中的抛光材料放入30％的双氧水中，在24℃下静置，检测多久后可以刮出抛光材料上的聚氨酯涂层，时间越长，抛光材料的抗氧化性能越好。
表1抛光材料的性能检测结果
| 样品 | 耐氧化时间(h) |
| 实施例1 | 192 |
| 实施例2 | 220 |
| 实施例3 | 228 |
| 实施例4 | 225 |
| 实施例5 | 180 |
| 实施例6 | 185 |
| 对比例1 | 100 |
结合实施例1和对比例1，实施例1中抛光材料的抗氧化性能较好，可见利用多元醇组合物和异氰酸酯合成的聚氨酯树脂，具有较强抗氧化性能，从而可以提高抛光材料的使用寿命。
结合实施例1和实施例2，实施例2中抛光材料的抗氧化性能较好，可见在合成聚氨酯树脂时，向原料中加入抗氧化剂和紫外光吸收剂，可以进一步提高制得抛光材料的抗氧化性能。
结合实施例2-4，实施例2-4中抛光材料的抗氧化性能相差不大，可见在合成聚氨酯树脂和复合抛光材料时，增大原料的使用量，对制得抛光材料的抗氧化性能影响不大。
结合实施例3、实施例5和实施例6，实施例3中抛光材料的抗氧化性能最好，可见在合成聚氨酯树脂时，多元醇组合物选用聚四氢呋喃二醇和聚酯二元醇组成混合物，制得聚氨酯树脂的抗氧化性能较好，从而制得抛光材料的使用寿命较长。
本具体实施例仅仅是对本申请的解释，其并不是对本申请的限制，本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改，但只要在本申请的权利要求范围内都受到专利法的保护。
Claims (8)
1.一种用于碳化硅精抛的抛光材料，其特征在于：所述抛光材料的原料包括载体、聚氨酯涂层、聚对苯二甲酸乙二酯薄膜；所述聚氨酯涂层的原料包括如下重量份的组分：聚氨酯树脂80~120份、溶剂40~60份、表面活性剂1~20份；所述聚氨酯树脂的原料包括如下重量份的组分：多元醇组合物20~35份、扩链剂0.1~1份、异氰酸酯3~9份、溶剂60~70份、封端剂0.02~0.04份。
2.根据权利要求1所述的一种用于碳化硅精抛的抛光材料，其特征在于：所述多元醇组合物包括聚四氢呋喃二醇和聚酯二元醇组成混合物。
3.根据权利要求2所述的一种用于碳化硅精抛的抛光材料，其特征在于：所述聚酯二元醇为二元酸和二元醇通过高温脱水缩聚而成的线性高分子聚合物，且分子链两端均为可与异氰酸酯反应的羟基；所述二元酸包括己二酸、丁二酸、分子量底于300的脂肪族或芳香族二元羧酸中的一种或多种；所述二元醇含有一个或多个侧链且有一个或多个侧链的碳链长度大于2。
4.根据权利要求3所述的一种用于碳化硅精抛的抛光材料，其特征在于：所述多元醇组合物还包括聚碳酸酯二元醇、聚己内酯二元醇、内酯
共聚物、聚酯二元醇中的一种或多种。
5.根据权利要求4所述的一种用于碳化硅精抛的抛光材料，其特征在于：所述聚四氢呋喃二醇和所述聚酯二元醇在所述多元醇组合物中的质量分数为30%-100%。
6.根据权利要求1所述的一种用于碳化硅精抛的抛光材料，其特征在于：所述扩链剂包括乙二醇、1,4 丁二醇、乙二胺中的一种或多种。
7.根据权利要求1所述的一种用于碳化硅精抛的抛光材料，其特征在于：所述聚氨酯树脂的原料还包括0.01~0.1重量份的助剂，所述助剂包括抗氧化剂、紫外光吸收剂、泡孔调节剂、改性硅油。
8.一种如权利要求1-7任意一项所述的用于碳化硅精抛的抛光材料的制备方法，其特征在于：包括以下步骤：
聚酯二元醇的合成：将二元酸和二元醇投入反应釜中，在氮气的保护下，先在90-100℃下搅拌，然后在150-160℃下恒温反应1.5-2.5h，再升温至220-230℃，开启真空，至物料的羟值为54-58mgKOH/g且酸值为0.1-0.5mgKOH/g，停止真空，降温至120℃出料，得到聚酯二元醇；
聚氨酯树脂的合成：将部分溶剂和部分多元醇组合物加入反应釜中搅拌均匀，在25-35℃下,加入部分异氰酸酯，升高温度至65-75℃，加入部分溶剂、剩下的多元醇组合物、扩链剂，降温至45-55℃，搅拌均匀后加入剩下的异氰酸酯，在75-85℃下反应至反应物的粘度为150000cps/25℃，接着加入剩下的溶剂、封端剂，在70-80℃下搅拌反应0.5-1.5h，最后加入助剂继续搅拌反应0.5-1.5h，冷却出料，得到聚氨酯树脂；
复合：将聚氨酯树脂、溶剂、表面活性剂、色料搅拌混合均匀后过滤真空脱泡涂布在载体上，然后放入水中凝固、清洗、烘干、切片、打磨，在载体上形成聚氨酯涂层，得到聚氨酯材料；在聚对苯二甲酸乙二酯薄膜上涂布热熔胶，然后复合在聚氨酯材料上，得到抛光材料。
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