CN104507603A - Polycrystalline cubic boron nitride (pcbn) body made with distinct layers of pcbn - Google Patents
Polycrystalline cubic boron nitride (pcbn) body made with distinct layers of pcbn Download PDFInfo
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Abstract
Description
相关申请的交叉参考Cross References to Related Applications
本申请要求2012年7月12日提交的临时申请61/670676的优先权。This application claims priority to provisional application 61/670676, filed July 12, 2012.
技术领域technical field
本发明涉及一种多晶立方氮化硼(PcBN)体。更特别地,本发明涉及一种使用以下方法制造的PcBN体,该方法包括覆盖(overlay)立方氮化硼(cBN)粉末的层或预先压实的盘材(pre-compacted disk),其中所述层具有与不同浓度的陶瓷混合的cBN。The invention relates to a polycrystalline cubic boron nitride (PcBN) body. More particularly, the present invention relates to a PcBN body manufactured using a method comprising overlaying a layer or pre-compacted disk of cubic boron nitride (cBN) powder, wherein the The layers have cBN mixed with different concentrations of ceramics.
背景技术Background technique
在下文的讨论中,参照特定的结构和/或方法。然而,以下的参照不应当被解读为承认这些结构和/或方法构成了现有技术。申请人明确地保留证明这样的结构和/或方法不作为现有技术反对本发明的权利。In the discussion that follows, reference is made to specific structures and/or methods. However, the following references should not be construed as an admission that these structures and/or methods constitute prior art. Applicant expressly reserves the right to demonstrate that such structures and/or methods do not constitute prior art against the present invention.
在常规的多晶立方氮化硼制造方法中,基底邻接PcBN层,该PcBN层以其整体由单一品级(即,cBN是该层中的主要材料)制成。由于在所述品级中期望的和通常竞争的特征,对于一个特征,例如韧性,的优化可能会导致另一种特征,例如焊接稳定性或耐磨性,的劣化。In conventional polycrystalline cubic boron nitride manufacturing methods, the substrate adjoins a PcBN layer which is made in its entirety of a single grade (ie, cBN is the predominant material in the layer). Due to desirable and often competing characteristics in the grades, optimization for one characteristic, such as toughness, may result in a deterioration of another characteristic, such as welding stability or wear resistance.
因此,需要改进的PcBN制造方法,该方法制造的PcBN体具有所述期望的特征,而不会为了加强另一种特征而劣化所述期望的特征中的一种或多种。Therefore, there is a need for an improved method of PcBN fabrication that produces a PcBN body having the desired characteristics without degrading one or more of the desired characteristics in order to enhance another characteristic.
发明内容Contents of the invention
本发明描述了一种改进的PcBN制造方法和使用该改进方法制造的PcBN体。The present invention describes an improved method of manufacturing PcBN and PcBN bodies made using the improved method.
在一个实施方式中,方法包括在难熔容器中沉积以下物质:基底(例如,含有钴(Co)),立方氮化硼(cBN),以及cBN和陶瓷的混合物。所沉积的cBN以及cBN和陶瓷的混合物可以是粉末或预先压实的盘材。所沉积的基底、cBN以及cBN和陶瓷的混合物构成所述难熔容器中的内容物(content)。在所述沉积步骤期间,在具有所述cBN和陶瓷的混合物的层中的cBN的浓度,低于在其下面沉积的层中的cBN的浓度。在沉积所述内容物之后,向所述难熔容器中的内容物施加高压和高温(HPHT)。在施加HPHT时,例如,所述基底中的Co首先扩散穿过所述cBN层,即,由所述Co扫掠(sweep)所述cBN层。在一些实施方式中,所述Co也可以扫掠过所述具有cBN和陶瓷的混合物的层。In one embodiment, a method includes depositing in a refractory vessel: a substrate (eg, containing cobalt (Co)), cubic boron nitride (cBN), and a mixture of cBN and ceramic. Deposited cBN and mixtures of cBN and ceramic can be powder or pre-compacted discs. The deposited substrate, cBN and the mixture of cBN and ceramic constitute the content in the refractory vessel. During said depositing step, the concentration of cBN in the layer having said mixture of cBN and ceramic is lower than the concentration of cBN in the layer deposited below it. After depositing the contents, high pressure and high temperature (HPHT) is applied to the contents in the refractory vessel. When HPHT is applied, for example, Co in the substrate first diffuses through the cBN layer, ie, the cBN layer is swept by the Co. In some embodiments, the Co may also be swept across the layer with a mixture of cBN and ceramic.
