CN116903391A - 一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法 - Google Patents
一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法 Download PDFInfo
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Abstract
一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,超硬材料制备技术领域,包括以下步骤:S1:将超硬磨料、辅助磨料、陶瓷结合剂粉体、硅溶胶、分散剂及去离子水混合,制得混合浆料;S2:向混合浆料中加入发泡剂并搅拌均匀,制得泡沫浆料;S3:向泡沫浆料中边搅拌边加入促凝剂,再将加有促凝剂的泡沫浆料注入模具中固化成型,得到生胚;S4:将生胚依次在温度为25~65℃、湿度为55~85%的条件下一级干燥,在温度为65~110℃的条件下二级干燥,再烧成处理即得到陶瓷结合剂超硬材料。本发明用于制备出成型密度分布均匀、显微结构均匀的陶瓷结合剂超硬材料。
Description
技术领域
本发明涉及超硬材料制备技术领域,具体的说是一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法。
背景技术
陶瓷结合剂超硬材料具有磨削能力强,加工精度高,磨具损耗小,使用寿命长等特点。目前,超硬材料制品已广泛应用于机械加工、装备制造等多个行业。随着现代制造技术的发展,超硬材料制品的应用领域越来越宽,已拓展到汽车行业、半导体行业、轴承行业、航空航天等高技术领域。
成型工艺是制备高性能陶瓷结合剂超硬材料的关键工艺之一。通过改善成型工艺获得显微结构均匀的坯体是改善超硬材料制品性能的有效途径。目前,制备陶瓷结合剂超硬材料主要以机压成型为主,机压成型工艺存在模具设计复杂,成型密度分布不均匀等问题,密度分布不均则易造成加工工件表面磨削品质不一致,甚至烧伤等一系列问题;凝胶注膜工艺制备的坯体强度高,但是其使用的酰胺类有机单体具有毒性,对人体健康和环境不利,且排胶工艺复杂,烧结收缩大,容易导致制品开裂。如公开号为CN111331527A的中国专利公布了一种超高气孔率陶瓷结合剂金刚石超精磨及其制备方法,其所使用的即为甲基丙烯酰胺有机单体。
陶瓷结合剂超硬材料中的气孔在磨削过程中具有容削、排削、散热、冷却的作用。生产过程中,为了调整陶瓷结合剂砂轮中所形成的气孔大小以及气孔量的多少,传统方式一般采用在砂轮中添加木粉、萘粒和塑料球等来达到形成气孔的目的。目前陶瓷结合剂超硬材料制备方法以添加固态造孔剂法如石墨,萘粒,木粉,淀粉、塑料球等有机物结合机压成型为主。采用该方法制备的制品,在压制成型后由于造孔剂的塑性回弹,易造成坯体开裂或产生肉眼不可见的微裂纹,影响产品的质量。同时,在烧成过程中会对环境造成污染。
发明内容
本发明旨在提供一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,以制备出成型密度分布均匀、显微结构均匀的陶瓷结合剂超硬材料。
为了解决以上技术问题,本发明采用的具体方案为:一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,包括以下步骤:
S1:将超硬磨料、辅助磨料、陶瓷结合剂粉体、硅溶胶、分散剂及去离子水混合,制得混合浆料;
S2:向混合浆料中加入发泡剂并搅拌均匀,制得泡沫浆料;
S3:向泡沫浆料中边搅拌边加入促凝剂,再将加有促凝剂的泡沫浆料注入模具中固化成型,得到生胚;
S4:将生胚依次在温度为25~65℃、湿度为55~85%的条件下一级干燥,在温度为65~110℃的条件下二级干燥,再烧成处理即得到陶瓷结合剂超硬材料。
作为上述技术方案的进一步优化,步骤S1具体为:首先将超硬磨料、陶瓷结合剂粉体以及辅助磨料混和,再加入硅溶胶、分散剂和去离子水,继续混合,加入氨水调节PH值,制得PH=9~10的混合浆料。
作为上述技术方案的进一步优化,所述的超硬磨料为立方氮化硼或金刚石。
