KR20140036781A - High-performance microdrill via solid-solution carbide/carbonitride nano powder - Google Patents
High-performance microdrill via solid-solution carbide/carbonitride nano powder Download PDFInfo
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- KR20140036781A KR20140036781A KR1020120103329A KR20120103329A KR20140036781A KR 20140036781 A KR20140036781 A KR 20140036781A KR 1020120103329 A KR1020120103329 A KR 1020120103329A KR 20120103329 A KR20120103329 A KR 20120103329A KR 20140036781 A KR20140036781 A KR 20140036781A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B41/00—Boring or drilling machines or devices specially adapted for particular work; Accessories specially adapted therefor
- B23B41/14—Boring or drilling machines or devices specially adapted for particular work; Accessories specially adapted therefor for very small holes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B51/00—Tools for drilling machines
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/04—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbonitrides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2204/00—End product comprising different layers, coatings or parts of cermet
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Abstract
The present invention relates to a material of a microdrill used for processing a PCB and a fuel injection nozzle. The present invention relates to a composition and microstructure of a material required for processing a plastic substrate at high speed. The invention relates to a high toughness / wear resistant microdrill material having a simple microstructure comprising a solid-based solid solid carbide or carbonitride and a combined phase.
Description
BACKGROUND OF THE
With the rapid development of information and communication, home appliances, automobiles, and life industries, and the demand for micro parts for light weight and miniaturization of products, interest in micro / nano scale parts is increasing, and MEMS, LIGA, Research on processing technology for micro parts such as these is becoming important.
High-performance materials for cutting tools or wear-resistant tools, which are necessary for the plastics, metal cutting processes and machining processes required for the mechanical industry, include tungsten carbide (WC) -based cemented carbide and fcc crystal structures (B1, NaCl). Various cermet alloys of TiC, Ti (CN) series, other ceramics or high speed steel are used. Among them, the cemented carbide sintered body refers to a ceramic-metal composite sintered body whose main component is Co, which is bonded to WC.
The cemented carbide composite sintered body is produced by mixing hard carbide powders such as NbC, TaC, Mo 2 C, and metal powders such as bonded phase Co, in addition to TiC, Ti (CN) and the like, and sintering them in a vacuum or hydrogen atmosphere.
WC is very hard with Vicker's hardness of 2,900kg / mm 2 and also has a very high melting point of 2,700 ° C. Therefore, it is widely used as a high speed micro drill material.
However, all the cemented carbide products based on the WC are produced in a narrower world than other carbides, which is expensive as a monopoly supply, and causes various problems due to the health problems due to the combined phase Co being used. Nevertheless, WC-Co cemented carbide, which exhibits high toughness even for most of the cutting tools and even micro drill materials for substrates, is the mainstream in this field. WCs of 200-300 nm are used for the production of cemented carbide micro drills and to date no commercially available micro drills of different material compositions are available.
Cermet, one of the alternative materials, is mainly composed of (Ti, W) C, (Ti, W) (CN), TiC, Ti (CN) and bonding phase metals such as Ni, Co, and Fe. It refers to a sintered body of ceramic-metal composite powder containing carbides, nitrides, and carbonitrides of, Va, and Group VIa metals as additives. The cermet mixes hard ceramic powders such as Mo 2 C, NbC, TaC, and metal powders such as Co, Ni, Fe, etc., for bonding them, in addition to TiC, Ti (CN), WC, and the like, and sinters them under vacuum or nitrogen atmosphere. It is manufactured by.
The TiC has Vicker's hardness of 3,200 kg / mm 2, which is extremely hard and has a very high melting point of 3,423 to 3,523 K, and has a relatively good oxidation resistance up to 973 K. Furthermore, it has excellent properties such as wear resistance, corrosion resistance, electron radiation, and light collection. Therefore, TiC has been widely used as a substitute for the WC-Co alloy as a material for high speed cutting tools.
However, when the cermet is manufactured using the TiC, a phase metal such as Ni is used as the liquid metal during sintering. In this case, the TiC is rapidly formed because the wetting angle is larger than that of the WC-Co combination. The growth of the mouth is caused, there was a problem that the toughness is reduced.
Nevertheless, in 1956, Ford Mortor, USA, first mass-produced TiC-Mo 2 C-Ni cermets, which, although their toughness did not significantly improve, were hard tool materials for precision machining. It has been used for semi-finishing and finishing.