在一些实施方式中,以相反的顺序沉积所述内容物,开始于所述cBN和陶瓷的混合物,所述cBN,和所述基底(例如含有钴(Co))。在所述沉积步骤期间,在具有cBN和陶瓷的混合物的层中的cBN的浓度低于在其上面沉积的层中的cBN的浓度。在以相反的顺序沉积所述内容物之后,向所述难熔容器的内容物施加HPHT。在施加HPHT时,例如,所述基底的钴扫掠过所述cBN层。在一些实施方式中,所述Co也可以扫掠过所述具有cBN和陶瓷的混合物的层。In some embodiments, the contents are deposited in reverse order, starting with the cBN and ceramic mixture, the cBN, and the substrate (eg, containing cobalt (Co)). During said depositing step, the concentration of cBN in the layer with the mixture of cBN and ceramic is lower than the concentration of cBN in the layer deposited thereon. After depositing the contents in reverse order, HPHT is applied to the contents of the refractory container. Upon application of HPHT, for example, the cobalt of the substrate is swept across the cBN layer. In some embodiments, the Co may also be swept across the layer with a mixture of cBN and ceramic.
在另一种实施方式中,由包括以下步骤的方法制备多晶立方氮化硼(PcBN)体。在难熔容器中沉积基底(例如,含有钴(Co)),立方氮化硼(cBN),以及cBN和陶瓷的混合物。所沉积的cBN以及cBN和陶瓷的混合物可以是粉末或预先压实的盘材。在沉积所述内容物之后,然后向所述难熔容器中的内容物施加高压和高温(HPHT)。在所述沉积步骤期间,在所述具有cBN粉末和陶瓷粉末的混合物的层中的cBN的浓度低于在其下面沉积的层中的cBN的浓度。在施加HPHT时,例如,所述基底的Co扩散穿过所述cBN粉末。在一些实施方式中,所述Co也可以扫掠过所述具有cBN和陶瓷的混合物的层。In another embodiment, a polycrystalline cubic boron nitride (PcBN) body is prepared by a method comprising the following steps. Substrates (eg, containing cobalt (Co)), cubic boron nitride (cBN), and mixtures of cBN and ceramics are deposited in refractory vessels. Deposited cBN and mixtures of cBN and ceramic can be powder or pre-compacted discs. After depositing the contents, high pressure and high temperature (HPHT) is then applied to the contents in the refractory vessel. During said depositing step, the concentration of cBN in said layer with the mixture of cBN powder and ceramic powder is lower than the concentration of cBN in the layer deposited below it. Upon application of HPHT, for example, the Co of the substrate diffuses through the cBN powder. In some embodiments, the Co may also be swept across the layer with a mixture of cBN and ceramic.
在一些实施方式中,以相反的顺序施加所述内容物的沉积,开始于所述cBN和陶瓷的混合物,所述cBN,和所述基底(例如含有钴(Co))。In some embodiments, the deposition of the contents is applied in reverse order, starting with the cBN and ceramic mixture, the cBN, and the substrate (eg, containing cobalt (Co)).
至少Co例如扩散穿过第一个中间扩散(inter-diffusion)层(即,在所述基底和第一PcBN层之间),和在一些实施方式中,扩散穿过第二中间扩散层(即,在所述第一PcBN层和在其上的第二PcBN层之间),这种扩散在烧结过程中导致所述基底熔接(fusion)至与它邻接的PcBN层,和熔接至邻接的任何另外的PcBN层。在HPHT的施加结束和所述难熔容器的内容物冷却后,所述方法产生了如下的PcBN体,该PcBN体具有含有不同浓度的cBN和陶瓷材料的层(即,不同的PcBN层)。可以通过调节与所述基底邻接的每个PcBN层中的cBN和陶瓷材料的浓度,来控制所产生的PcBN体的期望的特征。At least Co diffuses, for example, through a first inter-diffusion layer (i.e., between the substrate and the first PcBN layer), and in some embodiments, through a second inter-diffusion layer (i.e. , between the first PcBN layer and the second PcBN layer thereon), this diffusion during sintering causes the substrate to fuse (fusion) to its adjacent PcBN layer, and to any adjacent PcBN layer Additional PcBN layer. After the application of HPHT has ended and the contents of the refractory container have cooled, the method produces a PcBN body with layers containing different concentrations of cBN and ceramic material (ie different PcBN layers). The desired characteristics of the resulting PcBN body can be controlled by adjusting the concentrations of cBN and ceramic material in each PcBN layer adjacent to the substrate.
附图说明Description of drawings
可以参照附图理解优选实施方式的以下详述,附图中相同的数字代表相同的元件,并且其中:The following detailed description of the preferred embodiment can be understood with reference to the accompanying drawings, in which like numerals represent like elements, and in which:
图1显示,通过60×扫描电子显微镜(SEM),使用所公开方法制造的未抛光的PcBN体的截面。Figure 1 shows, by 6Ox scanning electron microscopy (SEM), a cross-section of an unpolished PcBN body fabricated using the disclosed method.