作为上述技术方案的进一步优化,所述陶瓷结合剂粉体由以下重量百分比的原料组成:SiO2 50~60%、B2O3 10~15%、Na2O1~5%、K2O 1~5%以及TiO2 1~5%。
作为上述技术方案的进一步优化,所述辅助磨料为碳化硅、刚玉和微晶刚玉中的一种或两种。
作为上述技术方案的进一步优化,所述硅溶胶为钠离子稳定型碱性硅溶胶,其二氧化硅浓度为20~40%。
作为上述技术方案的进一步优化,所述发泡剂为十二烷基硫酸钠、十二烷基笨磺酸钠和十二烷基三乙醇胺中的一种或多种。
作为上述技术方案的进一步优化,所述促凝剂为NH4Cl溶液或柠檬酸溶液。
作为上述技术方案的进一步优化,步骤S4中,一级干燥的持续时间为24~48h;二级干燥的持续时间为20~48h。
作为上述技术方案的进一步优化,步骤S4中,烧成温度为670~880℃。
与现有技术相比,本发明的有益效果如下:
1、通过本发明制备方法成型的坯体,不需要复杂的模具,成型密度分布均匀,可获得显微结构均匀的坯体,可解决由于超硬材料密度分布不均造成的加工工件表面磨削品质不一致,甚至烧伤等一系列问题。
2、利用无机溶胶的胶凝化反应实现泡沫浆体的快速固化,坯体干燥后收缩小,制品不易开裂。同时烧成过程中无需排胶,成孔或造孔剂不会释放其它有害物质,不会对环境造成污染。
3、将胶凝化反应实现泡沫浆体的快速固化与本发明的两段干燥(包括一级干燥和二级干燥)相结合,在一级干燥中设定适当的温度和湿度,一级干燥为低温干燥,防止水分蒸发过快导致制品开裂,二级干燥可以将游离水水分排除干净,防止烧成升温过程中水分气化,内部蒸气压过高,导致制品开裂。
4、通过硅溶胶引入的二氧化硅纳米粒子活性高,分散均匀,是陶瓷结合剂组成的一部分,不污染陶瓷结合剂。
附图说明
图1为实施例1中陶瓷结合剂超硬材料的显微结构图;
图2为实施例2中陶瓷结合剂超硬材料的显微结构图;
图3为实施例3中陶瓷结合剂超硬材料的显微结构图;
具体实施方式
下面对本发明的技术方案做进一步的详细阐述,本发明以下实施例中未详细记载和公开的部分,均应理解为本领域技术人员所知晓或应当知晓的现有技术。
本发明公开了一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,包括以下步骤:
S1:将超硬磨料、辅助磨料、陶瓷结合剂粉体、硅溶胶及去离子水混合,制得混合浆料;
S101:将超硬磨料、陶瓷结合剂粉体、辅助磨料进行配料,在三维混料机中进行混料1h,制得混合粉料;
所述的超硬磨料为立方氮化硼或金刚石;
所述的辅助磨料为碳化硅,刚玉或微晶刚玉等其中的一种或两种;
所述的陶瓷结合剂粉体的粒径不大于44μm,陶瓷结合剂粉体的主要成份见表1。
表1陶瓷结合剂的化学成分(wt%)
SiO2 | Al2O3 | B2O3 | Na2O | K2O | TiO2 |
50~60% | 10~20% | 10~15% | 1~5% | 1~5% | 1~5% |
S102:将硅溶胶、去离子水、分散剂加入混合粉料中,继续混合,加入氨水调节物料的PH值,得到为PH=9~10的混合浆料;
所述的硅溶胶为铵离子稳定型或钠离子稳定型碱性硅溶胶,其二氧化硅浓度为20~40%;
S2:向混合浆料中加入发泡剂,搅拌,制得泡沫浆料;
所述的发泡剂为十二烷基硫酸钠、十二烷基笨磺酸钠、十二烷基三乙醇胺中的一种或任意几种以任意质量比的混合物;
S3:向泡沫浆料中边搅拌边加入促凝剂,再将加入促凝剂的泡沫浆料注入模具中固化成型,得到生胚。所述的促凝剂为NH4Cl或者柠檬酸;控制NH4Cl或者柠檬酸的加入量,使泡沫浆料中NH4Cl或者柠檬酸的浓度为0.08~0.12mol/L。将加入促凝集后并搅拌均匀的泡沫浆料注入模具,使泡沫浆料快速固化成型得到生胚;
S4:将生胚经干燥、烧成后即得到陶瓷结合剂超硬材料。具体的干燥过程为:生胚首先在恒温恒湿箱中进行一级干燥,温度控制在25~65℃,相对湿度控制在55~85%,持续时间为24~48h;然后再转移至电热鼓风干燥箱中进行二级干燥,二级干燥的温度控制在65~110℃,持续时间为20~48h。
将干燥后的生胚在温度为670~880℃的条件下烧成处理,即制得陶瓷结合剂超硬材料。
本发明采用的是溶胶-凝胶成型工艺与发泡法结合的方式,其原理是利用硅溶胶的凝胶化反应实现泡沫浆料的快速固化成型。利用无机溶胶的胶凝化反应实现超硬材料泡沫浆体的快速固化,坯体干燥后收缩小,制品不易开裂,同时烧成过程中无需排胶,成孔或造孔剂不会释放其它有害物质,不会对环境造成污染。
