CN112592185A - 一种石墨烯增强碳化硅加热棒及其制备方法 - Google Patents
一种石墨烯增强碳化硅加热棒及其制备方法 Download PDFInfo
- Publication number
- CN112592185A CN112592185A CN202011267900.4A CN202011267900A CN112592185A CN 112592185 A CN112592185 A CN 112592185A CN 202011267900 A CN202011267900 A CN 202011267900A CN 112592185 A CN112592185 A CN 112592185A
- Authority
- CN
- China
- Prior art keywords
- graphene
- silicon carbide
- heating rod
- hot
- zone
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 59
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000010438 heat treatment Methods 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 90
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 89
- 239000011230 binding agent Substances 0.000 claims abstract description 28
- 239000004094 surface-active agent Substances 0.000 claims abstract description 28
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 25
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- 238000000576 coating method Methods 0.000 claims abstract description 17
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 40
- 239000000843 powder Substances 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000001694 spray drying Methods 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 6
- 239000000194 fatty acid Substances 0.000 claims description 6
- 229930195729 fatty acid Natural products 0.000 claims description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 3
- 239000004375 Dextrin Substances 0.000 claims description 3
- 229920001353 Dextrin Polymers 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 3
- 235000019425 dextrin Nutrition 0.000 claims description 3
- -1 fatty acid ester Chemical class 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 6
- 238000013021 overheating Methods 0.000 abstract description 2
- 238000005507 spraying Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000005313 fatty acid group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/6265—Thermal treatment of powders or mixtures thereof other than sintering involving reduction or oxidation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5001—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with carbon or carbonisable materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3821—Boron carbides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Metallurgy (AREA)
- Carbon And Carbon Compounds (AREA)
- Ceramic Products (AREA)
Abstract
本发明公开了一种石墨烯增强碳化硅加热棒及其制备方法，所述加热棒包括热区和冷区，所述冷区主要由以下质量百分比的原料制成：碳化硅72～93wt.％，氧化石墨烯4～13wt.％，碳化硼0.5～3wt.％，表面活性剂0.5～4wt.％，粘结剂2～8wt.％，各组分质量百分比之和为100％；所述热区主要由以下质量百分比的原料制成：碳化硅85～96wt.％，碳化硼0.5～3wt.％，表面活性剂0.5～4wt.％，粘结剂3～8wt.％，各组分质量百分比之和为100％，并且热区表面涂覆有浓度为0.1～4mg/L的石墨烯浆料，待烘干后，在其表面喷涂无机高温涂层。本发明将碳化硅、氧化石墨烯、碳化硼按特定比例混合、干燥、压制成形、真空条件下烧结制得石墨烯增强碳化硅加热棒。石墨烯的加入，有效的避免了加热棒出现局部过热、易断裂的现象，提高了加热棒的使用寿命。
Description
技术领域
本发明属于碳化硅加热棒技术领域，特别涉及一种石墨烯增强碳化硅加热棒及其制备方法。
背景技术
在晶体生长炉领域碳化硅加热棒是最普遍的电加热元件。常规的碳化硅加热元件主要由硅、碳等其它微量元素组成。碳化硅加热元件按其相对电流或电阻的大小分为热区和冷区两个部分。热区的电阻相对较高，冷区的电阻相对较低，冷区与导线、电源相连，当电流通过加热元件时，热区产生大部分的热量，冷区产生较少的热量。但是目前硅碳棒在使用过程中存在着热区发热不均匀、冷区电阻过大、易碎、使用寿命短等缺点。
发明内容
发明目的：针对现有硅碳棒热区发热不均，冷区电阻过大的问题，本发明提供了石墨烯增强碳化硅加热棒及其制备方法，解决了冷区产生热量多和热区发热不均的问题，增加了其使用寿命。
技术方案：为达到上述发明目的，本发明采用如下技术方案：
一种石墨烯增强碳化硅加热棒，所述加热棒包括热区和冷区，所述冷区主要由以下质量百分比的原料制成：碳化硅72～93wt.％，氧化石墨烯4～13wt.％，碳化硼0.5～3wt.％，表面活性剂0.5～4wt.％，粘结剂2～8wt.％，各组分质量百分比之和为100％；所述热区主要由以下质量百分比的原料制成：碳化硅85～96wt.％，碳化硼0.5～3wt.％，表面活性剂0.5～4wt.％，粘结剂3～8wt.％，各组分质量百分比之和为100％，热区表面涂覆有浓度为0.1～4mg/L的石墨烯浆料；为了使其性能更优异，热区表面涂覆的石墨烯浆料烘干后，再在其表面喷涂无机耐高温涂层。
作为优选：
所述氧化石墨烯和石墨烯的制备方法选自Hummers法、Staudenmaier法或Brodie法中的一种。
所述表面活性剂选自脂肪酸、脂肪酸酯、聚醚中的一种或几种。
所述粘结剂选自淀粉、糊精、聚乙烯醇、羧甲基纤维素中的一种或几种。
所述冷区和热区一体成形，热区位于两段冷区中间，冷区的直径略小于热区直径.
