CN1874973A - 陶瓷复合材料及其制造方法 - Google Patents
陶瓷复合材料及其制造方法 Download PDFInfo
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- CN1874973A CN1874973A CNA2004800322601A CN200480032260A CN1874973A CN 1874973 A CN1874973 A CN 1874973A CN A2004800322601 A CNA2004800322601 A CN A2004800322601A CN 200480032260 A CN200480032260 A CN 200480032260A CN 1874973 A CN1874973 A CN 1874973A
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- ceramic
- sintering
- carbon
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- composite
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- 239000000919 ceramic Substances 0.000 title claims abstract description 129
- 239000002131 composite material Substances 0.000 title claims abstract description 112
- 238000004519 manufacturing process Methods 0.000 title claims description 25
- 238000005245 sintering Methods 0.000 claims abstract description 153
- 239000000843 powder Substances 0.000 claims abstract description 112
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 90
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 48
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 28
- 150000004767 nitrides Chemical class 0.000 claims abstract description 17
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 13
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 13
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 13
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 13
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 13
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 12
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 12
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 12
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 12
- 238000000465 moulding Methods 0.000 claims description 34
- 239000011159 matrix material Substances 0.000 claims description 33
- 239000012298 atmosphere Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- 239000000470 constituent Substances 0.000 claims description 17
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000000428 dust Substances 0.000 claims description 8
- PIZYHTQSHRQOBI-UHFFFAOYSA-N [C].O=[N] Chemical compound [C].O=[N] PIZYHTQSHRQOBI-UHFFFAOYSA-N 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims 4
- 239000000463 material Substances 0.000 abstract description 30
- 238000005520 cutting process Methods 0.000 abstract description 3
- 238000005299 abrasion Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 150000001247 metal acetylides Chemical class 0.000 abstract 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 100
- 238000012360 testing method Methods 0.000 description 41
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 34
- 239000005297 pyrex Substances 0.000 description 34
- 239000005388 borosilicate glass Substances 0.000 description 32
- 229910002804 graphite Inorganic materials 0.000 description 31
- 239000010439 graphite Substances 0.000 description 31
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 27
- 229910010271 silicon carbide Inorganic materials 0.000 description 27
- 229910052727 yttrium Inorganic materials 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 21
- 239000000203 mixture Substances 0.000 description 18
- 238000011156 evaluation Methods 0.000 description 17
- 230000005540 biological transmission Effects 0.000 description 15
- 238000005452 bending Methods 0.000 description 13
- 230000001133 acceleration Effects 0.000 description 11