In the 1960s and 1970s, attempts were made to add various kinds of elements to the TiC-Ni cermet system in order to improve toughness, which is the biggest weakness of the TiC-Ni cermet system.
In the 1970s, however, TiN was added to TiC to form Ti (CN), which is a thermodynamically more stable phase. Ti (CN) has a finer structure than TiC. In addition, chemical stability and mechanical impact resistance could be improved.
On the other hand, many added carbides, such as WC, Mo 2 C, TaC, NbC, etc. have been used to improve toughness, and Ti (CN) -M1C-M2C-... -Ni / Co type products are commercially available.
When the addition carbide is applied to improve the toughness, the general microstructure of the TiC-based or Ti (CN) -based cermet sintered body is observed as a core / rim structure, and the hard phase of such a core structure is Ni, Co. The bonding phase of the back is enclosed.
The core of the core structure is a structure having high hardness as TiC or Ti (CN) which is not dissolved in the metal complex (Ni, Co, etc.) liquefied during sintering.
The surrounding rim tissue surrounding these cores, on the other hand, is a solid-solution (represented as a solid-solution (Ti, M1, M2…) (CN)) between the core components TiC or Ti (CN) and the added carbides. Toughness rather than hardness.
Thus, the cermet solved the problem of toughness, which is a fatal weakness of the simple cermet such as TiC-Ni or Ti (CN) -Ni, by forming the rim structure to some extent. However, even if the problem of toughness is solved, the cermet having the core structure has a problem that the toughness is still lower than that of the cemented carbide of WC-Co, and thus it has not yet completely replaced WC-Co. Thus, attempts have been made by tool companies, such as Sumitomo and Mitsubishi, to develop a toughened cermet through the formation of a complete employment without a concentric structure.
However, the solid solution phase is formed during the sintering of the composite powder, and since the amount formed is related to the sintering temperature and time, a cermet composed of a completely solid solution alone cannot be substantially obtained through the existing carbonitride mixed powder or the manufacturing method.
Accordingly, the present inventors have developed solid solution powders, cermets, and the like, which substantially achieve a complete solid solution. See Korean Patent Laid-Open Publication No. 2005-0081553, whereby toughness can be greatly improved. In addition, even when forming the complete solid solution phase or additional partial solid phase on the basis of the complete solid solution phase, the toughness can be further improved, and the cermet micro drill excellent in other physical properties such as high strength can be provided. This has not been reported yet.
The present invention is to solve the problems of the prior art as described above, the object of the present invention is a cermet or cemented carbide which can greatly improve the toughness by using a wholly carbide or carbonitride or a mixture thereof in whole or in part To provide a composite micro drill material.
The present invention is to provide a novel cermet composite sintered body and composition which enables the production of high performance micro drill tools. More specifically, it is an object of the present invention to solve the health and cost problems caused by the manufacture of cemented carbide and to provide a safe, economical and functionally superior microdrill.
The present invention provides a novel micro-drill manufacturing method and composition excellent in toughness, strength and hardness by using a completely solid phase powder that solves the problem that the conventional TiC-based and Ti (CN) -based cermets have excellent hardness but low toughness. To provide.
The micro drills produced by the process of the invention are Ti-based carbonitride completely solid solution, for example, (Ti, W) C, (Ti, W) (CN), (Ti, M1, M2, .. .) C, (Ti, M1, M2, ...) (CN) etc. are used in whole or in part, so they are excellent in terms of performance and the amount of tungsten and co-bolt is significantly reduced, which can reduce raw material costs. The process can also be greatly simplified.
In the present invention, completely solid solution powder means that the solid solution element (or carbide, carbonitride of solid solution element) does not exceed the solid solution limit within the carbon (nitride) -TiC or Ti (CN)-of the main element. It exists, which means forming a homogeneous single phase in composition. That is, it represents a single phase in the XRD phase, and means a phase or powder that does not show a core / rim microstructure even when observed.
The basic object of the present invention is a cubic structure (fcc) complete solid solution comprising a total of two transition metal elements selected from titanium, including titanium, Zr, Hf, V, Nb, Cr, Mo and W. Carbide, carbonitride or mixed phases thereof; And a cermet micro-drill having a microstructure comprising at least one bonding phase of Ni, Co, Fe, Al, Cr.
