CN116477952B - 一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法 - Google Patents
一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法 Download PDFInfo
- Publication number
- CN116477952B CN116477952B CN202310515235.3A CN202310515235A CN116477952B CN 116477952 B CN116477952 B CN 116477952B CN 202310515235 A CN202310515235 A CN 202310515235A CN 116477952 B CN116477952 B CN 116477952B
- Authority
- CN
- China
- Prior art keywords
- powder
- sibcn
- hfc
- amorphous
- under
- 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.)
- Active
Links
- 238000009792 diffusion process Methods 0.000 title claims abstract description 80
- 239000000919 ceramic Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 14
- 239000010703 silicon Substances 0.000 title claims abstract description 12
- DZVPMKQTULWACF-UHFFFAOYSA-N [B].[C].[N] Chemical compound [B].[C].[N] DZVPMKQTULWACF-UHFFFAOYSA-N 0.000 title claims abstract description 11
- QKQUUVZIDLJZIJ-UHFFFAOYSA-N hafnium tantalum Chemical compound [Hf].[Ta] QKQUUVZIDLJZIJ-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 117
- 238000005245 sintering Methods 0.000 claims abstract description 53
- 238000011049 filling Methods 0.000 claims abstract description 12
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 34
- 229910002804 graphite Inorganic materials 0.000 claims description 34
- 239000010439 graphite Substances 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 28
- 239000012300 argon atmosphere Substances 0.000 claims description 22
- 238000005498 polishing Methods 0.000 claims description 19
- 238000003825 pressing Methods 0.000 claims description 17
- 239000011863 silicon-based powder Substances 0.000 claims description 12
- 229910003460 diamond Inorganic materials 0.000 claims description 9
- 239000010432 diamond Substances 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000003892 spreading Methods 0.000 claims description 6
- 230000007480 spreading Effects 0.000 claims description 6
- 229910052715 tantalum Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 claims 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims 1
- 238000007731 hot pressing Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 7