- 238000000227 grinding Methods 0.000 description 11
- 238000002156 mixing Methods 0.000 description 11
- 239000011521 glass Substances 0.000 description 10
- 239000010936 titanium Substances 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 7
- 239000012299 nitrogen atmosphere Substances 0.000 description 7
- 238000004451 qualitative analysis Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 5
- 229910052753 mercury Inorganic materials 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 239000002041 carbon nanotube Substances 0.000 description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 208000037656 Respiratory Sounds Diseases 0.000 description 3
- 239000002134 carbon nanofiber Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 229910003564 SiAlON Inorganic materials 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 230000005713 exacerbation Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000009725 powder blending Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000010023 transfer printing Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000003913 materials processing Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-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
- 238000013001 point bending Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供了适合作切削工具、滑动部件和成型模具材料的高耐磨、低摩擦的陶瓷复合材料。该陶瓷复合材料的特征在于由具有平均晶粒尺寸为3μm或更小，优选30nm或更小的碳作为主组分的相以及陶瓷相(条件是排除碳)构成。所述陶瓷相为选自Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的氮化物、碳化物、氧化物、复合氮化物、复合碳化物、复合氧化物、碳氮化物、氧氮化物、碳氮氧化物和碳氧化物中的至少一种。该陶瓷复合材料是通过在800至1500℃烧结温度和200MPa或更高烧结压力下烧结原料粉末而制得。
Description
技术领域
本发明涉及在室温至中/低温范围具有优良机械性能的陶瓷复合材料，其在各种应用中被用作高耐磨、低摩擦的陶瓷材料，所述应用包括各种结构部件、切削工具、滑动部件以及成型模具材料；本发明还涉及该复合材料的制造方法。
背景技术
将固体润滑剂如碳的粒子分散入诸如氮化硅的陶瓷基质中以改善材料的摩擦系数和相对磨损率，由此所得的材料目前是公知的。
例如，由氮化硅和氮化钛以及0.5至20wt％石墨及碳的复合材料得到的具有突出摩擦特性和耐磨性能的材料报道于日本专利公报特开2003-34580中。然而在该特开2003-34580中所述条件下制备的粉末烧结试样，用扫描电子显微镜在2000倍放大倍数下鉴定，观察到大量直径20μm或更大、开气孔率为3％或更高的气孔，这证明此材料用于模具是不可能的。
同时，将0.5至6wt％的C、Cr、Mo、W、Al、Ti和Ni作为抗氧化合金掺入到氧化铝和氧化锆中所得的超硬材料报道于日本专利公报特开昭60-100646中，然而当碳含量低至0.1至0.2％时，材料缺乏用于模具的润滑性。
另外，将2至50wt％颗粒尺寸为5μm或更大的碳加入至碳化硅中所得的具有出色耐磨性的材料报道于日本专利公报特开平09-87029中；将3至30wt％平均晶粒尺寸3至6μm的石墨分散入碳化钛基质中所得的材料报道于日本专利公报特开平05-301773中。然而，当碳的平均晶粒尺寸大到3μm或更大时，在将材料加工成所期望的形状时表面粗糙度就受到晶粒尺寸的影响，这使得难以得到10nm或更低平均粗糙度的材料反射面。
此外，日本专利公报特开平10-231174介绍了将石墨和氮化硼分散入非氧化物陶瓷中所得的材料，在其界面层之间插入铁化合物(如铁的氧化物或硅化物)。然而，这种材料由于包含铁而存在一些问题，例如由于氧化而致的劣化以及高温下的稳定性受损，使其不适合用作模具材料。
本发明公开内容
鉴于上文讨论的情况，本发明的目的是制造可用的陶瓷复合材料，该材料除了在室温到中/高温度范围内具有优良的机械性能外，且对玻璃、树脂和陶瓷以及其他材料具有增强的脱模性能；同时提供制造该复合材料的方法。
通过反复研究，本发明人发现，在含有以碳作为主组分的相的陶瓷复合材料中，通过使该陶瓷复合材料的平均晶粒尺寸为3μm或更小，优选30nm或更小，则可解决上文详述的问题，由此完成了本发明。
具体地，本发明具有下列构成特征。
(1).陶瓷复合材料，其特征在于由含有平均晶粒尺寸为3μm或更小，优选30nm或更小的碳作为主组分的相以及陶瓷相(条件是排除碳)构成。
(2).如上文(1)所述的陶瓷复合材料，其特征在于含有碳作为主组分的相的含量是2-98wt％。
(3).如上文(1)和(2)所述的陶瓷复合材料，其特征在于抛光之后复合材料表面的开气孔率为1％或更小。
(4).如上文(1)和(2)所述的陶瓷复合材料，其特征在于烧结形式的复合材料的维氏硬度为10GPa或更大。
(5).如上文(1)至(4)所述的陶瓷复合材料，其特征在于所述陶瓷相由选自由Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的氮化物、碳化物、氧化物、复合氮化物、复合碳化物、复合氧化物、碳氮化物、氧氮化物、碳氮氧化物和碳氧化物组成的组中的至少一种构成。
(6).制造由具有平均晶粒尺寸为3μm或更小，优选30nm或更小的碳作为主组分的相以及陶瓷相构成的陶瓷复合材料的方法，其特征在于将平均晶粒尺寸为3μm或更小，优选30nm或更小的陶瓷粉末(条件是排除碳)与碳粉末的粉末混合物进行成型，并将获得的成型体在非氧化性气氛中于800至1500℃的烧结温度和200MPa或更高的烧结压力下进行烧结。
(7).制造如上文(5)所述、由具有平均晶粒尺寸为3μm或更小，优选30nm或更小的碳作为主组分的相以及陶瓷相构成的陶瓷复合材料的方法，其特征在于所述陶瓷粉末为选自由Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的氮化物、碳化物、氧化物、复合氮化物、复合碳化物、复合氧化物、碳氮化物、氧氮化物、碳氮氧化物和碳氧化物组成的组中的至少一种。
(8).如上文(6)和(7)所述的、制造由具有平均晶粒尺寸为3μm或更小，优选30nm或更小的碳作为主组分的相以及陶瓷相构成的陶瓷复合材料的方法，其特征在于粉末混合物进一步包括选自Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的至少一种金属。