图2a显示,通过60×SEM,使用所公开方法制造的抛光的PcBN体的截面。Figure 2a shows, by 6Ox SEM, a cross-section of a polished PcBN body fabricated using the disclosed method.
图2b-e显示,通过1000×SEM,使用所公开方法制造的抛光的PcBN体的不同层和中间层(inter-layer)界面的多个截面。Figures 2b-e show, by 1000x SEM, multiple cross-sections of different layer and inter-layer interfaces of a polished PcBN body fabricated using the disclosed method.
图2f-g显示了可以用于容纳根据一些实施方式的沉积内容物的难熔容器(杯体)。Figures 2f-g show refractory containers (cups) that may be used to hold deposited contents according to some embodiments.
图3a显示了使用所公开方法制造的PcBN体的使用能量弥散x射线(EDX)光谱线扫描产生的Ti K荧光x射线强度的图。Figure 3a shows a plot of Ti K fluorescence x-ray intensity generated using energy dispersive x-ray (EDX) spectral line scans of PcBN bodies fabricated using the disclosed method.
图3b显示了使用所公开方法制造的PcBN体的使用能量弥散x射线(EDX)光谱线扫描产生的Co K荧光x射线强度的图。Figure 3b shows a plot of Co K fluorescence x-ray intensity generated using energy dispersive x-ray (EDX) spectroscopic line scans of PcBN bodies fabricated using the disclosed method.
图4显示了制造PcBN体的改进方法的步骤的流程图。Figure 4 shows a flow chart of the steps of an improved method of making a PcBN body.
图5显示了制造PcBN体的另一种改进方法的步骤的流程图。Figure 5 shows a flow chart of the steps of another improved method of making a PcBN body.
发明详述Detailed description of the invention
此处描述的实施方式的目的是示例说明一种PcBN制造方法,以及由此类方法制造的PcBN体,其中所产生的PcBN体具有期望的特征,该期望的特征是在不为了加强另一种特征而劣化所期望特征中的的一种或多种的情况下获得的。The purpose of the embodiments described here is to illustrate a method of PcBN fabrication, and a PcBN body produced by such a method, wherein the PcBN body produced has desirable characteristics that are not intended to enhance another obtained without degrading one or more of the desired characteristics.
因此,实施方式涉及制造多晶立方氮化硼(PcBN)体的方法,其通过使用穿过不同堆叠层的不同浓度的cBN粉末和陶瓷粉末而改进所述PcBN体的焊接特征,从而充分地消除了由于相关技术的限制和不足而导致的一种或多种问题。Accordingly, embodiments relate to methods of fabricating polycrystalline cubic boron nitride (PcBN) bodies that substantially eliminate One or more problems due to limitations and deficiencies in the related art are addressed.
图1显示了使用一种改进方法制造的未抛光的PcBN体101的EDM切割截面。该截面显示了在HPHT烧结后所产生的材料。紧接着硬质合金(WC/Co)基底102,存在cBN层103(高cBN材料),和邻接的cBN和陶瓷的混合物层104(低cBN层)。cBN层103具有比低cBN层104低的陶瓷浓度。Figure 1 shows an EDM cut section of an unpolished PcBN body 101 fabricated using a modified method. This section shows the resulting material after HPHT sintering. Next to the cemented carbide (WC/Co) substrate 102 there is a cBN layer 103 (high cBN material), and an adjoining layer 104 of a mixture of cBN and ceramic (low cBN layer). The cBN layer 103 has a lower ceramic concentration than the low cBN layer 104 .
制造该未抛光的PcBN体101的方法包括在难熔容器中沉积以下物质:基底102,立方氮化硼(高cBN)粉末,以及cBN和陶瓷粉末的混合物层(低cBN),然后对所述难熔容器的内容物施加高压和高温(HPHT)。基底102的合适例子包括金属钴(Co)、硬质合金(WC/Co)、金属陶瓷((W,Ti)(C,N)/(Co,Ni))、硅(Si)或镍(Ni)。在一些实施方式中,所述高cBN的沉积层和所述低cBN层可以是粉末或预先压实的盘材。The method of making this unpolished PcBN body 101 involves depositing the following in a refractory vessel: a substrate 102, cubic boron nitride (high cBN) powder, and a mixture layer of cBN and ceramic powder (low cBN), and then depositing the The contents of the refractory container are subjected to high pressure and high temperature (HPHT). Suitable examples of substrate 102 include metallic cobalt (Co), cemented carbide (WC/Co), cermets ((W,Ti)(C,N)/(Co,Ni)), silicon (Si), or nickel (Ni ). In some embodiments, the high cBN deposited layer and the low cBN layer may be a powder or a pre-compacted disc.
