CN114717443B - 一种低温卷烟用发热体材料及其制备方法和应用 - Google Patents
一种低温卷烟用发热体材料及其制备方法和应用 Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 41
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000919 ceramic Substances 0.000 claims abstract description 35
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000000498 ball milling Methods 0.000 claims description 35
- 239000004088 foaming agent Substances 0.000 claims description 28
- 238000002844 melting Methods 0.000 claims description 26
- 230000008018 melting Effects 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 26
- 238000002791 soaking Methods 0.000 claims description 25
- 238000000748 compression moulding Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 18
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- 238000007598 dipping method Methods 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 5
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 5
- 239000001099 ammonium carbonate Substances 0.000 claims description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 238000000227 grinding Methods 0.000 description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 239000002253 acid Substances 0.000 description 8
- 239000003344 environmental pollutant Substances 0.000 description 8
- 239000011812 mixed powder Substances 0.000 description 8
- 231100000719 pollutant Toxicity 0.000 description 8
- 239000000523 sample Substances 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 238000004506 ultrasonic cleaning Methods 0.000 description 8
- 238000001291 vacuum drying Methods 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 230000006835 compression Effects 0.000 description 7
- 238000007906 compression Methods 0.000 description 7
- 238000007873 sieving Methods 0.000 description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 3
- 241000208125 Nicotiana Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