本发明最佳实施方式
本发明为陶瓷复合材料，其特征在于，由具有平均晶粒尺寸为3μm或更小、优选30nm或更小的碳作为主组分的相以及陶瓷相构成。该陶瓷复合材料中以碳为主组分的相对于玻璃、树脂和陶瓷以及其他材料显示出优良的脱模性能。如果陶瓷复合材料相的平均晶粒尺寸超过3μm，则在将复合材料加工成所期望的形状时，平均粗糙度将达到如此之大以至于如镜面般的光洁度将难以达到。
此外，本发明的“碳”应该是其构成物质由碳组成的物质，因此可合适地选自例如石墨(C)、石墨碳(GC)、金刚石、碳纳米管(CNT)、足球烯(C60)和碳纳米纤维(CNF)的材料。复合材料中的碳含量期望为2-98wt％；小于该含量是不期望的，因为这样材料的脱模性能将受到损害，高于该含量同样不期望，因为这样材料将不能烧结。优选的碳含量是30-80wt％；特别优选40-60wt％。这一数值范围内的碳含量能更加改善所述复合材料对于例如玻璃、树脂和陶瓷的材料的脱模性能。
本发明陶瓷复合材料中的陶瓷相期望由选自由Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的氮化物、碳化物和氧化物组成的组中的至少一种形成。此外，陶瓷相还可以是刚才所提及金属的复合氮化物、复合碳化物或复合氧化物，或者可以是刚才所列举金属的碳氮化物、氧氮化物、碳氮氧化物或碳氧化物。根据形成自复合材料的模具将要成型的材料，合适地选择用于陶瓷相的一种或多种这些种类的陶瓷材料并且陶瓷相材料的含量是2-98wt％是有利的。为了改善复合材料的烧结能力，还可根据需要而使用公知的烧结助剂，但是不希望氧化物基烧结助剂的含量大，因为助剂会与碳强烈反应，这使得难以制造超细材料且损害材料的机械性能。
本发明的陶瓷复合材料是通过将至少一种平均晶粒尺寸为3μm或更小，优选30nm或更小的Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo或W的氮化物、碳化物或氧化物的陶瓷粉末与碳粉末的粉末混合物进行成型，并在非氧化性气氛下于800至1500℃的烧结温度和200MPa或更高的烧结压力下将所得成型体进行烧结而得到。非氧化性气氛可选择真空气氛或惰性气体气氛如H2、N2或Ar，优选真空气氛。前述粉末混合物也可进一步包含至少一种选自Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的金属。这些金属与粉末混合物中的碳反应形成碳化物，或者，如果非氧化性气氛是N2，则与N2反应形成氮化物。此外，一些金属能通过混合物中的机械化学反应形成碳化物或氮化物等。
如果烧结温度低于800℃，则烧结反应不能进行，这将使得难以得到陶瓷复合材料。同样，如果温度高于1500℃将导致烧结过度进行，使颗粒尺寸变粗且损害材料的机械性能。1000至1400℃的烧结温度是尤其合适的。
此外，如果烧结压力低于200MPa，烧结反应将不能进行，导致不能得到陶瓷复合材料。最优的压力是500MPa或更高。
如下将给出实施方案的实例详细阐述本发明。应该指出的是以下的wt％表示内比例。
实施方案中使用的测定方法如下。
(1).粉末平均颗粒尺寸的测定
使用透射电子显微镜(TEM：H-9000UHRIII mfd.由Hitachi制造)。
在由TEM得到的图像的任意区域中，随机选出100个粉末颗粒，测定颗粒尺寸，尺寸的平均值被作为粉末的平均颗粒尺寸。
(2).平均晶粒尺寸的测定
使用透射电子显微镜(TEM：H-9000UHRIII mfd.由Hitachi制造)。
在由TEM得到的图像的任意位置，划出穿过50个颗粒的程度的直线，用线的长度除以颗粒数量，以此得到颗粒尺寸。该操作在5个任意位置施行，平均值作为平均晶粒尺寸。
(3).开气孔率的测定
使用压汞孔隙度仪(9420mfd.由Shimadzu Seisakusho制造)。
水银在压力下被压入样品，并且通过被压入的水银体积计算气孔体积和气孔尺寸。
(4).抗弯强度的测定
使用通用材料测定仪(5585mfd.由Instron制造)。
根据标准JIS R 1601计算从三点抗弯测得的数据。
实施方案1
在0.1MPa的氮气气氛下，将作为烧结助剂的2.5wt％Y2O3粉末和1wt％Al2O3粉末加入至平均颗粒尺寸为0.5μm的市售Si3N4粉末中，并进一步加入20wt％平均颗粒尺寸为1μm的金属Zr粉和40wt％平均颗粒尺寸为5μm的石墨粉，粉末的混合通过使用Si3N4制球的球磨方法在10G的加速度下进行。
将所得复合材料粉末通过X-射线衍射(XRD)进行定性分析，其中Si3N4、ZrN、ZrCN、ZrC和C的衍射峰能够被确认。此外，复合材料粉末在透射电子显微镜下的观测结果显示，平均颗粒尺寸为3μm或更小。
接着，利用上述所得复合材料粉末，在真空气氛和表I所记录的条件下通过烧结该粉末而制造陶瓷复合材料。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定。
表I
| 烧结中采用的温度和压力条件 | |
| 烧结温度 | 烧结压力 |
| 800℃ | 200MPa |
| 1150℃ | 500MPa |
| 1500℃ | 1000MPa |
| 1700℃* | 5000MPa |
*：比较例
在完成对所得陶瓷复合材料的磨削(grinding)和精研(lapping)操作后，使用透射电子显微镜在每一陶瓷复合材料的任意10个位置进行平均晶粒尺寸的测定。随后使用压汞孔隙度仪完成对每一陶瓷复合材料开气孔率的测定。接着使用维氏硬度计测定所获得复合材料的维氏硬度。这些测量的结果列于表II。
表II
*：比较例
表II的结果证明，应用800至1500℃烧结温度和200至5000Pa烧结压力的条件所制造的陶瓷复合材料的平均晶粒尺寸是3μm或更小。当烧结温度为1700℃时，晶粒生长显著增长，由此平均晶粒尺寸变得大于3μm，这意味着陶瓷复合材料表面上精研抛光(lap-polished)区域的表面粗糙度不能提供所期望的精度。
根据表II的结果，很明显，应用前述烧结条件所得烧结体的开气孔率小于1％，这是相当良好的。当开气孔率大于1％时，如果陶瓷复合材料被用作例如玻璃的成型模具，则玻璃进入气孔区域，引起脱模性能问题和界面上产生毛刺的问题以及其他困难。
实施方案2
在0.1Mpa的氮气气氛下，将作为烧结助剂的2.5wt％Y2O3粉末和1wt％Al2O3粉末加入至平均颗粒尺寸为0.5μm的市售Si3N4粉末中，并进一步加入20wt％平均颗粒尺寸为1μm的金属Zr粉，之后将平均颗粒尺寸为5μm的石墨粉以表III所列比例加入，并将粉末掺混，粉末的混合通过使用Si3N4制球的球磨方法在10G的加速度下进行。
表III
| 试验编号 | 烧结粉末中加入的石墨数量(wt％) |
| 2-1* | 1 |
| 2-2 | 2 |
| 2-3 | 20 |
| 2-4 | 40 |
| 2-5 | 70 |
| 2-6 | 98 |
| 2-7* | 99 |
*：比较例
所得复合材料粉末通过X-射线衍射(XRD)进行定性分析，其中Si3N4、ZrN、ZrCN、ZrC和C的衍射峰能够被确认。此外，复合材料粉末在透射电子显微镜下的观测结果显示，平均颗粒尺寸为3μm或更小。
接着，利用刚才所述的复合材料粉末，通过在真空气氛和1150℃烧结温度、1000MPa烧结压力的条件下烧结该粉末而制造陶瓷复合材料。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定。
在完成对所得陶瓷复合材料的磨削和精研操作后，进行复合材料平均晶粒尺寸、开气孔率和抗弯强度的评价。然后为确定对光学玻璃进行模具成型时的脱模性能，使用硅酸硼玻璃(Pyrex)进行评价。在评价方法中，将本发明的陶瓷复合材料切割成20mm的计量长度，然后表面精研抛光至0.02μm(Ra)的表面粗糙度，并且在720℃成型温度、10MPa成型压力的条件下用作模具对10mm计量长度的前述硅酸硼玻璃(Pyrex)压60秒。进行100次玻璃成型试验，对以下含量作出脱模性能评价。起初，在成型操作完成后，硅酸硼玻璃(Pyrex)在不施加外力的情况下与模具脱离，随后在硅酸硼玻璃(Pyrex)外表面的检测中，这些产品没有碎屑、裂纹或污斑，并且成型后硅酸硼玻璃(Pyrex)转印面的粗糙度为0.03μm或更小(Ra)被认为是合格的。脱模性能(％)被定义为合格的产品数除以成型试验次数所得的百分数。举例来说，如果在100次成型试验中得到50个合格产品，那么脱模性能就是50％。脱模性能评价的结果列于表IV。