所述的石墨烯增强碳化硅加热棒的制备方法，包括以下步骤：
(1)冷区材料制作：将碳化硅、碳化硼、表面活性剂加入到氧化石墨烯水溶液中搅拌均匀，再加入粘结剂继续搅拌均匀；将所得溶液喷雾干燥，然后置于氩气中将氧化石墨烯还原成石墨烯，得到含有石墨烯的冷区材料粉体；
(2)热区材料制作：将碳化硅、碳化硼、表面活性剂和粘结剂在水溶液中搅拌均匀，将所得溶液喷雾干燥，制得热区材料粉体；
(3)将冷区材料粉体和热区材料粉体一体成形，将坯体进行真空烧结，取出，将石墨烯浆料涂覆于热区材料表面，烘干，即得；为了使其性能更优异，热区表面涂覆的石墨烯浆料烘干后，再在其表面喷涂无机耐高温涂层。
优选，步骤(1)中，所述还原的温度为200～300℃。
优选，步骤(3)中，所述真空烧结，是在2000～2300℃下烧结2～5小时。
石墨烯是一种由单层碳原子紧密堆积成二维蜂窝状结构的碳材料，因具有独特的晶体和电子能带结构而拥有非常优异的力学、热学、光学、电学及化学性质，如超高的载流子迁移率、超大的比表面积、完美的量子隧道效应等。因此，本发明主要是在冷区材料中加入了氧化石墨烯浆料，由于氧化石墨烯具有超高的比表面积，在制备过程中有助于碳化硅等原料的均匀分散。通过高温将氧化石墨烯还原成石墨烯，由于石墨烯具有较高的导电性，可以大幅降低冷区材料的电阻，并且产生较少的热量。本发明采用高导热石墨烯涂层，可以有效防止热区产生局部过热，使硅碳棒受热更加均匀，增加了硅碳棒的使用寿命。无机耐高温涂料，具有附着力非常好，坚硬，不开裂，不起泡，耐1500℃高温，可以很好的隔绝空气，防止石墨烯被高温氧化。
有益效果：本发明通过液相合成的方法，引入了具有高比表面积的氧化石墨烯溶液作为分散剂，其加入可以使得碳化硅、碳化硼、表面活性剂、粘结剂等吸附在氧化石墨烯的表面，使其混合均匀，通过喷雾干燥的方法，得到含有氧化石墨烯的冷区粉体材料，通过氩气中高温煅烧的方法将氧化石墨烯还原成石墨烯，得到含有石墨烯的冷区材料。在热区表面涂覆一层石墨烯，增强了热区材料导热的均匀性。此种方法有利于解决硅碳棒热区发热不均，冷区电阻过大的问题，增加硅碳棒的使用寿命。
附图说明
图1为本发明石墨烯增强碳化硅加热棒的结构示意图。
具体实施方式
下面结合具体实施例，对本发明的具体实施方式作进一步详细描述。以下实例用于说明本发明，但不用来限制本发明的范围。
以下实施例所制得的石墨烯增强碳化硅加热棒，其结构如图1所示，冷区①和热区②一体成形，热区②位于两段冷区①中间，冷区①导电率高、电阻小，热区导电率低、电阻大；热区②的表面涂覆一层石墨烯浆料③，增强热导率，在石墨烯膜表面喷涂耐高温涂层④，防止石墨烯高温氧化。冷区①的直径略小于热区②直径。实施例1：
冷区材料①制备：碳化硅93wt.％，氧化石墨烯4wt.％，碳化硼0.5wt.％，表面活性剂0.5wt.％，粘结剂2wt.％。热区材料②制备：碳化硅96wt.％，碳化硼0.5wt.％，表面活性剂0.5wt.％，粘结剂3wt.％。
所述氧化石墨烯和石墨烯采用Hummers法制备；所述表面活性剂选自脂肪酸；所述粘结剂选自淀粉。
将碳化硅碳化硼、表面活性剂、加入到氧化石墨烯水溶液中搅拌均匀，再向溶液中加入粘结剂继续搅拌均匀。将所得溶液进行喷雾干燥，制得含有氧化石墨烯的冷区材料粉体，将粉体材料置于氩气中，200℃将氧化石墨烯还原成石墨烯，制得含有石墨烯的冷区粉体。
将碳化硅碳化硼、表面活性剂、粘结剂在水溶液中搅拌均匀，将所得溶液进行喷雾干燥，制得热区材料粉体。冷区粉体和热区粉体一体成形，将坯体置于真空烧结炉中2000℃烧结5小时，再将浓度为0.1mg/L石墨烯溶液涂覆于热区材料表面，50℃烘干，得石墨烯增强碳化硅加热棒。再在其表面喷涂无机耐高温涂层。
使用该加热棒发现其发光均匀性有了很大的改善，使用寿命得到了极大的提升。详见下表：
实施例2：
冷区材料①制备：碳化硅72wt.％，氧化石墨烯13wt.％，碳化硼3wt.％，表面活性剂4wt.％，粘结剂8wt.％。热区材料②制备：碳化硅85wt.％，碳化硼3wt.％，表面活性剂4wt.％，粘结剂8wt.％。
所述氧化石墨烯和石墨烯采用Staudenmaier法制备；所述表面活性剂选自脂肪酸酯；所述粘结剂选自糊精。
将碳化硅碳化硼、表面活性剂、加入到氧化石墨烯水溶液中搅拌均匀，再向溶液中加入粘结剂继续搅拌均匀。将所得溶液进行喷雾干燥，制得含有氧化石墨烯的冷区材料粉体，将粉体材料置于氩气中，300℃将氧化石墨烯还原成石墨烯，制得含有石墨烯的冷区粉体。
