CN101255520A - Nano WC-Co composite powder modified Ti(CN) based metal ceramic and preparation thereof - Google Patents
Nano WC-Co composite powder modified Ti(CN) based metal ceramic and preparation thereof Download PDFInfo
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Abstract
The invention discloses a nanometer WC-Co composite powder modified Ti(CN) based cermet and the preparing method thereof. Titanium carbonitride is used as the main parent metal, metal cobalt and/or nickel are/is used as the binder of raw material powder, carbide and tantalum-niobium sosoloid are used as the additive. The cermet is characterized in: the cermet is added with 6.0% to 27% by weight of raw material power nanometer WC-Co composite powder; the cermet is prepared with the raw material powder by ball grinding crushing, dispersing the nanometer WC-Co composite powder, uniformly mixing, press forming, vacuum or pressure sintering, etc. Compared with traditional cermet, since the cementing phase and the crystal boundary are strengthened, the nanometer WC-Co composite powder modified Ti(CN) based cermet has better wearing resistance, higher strength, fracture toughness and red hardness, thus a tool bit manufactured with the cermet has superior cutting property.
Description
Technical field
The present invention relates to a kind of is the sintering metal of base with the carbonitride, relates in particular to titanium carbonitride (Ti (CN)) based ceramic metal of a kind of nano composite powder modification and preparation method thereof.
Background technology
The cermet of conventional particles is because the particle diameter of raw material powder is bigger, more is easy to generate crackle later on being processed into alloy cutter, adds the inhomogeneous of structure, and the cutter after the processing also shows relatively poor toughness.The research work of nanotechnology and nano material has in recent years become the research focus, and the preparation of a lot of nanometer powders has entered the industrialization stage.Because the unique dimensions effect and the surface and interface effect of superfine powder make nano material have outstanding physics, mechanics and mechanical property.Yet, same because the dimensional effect and the surface and interface effect of nano-powder, make that the reunion of nano-powder is very serious, the production preparation of nano level compact block material also becomes very difficult, and for example the research of nano level hard alloy and sintering metal compact block material just still is in the starting stage.After discover, in the preparation process of micron or submicron powder material, change its delicate tissues structure by adding nano-powder, the performance of micron or submicron material is greatly improved.Chinese patent 02138161.5 discloses a kind of with nano TiN modified TiC or Ti (C, N) base ceramet tool bit, this cutter is by adding the nano TiN powder in raw material powder, TiC or Ti (C have been improved, N) performance index such as the hardness of base ceramet tool bit, wear resistance, solidity to corrosion, oxidation-resistance, compare with common inserted tool, improved cutter life and stock-removing efficiency greatly.But under the high speed cutting condition, particularly when some difficult to machine materials of processing, owing to face bad working environments such as cutting temperature height, cutting force is big, work hardening is serious, existing Ti (CN) based ceramic metal alloy seems and is difficult to tackle, the durability of cutter and life-span are not high, therefore how further to improve the hot strength and the hardness of cermet material, improve its red hardness and wear resistance and just become extremely important.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provide that a kind of fracture toughness property, wear resistance and cutting ability are better, intensity and hardness is higher, processing quality better, nano WC-Co composite powder modified Ti (CN) based ceramic metal of longer service life, a kind of this ceramic-metallic preparation method also is provided.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is a kind of nano WC-Co composite powder modified Ti (CN) based ceramic metal, with Ti (CN) as main base material, with cobalt and/or nickel as the bonding phase, it is characterized in that described sintering metal is after being mixed by the raw material powder of following each massfraction, to prepare through powder metallurgical technique:
Nano WC-Co composite powder 6～27%
Ti (CN) powder and carbonized titanium powder 35～65%
Tantalum niobium solid-solution powder 2～15%
Carbonization molybdenum powder or molybdenum powder 1～15%
Cobalt and/or nickel 6～25%
The massfraction of cobalt in the above-mentioned nano WC-Co composite powder in this composite powder is 5～20%, and the mol ratio of carbon atom and nitrogen-atoms is 3: 7～7: 3 in Ti (CN) powder and the carbonized titanium powder.Described " cobalt and/or nickel " is meant and can selects cobalt or nickel separately for use, also can select two kinds of metal-powders of cobalt and nickel simultaneously for use, when selecting two kinds of metal-powders of cobalt and nickel as raw material for use, the two can be arbitrarily than mixing, but the massfraction of total content must satisfy 6～25% requirement.