表IV
| 试验编号 | 石墨数量(wt％) | 开气孔率(％) | 平均颗粒尺寸(μm) | 抗弯强度 | 对硅酸硼玻璃(Pyrex)的脱模性能(％) |
| 2-1* | 1 | 2.3 | 4.7 | 1120 | 18 |
| 2-2 | 2 | 0.8 | 2.8 | 1100 | 59 |
| 2-3 | 20 | 0.3 | 2.1 | 918 | 97 |
| 2-4 | 40 | 0.2 | 1.7 | 717 | 100 |
| 2-5 | 70 | 0.3 | 1.9 | 414 | 100 |
| 2-6 | 98 | 0.9 | 2.6 | 112 | 91 |
| 2-7* | 99 | 未烧结 | 未烧结 | 未烧结 | 未烧结 |
硅酸硼玻璃(Pyrex)的脱模性能试验：720℃/10MPa压力条件下压60秒；试验次数n＝100
表IV的结果表明，在石墨含量为2至98wt％的陶瓷复合材料中，开气孔率小于1％且平均晶粒尺寸为3μm或更小。进一步，含有石墨比例20至98wt％的模具样品对硅酸硼玻璃(Pyrex)的脱模性能是非常优良的，为90％或更高，甚至当样品中所述含量比例为2％时，脱模性能也接近60％；由此显示出复合材料可充分用作模具。同时，在石墨含量为1wt％的样品中，脱模性能严重恶化。相反，对石墨含量高于90wt％的复合材料，其烧结被证明是有问题的；含量为98wt％的，烧结体在数次尝试中有一次是可制造的，但是随着石墨含量超过99wt％，制备烧结体被证明是完全不可能的。
实施方案3
按照表V所列的配方，通过将平均颗粒尺寸0.5μm的40wt％表V所示陶瓷粉末(1)、20wt％平均颗粒尺寸0.5μm的陶瓷粉末(2)和平均颗粒尺寸不超过5μm的作为余量的碳粉末以及根据需要而添加的烧结助剂共混合，并在10G的加速度下使用球磨机混合该共混物而制得掺混粉末。
表V
| 试验编号 | 陶瓷粉末(1) | 陶瓷粉末(2) | 碳 | 烧结助剂 |
| 3-1 | SiC | ZrCn | C | 2.5wt％Y2O3+1wt％Al2O3 |
| 3-2 | Si3N4 | TiCN | GC | 2.5wt％Y2O3+1wt％Al2O3 |
| 3-3 | AlN | CrN | C | 0.6wt％Y2O3 |
| 3-4 | Al2O3 | MoO2 | C | - |
| 3-5 | 3Y-ZrO2 * | WC | GC | - |
| 3-6 | SiC | VN | GC | 2.5wt％Y2O3+1wt％Al2O3 |
| 3-7 | Si3N4 | TiCO | C | 2.5wt％Y2O3+1wt％Al2O3 |
| 3-8 | 尖晶石 | NbHfC | C60 | 0.6wt％Y2O3 |
| 3-9 | β-SiAlON | TaNbC | CNT | - |
| 3-10 | 莫来石 | TaNbN | 碳黑 | - |
*)3Y-ZrO2：以3wt％Y2O3稳定的ZrO2
所得复合材料粉末在透射电子显微镜下的观测结果显示，平均晶粒尺寸为3μm或更小。
接着，利用刚才所述的复合材料粉末，在真空气氛和1150℃烧结温度、1000MPa烧结压力的条件下通过烧结该粉末而制造陶瓷复合材料。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定。
在完成对所得陶瓷复合材料的磨削和精研操作后，进行复合材料开气孔率、平均晶粒尺寸和抗弯强度的评价。然后，为了确定对光学玻璃进行模具成型时的转印精度和脱模性能，以与实施方案2同样的方式使用硅酸硼玻璃(Pyrex)进行100次成型试验，评价脱模性能。评价和试验的结果列于表VI。
表VI
| 试验编号 | 开气孔率(％) | 平均颗粒尺寸(μm) | 抗弯强度(MPa) | 对硅酸硼玻璃(Pyrex)的脱模性能(％)* |
| 3-1 | 0.3 | 1.4 | 433 | 100 |
| 3-2 | 0.2 | 1.7 | 720 | 100 |
| 3-3 | 0.4 | 1.8 | 428 | 100 |
| 3-4 | 0.5 | 2.3 | 287 | 100 |
| 3-5 | 0.2 | 1.6 | 686 | 100 |
| 3-6 | 0.2 | 1.6 | 728 | 100 |
| 3-7 | 0.3 | 1.7 | 720 | 100 |
| 3-8 | 0.4 | 1.7 | 402 | 100 |
| 3-9 | 0.4 | 2.2 | 416 | 100 |
| 3-10 | 0.2 | 1.7 | 337 | 100 |
*：720℃/10MPa压力条件下压60秒
试验次数n＝100
实施方案4
按照表VII所列的配方，利用平均颗粒尺寸为0.5μm的表VII所示陶瓷粉末，和使余量为平均颗粒尺寸5μm或更小的碳粉末，并根据需要向此共混物中添加烧结助剂，通过共混以上材料并且在10G的加速度下使用球磨机混合该共混物而制得掺混粉末。
表VII
| 采用的陶瓷粉末和烧结助剂 | |
| 陶瓷粉末 | 烧结助剂 |
| SiC | 2.5wt％Y2O3+1wt％Al2O3 |
| Si3N4 | 2.5wt％Y2O3+1wt％Al2O3 |
| AlN | 0.6wt％Y2O3 |
| Al2O3 | - |
| 3Y-ZrO2 * | - |
*)3Y-ZrO2：以3wt％Y2O3稳定的ZrO2：
| 石墨用量(wt％) |
| 1 |
| 2 |
| 10 |
| 20 |
| 40 |
| 70 |
| 90 |
| 98 |
| 99 |
：比较例
所得粉末掺混物在透射电子显微镜下的观测结果显示，平均晶粒尺寸为3μm或更小。接着，对陶瓷粉末分别为Si3N4和AlN的样品在N2气气氛下，对陶瓷粉末分别为SiC、Al2O3和3Y-ZrO2(以3wt％Y2O3稳定的ZrO2)的样品在Ar气气氛下，通过1150℃烧结温度、1000MPa烧结压力的条件烧结该粉末掺混物而制造陶瓷复合材料。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定的。
在完成对所得陶瓷复合材料的磨削和精研操作后，进行复合材料的开气孔率、平均晶粒尺寸和抗弯强度的评价。然后，为了确定对光学玻璃进行模具成型时的转移精度和脱模性能，以与实施方案2同样的方式使用硅酸硼玻璃(Pyrex)进行100次成型试验，评价脱模性能。评价和试验的结果列于表VIII。
表VIII
| 开气孔率(％) | 石墨含量(％) | |||||||||
| 1* | 2 | 10 | 20 | 40 | 70 | 90 | 98 | 99* | ||
| 陶瓷粉末 | SiC | 3.0 | 0.9 | 0.6 | 0.3 | 0.3 | 0.4 | 0.6 | 0.8 | 未烧结 |
| Si3N4 | 2.5 | 0.8 | 0.5 | 0.3 | 0.2 | 0.3 | 0.6 | 0.9 | 未烧结 | |
| AlN | 2.8 | 0.9 | 0.6 | 0.4 | 0.3 | 0.4 | 0.6 | 1 | 未烧结 | |
| Al2O3 | 3.2 | 0.9 | 0.7 | 0.5 | 0.3 | 0.4 | 0.5 | 0.8 | 未烧结 | |
| 3Y-ZrO2 | 3.1 | 0.9 | 0.6 | 0.4 | 0.3 | 0.4 | 0.6 | 0.9 | 未烧结 | |
*比较例
| 平均颗粒尺寸(μm) | 石墨含量(％) | |||||||||
| 1* | 2 | 10 | 20 | 40 | 70 | 90 | 98 | 99* | ||
| 陶瓷粉末 | SiC | 4.8 | 3.8 | 2.6 | 2.3 | 2 | 2.1 | 2.4 | 2.8 | 未烧结 |