在一些实施方式中,预先压实的盘材,也称为预烧结体,可以使用如下的一种或多种方法来制造,其公开在2004年1月13日授权的美国专利6676893B2,“Porous Cubic Boron Nitride Based MaterialSuitable for Subsequent Production of Cutting Tools and Method for itsProduction”(适用于切削工具的后续生产的基于多孔立方氮化硼的材料以及其生产方法)中,在此处以参考方式将该专利引入本文。In some embodiments, pre-compacted discs, also known as pre-sintered bodies, may be fabricated using one or more of the following methods, which are disclosed in US Patent 6,676,893 B2, issued January 13, 2004, "Porous Cubic Boron Nitride Based MaterialSuitable for Subsequent Production of Cutting Tools and Method for itsProduction" (applicable to the subsequent production of cutting tools based on porous cubic boron nitride material and its production method), which is incorporated herein by reference .
在一些实施方式中,所述难熔容器可以由钽(Ta)或钼(Mo)箔片材/卷材(foil sheet/wrap),或IV-VI族(grade)的任何其它过渡金属形成。钽难熔容器(杯体)的实施方式显示在图2f-g中。图2f示例说明了具有非折边顶部的钽金属容器(杯体)。图2g示例说明了具有折边顶部的钽难熔容器(杯体)。In some embodiments, the refractory vessel may be formed from tantalum (Ta) or molybdenum (Mo) foil sheet/wrap, or any other transition metal of grades IV-VI. Embodiments of tantalum refractory containers (cups) are shown in Figures 2f-g. Figure 2f illustrates a tantalum metal container (cup) with a non-collared top. Figure 2g illustrates a tantalum refractory container (cup) with a folded top.
在一些实施方式中,在所述低cBN粉末中的cBN的浓度低于所述高cBN粉末中的浓度。In some embodiments, the concentration of cBN in the low cBN powder is lower than the concentration in the high cBN powder.
所述陶瓷粉末可以例如包括氮化钛(TiN)或氧化铝(Al2O3)或Ti2AlN。在不背离所描述实施方式的范围的情况下也可使用其它陶瓷。例如,可以使用例如AlN、TiC、TiCN、ZrN、ZrO2、HfO2的陶瓷或IV-VI族的任何其它过渡金属如Me(C,N,O)。The ceramic powder may for example comprise titanium nitride (TiN) or aluminum oxide (Al 2 O 3 ) or Ti 2 AlN. Other ceramics may also be used without departing from the scope of the described embodiments. For example, ceramics such as AlN, TiC, TiCN, ZrN, ZrO 2 , HfO 2 or any other transition metal of groups IV-VI such as Me(C,N,O) may be used.
所述高cBN粉末具有例如约90%的高cBN含量。层103含有约90%的cBN和约10%的一种或多种的一些其它材料,其可以包括所述陶瓷。在一些实施方式中,cBN层103还可以例如包含约10%的相对低浓度的陶瓷,例如TiN或Al2O3。此外,所述低cBN层104可例如具有约50%的cBN含量。层104还可以例如包含约50%的相对高含量的陶瓷,例如TiN或Al2O3。The high cBN powder has, for example, a high cBN content of about 90%. Layer 103 contains about 90% cBN and about 10% of one or more of some other material, which may include the ceramic. In some embodiments, the cBN layer 103 may also contain a relatively low concentration of ceramics, such as TiN or Al 2 O 3 , for example, about 10%. Furthermore, the low cBN layer 104 may, for example, have a cBN content of about 50%. Layer 104 may also comprise a relatively high content of ceramics, such as TiN or Al 2 O 3 , for example about 50%.
当对所述难熔容器的内容物102-104施加HPHT以开始烧结时,基底102的Co首先扩散穿过cBN粉末层103,和然后,在一些实施方式中,扩散穿过cBN粉末和陶瓷粉末的混合物层104。因此,在一些实施方式中,可以形成两个中间扩散层。在基底102和高cBN层103之间的第一中间扩散层和在高cBN层103和低cBN层104之间的第二中间扩散层。基底材料(例如,Co)穿过所述两个中间扩散层的扩散,例如导致基底102熔接至与它邻接的的高cBN层103,以及与cBN层103邻接的一个或多个任何另外的PcBN层,例如低cBN层104。When HPHT is applied to the contents 102-104 of the refractory vessel to initiate sintering, the Co of the substrate 102 first diffuses through the cBN powder layer 103, and then, in some embodiments, diffuses through the cBN powder and the ceramic powder layer 104 of the mixture. Thus, in some embodiments, two intermediate diffusion layers may be formed. A first intermediate diffusion layer between the substrate 102 and the high cBN layer 103 and a second intermediate diffusion layer between the high cBN layer 103 and the low cBN layer 104 . Diffusion of the substrate material (e.g., Co) through the two intermediate diffusion layers, for example, results in fusion of the substrate 102 to the high cBN layer 103 adjoining it, and to one or more further PcBN layers adjoining the cBN layer 103 layer, such as the low cBN layer 104.