The granularity of above-mentioned nano WC-Co composite powder is below 100 nanometers.
Other raw material powders beyond the above-mentioned nano WC-Co composite powder are micron or submicron powder, and its purity is greater than 99%, and mean particle size is less than 1.5 microns.
The present invention also provides a kind of preparation method of above-mentioned nano WC-Co composite powder modified Ti (CN) based ceramic metal, comprises following processing step successively: the drying of the ball mill crushing of raw material powder, the dispersion of nano WC-Co composite powder, the Ball milling that is mixed in proportion each raw material powder, raw material powder, ball milling slurry, precise press molding (obtaining blank), pre-burning and high temperature sintering (obtaining sintering metal behind the sintering); Described high temperature sintering can be vacuum sintering mode, many atmosphere (N
2, H
2, among the Ar one or more) sintering processing or high temperature pressure sintering processing;
In the described Ball milling process, with dehydrated alcohol or methyl alcohol as grinding medium, with Wimet as grinding element, add the dispersion agent of raw material powder gross weight 0.3～1% and 4～5% binding agent, ratio of grinding media to material is 1: 6～12, rotational speed of ball-mill can be controlled at 30～40 rev/mins, and the Ball milling time can be controlled at 20～90 hours; The drying of described ball milling slurry is to adopt the spraying drying mode or adopt the vacuum-drying mode, and drying temperature is 80～95 ℃, 90～150 minutes time of drying; The temperature of described pre-burning is 200～500 ℃, and the time is 2～4 hours; The sintering temperature of described vacuum sintering or many atmosphere sinterings mode is 1400～1470 ℃, and soaking time is 50～90 minutes; The sintering temperature of described high temperature pressure sintering processing is 1390～1440 ℃, and pressure is 45～70 standard atmospheric pressures, and soaking time is 40～60 minutes.
The weave construction of typical Ti (CN) based ceramic metal is by hard phase and bonding phase composite, and hard is core-ring structure mutually, ring and outer shroud in the ring structure that has has.The height of sintering metal performance, key are the design of its internal organizational structure.By the bonding phase of reinforced metal pottery and the design that improves annular phase, can improve ceramic-metallic physics, mechanics and cutting ability.Technique scheme is as main base material with titanium carbonitride, with cobalt powder and/or nickel powder as binding agent, with carbide, tantalum niobium sosoloid (Ta, Nb) C is as additive, by adding nano WC-Co composite powder, prepare a kind of nano WC-Co composite powder modified Ti (CN) based ceramic metal of strengthening bonding phase and crystal boundary again through powder metallurgical technique.In preparation process, nano WC-Co composite powder has reached the uniform mixing of molecular level level, part even formed the prealloy powder.Because WC high-specific surface area in the nano WC-Co composite powder, Ti (CN) has higher dissolution rate in bonding in mutually relatively, has suppressed the dissolving of Ti (CN), refinement Ti (CN) phase crystal grain, and then form more uniform annular phase, and volume ratio enlarges markedly also.The dislocation desity of adding nano WC-Co composite powder is lower than conventional size raw material powder particulate dislocation desity, and is not mingled with, and has higher W content and C content like this in boning mutually, has increased the volume ratio of bonding phase.In addition, nano WC-Co composite powder has been stablized face-centered cubic (FCC) cobalt in the sintering process of cooling, has higher FCC/HCP in the cobalt than (face-centered cubic/six sides), the bonding mutually in and have unformed cobalt to exist mutually, W content is higher than W content in the crystallization cobalt in the unformed cobalt, and this has further strengthened the bonding phase.
Therefore, compared with prior art, the invention has the advantages that by in raw material, adding nano WC-Co composite powder, the bonding phase and the crystal boundary of Ti (CN) based ceramic metal have been strengthened, improved the distribution of its annular phase, improved fracture toughness property, intensity and the hardness of submicron Ti (CN) based ceramic metal, made it demonstrate better wear resistance and excellent impact resistance.Can be applicable to all kinds of cutting tools and wear part through nano WC-Co composite powder modified Ti (CN) based ceramic metal, not only can improve the surface quality of mechanical workout benefit and processing work after the application, and the work-ing life that can improve Impact mould and wear part.