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- -1 hafnium-silicon boron carbon nitrogen Chemical compound 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910003468 tantalcarbide Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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
- C04B35/5607—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 refractory metal 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
- 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
- C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
-
- 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
- C04B35/6261—Milling
- C04B35/62615—High energy or reactive ball milling
-
- 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
- C04B35/645—Pressure sintering
-
- 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
- C04B2235/6562—Heating rate
-
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
一种碳化钽铪‑硅硼碳氮陶瓷扩散偶的制备方法,它涉及扩散偶的制备方法。本发明要解决现有Ta4HfC5/SiBCN陶瓷扩散偶难以结合,界面结合强度差,扩散行为不明显的问题。制备方法:一、高能球磨制备非晶相SiBCN粉体;二、粉体装填至模具;三、热压烧结。本发明用于碳化钽铪‑硅硼碳氮陶瓷扩散偶的制备。
Description
技术领域
本发明涉及扩散偶的制备方法。
背景技术
Ta4HfC5陶瓷作为熔点最高的碳化物超高温陶瓷之一,具有高强度、高硬度、高模量以及高化学稳定性的优势,在高超音速航空中有很大的应用前景。但过渡金属碳化物原子之间的强共价键使其难以烧结,同时存在断裂韧性低,抗热冲击性能差,单独使用时抗氧化性能不佳等缺点。添加烧结助剂可有效解决以上问题,其主要机理是:第一,添加剂可以产生液相烧结促进原子扩散;第二,添加剂与基体反应形成新相,进一步影响陶瓷性能;第三,添加剂可以造成原子在晶界处的偏析,影响晶界或界面处的原子排列进而影响界面形态和微观结构,因此对界面行为的研究十分重要。
SiBCN作为添加剂对Ta4HfC5陶瓷烧结性能的影响尚未有相关报道。Ta4HfC5与SiBCN陶瓷析晶后的SiC均属于立方结构,相似的晶格常数和Ta、Hf、Si原子相近的原子半径使其具有相互扩散的能力。而Ta4HfC5与SiBCN陶瓷共价键结合特性使其难以致密化,一方面,表面的气孔阻碍原子的扩散,另一方面,界面处的点/线缺陷又提供了原子扩散通道,这意味着二者的界面具有复杂现象。为了探究Si原子与Hf、Ta原子的扩散行为,可采用扩散偶法来进行研究。扩散偶法在研究固态关系中占据重要地位,两种材料形成扩散偶后的扩散现象发生在两种材料垂直于界面方向,可以高效直观分析两相间的界面行为,但不同体系扩散偶的制备方法存在较大差异。Ta4HfC5-SiBCN陶瓷扩散偶的制备难点,一是需要较高能量来断开共价键结合促使原子互扩散发生,二是烧结过程中界面结合方式对界面强度产生影响;在此情况下,极易导致Ta4HfC5/SiBCN陶瓷扩散偶难以结合,界面结合强度差,扩散行为不明显。
发明内容
本发明要解决现有Ta4HfC5/SiBCN陶瓷扩散偶难以结合,界面结合强度差,扩散行为不明显的问题,进而提供一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法。
一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法,它是按以下步骤进行的:
一、高能球磨制备非晶相SiBCN粉体;
二、将Ta4HfC5粉体与非晶相SiBCN粉体依次分层装填于石墨模具内套内,得到装填好粉体的模具;
或者将Ta4HfC5粉体烧结得到Ta4HfC5块体,将Ta4HfC5块体及非晶相SiBCN粉体装填于石墨模具内套内,且Ta4HfC5块体埋于非晶相SiBCN粉体内部并压实,得到装填好粉体的模具;
或者将非晶相SiBCN粉体烧结得到SiBCN块体,将SiBCN块体及Ta4HfC5粉体装填于石墨模具内套内,且SiBCN块体埋于Ta4HfC5粉体内部并压实,得到装填好粉体的模具;