在HPHT结束和所述难熔容器中的内容物冷却后,所述方法产生了具有如下层的PcBN体,所述层具有不同浓度的cBN和陶瓷材料(即,不同的PcBN层)。可以通过调节在与基底层102邻接的每个PcBN层中的cBN和陶瓷材料的浓度,来控制所产生PcBN体的期望特征。在一些实施方式中,高cBN层103具有约86-99%体积的cBN和88-96%体积的cBN,以及具有约2-8%陶瓷含量的金属粘结剂。在一些实施方式中,低cBN层104在HPHT后具有约35-85%体积的cBN和陶瓷特征的粘结剂。After the end of HPHT and cooling of the contents in the refractory vessel, the process produces a PcBN body with layers having different concentrations of cBN and ceramic material (ie, different PcBN layers). The desired characteristics of the resulting PcBN body can be controlled by adjusting the concentrations of cBN and ceramic material in each PcBN layer adjacent to the base layer 102 . In some embodiments, the high cBN layer 103 has about 86-99% cBN and 88-96% cBN by volume, and a metal binder with a ceramic content of about 2-8%. In some embodiments, the low cBN layer 104 has about 35-85% by volume cBN and a binder of ceramic character after HPHT.
在使用一种改进方法制造的未抛光的PcBN体101的截面中,对应于基底102的层厚度的第一量,可例如约在0.0mm和8mm之间。对应于高cBN层103厚度的第二量,例如约在0.3mm和3.2mm之间,和约在0.5mm和1.0mm之间。对应于低cBN层104的厚度的第三量,可例如约在0.2mm和3.2mm之间,和约在0.3mm和1.0mm之间。In a cross-section of an unpolished PcBN body 101 produced using a modified method, the first amount, corresponding to the layer thickness of the substrate 102, may for example be approximately between 0.0 mm and 8 mm. The second amount corresponds to the thickness of the high cBN layer 103, for example between about 0.3 mm and 3.2 mm, and between about 0.5 mm and 1.0 mm. The third amount, corresponding to the thickness of the low cBN layer 104, may, for example, be between about 0.2 mm and 3.2 mm, and between about 0.3 mm and 1.0 mm.
图2a显示了使用60×扫描电子显微镜(SEM),使用所述改进方法制造的抛光的PcBN体201的截面。如所显示的,该抛光的PcBN体201具有第一WC/Co硬质合金基底层202,第二高cBN层203,和第三低cBN层204。在该实施例中,碳化物基底层202(没有显示其整体)具有约4mm的厚度。第二cBN粉末层203具有约0.6mm的厚度。第三低cBN层204具有约0.4mm的厚度。抛光的PcBN体201使用前面描述的方法来制造。在HPHT后,EDM切割该所述体201,和抛光所述截面,以促进显微镜检查。使用标准的金相方法完成抛光。Figure 2a shows a cross-section of a polished PcBN body 201 fabricated using the modified method using a 6Ox scanning electron microscope (SEM). As shown, the polished PcBN body 201 has a first WC/Co cemented carbide base layer 202 , a second high cBN layer 203 , and a third low cBN layer 204 . In this embodiment, the carbide base layer 202 (its entirety not shown) has a thickness of about 4 mm. The second cBN powder layer 203 has a thickness of about 0.6 mm. The third low cBN layer 204 has a thickness of about 0.4 mm. A polished PcBN body 201 was fabricated using the method described previously. After HPHT, EDM cuts the body 201 and polishes the cross section to facilitate microscopic examination. Polishing is accomplished using standard metallographic methods.
图2b-e显示,通过1000×的较高放大率的SEM,使用所述改进方法制造的PcBN体201的不同层和中间层界面的多个截面。特别地,图2b显示了基底202-高cBN层203的界面205;图2c显示了第二层203在较高放大率下的206;图2d显示了高cBN层203-低cBN层204的界面207;以及图2e显示了低cBN层204在较高放大率下的208。Figures 2b-e show multiple cross-sections of different layer and interlayer interfaces of a PcBN body 201 fabricated using the improved method by SEM at a higher magnification of 100Ox. In particular, Figure 2b shows the substrate 202-high cBN layer 203 interface 205; Figure 2c shows the second layer 203 at a higher magnification 206; Figure 2d shows the high cBN layer 203-low cBN layer 204 interface 207; and Fig. 2e shows 208 of the low cBN layer 204 at a higher magnification.