| Si3N4 | 5.1 | 3 | 2.7 | 2.5 | 2.1 | 2.2 | 2.4 | 2.9 | 未烧结 | |
| AlN | 5.6 | 3 | 2.8 | 2.6 | 2.3 | 2.3 | 2.7 | 3 | 未烧结 | |
| Al2O3 | 5.5 | 2.9 | 2.8 | 2.6 | 2.2 | 2.3 | 2.6 | 2.9 | 未烧结 | |
| 3Y-ZrO2 | 5.2 | 2.8 | 2.7 | 2.5 | 2.1 | 2.2 | 2.3 | 2.7 | 未烧结 | |
*比较例
| 抗弯强度(Mpa) | 石墨含量(％) | |||||||||
| 1* | 2 | 10 | 20 | 40 | 70 | 90 | 98 | 99* | ||
| 陶瓷粉末 | SiC | 715 | 703 | 654 | 592 | 469 | 285 | 162 | 101 | 未烧结 |
| Si3N4 | 1030 | 1012 | 938 | 845 | 660 | 383 | 198 | 106 | 未烧结 | |
| AlN | 415 | 409 | 383 | 352 | 288 | 193 | 130 | 98 | 未烧结 | |
| Al2O3 | 620 | 610 | 568 | 516 | 412 | 256 | 152 | 100 | 未烧结 | |
| 3Y-ZrO2 | 980 | 962 | 892 | 804 | 629 | 365 | 190 | 102 | 未烧结 | |
*比较例
| 对硅酸硼玻璃(Pyrex)的脱模性能(％)* | 石墨含量(％) | |||||||||
| 1* | 2 | 10 | 20 | 40 | 70 | 90 | 98 | 99* | ||
| 陶瓷粉末 | SiC | 21 | 62 | 83 | 96 | 100 | 100 | 94 | 89 | 未烧结 |
| Si3N4 | 19 | 56 | 80 | 97 | 100 | 100 | 92 | 86 | 未烧结 | |
| AlN | 17 | 59 | 78 | 94 | 100 | 100 | 93 | 87 | 未烧结 | |
| Al2O3 | 12 | 51 | 72 | 90 | 100 | 100 | 89 | 82 | 未烧结 | |
| 3Y-ZrO2 | 18 | 61 | 81 | 92 | 100 | 100 | 94 | 88 | 未烧结 | |
*比较例
硅酸硼玻璃(Pyrex)的脱模性能试验：720℃/10MPa压力条件下压60秒；试验次数n＝100
实施方案5
在0.1Mpa的氮气气氛下，将作为烧结助剂的2.5wt％Y2O3粉末以及1wt％Al2O3粉末加入至平均颗粒尺寸为0.5μm的市售SiC粉末中，并进一步加入20wt％平均颗粒尺寸为3μm的金属CrN粉和40wt％平均颗粒尺寸为5μm的石墨粉，粉末的混合通过使用SiC制球的球磨方法在10G的加速度下进行。
所得复合材料粉末通过XRD进行定性分析，其中SiC、CrN、CrCN、CrC和C的衍射峰能够被确认。此外，复合材料粉末在透射电子显微镜下的观测结果显示，平均晶粒尺寸为3μm或更小。
接着，将刚才所述的复合材料粉末在真空气氛和表IX所记录的条件下进行烧结以生成陶瓷复合材料。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定。
表IX
| 烧结中采用的温度和压力条件 | |
| 烧结温度 | 烧结压力 |
| 400℃* | 100Mpa* |
| 600℃* | 200MPa |
| 800℃ | 500MPa |
| 1150℃ | 1000MPa |
| 1500℃ | 5000MPa |
| 1700℃* | |
*：比较例
在完成对所得陶瓷复合材料的磨削和精研操作后，为了确定在对光学玻璃进行模具成型时的形状转印精度和脱模性能，以与实施方案2同样的方式使用硅酸硼玻璃(Pyrex)进行100次成型试验，评价脱模性能。试验和评价的结果列于表X。
表X
*：比较例
硅酸硼玻璃(Pyrex)的脱模性能试验：720℃/10MPa压力条件下压60秒；试验次数n＝100
表X的结果证明，应用800至1500℃烧结温度和200MPa或更高烧结压力的条件所制造的烧结体与硅酸硼玻璃(Pyrex)之间的脱模性能是优良的。然而，当烧结温度为1700℃时，晶粒显著生长以至于脱模性能明显恶化。同时，在烧结温度为600℃的样品中，尽管烧结压力为1000MPa或更高的那些样品显示出了脱模性能，但对应用低于该水平的烧结压力而得到的陶瓷复合材料，模具经不起成型时的加压力而解体。最后，400℃的烧结温度被证明会抑制烧结体的制造。
实施方案6
在0.1Mpa的氮气气氛下，将作为烧结助剂的2.5wt％Y2O3粉末以及1wt％Al2O3粉末加入至平均颗粒尺寸为0.5μm的市售Si3N4粉末中，并进一步加入30wt％平均颗粒尺寸为0.5μm的金属Ti粉和40wt％平均颗粒尺寸为5μm的石墨粉，粉末的混合通过使用Si3N4制球的球磨方法在150G的加速度下完成。
所得复合材料粉末通过XRD进行定性分析，其中Si3N4、TiN、TiCN、TiC和C的宽衍射峰能够被确认。此外，复合材料粉末在透射电子显微镜下的观测结果显示，平均颗粒尺寸为30nm或更小。
接着，将上述方式制造的复合材料粉末在真空气氛和表XI所记录的条件下进行烧结以生成陶瓷复合材料。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定。
表XI
| 烧结中采用的温度和压力条件 | |
| 烧结温度 | 烧结压力 |
| 800℃ | 200MPa |
| 1000℃ | 500MPa |
| 1200℃ | 1000MPa |
| 1400℃ | 5000MPa |
| 1500℃ | 10000MPa |
| 1600℃* | |
*：比较例
在完成对所得陶瓷复合材料的磨削和精研操作后，使用透射电子显微镜在每一陶瓷复合材料的任意10个位置进行平均晶粒尺寸的测定。随后使用压汞孔隙度仪完成对每一陶瓷复合材料开气孔率的测定。这些测量的结果列于表XII。
表XII
*：比较例
*：比较例
表XII的结果证明，应用800至1500℃烧结温度和200至5000MPa烧结压力的条件所制造的陶瓷复合材料的平均晶粒尺寸是30nm或更小。当烧结温度超过1600℃时，导致颗粒生长显著增加，由此平均晶粒尺寸变得大于30nm，这意味着陶瓷复合材料表面上精研抛光区域的表面粗糙度不能提供所期望的精度。
根据表XII的结果，很明显，应用上述烧结条件的烧结体的开气孔率小于1％，这是相当良好的。当开气孔率大于1％时，如果将陶瓷复合材料用作例如玻璃的成型模具，则玻璃进入气孔区域，引起脱模性能问题和界面上产生毛刺的问题以及其他困难。
实施方案7
在0.1Mpa的氮气气氛下，将作为烧结助剂的2.5wt％Y2O3粉末以及1wt％Al2O3粉末加入至平均颗粒尺寸为0.5μm的市售Si3N4粉末中，并且进一步加入30wt％平均颗粒尺寸为0.5μm的金属Ti粉，之后将平均颗粒尺寸为5μm的石墨粉以表XIII所列比例加入，并将粉末掺混，粉末的混合通过采用Si3N4制球的球磨方法在150G的加速度下进行12小时。
表XIII
| 试验编号 | 烧结粉末中加入的石墨量(wt％) |
| 7-1* | 1 |
| 7-2 | 2 |
| 7-3 | 20 |
| 7-4 | 40 |
| 7-5 | 60 |
| 7-6 | 80 |
| 7-7 | 98 |
| 7-8* | 99 |
*：比较例
所得复合材料粉末通过XRD进行定性分析，其中Si3N4、TiN、TiCN、TiC和C的宽衍射峰能够被确认。此外，复合材料粉末在透射电子显微镜下的观测结果显示，平均颗粒尺寸为30nm或更小。
接着，利用刚才所述的复合材料粉末，通过在真空气氛和1200℃烧结温度、1000MPa烧结压力的条件下烧结该粉末而生成陶瓷复合材料。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定。
