CN1307045C - 碳蜂窝体 - Google Patents
碳蜂窝体 Download PDFInfo
- Publication number
- CN1307045C CN1307045C CNB038134187A CN03813418A CN1307045C CN 1307045 C CN1307045 C CN 1307045C CN B038134187 A CNB038134187 A CN B038134187A CN 03813418 A CN03813418 A CN 03813418A CN 1307045 C CN1307045 C CN 1307045C
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- China
- Prior art keywords
- matrix
- pyrolysis
- honeycomb
- fiber
- stabilisation
- 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.)
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims description 24
- 239000011159 matrix material Substances 0.000 claims description 23
- 238000000197 pyrolysis Methods 0.000 claims description 22
- 239000000835 fiber Substances 0.000 claims description 17
- 239000000919 ceramic Substances 0.000 claims description 16
- 230000006641 stabilisation Effects 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- 239000005011 phenolic resin Substances 0.000 claims description 9
- 239000004760 aramid Substances 0.000 claims description 7
- 229920003235 aromatic polyamide Polymers 0.000 claims description 7
- 238000003763 carbonization Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000005087 graphitization Methods 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 2
- 241000208202 Linaceae Species 0.000 claims description 2
- 235000004431 Linum usitatissimum Nutrition 0.000 claims description 2
- 235000009120 camo Nutrition 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 235000005607 chanvre indien Nutrition 0.000 claims description 2
- 239000011487 hemp Substances 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 238000000280 densification Methods 0.000 claims 3
- 229920003043 Cellulose fiber Polymers 0.000 claims 1
- 239000003607 modifier Substances 0.000 claims 1
- 239000012779 reinforcing material Substances 0.000 claims 1
- 238000007581 slurry coating method Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000005229 chemical vapour deposition Methods 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 229920000784 Nomex Polymers 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000004763 nomex Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000010426 asphalt Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 241001466460 Alveolata Species 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 210000001170 unmyelinated nerve fiber Anatomy 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
- C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
- C04B41/4529—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied from the gas phase
- C04B41/4531—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied from the gas phase by C.V.D.