将碳化硅碳化硼、表面活性剂、粘结剂在水溶液中搅拌均匀，将所得溶液进行喷雾干燥，制得热区材料粉体。冷区粉体和热区粉体一体成形，将坯体置于真空烧结炉中2300℃烧结2小时，再将浓度为4mg/L石墨烯溶液涂覆于热区材料表面，80℃烘干得石墨烯增强碳化硅加热棒，再在其表面喷涂无机耐高温涂层。
使用该加热棒发现其发光均匀性有了很大的改善，使用寿命得到了极大的提升。详见下表：
实施例3：
冷区材料①制备：碳化硅90wt.％，氧化石墨烯6wt.％，碳化硼1wt.％，表面活性剂1wt.％，粘结剂2wt.％。热区材料②制备：碳化硅90wt.％，碳化硼2wt.％，表面活性剂3wt.％，粘结剂5wt.％。
所述氧化石墨烯和石墨烯采用Brodie法制备；所述表面活性剂选自聚醚；所述粘结剂选自羧甲基纤维素。
将碳化硅碳化硼、表面活性剂、加入到氧化石墨烯水溶液中搅拌均匀，再向溶液中加入粘结剂继续搅拌均匀。将所得溶液进行喷雾干燥，制得含有氧化石墨烯的冷区材料粉体，将粉体材料置于氩气中，250℃将氧化石墨烯还原成石墨烯，制得含有石墨烯的冷区粉体。
将碳化硅碳化硼、表面活性剂、粘结剂在水溶液中搅拌均匀，将所得溶液进行喷雾干燥，制得热区材料粉体。冷区粉体和热区粉体一体成形，将坯体置于真空烧结炉中2100℃烧结3小时，再将浓度为2mg/L石墨烯溶液涂覆于热区材料表面，60℃烘干得石墨烯增强碳化硅加热棒，再在其表面喷涂无机耐高温涂层。
使用该加热棒发现其发光均匀性有了很大的改善，使用寿命得到了极大的提升。详见下表：
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (8)
1.一种石墨烯增强碳化硅加热棒，其特征在于，所述加热棒包括热区和冷区，所述冷区主要由以下质量百分比的原料制成：碳化硅72～93wt.％，氧化石墨烯4～13wt.％，碳化硼0.5～3wt.％，表面活性剂0.5～4wt.％，粘结剂2～8wt.％，各组分质量百分比之和为100％；所述热区主要由以下质量百分比的原料制成：碳化硅85～96wt.％，碳化硼0.5～3wt.％，表面活性剂0.5～4wt.％，粘结剂3～8wt.％，各组分质量百分比之和为100％，热区表面涂覆有浓度为0.1～4mg/L的石墨烯浆料。
2.根据权利要求1所述的石墨烯增强碳化硅加热棒，其特征在于，所述氧化石墨烯和石墨烯的制备方法选自Hummers法、Staudenmaier法或Brodie法中的一种。
3.根据权利要求1所述的石墨烯增强碳化硅加热棒，其特征在于，所述表面活性剂选自脂肪酸、脂肪酸酯、聚醚中的一种或几种。
4.根据权利要求1所述的石墨烯增强碳化硅加热棒，其特征在于，所述粘结剂选自淀粉、糊精、聚乙烯醇、羧甲基纤维素中的一种或几种。
5.根据权利要求1所述的石墨烯增强碳化硅加热棒，其特征在于，所述冷区和热区一体成形，热区位于两段冷区中间，冷区的直径略小于热区直径。
6.权利要求1-5任一项所述的石墨烯增强碳化硅加热棒的制备方法，其特征在于，包括以下步骤：
(1)冷区材料制作：将碳化硅、碳化硼、表面活性剂加入到氧化石墨烯水溶液中搅拌均匀，再加入粘结剂继续搅拌均匀；将所得溶液喷雾干燥，然后置于氩气中将氧化石墨烯还原成石墨烯，得到含有石墨烯的冷区材料粉体；
(2)热区材料制作：将碳化硅、碳化硼、表面活性剂和粘结剂在水溶液中搅拌均匀，将所得溶液喷雾干燥，制得热区材料粉体；
(3)将冷区材料粉体和热区材料粉体一体成形，将坯体进行真空烧结，取出，将石墨烯浆料涂覆于热区材料表面，烘干，即得。
7.根据权利要求6所述的石墨烯增强碳化硅加热棒的制备方法，其特征在于，步骤(1)中，所述还原的温度为200～300℃。
8.根据权利要求6所述的石墨烯增强碳化硅加热棒的制备方法，其特征在于，步骤(3)中，所述真空烧结，是在2000～2300℃下烧结2～5小时。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011267900.4A CN112592185A (zh) | 2020-11-13 | 2020-11-13 | 一种石墨烯增强碳化硅加热棒及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011267900.4A CN112592185A (zh) | 2020-11-13 | 2020-11-13 | 一种石墨烯增强碳化硅加热棒及其制备方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112592185A true CN112592185A (zh) | 2021-04-02 |