Embodiment
Embodiment 1:
Prepare raw material powder by following quality proportioning: 17% nanometer WC-10%Co composite powder, 45% Ti (CN) powder, 8% (Ta, Nb) C powder, 8% Mo
2C powder, 7% TiC powder, 7% Co and 8% Ni, wherein the granularity of nano WC-Co composite powder is 50～100 nanometers, the mean particle size of all the other raw material powders is less than 1.5 microns.
The above-mentioned raw materials powder is put into ball mill, with dehydrated alcohol as grinding medium, with Wimet as grinding element, the tween (making dispersion agent) that adds raw material powder total amount 0.8%, 3% polyoxyethylene glycol and 1% polytetrahydrofuran (making binding agent), ratio of grinding media to material is 1: 10, rotational speed of ball-mill is 36 rev/mins, the ball milling mixing time is 56 hours, spray-dried (90 ℃ of the nozzle outlet temperatures of slurry after the Ball milling, successive drying, time of drying according to stove slurry what and decide), precise press molding, again through 3 hours pre-burning (200～500 ℃), and at 1450 ℃ H
2With heat preservation sintering under the Ar atmosphere 75 minutes, make nano WC-Co composite powder modified Ti (CN) based ceramic metal at last.
Measuring above-mentioned ceramic-metallic mechanical performance index is: bending strength is 1940MPa, and hardness is HRA92.0, fracture toughness property K
IC is 9.02MPam
1/2Above-mentioned sintering metal is prepared into milling cutting insert (SPEN1203EDR) processing 42CrMo, and machined parameters is cutting speed V=300m/min, cutting-in Ap=0.5mm, feeding f=0.15mm/z, and the working durability that last test obtains milling cutting insert is 75 minutes.
Simultaneous test: with same sample ingredient, there is not composite powder modified raw material powder to mix: 15.3%WC (1.5 microns of powder mean particle sizes), 8%Mo by following quality proportioning
2C, 8% (Ta, Nb) C, 45%Ti (CN), 7%TiC, 8.7%Co and 8%Ni are prepared into sintering metal with existing powder metallurgy technology again, and its performance index are: bending strength is 1670MPa, and hardness is HRA91.8, fracture toughness property K
IC is 8.77MPam
1/2This sintering metal is prepared into milling cutting insert (SPEN1203EDR) processing 42CrMo, and machined parameters is cutting speed V=300m/min, cutting-in Ap=0.5mm, feeding f=0.15mm/z, and the working durability that test obtains milling cutting insert only is 35 minutes.
Embodiment 2:
Prepare raw material powder by following quality proportioning: 10% nanometer WC-10%Co composite powder, 46% Ti (CN) powder, 12% (Ta, Nb) C powder, 7% Mo
2C powder, 10% TiC powder, 8% Co and 7% Ni, wherein the granularity of nano WC-Co composite powder is 50～100 nanometers, the mean particle size of all the other raw material powders is less than 1.5 microns.
The above-mentioned raw materials powder is put into ball mill, with dehydrated alcohol as grinding medium, with Wimet as grinding element, the tween (making dispersion agent) of adding raw material powder total amount 0.8%, 3% polyoxyethylene glycol and 1% polytetrahydrofuran (making binding agent), ratio of grinding media to material is 1: 11, rotational speed of ball-mill is 36 rev/mins, the ball milling mixing time is 50 hours, behind slurry after the Ball milling spray-dried (90 ℃ of nozzle outlet temperatures), the precise press molding, again through 3 hours pre-burning (200～500 ℃), at last at 1450 ℃ H
2With heat preservation sintering under the Ar atmosphere 60 minutes, make nano WC-Co composite powder modified Ti (CN) based ceramic metal.
Measuring above-mentioned ceramic-metallic mechanical performance index is: bending strength is 1970MPa, and hardness is HRA92.2, fracture toughness property K
IC is 9.53MPam
1/2Above-mentioned sintering metal is prepared into turning insert (CNMG120408-DF) processing 42CrMo, and machined parameters is cutting speed V=200m/min, cutting-in Ap=1mm, feeding f=0.2mm/z, and the working durability that last test obtains turning insert is 20 minutes.