下面结合附图及具体的实施例对本发明的技术方案做进一步的详细阐述。
实施例1:
S1:将金刚石粉、陶瓷结合剂粉体和碳化硅粉混合配料(以下简称总粉体Ⅰ),金刚石粉、陶瓷结合剂粉体和碳化硅粉三种原料的加入量质量比为50:20:30,其中金刚石粉的粒度为W40,陶瓷结合剂粉体的平均粒径为20微米,碳化硅粉的粒度为W20。
将总粉体Ⅰ在三维混料机中混料1h,再加入总粉体Ⅰ质量5%的去离子水、总粉体Ⅰ质量0.1%的分散剂,分散剂为三聚磷酸钠、总粉体Ⅰ质量的15%的钠离子型硅溶胶(SiO2质量浓度为30wt%)。利用氨水调节浆料的PH值,继续混合20min,得到PH=9~10的混合浆料。
S2:将混合得到的混合浆料转移至搅拌桶中,加入总粉体Ⅰ质量0.1%的十二烷基苯磺酸钠,通过机械搅拌发泡得到泡沫浆料。
S3:在泡沫浆料中边搅拌边加入NH4Cl溶液,控制泡沫浆料中的NH4Cl的浓度为0.1mol/L,将搅拌均匀后的泡沫浆料注入模具,泡沫浆料快速固化成型,脱模得到生胚,其生坯为φ102mm,厚度5.5mm。
S4:将生胚先在恒温恒湿箱中一级干燥36h,温度和相对湿度分别控制在60℃和80%;后移入电热鼓风干燥箱中进行二级干燥,二级干燥为在温度105℃的条件下保温24h,干燥后的坯体放入电炉中以2℃的升温速率升至740℃并保温3h,烧成得到陶瓷结合剂超硬材料,记为陶瓷结合剂超硬材料Ⅰ。
所得陶瓷结合剂超硬材料Ⅰ抗折强度为45MPa,密度为1.85g/cm3,气孔率45%,气孔孔径为200~500μm。
所得陶瓷结合剂超硬材料Ⅰ样品的显微结构图见附图1。
实施例2:
S1:将立方氮化硼粉、陶瓷结合剂粉体和刚玉粉混合配料(以下简称总粉体II),三种原料的加入量之比为(60:20:20),其中立方氮化硼粉的粒度为325/400,陶瓷结合剂粉体的平均粒径为25微米,刚玉粉的粒度为W40。
将总粉体II在三维混料机中混料1h;再加入总粉体II质量0.2%的分散剂、总粉体II总质量15%的钠离子型硅溶胶(SiO2质量浓度为30wt%),通过氨水调节浆料的PH值,继续混料20min,得到PH=9~10的混合浆料。
S2:将混合得到的浆料转移至搅拌桶中,加入总粉体II质量0.02wt%的十二烷基苯磺酸钠,通过机械搅拌发泡得到泡沫浆料,
S3:在泡沫浆料中边搅拌边加入NH4Cl溶液,控制泡沫浆料中的NH4Cl的浓度为0.1mol/L,搅拌均匀后的泡沫浆料注入模具,泡沫浆料快速固化成型,再进行脱模得到生胚。其生坯尺寸为φ150mm,厚度10mm。
S4:将生胚先在恒温恒湿箱中一级干燥48h,温度和相对湿度分别控制在55℃和85%;后移入电热鼓风干燥箱中二级干燥,二级干燥为在105℃的温度下保温36h;干燥后的坯体放入电炉中以2℃的升温速率升至880℃并保温3h,烧成得到陶瓷结合剂超硬材料,记为陶瓷结合剂超硬材料II。
所得陶瓷结合剂超硬材料II的抗折强度为70MPa,密度为2.05g/cm3,气孔孔径为200~600μm,气孔率为35%。
所得陶瓷结合剂超硬材料II样品的显微结构照片如图2。
实施例3:
S1:将金刚石微粉、陶瓷结合剂粉体和微晶刚玉粉混合配料(以下简称总粉体III),三种原料的加入量之比为(55:20:25),其中金刚石微粉的粒度为W10,陶瓷结合剂粉体的平均粒径为10微米,微晶刚玉粉的粒度W7。
将总粉体III在三维混料机中混料1h;再加入总粉体III质量0.2%的分散剂、总粉体III质量15%的钠离子型硅溶胶(SiO2质量浓度为30wt%),通过氨水调节浆料的PH值,继续混料20min,得到PH=9~10的混合浆料。
S2:将混合得到的混合浆料转移至搅拌桶中,加入总粉体III质量0.8%的十二烷基苯磺酸钠,通过机械搅拌发泡得到泡沫浆料。
S3:在泡沫浆料中边搅拌边加入NH4Cl溶液。控制泡沫浆料中的NH4Cl的浓度为0.1mol/L,将搅拌均匀后的泡沫浆料注入模具,泡沫浆料快速固化成型,脱模后得到生胚。生坯直径为102mm,厚度为5mm
S4:将生胚先在恒温恒湿箱中一级干燥36h,温度和相对湿度分别控制在60℃和80%;后移入电热鼓风干燥箱中进行二级干燥,二级干燥为在105℃的温度下保温24h。干燥后的坯体放入电炉中以2℃的升温速率升至880℃并保温3h,烧成得到陶瓷结合剂超硬材料,记为陶瓷结合剂超硬材料III。