In order to implement a microstructure including only the binary solid solution carbide, carbonitride or a mixed phase thereof, it is easy and preferable to use powders of these solid solutions. Therefore, it is preferable to obtain a cermet micro-drill by mixing, solidifying and sintering the solid solution powder and one or more of the binder phase powders of Ni, Co, Fe, Al, and Cr. The result of the microstructure is that, for example, only a completely solid solution phase such as (Ti, W) C, (Ti, W) (CN), which is a single phase, is uniformly present as the major phase in the binding phase. .
Another object of the present invention is a cubic structure (fcc) comprising a total of three or more transition metal elements selected from titanium, including titanium from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo and W Fully solid carbide, carbonitride or mixed phase thereof; And it can be achieved by providing a cermet micro drill having a microstructure comprising at least one bonding phase of Ni, Co, Fe, Al, Cr.
It is easy and preferable to use powders of these solid solids in order to realize a microstructure including only the ternary or more of the multinary solid solid carbides, carbonitrides or mixed phases thereof. Therefore, it is preferable to obtain a cermet micro-drill by mixing, solidifying and sintering the solid solution powder and one or more of the binder phase powders of Ni, Co, Fe, Al, and Cr. The results of the microstructure are, for example, (Ti, W, Mo) C, (Ti, W, Mo) (CN), (Ti, M1, M2, ...) C, (Ti Only completely solid phases such as M1, M2, ...) (CN), (M1, M2, ...) C, (M1, M2, ...) (CN), etc. major phases).
The composition of the multinary fully solid solution carbides and carbonitrides including the binary is preferably at least WC and the weight ratio is 5-70 wt.% Of the carbides or carbonitrides.
Preferably, the amount of the combined phase is 2-40 wt.% Of the total weight.
Even when the solid solution powder is mixed with a carbide or carbonitride which is not a solid solution, it exhibits excellent high toughness and wear resistance because the thermodynamically stable solid solution phase promotes high temperature dissolution of other carbides. For example, when 10-20 wt.% Of the complete solid solution is added to the total weight ratio, more than 80% of the microstructure is changed to the total solid solution. Therefore, it is preferable to use a mixed powder made of at least 5 wt.% Or more of completely solid solution carbide or carbonitride powder. Examples of the mixed powder include Ti (CN)-(Ti, W) (CN) -Ni-Co (Ti, W) (CN) -WC-Ni-Co, [Ti (CN) -WC-Mo2C]- Same as (Ti, W) (CN) -Ni-Co, [TiC-WC-TaC]-(Ti, W, Mo) C-Ni, etc., if used, depending on the composition, TiC, Ti (CN) or solid solution It has a core / rim structure having (Ti, W) C and (Ti, W) (CN) as cores.
That is, according to the present invention, the volume fraction is large as well as the microstructure composed of only a solid solution having no core structure in the form of (Ti, M1, M2…) C and (Ti, M1, M2…) (C, N) having a desired composition. High toughness of core structure with increased (> 80%) full employment rim and TiC, Ti (CN) or solid phase (Ti, W) C, (Ti, W) (CN) as core Abrasion resistant cermet micro drills are available. In general, most of the Ti-based cermet material has a core structure.
In accordance with the prior art, the manufacturing facilities for the cermet composite sintered compact and the process have already been commercialized for various carbide and carbonitride powders. proper.
The micro drills produced by the process of the invention are Ti-based carbonitride completely solid solution, for example, (Ti, W) C, (Ti, W) (CN), (Ti, M1, M2, .. .) C, (Ti, M1, M2, ...) (CN), etc.- are used in whole or in part, so they are excellent in terms of performance, and the amount of tungsten and co-bolt is significantly reduced to reduce raw material costs. The process can also be greatly simplified.
1 is carbonized in the graphite vacuum furnace for 1 hour at 1,300 ℃, 1,400 ℃, and 1,500 ℃ for 1 hour at 1,300 ℃, 1,400 ℃, and 1,500 ℃ powder according to Example 1 of the present invention, a graph illustrating the analysis result by the X-ray diffraction analysis of the reduced and manufacturing (Ti 0 .7 W 0 .3) C solid solution powder.