在完成对所获陶瓷复合材料的磨削和精研操作后，进行复合材料平均晶粒尺寸、开气孔率和抗弯强度的评价。然后为确定对光学玻璃进行模具成型时的脱模性能，使用硅酸硼玻璃(Pyrex)进行评价。在该评价方法中，将本发明的陶瓷复合材料切割成20mm的计量长度，然后表面精研抛光至0.02μm(Ra)的表面粗糙度，并且在720℃成型温度、10MPa成型压力的条件下用作模具对10mm计量长度的前述硅酸硼玻璃(Pyrex)压60秒。进行500次玻璃成型试验，对以下含量作出脱模性能评价。起初，在成型操作完成后，硅酸硼玻璃(Pyrex)在不施加外力的情况下与模具脱离，随后在硅酸硼玻璃(Pyrex)外表面的检测中，这些产品没有碎屑、裂纹或污斑，并且成型后硅酸硼玻璃(Pyrex)的转移表面粗糙度为0.03μm或更小(Ra)被认为是合格的。脱模性能(％)被定义为合格产品数除以成型试验次数所得的百分数。举例来说，如果在500次成型试验中得到50个合格产品，那么脱模性能就是10％。脱模性能评价的结果列于表XIV。
表XIV
| 试验编号 | 石墨含量(wt％) | 开气孔率(％) | 平均颗粒尺寸(nm) | 抗弯强度(MPa) | 对硅酸硼玻璃(Pyrex)的脱模性能(％) |
| 7-1* | 1 | 1.4 | 53 | 1350 | 23 |
| 7-2 | 2 | 0.4 | 28 | 1326 | 64 |
| 7-3 | 20 | 0.2 | 19 | 1107 | 99 |
| 7-4 | 40 | 0.1 | 14 | 863 | 100 |
| 7-5 | 60 | 0.2 | 15 | 620 | 100 |
| 7-6 | 80 | 0.3 | 15 | 377 | 98 |
| 7-7 | 98 | 0.6 | 17 | 134 | 96 |
| 7-8* | 99 | 未烧结 | 未烧结 | 未烧结 | 未烧结 |
硅酸硼玻璃(Pyrex)的脱模性能试验：720℃/10MPa压力条件下压60秒；试验次数n＝500
表XIV的结果表明，在石墨含量为2至98wt％的陶瓷复合材料中，开气孔率小于1％且平均晶粒尺寸为30nm或更小。进一步，含有石墨比例20至98wt％的模具样品对于硅酸硼玻璃(Pyrex)的脱模性能是非常优良的，为90％或更高，甚至当样品中所述含量比例为2％时，脱模性能也是60％或更好；由此显示出复合材料可充分用作模具。同时，在石墨含量为1wt％的样品中，脱模性能严重恶化。反之，对于石墨含量高于90wt％的复合材料，其烧结被证明是有问题的；含量为98wt％的，烧结体在数次尝试中有一次是可制造的，但是随着石墨含量超过99wt％，制备烧结体被证明是完全不可能的。
实施方案8
按照表XV所列的配方，通过将40wt％平均颗粒尺寸0.5μm的表XV所示陶瓷粉末(1)、20wt％平均颗粒尺寸0.5μm的陶瓷粉末(2)和平均颗粒尺寸不超过5μm作为余量的碳粉末以及根据需要而添加的烧结助剂共混，并且在150G加速度下使用球磨机混合该共混物12小时而制得掺混粉末。
表XV
| 试验编号 | 陶瓷粉末(1) | 陶瓷粉末(2) | 碳 | 烧结助剂 |
| 8-1 | SiC | ZrCn | C | 1wt％Al2O3 |
| 8-2 | Si3N4 | TiCN | GC | 2.5wt％Y2O3+1wt％Al2O3 |
| 8-3 | AlN | CrN | C | 0.6wt％Y2O3 |
| 8-4 | Al2O3 | MoO2 | C | - |
| 8-5 | 3Y-ZrO2 | WC | GC | - |
| 8-6 | SiC | VN | GC | 1wt％Al2O3 |
| 8-7 | Si3N4 | TiCO | C | 2.5wt％Y2O3+1wt％Al2O3 |
| 8-8 | 尖晶石 | NbHfC | C60 | 0.6wt％Y2O3 |
| 8-9 | β-SiAlON | TaNbC | CNT | - |
| 8-10 | 莫来石 | TaNbN | 炭黑 | - |
| 8-11 | Si3N4 | TiCN | CNF | - |
所得复合材料粉末在透射电子显微镜下的观测结果显示，平均颗粒尺寸为30nm或更小。
接着，利用刚才所述的复合材料粉末，通过在真空气氛和1200℃烧结温度、1000MPa烧结压力的条件下烧结该粉末而生成陶瓷复合材料。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定。
在完成对所得陶瓷复合材料的磨削和精研操作后，进行复合材料开气孔率、平均颗粒尺寸和抗弯强度的评价。然后，为了确定对Pyrex光学玻璃进行模具成型时的脱模性，在720℃、10MPa条件下压按硅酸硼玻璃(Pyrex)后，以与实施方案7同样的方式进行500次成型试验，评价脱模性能的情况。评价的结果列于表XVI。
表XVI
| 试验编号 | 开气孔率(％) | 平均颗粒尺寸(μm) | 抗弯强度(MPa) | 对硅酸硼玻璃(Pyrex)的脱模性能(％)* |
| 8-1 | 0.2 | 15 | 514 | 100 |
| 8-2 | 0.1 | 14 | 860 | 100 |
| 8-3 | 0.2 | 16 | 508 | 100 |
| 8-4 | 0.1 | 20 | 341 | 100 |
| 8-5 | 0.1 | 14 | 815 | 100 |
| 8-6 | 0.1 | 13 | 508 | 100 |
| 8-7 | 0.1 | 16 | 860 | 100 |
| 8-8 | 0.2 | 15 | 61 | 100 |
| 8-9 | 0.2 | 21 | 547 | 100 |
| 8-10 | 0.1 | 18 | 39 | 100 |
| 8-11 | 0.2 | 20 | 800 | 100 |
*：720℃/10MPa压力条件下压60秒
试验次数n＝500
实施方案9
利用平均颗粒尺寸为0.5μm的表XVII所示陶瓷粉末，并使余量为平均颗粒尺寸5μm或更小的碳粉末，且根据需要在该共混物中加入烧结助剂，由此按照表XVII所列的共混物配方，在150G的加速度下使用球磨机混合该共混物12小时而制得掺混粉末。
所得复合材料粉末在透射电子显微镜下的观测结果显示，平均晶粒尺寸为30nm或更小。
表XVII
| 采用的陶瓷粉末和烧结助剂 | |
| 陶瓷粉末 | 烧结助剂 |
| SiC | 1重量％的Al2O3 |
| Si3N4 | 2.5重量％的Y2O3+1重量％的Al2O3 |
| AlN | 0.6重量％的Y2O3 |
| Al2O3 | -- |
| 3Y-ZrO2 * | -- |
*)3Y-ZrO2：以3wt％Y2O3稳定的ZrO2
| 石墨含量(重量％) |
| 1 |
| 2 |
| 10 |
| 20 |
| 40 |
| 60 |
| 80 |
| 90 |
| 98 |
| 99 |
：比较例
接着，通过在1200℃烧结温度、1000MPa烧结压力的条件下烧结上述粉末掺混物而生成陶瓷复合材料，烧结时陶瓷粉末分别为Si3N4和AlN的样品处于N2气气氛下，陶瓷粉末分别为SiC、Al2O3和3Y-ZrO2的样品处于Ar气气氛下(以3wt％Y2O3稳定的ZrO2)。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定。
在完成对所得陶瓷复合材料的磨削和精研操作后，进行复合材料开气孔率、平均颗粒尺寸和抗弯强度的评价。然后，为了确定对光学玻璃进行模具成型时的转印精度和脱模性能，使用硅酸硼玻璃(Pyrex)以与实施方案7同样的方式进行500次成型试验来完成评价。评价和试验的结果列于表XVIII。
表XVIII
| 开气孔率(％) | 石墨含量(％) | ||||||||||
| 1* | 2 | 10 | 20 | 40 | 60 | 80 | 90 | 98 | 99* | ||
| 陶瓷粉末 | SiC | 1.4 | 0.5 | 0.2 | 0.1 | 0.1 | 0.1 | 0.2 | 0.3 | 0.7 | 未烧结 |