在1000×放大率下容易看到所述碳化物的晶粒结构,所述Co(金属粘结剂)和浅灰色的陶瓷粘结剂(呈黑色的cBN晶粒)。基底202具有可见的明亮对比(visible light contrast)(参见图2b),这是由于其WC和Co内容物。第二层203以较高的放大率显示在图2e中206。黑色晶粒是cBN并且在所述粘结相中的明亮对比是由于Co从所述基底向中间扩散(interdiffuse),其也称为扫掠。第三层204在较高放大率下显示208。黑色晶粒是cBN并且灰色相是没有Co中间扩散的陶瓷粘结剂。基底层202到第二层203的界面205和第二层203到第三层204的界面207都是突变的(参见图2b和2d)。在所述PcBN体中没有显示裂纹或孔(参见图2b-e),这意味着好的粘结特征。The grain structure of the carbides, the Co (metallic binder) and the light gray vitrified binder (cBN grains in black) are easily seen at 1000× magnification. Substrate 202 has a visible light contrast (see Figure 2b) due to its WC and Co content. The second layer 203 is shown at 206 in Fig. 2e at a higher magnification. The black grains are cBN and the bright contrast in the binder phase is due to Co interdiffuse from the substrate, also known as sweeping. The third layer 204 is shown 208 at a higher magnification. The black grains are cBN and the gray phase is the ceramic binder without Co interdiffusion. Both the interface 205 of the base layer 202 to the second layer 203 and the interface 207 of the second layer 203 to the third layer 204 are abrupt (see Figures 2b and 2d). No cracks or pores were shown in the PcBN body (see Fig. 2b-e), implying good bonding characteristics.
图2f-g显示了可用于容纳根据一些实施方式的沉积内容物的难熔容器(杯体)210。图2f示例了由钽制成的并具有非折边顶部的难熔容器210。图2g示例了由钽制成的并具有折边顶部的难熔容器。在不背离所述实施方式的范围的情况下,可以使用不是图2f或图2g的其它难熔容器类型。Figures 2f-g show a refractory container (cup) 210 that may be used to hold deposition contents according to some embodiments. Fig. 2f illustrates a refractory container 210 made of tantalum and having a non-collared top. Figure 2g illustrates a refractory container made of tantalum with a folded top. Other refractory vessel types than Figure 2f or Figure 2g may be used without departing from the scope of the described embodiments.
图3a显示了使用所公开方法制造的PcBN体的使用能量弥散x射线(EDX)光谱产生的Ti K荧光x射线强度的图。图310是所述PcBN体的线扫描(沿着白线302),其定性地示例说明了穿过所述PcBN体的厚度的Ti的浓度。线扫描301沿着白线302从顶部取到底部。可以作为陶瓷TiN粘结的Ti没有显示任何扩散的证据,因为第二到第三层的界面303对应于图301中的空心箭头。第三层204中存在TiN,其朝向所述PcBN体的顶部/预期的工作表面,这种存在是为了增加所述PcBN层的化学稳定性和加强所述PcBN体,以用于其用途,例如在硬质部件车削应用中用作切削工具。第二层203中较高的cBN含量赋予所述材料较高的韧性和硬度。Figure 3a shows a plot of the Ti K fluorescence x-ray intensity generated using energy-dispersive x-ray (EDX) spectroscopy of a PcBN body fabricated using the disclosed method. Graph 310 is a line scan (along white line 302) of the PcBN body, qualitatively illustrating the concentration of Ti through the thickness of the PcBN body. Line scan 301 is taken from top to bottom along white line 302 . Ti, which can be bonded as ceramic TiN, does not show any evidence of diffusion, as the interface 303 of the second to third layer corresponds to the open arrow in diagram 301 . TiN is present in the third layer 204 towards the top/intended working surface of the PcBN body, this presence is to increase the chemical stability of the PcBN layer and strengthen the PcBN body for its use, e.g. Used as cutting tools in hard component turning applications. A higher cBN content in the second layer 203 imparts higher toughness and hardness to the material.