Family
ID=75182992
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011267900.4A Pending CN112592185A (zh) | 2020-11-13 | 2020-11-13 | 一种石墨烯增强碳化硅加热棒及其制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112592185A (zh) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3404202A (en) * | 1964-11-06 | 1968-10-01 | Basic Inc | Electric resistance heater and method of making |
| CN1397001A (zh) * | 2000-01-25 | 2003-02-12 | 圣戈本陶瓷及塑料股份有限公司 | 陶瓷点火器及其使用和制造方法 |
| US20060131295A1 (en) * | 2004-10-28 | 2006-06-22 | Saint-Gobain Corporation | Ceramic igniter |
| CN102067720A (zh) * | 2008-06-06 | 2011-05-18 | 山特维克材料技术英国有限公司 | 电阻加热元件 |
| CN104926312A (zh) * | 2015-06-29 | 2015-09-23 | 莱芜亚赛陶瓷技术有限公司 | 一种高热导率无压烧结碳化硅陶瓷材料及其制备方法 |
| CN107176838A (zh) * | 2017-06-20 | 2017-09-19 | 安徽省含山瓷业股份有限公司 | 一种石墨烯增强热导率的碳化硅陶瓷锅的制备方法 |
| CN108738170A (zh) * | 2018-05-24 | 2018-11-02 | 镇江东方电热科技股份有限公司 | 石墨烯纳米涂层ptc电加热器及其制造方法 |
| CN108821777A (zh) * | 2018-06-28 | 2018-11-16 | 浙江东新新材料科技有限公司 | 石墨烯/碳化硅复合陶瓷及其制备方法 |
| CN108911756A (zh) * | 2018-08-27 | 2018-11-30 | 宁波伏尔肯科技股份有限公司 | 一种电阻可调的碳化硅陶瓷及其制备方法 |
| CN111343735A (zh) * | 2020-03-06 | 2020-06-26 | 成都石墨烯应用产业技术研究院有限公司 | 一种石墨烯理疗发热板及多功能理疗取暖器 |
-
2020
- 2020-11-13 CN CN202011267900.4A patent/CN112592185A/zh active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3404202A (en) * | 1964-11-06 | 1968-10-01 | Basic Inc | Electric resistance heater and method of making |
| CN1397001A (zh) * | 2000-01-25 | 2003-02-12 | 圣戈本陶瓷及塑料股份有限公司 | 陶瓷点火器及其使用和制造方法 |
| US20060131295A1 (en) * | 2004-10-28 | 2006-06-22 | Saint-Gobain Corporation | Ceramic igniter |
| CN102067720A (zh) * | 2008-06-06 | 2011-05-18 | 山特维克材料技术英国有限公司 | 电阻加热元件 |
| CN104926312A (zh) * | 2015-06-29 | 2015-09-23 | 莱芜亚赛陶瓷技术有限公司 | 一种高热导率无压烧结碳化硅陶瓷材料及其制备方法 |