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- B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
- B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
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- C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
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- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- C04B41/85—Coating or impregnation with inorganic materials
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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Abstract
本发明涉及一种制备具有蜂窝结构的碳材料体的方法。为了能以简便的方法制得相应的碳材料体,推荐对由纸张或纤维网制成的、具有蜂窝结构的预成型体进行热解和稳定化处理。
Description
本发明涉及一种制备具有蜂窝结构的碳材料体的方法。
具有蜂窝结构的相应材料体在重量很小的情况下能显示出高刚性的优点。为了能用碳材料制得相应的蜂窝结构,根据US5567500推荐的方法,要使用多层纤维材料层并使其处于相互偏转的纤维方向,同时在相应层之间还要设置一个预设有蜂窝结构的型芯,用以随后通过加热作用硬化这些层,同时实现层间连接。为此要用树脂浸渍这些层。其中所说的层特别是指织物或预浸渍片。
为了能得到特别适用于飞机中的、且兼具重量轻和稳定性好这一特性的夹层结构体或是板材,不得不采用成本昂贵的这种制备方法来构造蜂窝结构。
还存在一种由芳族聚酰胺纸(NOMEX)或铝组成的蜂窝体。
US4518704中记载了一种具有蜂窝状结构的并由活性炭制成的材料体。其中,先要将一种含活性炭的混合物挤出,然后干燥成形体,最后进行热解。
在根据DE4301396C2制备多孔纤维结构体的过程中,首先制备连续纤维的纤维束,然后相互叠加放置成至少两层,最后进行相互连结。
JP57027130A或JP11217278A是用活性炭制得多孔材料体或蜂窝体。其中,在将它们成型后再将这些材料体干燥并热解。
本发明的任务在于提供一种具有蜂窝结构的碳材料体,其能简便地制得且具有高机械强度,并且在保持所需的材料性质的同时还能对其进行调节。
为解决该难题,推荐使用一种预成型的具有蜂窝结构且由树脂浸渍过的纸张或纤维网制成的基体,其中首先对基体进行热解,然后使其稳定化和/或使其致密化。
与已知的现有技术不同,这里使用了一种具有蜂窝结构的预成型基体来制备碳材料体,并且该基体在很大程度上含有一种能转变为碳的材料,由此使得不再需要如现有技术中所需的那种碳织物或预浸渍片的层式结构了。
换句话说,使用可用于商业目的且本身也能商购得的蜂窝体,就能用碳通过热解和稳定化作用制得如下所述的一种蜂窝体,即其能例如被板材所覆盖,用以构成航天航空技术中所需的夹层结构。但是也特别优选可将如此制得的一种具有蜂窝结构的碳材料体用于化学工业中,例如作为催化剂或过滤器。
特别优选将一种由经树脂浸渍过的芳族聚酰胺构成的蜂窝体用作基体。不受此限制地,能通过材料从气相中沉积而使热解后的基体稳定化或致密化。这里优选用C、SiC、B4C和/或Si特别是通过CVI(化学气相渗透)和/或CVD(化学气相沉积)沉淀而使经热解后的基体稳定化或致密化。
此外,还推荐在850℃≤T1≤1100℃、特别优选900℃≤T1≤1000℃的温度T1下碳化该预成型的基体。还可以在1700℃≤T2≤3100℃、特别是1800℃≤T2≤2450℃的温度T2下石墨化该基体。
预成型的基体至少由一种树脂以及一种预设有蜂巢结构的增强介质组成。所谓的树脂指的是如具有高C产率的环氧化物,热塑性塑料如PEEK,PI,酚树脂,呋喃树脂,环氧化的酚醛树脂或其他粘结体系等一类在热解之时和之后能具有或保证粘结或成型稳定性的材料。
预成型的、具有蜂窝结构且由纸张或纤维网制成的基体应该具有耐高温的纤维如C纤维或SiC纤维,或者是具有足够高碳残留量的可热解纤维。属于这些纤维的例子有酚树脂纤维、芳族聚酰胺纤维、亚麻纤维、大麻纤维或其他天然纤维。
但是,在上述的这些物质中优选使用例如由用树脂如酚树脂浸渍过的芳族聚酰胺纸制成的预成型蜂窝体。相应的蜂窝体可从Dupont de Nemours公司购得,且其商品名为NOMEX。
此外,本发明还设计对经热解的且具有蜂窝结构的碳材料体和稳定化体进行后处理或对其进行调质。这同样可通过表面技术如CVI技术(化学气相渗透)、CVD法(化学气相沉积)、沥青涂覆进行或利用含碳的溶液如树脂、环氧树脂、酚树脂进行处理,然后将它们转化成碳而进行。还可以利用能转换成陶瓷如SiC的陶瓷浆进行后处理。
特别优选通过硅化作用构造SiC表面层。为此目的,可使用CVD或CVI法来处理碳材料体,用以形成SiC或PyC(高温石墨层)。还可以用液态沥青或聚合物进行涂层。接着,使经如此涂层的碳材料体碳化或石墨化。
虽然确定具有蜂窝结构的相应碳材料体特别适用于诸如航空航天领域内的夹层结构或面板,但是其也能用于耐高温的领域内,比如作为催化剂和过滤器的载体结构,反应器和化学装置的填料体,在使用有腐蚀性介质的情况下用作高温环境下的高透过性载体结构,化学装置的物质交换部件,解吸塔中用于水处理的填料体,吸收塔中用于净化废气的填料体,液体和气体分配器,热绝缘材料,或诸如加热工艺气体的电阻加热元件。
一般而言,蜂窝结构本身是六边形的,但也可以是其他几何形状,如圆形或矩形。
本发明制备的具有蜂窝结构的碳材料体典型地具有如下尺寸:
板材大小900mm×600mm,蜂窝高度40mm。蜂窝可以具有7mm×4mm和0.2mm的典型壁厚的典型六边形结构。
以下将结合实施例来进一步详细地阐释本发明。从权利要求(其本身和/或相互的结合)中可以得到本发明的其他一些细节、优点和特征。