图3b显示了使用所公开方法制造的PcBN体的使用能量弥散x射线(EDX)光谱产生的Co K荧光x射线强度的图305。该图305是PcBN的线扫描,其定性地示例说明了穿过所述PcBN体的厚度的钴(Co)的浓度。线扫描306沿着白线305从顶部取到底部。Figure 3b shows a graph 305 of Co K fluorescence x-ray intensity generated using energy dispersive x-ray (EDX) spectroscopy for PcBN bodies fabricated using the disclosed methods. The graph 305 is a line scan of PcBN qualitatively illustrating the concentration of cobalt (Co) through the thickness of the PcBN body. Line scan 306 is taken along white line 305 from top to bottom.
在扫描电子显微镜中获得PcBN体的线扫描,该显微镜中电极产生与所述PcBN体中的Co浓度成比例的特征性x射线荧光。在这个实施例中,来自基底202的Co金属在所述基底层和所述第二层之间的第一界面308处富集,并且通过第二层203扩散过界面308,但是没有穿过第二界面307进入第三层204中。Line scans of the PcBN body were obtained in a scanning electron microscope in which electrodes produced a characteristic x-ray fluorescence proportional to the Co concentration in the PcBN body. In this example, Co metal from the substrate 202 is enriched at the first interface 308 between the substrate layer and the second layer, and diffuses through the second layer 203 across the interface 308, but not across the first interface 308. The second interface 307 enters the third layer 204 .
图4显示了制造多晶立方氮化硼(PcBN体)的改进方法的步骤401-404的流程图400。该方法包括:在难熔容器中沉积第一量的基底401;在所述难熔容器中沉积第二量的至少立方氮化硼(cBN)402;在所述难熔容器中沉积第三量的cBN和陶瓷的混合物403;和对难熔容器404的内容物施加高压和高温(HPHT),其中在所述第三量中的cBN的第一浓度低于在所述第二量中的cBN的第二浓度,和其中在施加HPHT时,所述基底的Co首先扩散穿过所述第二量的至少cBN,和然后扩散穿过所述第三量的cBN和陶瓷的混合物。Figure 4 shows a flowchart 400 of steps 401-404 of an improved method of making polycrystalline cubic boron nitride (PcBN body). The method comprises: depositing a first amount of substrate 401 in a refractory vessel; depositing a second amount of at least cubic boron nitride (cBN) 402 in said refractory vessel; depositing a third amount in said refractory vessel a mixture 403 of cBN and ceramic; and applying high pressure and high temperature (HPHT) to the contents of the refractory vessel 404, wherein the first concentration of cBN in said third amount is lower than that of cBN in said second amount and wherein upon application of HPHT, Co of the substrate first diffuses through the second amount of at least cBN, and then diffuses through the third amount of a mixture of cBN and ceramic.
在不背离本发明的范围的情况下,一个或多个步骤可以插入其中或者替换前述步骤401-404中的每个。One or more steps may be inserted into or substituted for each of the aforementioned steps 401-404 without departing from the scope of the present invention.
图5显示了制造PcBN体的另一种改进方法的步骤501-504的流程图500。该方法包括:在难熔容器中沉积第一量的立方氮化硼(cBN)和陶瓷的混合物501;在所述难熔容器中沉积第二量的至少cBN 502;在所述难熔容器中沉积第三量的基底503;和对所述难熔容器的内容物施加高压和高温(HPHT),其中在所述第一量中的cBN的第一浓度低于在所述第二量中的cBN的第二浓度,和其中在施加HPHT时,所述基底的Co首先扩散穿过所述第二量的至少cBN,和然后扩散穿过所述第一量的cBN和陶瓷的混合物504。此处的优点是所述难熔容器不需要另外的钽(Ta)层作为盖层。FIG. 5 shows a flowchart 500 of steps 501-504 of another improved method of making a PcBN body. The method comprises: depositing a first amount of a mixture of cubic boron nitride (cBN) and ceramic 501 in a refractory vessel; depositing a second amount of at least cBN 502 in said refractory vessel; depositing a third amount of substrate 503; and applying high pressure and high temperature (HPHT) to the contents of said refractory vessel, wherein a first concentration of cBN in said first amount is lower than in said second amount A second concentration of cBN, and wherein upon application of HPHT, Co of the substrate first diffuses through the second amount of at least cBN, and then diffuses through the mixture 504 of the first amount of cBN and ceramic. The advantage here is that the refractory container does not require an additional tantalum (Ta) layer as a capping layer.
在不背离本发明的范围的情况下,一个或多个步骤可以插入其中或者替换前述步骤501-504中的每个。One or more steps may be inserted into or substituted for each of the aforementioned steps 501-504 without departing from the scope of the present invention.