| Si3N4 | 1.4 | 0.4 | 0.2 | 0.1 | 0.1 | 0.1 | 0.2 | 0.2 | 0.6 | 未烧结 | |
| AlN | 1.6 | 0.6 | 0.3 | 0.2 | 0.2 | 0.2 | 0.3 | 0.3 | 0.7 | 未烧结 | |
| Al2O3 | 1.5 | 0.6 | 0.3 | 0.2 | 0.1 | 0.1 | 0.2 | 0.2 | 0.8 | 未烧结 | |
| 3Y-ZrO2 | 1.4 | 0.4 | 0.2 | 0.1 | 0.1 | 0.1 | 0.2 | 0.3 | 0.6 | 未烧结 | |
*比较例
| 平均颗粒尺寸(μm) | 石墨含量(％) | ||||||||||
| 1* | 2 | 10 | 20 | 40 | 60 | 80 | 90 | 98 | 99* | ||
| 陶瓷粉末 | SiC | 52 | 26 | 20 | 17 | 15 | 16 | 17 | 19 | 21 | 未烧结 |
| Si3N4 | 54 | 24 | 18 | 15 | 14 | 14 | 15 | 17 | 20 | 未烧结 | |
| AlN | 62 | 27 | 19 | 17 | 16 | 16 | 17 | 17 | 22 | 未烧结 | |
| Al2O3 | 60 | 30 | 21 | 18 | 17 | 17 | 18 | 18 | 24 | 未烧结 | |
| 3Y-ZrO2 | 56 | 26 | 19 | 16 | 14 | 14 | 15 | 16 | 21 | 未烧结 | |
*比较例
| 抗弯强度(MPa) | 石墨含量(％) | ||||||||||
| 1* | 2 | 10 | 20 | 40 | 60 | 80 | 90 | 98 | 99* | ||
| 陶瓷粉末 | SiC | 780 | 767 | 715 | 650 | 520 | 390 | 260 | 195 | 130 | 未烧结 |
| Si3N4 | 1265 | 1242 | 1152 | 1040 | 815 | 589 | 364 | 252 | 139 | 未烧结 | |
| AlN | 530 | 522 | 490 | 449 | 368 | 288 | 207 | 166 | 126 | 未烧结 | |
| Al2O3 | 775 | 762 | 711 | 646 | 517 | 389 | 260 | 195 | 131 | 未烧结 | |
| 3Y-ZrO2 | 1210 | 1189 | 1103 | 995 | 780 | 566 | 351 | 243 | 136 | 未烧结 | |
*比较例
| 对硅酸硼玻璃(Pyrex)的脱模性能(％) | 石墨含量(％) | ||||||||||
| 1* | 2 | 10 | 20 | 40 | 60 | 80 | 90 | 98 | 99* | ||
| 陶瓷粉末 | SiC | 24 | 65 | 84 | 98 | 100 | 100 | 100 | 100 | 93 | 未烧结 |
| Si3N4 | 20 | 61 | 81 | 99 | 100 | 100 | 100 | 100 | 95 | 未烧结 | |
| AlN | 21 | 63 | 79 | 93 | 100 | 100 | 100 | 98 | 91 | 未烧结 | |
| Al2O3 | 18 | 60 | 75 | 90 | 100 | 100 | 99 | 96 | 90 | 未烧结 | |
| 3Y-ZrO2 | 22 | 63 | 83 | 94 | 100 | 100 | 100 | 100 | 92 | 未烧结 | |
*比较例
硅酸硼玻璃(Pyrex)的脱模性能试验：720℃/10MPa压力条件下压60秒
实施方案10
在0.1Mpa的氮气气氛下，将作为烧结助剂的2.5wt％Y2O3粉末以及1wt％Al2O3粉末加入至平均颗粒尺寸为0.5μm的市售SiC粉末中，并进一步加入20wt％平均颗粒尺寸为3μm的金属CrN粉和40wt％平均颗粒尺寸为5μm的石墨粉，粉末的混合通过使用SiC制球的球磨方法在150G的加速度下进行12小时。
所得复合材料粉末通过XRD进行定性分析，其中SiC、CrN、CrCN、CrC和C的宽衍射峰能够被确认。此外，复合材料粉末在透射电子显微镜下的观测结果显示，平均晶粒尺寸为30nm或更小。
接着，将刚才所述的复合材料粉末在真空气氛和表X IX所记录的条件下进行烧结以生成陶瓷复合材料。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定。
表XIX
| 烧结过程中采用的温度和压力条件 | |
| 烧结温度 | 烧结压力 |
| 400℃* | 100MPa* |
| 600℃* | 200MPa |
| 800℃ | 500MPa |
| 1000℃ | 1000MPa |
| 1200℃ | 5000MPa |
| 1400℃ | 10,000MPa |
| 1500℃ | *比较例 |
| 1600℃* | |
在完成对所得陶瓷复合材料的磨削和精研操作后，为了确定对Pyrex光学玻璃进行模具成型时的脱模性，在720℃、10MPa条件下压按硅酸硼玻璃(Pyrex)后，以与实施方案7同样的方式进行500次成型试验，评价脱模性能的情况。评价的结果列于表XX。
表XX
*：比较例
硅酸硼玻璃(Pyrex)的脱模性能试验：720℃/10MPa压力条件下压60秒；试验次数n＝500
表XX的结果证明，应用800至1500℃烧结温度和200MPa或更高烧结压力的条件所制造的烧结体与硅酸硼玻璃(Pyrex)之间的脱模性能是优良的。然而，当烧结温度为1600℃时，晶粒生长显著以至于脱模性能明显恶化。同时，在烧结温度为600℃的样品中，尽管烧结压力为1000MPa或更高的那些样品显示出脱模性能，但对应用低于该水平的烧结压力而得到的烧结体，模具经不起成型时的加压力而解体。最后，400℃的烧结温度被证明会抑制烧结体的生成。
实施方案11
在0.1Mpa的氮气气氛下，将平均颗粒尺寸为5μm的石墨粉以表XXI所列比例加入至平均颗粒尺寸为0.5μm的市售SiC粉末中，不加烧结助剂，各粉末的混合通过使用Si3N4制球的球磨方法在150G的加速度下进行12小时。
表XXI
| 陶瓷(SiC)(重量份) | 石墨(重量份) |
| 99 | 1 |
| 98 | 2 |
| 90 | 10 |
| 80 | 20 |
| 60 | 40 |
| 40 | 60 |
| 20 | 80 |
| 10 | 90 |
| 2 | 98 |
| 1 | 99 |
将所得复合材料粉末通过XRD进行定性分析，其中SiC和C的宽衍射峰能够被确认。此外，复合材料粉末在透射电子显微镜下的观测结果显示，平均颗粒尺寸为30nm或更小。
接着，利用刚才所述的复合材料粉末，通过在真空气氛和1200℃烧结温度、1000MPa烧结压力的条件下烧结该粉末而生成陶瓷复合材料。复合材料制造中的温度是通过使用红外光学高温计测量成型模具表面温度而测定。
以采用所得陶瓷复合材料的模具对ZnS陶瓷进行烧结-成型时，为了确定脱模性能，使用市售ZnS粉末进行评价。在评价方法中，将本发明的陶瓷复合材料切割成20mm的计量长度，然后表面精研抛光至0.02μm(Ra)的表面粗糙度，并且在1000℃烧结温度、50MPa成型压力的条件下用作模具来压按20mm计量长度的前述ZnS陶瓷。进行100次成型试验，对以下含量作出脱模性能评价。起初，在成型操作完成后，ZnS陶瓷在不施加外力的情况下与模具脱离，随后在这些成型后的ZnS陶瓷产品上没有碎屑、裂纹或污染，并且成型后ZnS陶瓷的转移表面粗糙度为0.03μm或更小(Ra)被认为是合格的。脱模性能(％)被定义为合格的产品数除以成型试验次数所得的百分数。举例来说，如果在100次成型试验中得到50个合格产品，那么脱模性能就是50％。脱模性能评价的结果列于表XXII。
表XXII