三、将装填好粉体的模具进行预压,然后在氩气气氛及升温速率为20℃/min~25℃/min的条件下,将预压后的粉体升温至烧结温度为1400℃~1600℃,再在氩气气氛、升温速率为20℃/min~25℃/min及加压速度为1MPa/min~8MPa/min的条件下,将烧结温度继续升温至1800℃~2100℃,且加压至30MPa~60MPa,最后在氩气气氛、烧结温度为1800℃~2100℃及压力为30MPa~60MPa的条件下,保持1~2h,以卸压速度为1MPa/min~4MPa/min泄压并随炉冷却,即得到碳化钽铪-硅硼碳氮陶瓷扩散偶。
本发明的有益效果是:
1、本发明采用机械合金化法结合热压烧结工艺制备多层Ta4HfC5/SiBCN扩散偶,基于二者烧结特征,利用热压烧结在高温和压力的结合下,促使Si、Hf、Ta原子在扩散偶界面处发生扩散。制备的Ta4HfC5/SiBCN扩散偶具有多层强结合的“啮合”界面,“啮合”状态的原因归结为粉体填装的非平直性和高烧结温度导致的晶粒长大。界面的“啮合”特征使得扩散偶在机械加工后能够保持相连状态,界面处形成较强结合。
2、本发明采用两次热压烧结制备Ta4HfC5/SiBCN扩散偶,基于二者烧结特征,利用热压烧结在高温和压力的结合下,促使Si、Hf、Ta原子在扩散偶界面处发生扩散。且其关键在于内嵌小块体的抛光程度以及***块体的烧结致密性,这是因为块体内芯的表面特征不随烧结压力、温度或者烧结时间的变化而变形,在压力作用下,四周的粉体对块体内芯产生挤压,接触位置的粉体烧结形貌取决于块体内芯的表面结构,在二者接触位置的界面发生扩散,而且块体内芯的表面杂质和宏观缺陷将影响原子扩散行为。
说明书附图
图1为本发明碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法中步骤三热压烧结示意图;
图2为实施例一制备的Ta4HfC5/SiBCN扩散偶切割前的光学照片;
图3为实施例一制备的Ta4HfC5/SiBCN扩散偶切割后截面的光学照片;
图4为实施例一抛光后的Ta4HfC5/SiBCN扩散偶界面微观形貌SEM图;
图5为实施例一抛光后的Ta4HfC5/SiBCN扩散偶SEM和原子相对含量随扩散距离曲线;
图6为实施例一抛光后的Ta4HfC5/SiBCN扩散偶界面的XRD图;
图7为实施例一制备的Ta4HfC5/SiBCN扩散偶界面的“啮合”形貌示意图;
图8为实施例二打磨去掉表面SiBCN陶瓷后的Ta4HfC5/SiBCN扩散偶光学照片。
具体实施方式
具体实施方式一:本实施方式一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法,它是按以下步骤进行的:
一、高能球磨制备非晶相SiBCN粉体;
二、将Ta4HfC5粉体与非晶相SiBCN粉体依次分层装填于石墨模具内套内,得到装填好粉体的模具;
或者将Ta4HfC5粉体烧结得到Ta4HfC5块体,将Ta4HfC5块体及非晶相SiBCN粉体装填于石墨模具内套内,且Ta4HfC5块体埋于非晶相SiBCN粉体内部并压实,得到装填好粉体的模具;
或者将非晶相SiBCN粉体烧结得到SiBCN块体,将SiBCN块体及Ta4HfC5粉体装填于石墨模具内套内,且SiBCN块体埋于Ta4HfC5粉体内部并压实,得到装填好粉体的模具;
三、将装填好粉体的模具进行预压,然后在氩气气氛及升温速率为20℃/min~25℃/min的条件下,将预压后的粉体升温至烧结温度为1400℃~1600℃,再在氩气气氛、升温速率为20℃/min~25℃/min及加压速度为1MPa/min~8MPa/min的条件下,将烧结温度继续升温至1800℃~2100℃,且加压至30MPa~60MPa,最后在氩气气氛、烧结温度为1800℃~2100℃及压力为30MPa~60MPa的条件下,保持1~2h,以卸压速度为1MPa/min~4MPa/min泄压并随炉冷却,即得到碳化钽铪-硅硼碳氮陶瓷扩散偶。
结合图1具体说明,本具体实施方式中为上下两个压头,从上方施加压力,但装填的粉体上下表面都受力。
本具体实施方式步骤一制备的非晶相SiBCN粉体储存在氩气或者真空环境内。
本实施方式的有益效果是:
1、本实施方式采用机械合金化法结合热压烧结工艺制备多层Ta4HfC5/SiBCN扩散偶,基于二者烧结特征,利用热压烧结在高温和压力的结合下,促使Si、Hf、Ta原子在扩散偶界面处发生扩散。制备的Ta4HfC5/SiBCN扩散偶具有多层强结合的“啮合”界面,“啮合”状态的原因归结为粉体填装的非平直性和高烧结温度导致的晶粒长大。界面的“啮合”特征使得扩散偶在机械加工后能够保持相连状态,界面处形成较强结合。
2、本实施方式采用两次热压烧结制备Ta4HfC5/SiBCN扩散偶,基于二者烧结特征,利用热压烧结在高温和压力的结合下,促使Si、Hf、Ta原子在扩散偶界面处发生扩散。且其关键在于内嵌小块体的抛光程度以及***块体的烧结致密性,这是因为块体内芯的表面特征不随烧结压力、温度或者烧结时间的变化而变形,在压力作用下,四周的粉体对块体内芯产生挤压,接触位置的粉体烧结形貌取决于块体内芯的表面结构,在二者接触位置的界面发生扩散,而且块体内芯的表面杂质和宏观缺陷将影响原子扩散行为。