| CN107176838A (zh) * | 2017-06-20 | 2017-09-19 | 安徽省含山瓷业股份有限公司 | 一种石墨烯增强热导率的碳化硅陶瓷锅的制备方法 |
| CN108738170A (zh) * | 2018-05-24 | 2018-11-02 | 镇江东方电热科技股份有限公司 | 石墨烯纳米涂层ptc电加热器及其制造方法 |
| CN108821777A (zh) * | 2018-06-28 | 2018-11-16 | 浙江东新新材料科技有限公司 | 石墨烯/碳化硅复合陶瓷及其制备方法 |
| CN108911756A (zh) * | 2018-08-27 | 2018-11-30 | 宁波伏尔肯科技股份有限公司 | 一种电阻可调的碳化硅陶瓷及其制备方法 |
| CN111343735A (zh) * | 2020-03-06 | 2020-06-26 | 成都石墨烯应用产业技术研究院有限公司 | 一种石墨烯理疗发热板及多功能理疗取暖器 |
Non-Patent Citations (1)
| Title |
|---|
| 全苏科学技术情报研究所文摘编辑辑委员会: "《电工文摘 第6分册 电力拖动和电工艺》", 31 December 1964, 中国科学技术情报研究所重庆分所 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103096529B (zh) | 具有较高可靠性和安全性的氮化硅发热体的制作方法 | |
| CN106478105A (zh) | 一种多步反应烧结法制备低残硅的碳化硅陶瓷材料的方法 | |
| CN112011705A (zh) | 纳米碳增强铜基复合材料批量制备方法 | |
| CN101948315A (zh) | 一种高性能氮化铝陶瓷的低温烧结方法 | |
| CN105400982A (zh) | 通过氢化钛来制备石墨烯增强钛基纳米复合材料的方法 | |
| CN103934451B (zh) | 一种氧化铝弥散强化铜合金粉的制备方法 | |
| CN103096528B (zh) | 一种氮化硅发热体的制作方法 | |
| CN116496103B (zh) | 一种高强度、低密度碳化硅及其制备方法和应用 | |
| CN101891193B (zh) | 一种溶胶凝胶法制备纳米碳化钒 | |
| CN112592185A (zh) | 一种石墨烯增强碳化硅加热棒及其制备方法 | |
| CN110451498B (zh) | 一种石墨烯-氮化硼纳米片复合结构及其制备方法 | |
| CN112851334A (zh) | 一种基于氮化硅的加热体及其制备工艺 | |
| CN110423916B (zh) | 二氧化硅气凝胶负载铜基复合材料及其制备方法 | |
| CN110172606A (zh) | 一种氧化铝弥散强化铜合金管的制备工艺 | |
| CN107619265A (zh) | 一种降低99氧化铝陶瓷烧结温度的方法 | |
| CN102226298B (zh) | 一种金属氧化物纳米线的制备方法 | |
| CN113636833B (zh) | 一种氧化铬陶瓷材料及其制备方法以及一种氧化铬陶瓷材料烧结用保温装置 | |
| CN111847458B (zh) | 一种高纯度、低成本二硅化钼的制备方法 | |
| CN112898025A (zh) | 一种碳热硼热制备硼化钒超细粉体方法 | |
| CN112974834B (zh) | 等离子炬阴极材料前驱粉体及其制备方法及等离子炬阴极 | |
| EP2562138B1 (en) | Preparation method for copper oxide nanowires | |
| KR101500657B1 (ko) | 니켈-알루미늄 합금 분말 저온 제조 방법 | |
| CN100378256C (zh) | 一种合成六棱柱状碳化硅纳米棒的方法 | |
| CN112981299B (zh) | 一种利用热等离子体在金刚石表面制备高结合强度碳化物涂层的方法 | |
| CN216162880U (zh) | 一种加热器 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210402 |