| 模具材料 | 石墨含量(重量份) | 1 | 2 | 10 | 20 | 40 | 60 | 80 | 98 | 99 |
| SiC含量(重量份) | 99 | 98 | 90 | 80 | 60 | 40 | 20 | 2 | 1 | |
| 评价结果 | 脱模性能(％) | 0 | 0 | 12 | 86 | 100 | 100 | 100 | 67* | 模具破裂 |
*模具在第68次试验中破裂
烧结条件：1200℃；1000MPa
产业适用性
由于本发明中的陶瓷复合材料具有出众的耐磨和低摩擦性能，还对玻璃、树脂和陶瓷以及其他材料有着优良的脱模性能，所以该复合材料用作切削工具、滑动部件和成型模具材料是极好的。
Claims (12)
1.陶瓷复合材料，其特征在于由含有平均晶粒尺寸为3μm或更小的碳作为主组分的相以及陶瓷相(条件是排除碳)构成。
2.陶瓷复合材料，其特征在于由含有平均晶粒尺寸为30nm或更小的碳作为主组分的相以及陶瓷相(条件是排除碳)构成。
3.如权利要求1或2所述的陶瓷复合材料，其特征在于含有碳作为主组分的相的含量为2-98wt％。
4.如权利要求1至3任一项所述的陶瓷复合材料，其特征在于抛光之后复合材料表面的开气孔率为1％或更小。
5.如权利要求1至4任一项所述的陶瓷复合材料，其特征在于烧结形式的复合材料的维氏硬度为10GPa或更高。
6.如权利要求1至5任一项所述的陶瓷复合材料，其特征在于所述陶瓷相由选自由Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的氮化物、碳化物、氧化物、复合氮化物、复合碳化物、复合氧化物、碳氮化物、氧氮化物、碳氮氧化物和碳氧化物组成的组中的至少一种构成。
7.制造如权利要求1或3至6任一项所述的由含有平均晶粒尺寸为3μm或更小的碳作为主组分的相以及陶瓷相构成的陶瓷复合材料的方法，其特征在于将平均晶粒尺寸为3μm或更小的陶瓷粉末(条件是排除碳)与碳粉末的混合粉末进行成型，并将获得的成型体在非氧化性气氛中于800至1500℃的烧结温度和200MPa或更高的烧结压力下进行烧结。
8.如权利要求7所述的制造由含有平均晶粒尺寸为3μm或更小的碳作为主组分的相以及陶瓷相构成的陶瓷复合材料的方法，其特征在于所述陶瓷粉末为选自由Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的氮化物、碳化物、氧化物、复合氮化物、复合碳化物、复合氧化物、碳氮化物、氧氮化物、碳氮氧化物和碳氧化物组成的组中的至少一种。
9.如权利要求7或8所述的制造由含有平均晶粒尺寸为3μm或更小的碳作为主组分的相以及陶瓷相构成的陶瓷复合材料的方法，其特征在于混合粉末进一步包括选自Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的至少一种金属。
10.制造如权利要求2至6任一项所述的由含有平均晶粒尺寸为30nm或更小的碳作为主组分的相以及陶瓷相构成的陶瓷复合材料的方法，其特征在于将平均晶粒尺寸为30nm或更小的陶瓷粉末(条件是排除碳)与碳粉末的混合粉末进行成型，并将获得的成型体在非氧化性气氛中于800至1500℃的烧结温度和200MPa或更高的烧结压力下进行烧结。
11.如权利要求10所述的制造由含有平均晶粒尺寸为30nm或更小的碳作为主组分的相以及陶瓷相构成的陶瓷复合材料的方法，其特征在于所述陶瓷粉末为选自由Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的至少一种金属的氮化物、碳化物、氧化物、复合氮化物、复合碳化物、复合氧化物、碳氮化物、氧氮化物、碳氮氧化物和碳氧化物组成的组中的一种或多种。
12.如权利要求10或11所述的制造由含有平均晶粒尺寸为30nm或更小的碳作为主组分的相以及陶瓷相构成的陶瓷复合材料的方法，其特征在于混合粉末进一步包括选自Al、Si、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo和W的至少一种金属。
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| JP282952/2004 | 2004-09-29 |
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| EP (1) | EP1679293A4 (zh) |
| JP (1) | JP2005154258A (zh) |
| KR (1) | KR20060116807A (zh) |
| CN (1) | CN100425572C (zh) |
| TW (1) | TW200526540A (zh) |
| WO (1) | WO2005040064A1 (zh) |
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| CN115135622A (zh) * | 2020-02-27 | 2022-09-30 | 3M创新有限公司 | 用于玻璃成形的模具以及使用模具形成玻璃的方法 |
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- 2004-09-29 JP JP2004282952A patent/JP2005154258A/ja active Pending
- 2004-10-22 WO PCT/JP2004/016077 patent/WO2005040064A1/ja active Application Filing
- 2004-10-22 KR KR1020067008248A patent/KR20060116807A/ko not_active Application Discontinuation
- 2004-10-22 CN CNB2004800322601A patent/CN100425572C/zh not_active Expired - Fee Related
- 2004-10-22 US US10/595,577 patent/US7723248B2/en not_active Expired - Fee Related
- 2004-10-22 EP EP04793185A patent/EP1679293A4/en not_active Withdrawn
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017079878A1 (zh) * | 2015-11-09 | 2017-05-18 | 深圳市博世知识产权运营有限公司 | 一种氧化铝、氮化铝复合粉体的制造方法 |
| CN115135622A (zh) * | 2020-02-27 | 2022-09-30 | 3M创新有限公司 | 用于玻璃成形的模具以及使用模具形成玻璃的方法 |
| CN115135622B (zh) * | 2020-02-27 | 2023-12-15 | 3M创新有限公司 | 用于玻璃成形的模具以及使用模具形成玻璃的方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1679293A4 (en) | 2011-01-26 |
| KR20060116807A (ko) | 2006-11-15 |
| EP1679293A1 (en) | 2006-07-12 |
| US20070129233A1 (en) | 2007-06-07 |
| TW200526540A (en) | 2005-08-16 |
| JP2005154258A (ja) | 2005-06-16 |
| WO2005040064A1 (ja) | 2005-05-06 |
| CN100425572C (zh) | 2008-10-15 |
| US7723248B2 (en) | 2010-05-25 |
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