具体实施方式二:本实施方式与具体实施方式一不同的是:步骤一中高能球磨制备非晶相SiBCN粉体具体是按以下步骤进行:在手套箱内称取Si粉、h-BN及石墨,并将称取的Si粉、h-BN及石墨装入球磨罐中,再在氩气气氛及球磨转速为600rpm~800rpm及球料比为(10~20):1的条件进行高能球磨20h~40h,得到非晶相SiBCN粉体。其它与具体实施方式一相同。
具体实施方式三:本实施方式与具体实施方式一或二之一不同的是:所述的Si粉与h-BN的摩尔比为1:(0.5~1)。其它与具体实施方式一或二相同。
具体实施方式四:本实施方式与具体实施方式一至三之一不同的是:所述的Si粉与石墨的摩尔比为1:(1~2)。其它与具体实施方式一至三相同。
具体实施方式五:本实施方式与具体实施方式一至四之一不同的是:步骤二中所述的Ta4HfC5粉体和非晶相SiBCN粉体为通过200目筛后得到的粉体。其它与具体实施方式一至四相同。
具体实施方式六:本实施方式与具体实施方式一至五之一不同的是:步骤二中将Ta4HfC5粉体与非晶相SiBCN粉体依次分层装填于石墨模具内套内具体是按以下步骤进行:在石墨模具内套的底面铺一层非晶相SiBCN粉体,上下震动使粉体平铺,然后用上压头将粉体压实,在压实的粉体上铺上一层Ta4HfC5粉体,上下震动使粉体平铺,再用上压头将粉体压实,重复交替非晶相SiBCN粉体和Ta4HfC5粉体的铺平及压实,直至达到3层非晶相SiBCN粉体和2层Ta4HfC5粉体,得到装填好粉体的模具。其它与具体实施方式一至五相同。
具体实施方式七:本实施方式与具体实施方式一至六之一不同的是:步骤二中所述的Ta4HfC5块体及SiBCN块体均是按以下步骤制备:在氩气气氛及升温速率为20℃/min~25℃/min的条件下,升温至烧结温度为1400℃~1550℃,再在氩气气氛、升温速率为20℃/min~25℃/min及加压速度为1MPa/min~4MPa/min的条件下,将烧结温度继续升温至1600℃~2100℃,且加压至30MPa~40MPa,最后在氩气气氛、烧结温度为1600℃~2100℃及压力为30MPa~40MPa的条件下,保持0.5h~1h,以卸压速度为1MPa/min~4MPa/min卸压并随炉冷却,得到陶瓷,将陶瓷切割成六面的块体,并对六面分别进行打磨和抛光处理。其它与具体实施方式一至六相同。
具体实施方式八:本实施方式与具体实施方式一至七之一不同的是:所述的打磨和抛光处理具体为依次经过500目~3000目金刚石磨盘打磨、500目~3000目砂纸打磨及粒径为0.25μm的金刚石抛光剂抛光。其它与具体实施方式一至七相同。
具体实施方式九:本实施方式与具体实施方式一至八之一不同的是:步骤二中所述的石墨模具内套的内表面设置厚度为0.01mm~0.03mm的石墨纸;步骤二中所述的压实为利用上压头将粉体压实,且压实过程中用厚度为0.1mm~0.5mm的石墨纸将粉体与上压头分隔。其它与具体实施方式一至八相同。
具体实施方式十:本实施方式与具体实施方式一至九之一不同的是:步骤三中所述的预压具体是按以下步骤进行:在压力机下,以加压速度为0.05t/s~0.1t/s,将装填好粉体的模具加压至1t~5t,并在压力为1t~5t的条件下,保压10min~60min,然后以卸压速度为0.2t/s~0.5t/s卸压。其它与具体实施方式一至九相同。
采用以下实施例验证本发明的有益效果:
实施例一:
一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法,它是按以下步骤进行的:
一、在手套箱内称取Si粉、h-BN及石墨,并将称取的Si粉、h-BN及石墨装入球磨罐中,再在氩气气氛及球磨转速为600rpm及球料比为20:1的条件进行高能球磨20h,得到非晶相SiBCN粉体;
所述的Si粉与h-BN的摩尔比为2:1;所述的Si粉与石墨的摩尔比为2:3;
二、在直径为20mm的石墨模具内套的底面铺一层1.2g非晶相SiBCN粉体,上下震动使粉体平铺,然后在压力为3MPa的条件下,用上压头将粉体压实,在压实的粉体上铺上一层4gTa4HfC5粉体,上下震动使粉体平铺,再在压力为3MPa的条件下,用上压头将粉体压实,重复交替非晶相SiBCN粉体和Ta4HfC5粉体的铺平及压实,直至达到3层非晶相SiBCN粉体和2层Ta4HfC5粉体,得到装填好粉体的模具;
三、将装填好粉体的模具进行预压,然后在氩气气氛及升温速率为25℃/min的条件下,将预压后的粉体升温至烧结温度为1400℃,再在氩气气氛、升温速率为25℃/min及加压速度为1.1MPa/min的条件下,将烧结温度继续升温至2100℃,且加压至30MPa,最后在氩气气氛、烧结温度为2100℃及压力为30MPa的条件下,保持2h,以卸压速度为1.1MPa/min泄压并随炉冷却,得到Ta4HfC5/SiBCN扩散偶。
步骤二中所述的Ta4HfC5粉体和非晶相SiBCN粉体为通过200目筛后得到的粉体。
步骤二中所述的石墨模具内套为高强石墨模具内套。
步骤二中所述的石墨模具内套的内表面设置厚度为0.03mm的石墨纸;步骤二中所述的压实为利用上压头将粉体压实,且压实过程中用厚度为0.2mm的石墨纸将粉体与上压头分隔。