为将由碳构成的且呈六面体结构的蜂窝体用于承重的夹层板,首先就要将ECA4.8-48型的NOMEX蜂窝体在保护气氛下进行热解。热解在800℃到1050℃的温度范围内进行。然后借助CVI法,利用PyC(高温石墨)沉积使所得到的脆性很高的碳蜂窝结构体稳定化。这个过程要在约1250℃的温度下进行并持续约60小时。
如此制得的碳蜂窝片显示出了良好的耐压值。为进一步提高机械性能,就要利用酚树脂对碳蜂窝片进行树脂浸渍,接着在950℃至1050℃的温度下进行再碳化。为了更进一步提高机械性能,就要将浸渍和再碳化过程重复两次。然后,借助酚树脂粘贴膜,并且在一定的压力(约2bar)和温度(约140℃)下在表面,也就是蜂窝体的端面上施以热压,从而将已预成型的CFC片(碳纤维增强的碳材料片,约2mm厚)粘贴到如此制得的碳蜂窝体材料上。最后在约1000℃的温度下对如此形成的CFC夹层板进行再碳化处理,用以将形成粘结介质的酚树脂膜转变成碳。
按上述方法就制得了高刚性的且能用在高温炉部件中作为承载结构的CFC夹层板。
Claims (16)
1.制备碳蜂窝体的方法,其中使用一种经树脂浸渍过的且由纸张或纤维网构成的、具有蜂窝结构的基体,该基体首先经热解,然后使其致密化或稳定化,其特征在于,用含碳的溶液涂覆经稳定化的蜂窝体,然后对其再次进行热解。
2.如权利要求1的方法,其特征在于,将一种由树脂浸渍过的芳族聚酰胺纸构成的蜂窝体用作基体。
3.如权利要求1的方法,其特征在于,通过气相材料沉积使经热解的基体稳定化或致密化。
4.如权利要求3的方法,其特征在于,通过CVI沉积和/或CVD沉积,利用C、SiC、B4C和/或Si而使所述经热解的基体稳定化或致密化。
5.如权利要求1的方法,其特征在于,在经热解后的基体上形成一层SiC或PyC层。
6.如权利要求1的方法,其特征在于,用能转化为陶瓷的陶瓷浆涂覆经热解和稳定化或致密化处理的基体。
7.如权利要求6的方法,其特征在于,所用陶瓷浆能转化为SiC。
8.如权利要求1的方法,其特征在于,在850℃≤T1≤1100℃的温度T1下碳化所述具有蜂窝结构的基体。
9.如权利要求8的方法,其特征在于900℃≤T1≤1000℃。
10.如权利要求1的方法,其特征在于,在1700℃2≤T2≤3100℃的温度T2下石墨化所述基体。
11.如权利要求10的方法,其特征在于1800℃≤T2≤2450℃。
12.如权利要求1的方法,其特征在于,使用具有耐高温的纤维或者是具有足够高碳残留量的可热解的纤维作为增强材料的这样一类基体。
13.如权利要求12的方法,其特征在于,所述耐高温的纤维是碳纤维或SiC纤维,所述可热解的纤维是酚树脂纤维、芳族聚酰胺纤维、亚麻纤维、大麻纤维或其他纤维素纤维。
14.如权利要求1的方法,其特征在于,接着使经热解和稳定化或致密化处理的基体进行进一步的增强或调质处理。
15.如权利要求1的方法,其特征在于,对经热解和稳定化或致密化处理过的基体进行硅化处理。
16.一种可商购的由芳族聚酰胺纸制成的蜂窝体作为过滤器、催化剂或航空航天工业中铺盖用的结构部件的用途,其中要对所述的纸进行树脂浸渍,热解,然后再使其稳定化和/或致密化。
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DE102008011357A1 (de) * | 2008-02-27 | 2009-09-03 | Mann + Hummel Gmbh | Verfahren zur Herstellung eines keramischen Filterelements |
CN102211045B (zh) * | 2010-04-01 | 2012-12-12 | 上海霍林化工设备工程有限公司 | 一种海水脱硫工艺的催化剂填料及其填料床 |
CN101935230B (zh) * | 2010-08-27 | 2013-01-30 | 南通京通石墨设备有限公司 | 加工型浸渍石墨管生产方法 |
CN102964145B (zh) * | 2012-12-04 | 2014-04-02 | 西北工业大学 | 一种涂层增强C/SiC复合材料的制备方法 |
DE102014013532A1 (de) | 2014-09-12 | 2016-03-17 | Airbus Operations Gmbh | Honigwabenstruktur aus einem vlies aus rezyklierten kohlenstofffasern |
CN104909798B (zh) * | 2015-05-25 | 2017-07-28 | 航天材料及工艺研究所 | 一种碳化硅纤维轻质高温隔热材料及其制备方法 |
CN106316437A (zh) * | 2015-06-26 | 2017-01-11 | 上海航天设备制造总厂 | 一种卫星高导热碳/碳复合材料蜂窝制备方法 |
CN108840697B (zh) * | 2018-06-29 | 2021-07-13 | 航天材料及工艺研究所 | 一种碳/碳复合材料蜂窝及其制备方法 |
CN113019015B (zh) * | 2019-12-24 | 2022-05-17 | 东北林业大学 | 一种饼形木纤维陶瓷发动机空气滤芯 |
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DE10225953A1 (de) | 2003-12-24 |
US20050249914A1 (en) | 2005-11-10 |
JP2005536420A (ja) | 2005-12-02 |
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DE50308804D1 (de) | 2008-01-24 |
EP1515835B1 (de) | 2007-12-12 |
ATE380654T1 (de) | 2007-12-15 |
WO2003103940A1 (de) | 2003-12-18 |
CN1671544A (zh) | 2005-09-21 |
AU2003250346A1 (en) | 2003-12-22 |
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