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- 238000000889 atomisation Methods 0.000 description 1
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- 230000001276 controlling effect Effects 0.000 description 1
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- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 235000019505 tobacco product Nutrition 0.000 description 1
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Abstract
本发明提供了一种低温卷烟用发热体材料及其制备方法和应用,发热体材料的制备原料包括绝缘陶瓷和金属;所述金属和绝缘陶瓷的质量比为4:1~1:4。本发明提供的发热体材料具有低温卷烟器具所需的电阻率,且阻值可进行调控,有利于提高加热效果;其可整体加热,有利于提高热效率;其制备工艺简单,成本较低。实验结果表明:电阻率为572~2301μΩ·cm;强度为321~864MPa。
Description
技术领域
本发明属于烟草制品技术领域,尤其涉及一种低温卷烟用发热体材料及其制备方法和应用。
背景技术
目前市场上应用于烟草加热不燃烧的发热器件主要包括电阻加热及电磁感应加热,其中以电阻加热的应用较为广泛。其中电阻加热元件主要为MCH陶瓷。虽然能够有效对低温卷烟中雾化基质进行加热雾化,但仍存在较多问题。如制备工艺复杂、成本较高,产品质量波动较大等问题,另一方面,由于发热金属被氧化铝陶瓷包裹,因此不能对烟草薄片直接加热,很大程度降低了加热效率,且印刷线路也导致了加热区间的不均匀性。因此急需开发一种低成本、工艺简单、可靠性高及可控性强的新型发热材料。
发明内容
有鉴于此,本发明的目的在于提供一种低温卷烟用发热体材料及其制备方法和应用,该发热体材料具有合适的电阻率,且力学性能优异。
本发明提供了一种低温卷烟用发热体材料,制备原料包括绝缘陶瓷和金属;
所述金属与绝缘陶瓷的质量比为4:1~1:4。
在本发明中,所述绝缘陶瓷选自Al2O3、ZrO2、SiC和B3N4中的一种或多种。
在本发明中,所述金属选自V、Cr、Mn、Fe、Co、Ni和Cu中的一种或多种。所述金属的熔点不高于2000℃。
在本发明中,所述制备原料还包括发泡剂;
所述发泡剂占绝缘陶瓷体积的10~25%;
所述发泡剂选自碳酸氢铵、碳酸钙和十二烷基磺酸钠中的一种或多种。
在本发明中,所述发热体材料的电阻率为500~6000μΩ·cm,抗弯强度为300~1000MPa。
本发明提供了一种上述技术方案所述发热体材料的制备方法,包括以下步骤:
将绝缘陶瓷粉末和发泡剂清洗后球磨,干燥,模压成型,得到压坯;
将所述压坯和金属混合后进行熔浸处理,抛光,得到发热体材料。
在本发明中,所述熔浸处理的温度为1200~2000℃,时间为1~10h,真空度≥1Pa。
本发明优选对绝缘陶瓷粉末和发泡剂进行酸洗和超声波清洗,以去除表面的氧化膜及污染物。在本发明中,所述发泡剂优选自碳酸氢铵、碳酸钙和十二烷基磺酸钠中的一种或多种。所述发泡剂占绝缘陶瓷粉末体积的10~25%。本发明通过控制发泡剂的用量控制孔隙的体积分数,从而控制渗入金属数量,实现对电阻率的控制。具体实施例中,所述发泡剂占绝缘陶瓷粉末体积的10%、25%、15%、或20%。发泡剂在熔浸过程中烧损或分解。
在本发明中,球磨时的球料比为(5:1)~(10:1);球磨的转速为200~500rpm;球磨的介质为高纯乙醇,球磨的时间为2~12h。
本发明优选将球磨后的混合粉末在真空干燥箱中烘干;烘干的温度为60~120℃。具体实施例中,烘干的温度为60℃、80℃、90℃、或120℃。
在本发明中,模压成型的压力为200~400MPa,模压成型的时间为30~120s。具体实施例中,模压成型的压力为200MPa、或400MPa、或300MPa、或;时间为30s、或120s、或60s。