步骤三中所述的预压具体是按以下步骤进行:在压力机下,以加压速度为0.05t/s,将装填好粉体的模具加压至1.2t,并在压力为1.2t的条件下,保压20min,然后以卸压速度为0.4t/s卸压。
实施例一步骤一中原料为单质硅(Si),六方氮化硼(h-BN)及石墨。步骤二中所述的Ta4HfC5粉体为购买的商业粉体;步骤二中每层称取对应4gTa4HfC5粉体或1.2g非晶相SiBCN粉体,保证烧结过后每层具有相似的厚度(≈2mm)。
将实施例一制备的Ta4HfC5/SiBCN扩散偶沿轴向切割出截面,依次使用500目及800目金刚石磨盘打磨,然后依次使用1000目、1500目及2000目砂纸进行打磨,最后使用粒径为0.25μm金刚石抛光剂,并在转速为1000rpm的条件下进行抛光处理,将抛光后的样品使用酒精超声清洗后烘干,得到抛光后的Ta4HfC5/SiBCN扩散偶。
图2为实施例一制备的Ta4HfC5/SiBCN扩散偶切割前的光学照片;图3为实施例一制备的Ta4HfC5/SiBCN扩散偶切割后截面的光学照片;由图可知,烧结后得到五层扩散偶试样结合紧密,界面结合强度可满足后续机械加工。
图4为实施例一抛光后的Ta4HfC5/SiBCN扩散偶界面微观形貌SEM图。由图可知,界面处结合紧密,呈现啮齿状特征。
图5为实施例一抛光后的Ta4HfC5/SiBCN扩散偶SEM和原子相对含量随扩散距离曲线。由图可知,在实施例一工艺下制备的扩散偶界面处发生了明显的Si、Hf、Ta原子的扩散行为。
图6为实施例一抛光后的Ta4HfC5/SiBCN扩散偶界面的XRD图。由图可知,界面处主要由Ta4HfC5相以及非晶SiBCN析晶相组成。
图7为实施例一制备的Ta4HfC5/SiBCN扩散偶界面的“啮合”形貌示意图;本实施例制备的五层扩散偶界面具有“啮合”特征,经机械加工后能够保持相连状态,界面处形成较强结合。
对比实验:本对比实验与实施例一不同的是:步骤三中在氩气气氛、升温速率为25℃/min及加压速度为1.1MPa/min的条件下,将烧结温度继续升温至1700℃,且加压至30MPa,最后在氩气气氛、烧结温度为1700℃及压力为30MPa的条件下,保持2h。其它与实施例一相同。
对比实验烧结温度为1700℃,扩散偶间的结合强度较低,机械加工时沿着两种材料的界面发生开裂,且界面处的扩散行为不明显。
实施例二:本实施例与实施例一不同的是:步骤二中将Ta4HfC5粉体烧结得到Ta4HfC5块体,将Ta4HfC5块体及非晶相SiBCN粉体装填于石墨模具内套内,且Ta4HfC5块体埋于非晶相SiBCN粉体内部并压实,得到装填好粉体的模具;
所述的Ta4HfC5块体是按以下步骤制备:在氩气气氛及升温速率为25℃/min的条件下,升温至烧结温度为1400℃,再在氩气气氛、升温速率为25℃/min及加压速度为1.25MPa/min的条件下,将烧结温度继续升温至2000℃,且加压至30MPa,最后在氩气气氛、烧结温度为2000℃及压力为30MPa的条件下,保持1h,以卸压速度为1.25MPa/min卸压并随炉冷却,得到陶瓷,将陶瓷切割成六面的块体,并对六面分别进行打磨和抛光处理;所述的打磨和抛光处理具体为依次使用500目及1000目金刚石磨盘打磨,然后依次使用1000目、1500目及2000目砂纸打磨,最后使用粒径为0.25μm的金刚石抛光剂抛光。其他与实施例一相同。
将实施例二制备的Ta4HfC5/SiBCN扩散偶打磨去掉表面SiBCN陶瓷,露出内部Ta4HfC5块体,并进行光学照片拍摄。图8为实施例二打磨去掉表面SiBCN陶瓷后的Ta4HfC5/SiBCN扩散偶光学照片。图中黄色芯部是Ta4HfC5陶瓷块体,黑色是SiBCN陶瓷,二者具有较好的结合。
Claims (2)
1.一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法,其特征在于,按以下步骤进行:
一、高能球磨制备非晶相SiBCN粉体;
二、在石墨模具内套的底面铺一层非晶相SiBCN粉体,上下震动使粉体平铺,然后用上压头将粉体压实,在压实的粉体上铺上一层Ta4HfC5粉体,上下震动使粉体平铺, 再用上压头将粉体压实,重复交替非晶相SiBCN粉体和Ta4HfC5粉体的铺平及压实,直至达到3层非晶相SiBCN粉体和2层Ta4HfC5粉体,得到装填好粉体的模具;
或者将Ta4HfC5粉体烧结得到Ta4HfC5块体,将Ta4HfC5块体及非晶相SiBCN粉体装填于石墨模具内套内,且Ta4HfC5块体埋于非晶相SiBCN粉体内部并压实,得到装填好粉体的模具;
或者将非晶相SiBCN粉体烧结得到SiBCN块体,将SiBCN块体及Ta4HfC5粉体装填于石墨模具内套内,且SiBCN块体埋于Ta4HfC5粉体内部并压实,得到装填好粉体的模具;
所述的Ta4HfC5块体及SiBCN块体均是按以下步骤制备:在氩气气氛及升温速率为20℃/min~25℃/min的条件下,升温至烧结温度为1400℃~1550℃,再在氩气气氛、升温速率为20℃/min~25℃/min及加压速度为1MPa/min~4MPa/min的条件下,将烧结温度继续升温至1600℃~2100℃,且加压至30MPa~40MPa,最后在氩气气氛、烧结温度为1600℃~2100℃及压力为30MPa~40MPa的条件下,保持0.5h~1h,以卸压速度为1MPa/min~4MPa/min卸压并随炉冷却,得到陶瓷,将陶瓷切割成六面的块体,并对六面分别进行打磨和抛光处理;