2 is a reduction of the powder of FIGS. 1 (a) and 1 (b) using a graphite vacuum furnace and
FIG. 3 is (Ti 0.7 W 0.3 ) C solid solution powder prepared by mixing and grinding TiO 2 , WO 3 , C, according to Example 3 of the present invention, and reducing and carbonizing at 1,400 ° C. and 1,500 ° C. for 2 hours. the (Ti 0 .7 W 0 .3) C-20 wt% Ni standing optical and scanning electron microscope (FESEM) for metteu sintered microstructure photograph is produced using a.
Figure 4 shows a photograph of the fabricated micro drill, performance evaluation method and the results of Al 6061 work piece used for cutting.
5 is a photographic result of comparing the wear state of the micro-drill for each specimen composition after the performance evaluation of the Al 6061 specimen according to the cutting conditions.
The method of manufacturing a micro drill manufactured by the method of the present invention and a micro drill material using a mixed powder for cermet including the solid solution powder will be described in more detail with reference to the following examples. However, the scope of the present invention is not limited to the following examples, only the examples are intended to facilitate the implementation of the invention to those skilled in the art while at the same time making the disclosure of the present invention complete. It will be understood by those skilled in the art that various modifications are possible within the scope of the appended claims.
(Ti 0 .7 W 0 .3) the Ti metal and anatase (anatase) TiO 2, WO 3 oxide, and carbon powder were prepared in order to produce a complete solid solution C having a solid solution composition. Two kinds of mixtures were prepared by mixing the prepared TiO 2 and Ti in a ratio of 1: 0 or 1: 1, and mixed them with WO 3 and carbon powder. The two kinds of mixtures thus prepared were pulverized using an WC-Co ball for 20 hours under a condition of 30: 1 at a ball-to-powder ratio (BPR) at 250 rpm using an attrition mill. Heat treatment was carried out at a temperature of 1,300 ° C. to 1,500 ° C. for 2 hours and at 1,600 ° C. for 1 hour in a vacuum atmosphere to undergo reduction and carbonization.
Figure 1 shows the XRD results for the solid solution nano-powder thus prepared. FIG. 1 (a) shows XRD results of anatase TiO 2 , WO 3 oxide, and powder (TiO 2 : Ti = 1: 0) using carbon powder, and FIG. 1 (b) shows Ti, anatase TiO 2 , WO 3 oxide, And XRD results of a powder (TiO 2 : Ti = 1: 1) using carbon powder.
The result is that when the reduction of the mixed oxide powder is ground to an appropriate temperature and time, the carbide (Ti 0 .7, W 0 .3 ) to easily obtain a complete solid solution C Nano.
(Ti 0 .7 W 0 .3) (CN) of Ti metal and anatase TiO 2, WO 3 oxide, and carbon powder were prepared for the production of nano complete solid solution having a solid solution composition. Two kinds of mixtures were prepared by mixing the prepared TiO 2 and Ti in a ratio of 1: 0 or 1: 1, and mixed them with WO 3 and carbon powder. The two kinds of mixtures thus prepared were pulverized using an WC-Co ball dry for 20 hours under a condition of a ball-to-powder ratio (BPR) of 30: 1 at 250 rpm using an attrition mill. The pulverized powder was heat-treated at 1,400 ° C. and 1,500 ° C. for 2 hours and at 1,600 ° C. for 1 hour while maintaining a nitrogen pressure of 10 Torr in a graphite vacuum furnace to undergo a reduction and carbonization process.
FIG. 2 is an XRD result of powder reduced and carbonitized using a graphite vacuum furnace and a nitrogen pressure of 10 torr for 2 hours in a temperature range of 1,300 ° C. to 1,500 ° C. FIG.
FIG. 2 (a) shows XRD results of anatase TiO 2 , WO 3 oxide, and powder (TiO 2 : Ti = 1: 0) using carbon powder, and FIG. 2 (b) shows Ti, anatase TiO 2 , WO 3 oxide, And XRD results of a powder (TiO 2 : Ti = 1: 1) using carbon powder. In the case of Figure 2 (a) it was possible to obtain (Ti, W) (CN) nano solid solution powder at 1,500 ℃ without the production of WC, W 2 C. However, in Figure 3 (b) WC was also precipitated at 1,500 ℃.