本发明优选将压坯和金属放入陶瓷坩埚内再进行熔浸处理;所述压坯和金属的质量比为6:4、或7:3、或1:1、或1:4。
本发明优选在真空烧结炉中进行熔浸处理;所述熔浸处理的温度为1200~2000℃,时间为1~10h,真空度≥1Pa。具体实施例中,所述熔浸处理的温度为1200℃、或2000℃、或1800℃、或1600℃;时间为1h、或10h、或8h;真空度为1Pa、或2Pa、或3Pa。
本发明提供了一种上述技术方案所述发热体材料或上述技术方案所述制备方法制备的发热体材料在制备低温卷烟发热体元件中的应用。
对于发热体元件而言,合适的电阻值,大概在0.5~1.5Ω之间,优选0.8Ω左右。不同尺寸的元件所需的合适电阻率是不一样的。一般而言,合适的电阻率为2000μΩ·cm左右,强度不能低于300MPa。
本发明提供了一种低温卷烟用发热体材料,制备原料包括绝缘陶瓷和金属;所述金属与绝缘陶瓷的质量比为4:1~1:4。本发明通过绝缘陶瓷和金属的科学配比及组织优化,获得电阻率合适的导电复合材料,可用于低温卷烟发热体元件制备,同时熔浸工艺实施简便,成本较低。
具体实施方式
为了进一步说明本发明,下面结合实施例对本发明提供的一种低温卷烟用发热体材料及其制备方法和应用进行详细地描述,但不能将它们理解为对本发明保护范围的限定。
实施例1
1)清洗;将氧化铝陶瓷粉末及碳酸氢铵发泡剂进行酸洗及超声波清洗,以去除表面氧化膜及污染物,其中发泡剂体积分数为10%;
2)混料:将上述粉末放入球磨罐中进行混料。采用的球料比为5:1,转速为200rpm,球磨介质为高纯乙醇,球磨时间2h;
3)干燥:将球磨后的混合粉末与在真空干燥箱中烘干,温度为60℃;
4)模压成形:将干燥后的粉料过筛后进行模压成型,压制压力为200MPa,保压时间为30s;
5)熔浸:将上述压坯与Al片按质量比1:4放入陶瓷坩埚内,在真空烧结炉中进行熔浸处理,熔浸温度1200℃,熔浸时间1h,真空度为1Pa。
6)研磨抛光:将熔浸后的样品在研磨机上进行研磨抛光,提高表面质量。所获发热体材料性能如表1所示。
实施例2
1)清洗;将氧化锆陶瓷粉末及碳酸钙发泡剂进行酸洗及超声波清洗,以去除表面氧化膜及污染物,其中发泡剂体积分数为25%;
2)混料:将上述粉末放入球磨罐中进行混料。采用的球料比为7:1,转速为500rpm,球磨介质为高纯乙醇,球磨时间12h;
3)干燥:将球磨后的混合粉末与在真空干燥箱中烘干,温度为120℃;
4)模压成形:将干燥后的粉料过筛后进行模压成型,压制压力为400MPa,保压时间为120s;
5)熔浸:将上述压坯与镍片按质量比1:1放入陶瓷坩埚内,在真空烧结炉中进行熔浸处理,熔浸温度2000℃,熔浸时间10h,真空度为2Pa。
6)研磨抛光:将熔浸后的样品在研磨机上进行研磨抛光,提高表面质量。所获发热体材料性能如表1所示。
实施例3
1)清洗;将氧化锆陶瓷粉末及碳酸钙发泡剂进行酸洗及超声波清洗,以去除表面氧化膜及污染物,其中发泡剂体积分数为15%;
2)混料:将上述粉末放入球磨罐中进行混料。采用的球料比为7:1,转速为350rpm,球磨介质为高纯乙醇,球磨时间5h;
3)干燥:将球磨后的混合粉末与在真空干燥箱中烘干,温度为80℃;
4)模压成形:将干燥后的粉料过筛后进行模压成型,压制压力为300MPa,保压时间为60s;
5)熔浸:将上述压坯与Ni50Cr50(质量分数)合金丝按质量比7:3放入陶瓷坩埚内,在真空烧结炉中进行熔浸处理,熔浸温度1800℃,熔浸时间8h,真空度为3Pa。
6)研磨抛光:将熔浸后的样品在研磨机上进行研磨抛光,提高表面质量。所获发热体材料性能如表1所示。
实施例4
1)清洗;将氮化硅陶瓷粉末及十二烷基磺酸钠发泡剂进行酸洗及超声波清洗,以去除表面氧化膜及污染物,其中发泡剂体积分数为20%;
2)混料:将上述粉末放入球磨罐中进行混料。采用的球料比为6:1,转速为250rpm,球磨介质为高纯乙醇,球磨时间12h;
3)干燥:将球磨后的混合粉末与在真空干燥箱中烘干,温度为90℃;
4)模压成形:将干燥后的粉料过筛后进行模压成型,压制压力为300MPa,保压时间为120s;
5)熔浸:将上述压坯与镍片按质量比6:4放入陶瓷坩埚内,在真空烧结炉中进行熔浸处理,熔浸温度1600℃,熔浸时间10h,真空度为2Pa。
6)研磨抛光:将熔浸后的样品在研磨机上进行研磨抛光,提高表面质量。所获发热体材料性能如表1所示。
实施例5
1)清洗;将氮化硅陶瓷粉末及碳酸氢铵与碳酸钙混合发泡剂进行酸洗及超声波清洗,以去除表面氧化膜及污染物,其中两类发泡剂体积比为1:1,总体积分数为20%;