所述的Ta4HfC5粉体和非晶相SiBCN粉体为通过200目筛后得到的粉体;
三、在压力机下,以加压速度为0.05t/s~0.1t/s,将装填好粉体的模具加压至1t~5t,并在压力为1t~5t的条件下,保压10min~60min,然后以卸压速度为0.2t/s~0.5t/s卸压,然后在氩气气氛及升温速率为20℃/min~25℃/min的条件下,将预压后的粉体升温至烧结温度为1400℃~1600℃,再在氩气气氛、升温速率为20℃/min~25℃/min及加压速度为1MPa/min~8MPa/min的条件下,将烧结温度继续升温至1800℃~2100℃,且加压至30MPa~60MPa,最后在氩气气氛、烧结温度为1800℃~2100℃及压力为30MPa~60MPa的条件下,保持1~2h,以卸压速度为1MPa/min~4MPa/min泄压并随炉冷却,即得到碳化钽铪-硅硼碳氮陶瓷扩散偶;
步骤一中高能球磨制备非晶相SiBCN粉体具体是按以下步骤进行:在手套箱内称取Si粉、h-BN及石墨,并将称取的Si粉、h-BN及石墨装入球磨罐中,再在氩气气氛及球磨转速为600rpm~800rpm及球料比为(10~20):1的条件进行高能球磨20h~40h,得到非晶相SiBCN粉体;所述的Si粉与h-BN的摩尔比为1:(0.5~1);所述的Si粉与石墨的摩尔比为1:(1~2);
步骤二中所述的石墨模具内套的内表面设置厚度为0.01mm~0.03mm的石墨纸;步骤二中所述的压实为利用上压头将粉体压实,且压实过程中用厚度为0.1mm~0.5mm的石墨纸将粉体与上压头分隔。
2.根据权利要求1所述的一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法,其特征在于所述的打磨和抛光处理具体为依次经过500目~3000目金刚石磨盘打磨、500目~3000目砂纸打磨及粒径为0.25μm的金刚石抛光剂抛光。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202310515235.3A CN116477952B (zh) | 2023-05-09 | 2023-05-09 | 一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202310515235.3A CN116477952B (zh) | 2023-05-09 | 2023-05-09 | 一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN116477952A CN116477952A (zh) | 2023-07-25 |
CN116477952B true CN116477952B (zh) | 2024-05-17 |
Family
ID=87216357
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202310515235.3A Active CN116477952B (zh) | 2023-05-09 | 2023-05-09 | 一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN116477952B (zh) |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104843646A (zh) * | 2015-04-08 | 2015-08-19 | 昆明理工大学 | 一种金属氧化物扩散偶的制备方法 |
CN111196726A (zh) * | 2020-01-06 | 2020-05-26 | 哈尔滨工业大学 | 一种SiBCN-Ta4HfC5复相陶瓷及其制备方法 |
CN111217610A (zh) * | 2019-06-19 | 2020-06-02 | 哈尔滨工业大学 | 一种纳米晶碳化钽增强硅硼碳氮复相陶瓷材料及其制备方法 |
CN111689778A (zh) * | 2020-06-30 | 2020-09-22 | 哈尔滨工业大学 | 一种高致密SiBCN陶瓷材料及其制备方法 |
CN115849890A (zh) * | 2022-11-25 | 2023-03-28 | 东北大学 | 一种五氧化二钒/氧化钙扩散偶的制备方法 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110845238A (zh) * | 2019-11-29 | 2020-02-28 | 中南大学 | 一种长时耐烧蚀超高熔点含氮碳化物超高温陶瓷及其应用 |
-
2023