虽然已经结合本发明的优选实施方式描述了本发明,但是本领域普通技术人员能够理解,在不背离所附权利要求书中所限定的本发明的主旨和范围的情况下,可以进行未具体描述的增加、删除、改变和代替。Although the present invention has been described in conjunction with preferred embodiments of the present invention, those of ordinary skill in the art will understand that, without departing from the spirit and scope of the present invention as defined in the appended claims, modifications not specifically described may be made. additions, deletions, changes and substitutions.
Claims (38)
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| US201261670676P | 2012-07-12 | 2012-07-12 | |
| US61/670,676 | 2012-07-12 | ||
| PCT/US2013/048666 WO2014011420A1 (en) | 2012-07-12 | 2013-06-28 | POLYCRYSTALLINE CUBIC BORON NITRIDE (PcBN) BODY MADE WITH DISTINCT LAYERS OF PcBN |
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| CN104507603A true CN104507603A (en) | 2015-04-08 |
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| Country | Link |
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| US (1) | US20140017435A1 (en) |
| EP (1) | EP2872274A1 (en) |
| JP (1) | JP6377057B2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110757907A (en) * | 2018-07-27 | 2020-02-07 | 北京沃尔德金刚石工具股份有限公司 | PcBN composite sheet and preparation method thereof |
| CN118181886A (en) * | 2024-03-18 | 2024-06-14 | 上海新山田精密刀具有限公司 | Low-content PcBN composite sheet with multiple cBN layers |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP7755359B1 (en) * | 2025-04-16 | 2025-10-16 | 大学共同利用機関法人自然科学研究機構 | Method for manufacturing high melting point member having interface |
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| US20020112408A1 (en) * | 1999-04-07 | 2002-08-22 | Ulf Rolander | Porous cubic boron nitride based material suitable for subsequent production of cutting tools and method for its production |
| US20050249978A1 (en) * | 2004-04-02 | 2005-11-10 | Xian Yao | Gradient polycrystalline cubic boron nitride materials and tools incorporating such materials |
| CN2805902Y (en) * | 2005-06-23 | 2006-08-16 | 河南富耐克超硬材料有限公司 | Multi-layered stock container for production of super-hard polycrystalline patch |
| CN201105217Y (en) * | 2007-05-16 | 2008-08-27 | 上海美恩精密工具有限公司 | Feed charge body for superhard grinding production |
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| US4289503A (en) * | 1979-06-11 | 1981-09-15 | General Electric Company | Polycrystalline cubic boron nitride abrasive and process for preparing same in the absence of catalyst |
| JP2002235142A (en) * | 2001-02-05 | 2002-08-23 | Toshiba Tungaloy Co Ltd | DOUBLE LAYER cBN BASED SINTERED COMPACT AND HARD MEMBER |
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2013
- 2013-06-28 US US13/931,065 patent/US20140017435A1/en not_active Abandoned
- 2013-06-28 CN CN201380036609.8A patent/CN104507603A/en active Pending
- 2013-06-28 JP JP2015521649A patent/JP6377057B2/en not_active Expired - Fee Related
- 2013-06-28 EP EP13739547.1A patent/EP2872274A1/en not_active Withdrawn
- 2013-06-28 WO PCT/US2013/048666 patent/WO2014011420A1/en not_active Ceased
- 2013-06-28 KR KR1020157000586A patent/KR102125590B1/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020112408A1 (en) * | 1999-04-07 | 2002-08-22 | Ulf Rolander | Porous cubic boron nitride based material suitable for subsequent production of cutting tools and method for its production |
| US20050249978A1 (en) * | 2004-04-02 | 2005-11-10 | Xian Yao | Gradient polycrystalline cubic boron nitride materials and tools incorporating such materials |
| CN2805902Y (en) * | 2005-06-23 | 2006-08-16 | 河南富耐克超硬材料有限公司 | Multi-layered stock container for production of super-hard polycrystalline patch |
| CN201105217Y (en) * | 2007-05-16 | 2008-08-27 | 上海美恩精密工具有限公司 | Feed charge body for superhard grinding production |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110757907A (en) * | 2018-07-27 | 2020-02-07 | 北京沃尔德金刚石工具股份有限公司 | PcBN composite sheet and preparation method thereof |
| CN118181886A (en) * | 2024-03-18 | 2024-06-14 | 上海新山田精密刀具有限公司 | Low-content PcBN composite sheet with multiple cBN layers |
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| EP2872274A1 (en) | 2015-05-20 |
| US20140017435A1 (en) | 2014-01-16 |
| JP6377057B2 (en) | 2018-08-22 |
| KR20150036031A (en) | 2015-04-07 |
| KR102125590B1 (en) | 2020-06-22 |
| JP2015529617A (en) | 2015-10-08 |
| WO2014011420A1 (en) | 2014-01-16 |
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