所得陶瓷结合剂超硬材料III抗折强度为28MPa,气孔孔径为200~500μm,密度为1.54g/cm3,气孔率为60%。所得陶瓷结合剂超硬材料III样品的显微结构照片如图3所示。
本发明中利用无机溶胶的胶凝化反应实现泡沫浆体的快速固化,坯体干燥后收缩小,制品不易开裂。同时烧成过程中无需排胶,成孔或造孔剂不会释放其它有害物质,不会对环境造成污染。同时将胶凝化反应实现泡沫浆体的快速固化与本发明的一级干燥和二级干燥相结合的两段干燥,一级干燥为低温干燥,防止水分蒸发过快导致制品开裂,二级干燥可以将游离水水分排除干净,防止烧成升温过程中水分气化,内部蒸气压过高,导致制品开裂。本发明通过硅溶胶引入的二氧化硅纳米粒子活性高,分散均匀,是陶瓷结合剂组成的一部分,不污染陶瓷结合剂。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,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。
Claims (10)
1.一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,其特征在于:包括以下步骤:
S1:将超硬磨料、辅助磨料、陶瓷结合剂粉体、硅溶胶、分散剂及去离子水混合,制得混合浆料;
S2:向混合浆料中加入发泡剂并搅拌均匀,制得泡沫浆料;
S3:向泡沫浆料中边搅拌边加入促凝剂,再将加有促凝剂的泡沫浆料注入模具中固化成型,得到生胚;
S4:将生胚依次在温度为25~65℃、湿度为55~85%的条件下一级干燥,在温度为65~110℃的条件下二级干燥,再烧成处理即得到陶瓷结合剂超硬材料。
2.根据权利要求1所述的一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,其特征在于:步骤S1具体为:首先将超硬磨料、陶瓷结合剂粉体以及辅助磨料混和,再加入硅溶胶、分散剂和去离子水,继续混合,加入氨水调节PH值,制得PH=9~10的混合浆料。
3.根据权利要求1所述的一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,其特征在于:所述的超硬磨料为立方氮化硼或金刚石。
4.根据权利要求1所述的一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,其特征在于:所述陶瓷结合剂粉体由以下重量百分比的原料组成:SiO250~60%、B2O310~15%、Na2O1~5%、K2O1~5%以及TiO21~5%。
5.根据权利要求1所述的一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,其特征在于:所述辅助磨料为碳化硅、刚玉和微晶刚玉中的一种或两种。
6.根据权利要求1所述的一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,其特征在于:所述硅溶胶为钠离子稳定型碱性硅溶胶,其二氧化硅浓度为20~40%。
7.根据权利要求1所述的一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,其特征在于:所述发泡剂为十二烷基硫酸钠、十二烷基笨磺酸钠和十二烷基三乙醇胺中的一种或多种。
8.根据权利要求1所述的一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,其特征在于:所述促凝剂为NH4Cl溶液或柠檬酸溶液。
9.根据权利要求1所述的一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,其特征在于:步骤S4中,一级干燥的持续时间为24~48h;二级干燥的持续时间为20~48h。
10.根据权利要求1所述的一种基于溶胶结合发泡法制备陶瓷结合剂超硬材料的方法,其特征在于:步骤S4中,烧成温度为670~880℃。
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