In fact can be seen from this result is that more than two hours at more than 1,500 ℃ reduced, if carbide (Ti 0 .7, W 0 .3 ) to obtain a complete solid solution such as (CN).
(Ti 0 .7 W 0 .3) C-20wt% Ni cermet to the production of composite sintered TiO 2, WO 3, a mixture of carbon powder control tree illustration mill 250rpm, BPR (Ball-to- Powder Ratio) 30: and then pulverized by means of a WC-Co ball to dry for 20 hours under the conditions of 1, by heating at a temperature or 1,500 1,400 ℃ ℃ under vacuum for 2 hours after the reduction and carbonization process (Ti 0 .7 W 0 .3) C nano solid solution powder was prepared. The solid solution powder was wet mixed with a micron size Ni powder using a horizontal mill for 24 hours, dried, and the powder was prepared by using a graphite vacuum furnace at 1,510 ° C. for 1 hour.
Figure 3 according to a third embodiment of the invention (Ti 0 .7 W 0 .3) C solid solution was prepared by using a nano-powder (Ti 0 .7 W 0 .3) Fine-20 wt% Ni cermet of the sintered body C Optical and scanning electron microscope (FESEM) photographs of the structure.
Figure 3 (a) is a photograph showing the optical and SEM microstructure of the sintered body sintered (Ti, W) C-Ni powder reduced and carbonized at 1,400 ℃ at 1,510 ℃, the size of the solid solution is approximately 1μm to 3μm and sinterability outstanding. FIG. 3 (b) shows the optical and SEM microstructures of the sintered compact sintered and reduced at 1,500 ° C. (Ti, W) C-Ni powder at 1,510 ° C. to solidify the solid phase and show a large size of about 2 μm to 4 μm. It shows a uniform, pore-free microstructure. The powder reduced and carbonized at high temperature has a large particle size after sintering.
Table 1 Example 3 Method to 1,300 ℃ to 1,600
(Ti 0 .7 W 0 .3) (CN) -20wt% Ni cermet to produce a composite sintered TiO 2, WO 3 to, carbon powder (TiO 2: Ti = 1: 0) by mixing air tree illustration mill to 250rpm , BPR (Ball-to-Powder Ratio) 30: 1 dry pulverized with a WC-Co ball for 20 hours, then heat treatment at 1,400 ℃ or 1,500 ℃ temperature under vacuum to reduce, carbonization and after the nitriding process (Ti 0 .7 W 0 .3) (CN) to prepare a solid solution in nano-powder. The solid solution powder was wet mixed with a micron size Ni powder using a horizontal mill for 24 hours, dried, and the powder was prepared by using a graphite vacuum furnace at 1,510 ° C. for 1 hour. In this result, as shown in FIG. 3 of Example 3, it was possible to obtain a microstructure composed of a single phase complete solid solution and a combined phase only.
Table 2 Example 4 The method as 1,300 ℃ to 1,500 ℃ in 2 sigan prepared using the reduction, which was prepared by carbo-nitride solid-solution powder (Ti 0 .7 W 0 .3) (CN) -20 wt% Ni cermet of After molding the powder, the hardness, toughness and porosity of the sintered body sintered at (a) 1,400 ° C. for 1 hour and (b) 1,510 ° C. for 1 hour are shown. Although the physical properties and porosity change according to the reduction and carbonitriding temperature and the sintering temperature, the manufactured sintered body generally has low porosity (A2B2) and high toughness. When the nitrogen reduction at a high temperature can be seen that the physical properties are significantly improved.
Example 1 and in accordance with the method of 2 (Ti 0 .88 W 0 .12 ) (CN), (
In addition, the prepared (Ti 0 .88 W 0 .12) with the complete solid-solution powders of composition C using 15% to 20% of the total weight as shown in Table 4 [Ti (CN) -WC- Mo2C-TaC] - (
The manufactured micro drill was tested for performance under the conditions of Table 5 below.
5 shows the results of performance evaluation of the Al 6061 specimen according to the above conditions. As shown in FIG. 5, it can be seen that the cermet drills of
The results show that the microdrills using solid solids are no better than conventional carbide drills in terms of toughness and wear resistance. In addition, the use of a relatively small amount of W or WC provides an economical and excellent micro drill.
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