- 2023-05-09 CN CN202310515235.3A patent/CN116477952B/zh active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104843646A (zh) * | 2015-04-08 | 2015-08-19 | 昆明理工大学 | 一种金属氧化物扩散偶的制备方法 |
CN111217610A (zh) * | 2019-06-19 | 2020-06-02 | 哈尔滨工业大学 | 一种纳米晶碳化钽增强硅硼碳氮复相陶瓷材料及其制备方法 |
CN111196726A (zh) * | 2020-01-06 | 2020-05-26 | 哈尔滨工业大学 | 一种SiBCN-Ta4HfC5复相陶瓷及其制备方法 |
CN111689778A (zh) * | 2020-06-30 | 2020-09-22 | 哈尔滨工业大学 | 一种高致密SiBCN陶瓷材料及其制备方法 |
CN115849890A (zh) * | 2022-11-25 | 2023-03-28 | 东北大学 | 一种五氧化二钒/氧化钙扩散偶的制备方法 |
Also Published As
Publication number | Publication date |
---|---|
CN116477952A (zh) | 2023-07-25 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
KR102208400B1 (ko) | 경사 기능 재료로 이루어진 신규한 조성물을 갖는 금속 또는 세라믹 물품의 성형방법과 그 성형방법을 포함하는 물품 | |
KR100260368B1 (ko) | 복합재와 그의 제조방법 | |
US9327385B2 (en) | Near-net cutting tool insert | |
US4110084A (en) | Composite of bonded cubic boron nitride crystals on a silicon carbide substrate | |
JP6257896B2 (ja) | 高靭性マトリックス材料中の固結された高靭性被覆硬質粒子 | |
JP2011520031A (ja) | 超硬質強化超硬合金 | |
JPH09194909A (ja) | 複合材料およびその製造方法 | |
WO2004007401A1 (ja) | 炭化ケイ素基複合材料とその製造方法、および炭化ケイ素基複合材料部品の製造方法 | |
Ding et al. | Fabrication and wear characteristics of open-porous cBN abrasive wheels in grinding of Ti–6Al–4V alloys | |
WO2018136631A2 (en) | Composite carbide compositions and methods of making the same | |
WO2004054943A1 (ja) | 耐熱性ダイヤモンド複合焼結体とその製造法 | |
CN116477952B (zh) | 一种碳化钽铪-硅硼碳氮陶瓷扩散偶的制备方法 | |
CN103477019A (zh) | 形成多晶材料的方法,包括在hpht 加工前提供具有超级研磨剂晶粒的材料,和通过这样的方法形成的多晶压实体和切割元件 | |
USRE30503E (en) | Composite of bonded cubic boron nitride crystals on a silicon carbide substrate | |
US11873256B2 (en) | Polycrystalline diamond with iron-containing binder | |
JP3221180B2 (ja) | セラミックス−金属接合体及びその製造方法 | |
JPH06504585A (ja) | 真正或いは擬似の均衡加圧法 | |
CN115703683B (zh) | 一种高强高导热大尺寸氮化硅陶瓷及其制备方法 | |
CN118271089A (zh) | 超硬高强的仿生叠层金刚石-B4C-SiC/Si3N4-SiC陶瓷复合材料制备方法 | |
CN113977469A (zh) | 一种陶瓷骨架增强金属基复合结合剂的制备方法 | |
CA1111664A (en) | Polycrystalline diamond body/silicon carbide or silicon nitride substrate composite | |
WO2001016249A1 (en) | Abrasive material comprising elongate abrasive bodies | |
CA1103940A (en) | Cubic boron nitride abrasive composite |
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 | ||
GR01 | Patent grant | ||
GR01 | Patent grant |