2)混料:将上述粉末放入球磨罐中进行混料。采用的球料比为6:1,转速为250rpm,球磨介质为高纯乙醇,球磨时间12h;
3)干燥:将球磨后的混合粉末与在真空干燥箱中烘干,温度为90℃;
4)模压成形:将干燥后的粉料过筛后进行模压成型,压制压力为300MPa,保压时间为120s;
5)熔浸:将上述压坯与镍片按质量比6:4放入陶瓷坩埚内,在真空烧结炉中进行熔浸处理,熔浸温度1600℃,熔浸时间10h,真空度为2Pa。
6)研磨抛光:将熔浸后的样品在研磨机上进行研磨抛光,提高表面质量。
所获发热体材料性能如表1所示。
对比例1
1)清洗;将氮化硅陶瓷粉末及十二烷基磺酸钠发泡剂进行酸洗及超声波清洗,以去除表面氧化膜及污染物,其中发泡剂体积分数为9%;
2)混料:将上述粉末放入球磨罐中进行混料。采用的球料比为6:1,转速为250rpm,球磨介质为高纯乙醇,球磨时间12h;
3)干燥:将球磨后的混合粉末与在真空干燥箱中烘干,温度为90℃;
4)模压成形:将干燥后的粉料过筛后进行模压成型,压制压力为300MPa,保压时间为120s;
5)熔浸:将上述压坯与镍片按质量比6:4放入陶瓷坩埚内,在真空烧结炉中进行熔浸处理,熔浸温度1600℃,熔浸时间10h,真空度为2Pa。
6)研磨抛光:将熔浸后的样品在研磨机上进行研磨抛光,提高表面质量。所获发热体材料性能如表1所示。
对比例2
1)清洗;将氧化锆陶瓷粉末及碳酸钙发泡剂进行酸洗及超声波清洗,以去除表面氧化膜及污染物,其中发泡剂体积分数为30%;
2)混料:将上述粉末放入球磨罐中进行混料。采用的球料比为7:1,转速为500rpm,球磨介质为高纯乙醇,球磨时间12h;
3)干燥:将球磨后的混合粉末与在真空干燥箱中烘干,温度为120℃;
4)模压成形:将干燥后的粉料过筛后进行模压成型,压制压力为400MPa,保压时间为120s;
5)熔浸:将上述压坯与镍片按质量比1:1放入陶瓷坩埚内,在真空烧结炉中进行熔浸处理,熔浸温度2000℃,熔浸时间10h,真空度为2Pa。
6)研磨抛光:将熔浸后的样品在研磨机上进行研磨抛光,提高表面质量。所获发热体材料性能如表1所示。
本发明所述电磁加热材料的电阻率采用四探针电阻测试仪进行测试;抗弯强度通过三点抗弯强度仪进行测试。
表1实施例1~5和对比例1~2制备的材料的性能测试结果
电阻率/μΩ■cm | 强度/MPa | |
实施例1 | 2301 | 321 |
实施例2 | 572 | 864 |
实施例3 | 1284 | 475 |
实施例4 | 903 | 530 |
实施例5 | 832 | 677 |
对比例1 | 3112 | 267 |
对比例2 | 431 | 874 |
由以上实施例可知,本发明提供了一种低温卷烟用发热体材料,制备原料包括绝缘陶瓷和金属;所述金属与绝缘陶瓷的质量比为4:1~1:4。本发明提供的发热体材料具有低温卷烟器具所需的电阻率,且阻值可进行调控,有利于提高加热效果;其可整体加热,有利于提高热效率;其制备工艺简单,成本较低。实验结果表明:电阻率为572~2301μΩ■cm;强度为321~864MPa。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (3)
1.一种低温卷烟用发热体材料的制备方法,其特征在于,包括以下步骤:
将绝缘陶瓷粉末和发泡剂清洗后球磨,干燥,模压成型,得到压坯;
将所述压坯和金属混合后进行熔浸处理,抛光,得到发热体材料;所述熔浸处理的温度为1200~2000℃,时间为1~10h,真空度≥1Pa;
所述低温卷烟用发热体材料,制备原料包括绝缘陶瓷和金属;
所述金属与绝缘陶瓷的质量比为4:1~1:4;
所述制备原料还包括发泡剂;所述发泡剂占绝缘陶瓷体积的10~25%;所述发泡剂选自碳酸氢铵、碳酸钙和十二烷基磺酸钠中的一种或多种;
所述绝缘陶瓷选自Al2O3、ZrO2、SiC和B3N4中的一种或多种;
所述金属选自V、Cr、Mn、Fe、Co、Ni和Cu中的一种或多种。
2.根据权利要求1所述的制备方法,其特征在于,所述发热体材料的电阻率为500~6000μΩ▪cm,抗弯强度为300~1000MPa。
3.一种权利要求1~2任一项所述制备方法制备的低温卷烟用发热体材料在制备低温卷烟发热体元件中的应用。
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