Simultaneous test: with same sample ingredient, there is not composite powder modified raw material powder to mix: 9%WC (1.5 microns of powder mean particle sizes), 7%Mo by following quality proportioning
2C, 12% (Ta, Nb) C, 46%Ti (CN), 10%TiC, 9%Co and 7%Ni are prepared into sintering metal with existing powder metallurgy technology again, and its performance index are: bending strength is 1680MPa, and hardness is HRA92.0, fracture toughness property K
IC is 8.27MPam
1/2This sintering metal is prepared into turning insert (CNMG120408-DF) processing 42CrMo, and machined parameters is cutting speed V=200m/min, cutting-in Ap=1mm, feeding f=0.2mm/z, and the working durability that test obtains turning insert only is 13 minutes.
Embodiment 3:
Prepare raw material powder by following quality proportioning: 27% nanometer WC-5%Co composite powder, 40% Ti (CN) powder, 7% (Ta, Nb) C powder, 4% Mo
2C powder, 10% TiC powder, 6% Co and 6% Ni, wherein the granularity of nano WC-Co composite powder is 50～100 nanometers, the mean particle size of all the other raw material powders is less than 1.5 microns.
The above-mentioned raw materials powder is put into ball mill, as grinding medium, use Wimet, the tween (making dispersion agent) of adding raw material powder total amount 0.8%, 3% polyoxyethylene glycol and 1% polytetrahydrofuran (making binding agent) as grinding element with dehydrated alcohol; Ratio of grinding media to material is 1: 10, rotational speed of ball-mill is 36 rev/mins, the ball milling mixing time is 52 hours, the ball milling slurry is behind vacuum-drying (88 ℃) 2 hours, precise press molding, again through 3 hours pre-burning (200～500 ℃), 1460 ℃ of following vacuum sinterings, be incubated 70 minutes at last, make nano WC-Co composite powder modified Ti (CN) based ceramic metal.
Measuring above-mentioned ceramic-metallic mechanical performance index is: bending strength is 1730MPa, and hardness is HRA93.2, fracture toughness property K
IC is 8.67MPam
1/2
Embodiment 4:
Prepare raw material powder by following quality proportioning: 6% nanometer WC-20%Co composite powder, 61% Ti (CN) powder, 2% (Ta, Nb) C powder, 11% Mo
2C powder, 2% TiC powder, 8% Co and 10% Ni, wherein the granularity of nano WC-Co composite powder is 50～100 nanometers, the mean particle size of all the other raw material powders is less than 1.5 microns.
The above-mentioned raw materials powder is put into ball mill, as grinding medium, use Wimet, the tween (making dispersion agent) of adding raw material powder total amount 0.8%, 3% polyoxyethylene glycol and 1% polytetrahydrofuran (making binding agent) as grinding element with dehydrated alcohol; Ratio of grinding media to material is 1: 12, rotational speed of ball-mill is 36 rev/mins, the ball milling mixing time is 44 hours, the ball milling slurry is behind vacuum-drying (88 ℃) 2 hours, precise press molding, again through 3 hours pre-burning (200～500 ℃), sintering under the pressure of 1420 ℃, 70 standard atmospheric pressures is incubated 50 minutes at last, makes nano WC-Co composite powder modified Ti (CN) based ceramic metal.
Measuring above-mentioned ceramic-metallic mechanical performance index is: bending strength is 2210MPa, and hardness is HRA91.3, fracture toughness property K
IC is 11.09MPam
1/2
Claims (4)
1, a kind of nano WC-Co composite powder modified Ti (CN) based ceramic metal, with Ti (CN) as main base material, as the bonding phase, it is characterized in that described sintering metal is after raw material powder by following each massfraction mixes, to prepare through powder metallurgical technique with cobalt and/or nickel:
Nano WC-Co composite powder 6～27%
Ti (CN) powder and carbonized titanium powder 35～65%
Tantalum niobium solid-solution powder 2～15%
Carbonization molybdenum powder or molybdenum powder 1～15%
Cobalt and/or nickel 6～25%
The massfraction of cobalt in the above-mentioned nano WC-Co composite powder in this composite powder is 5～20%, and the mol ratio of carbon atom and nitrogen-atoms is 3: 7～7: 3 in Ti (CN) powder and the carbonized titanium powder.
2, nano WC-Co composite powder modified Ti according to claim 1 (CN) based ceramic metal, the granularity that it is characterized in that described nano WC-Co composite powder is below 100 nanometers.
3, nano WC-Co composite powder modified Ti according to claim 1 (CN) based ceramic metal, it is characterized in that other raw material powders beyond the described nano WC-Co composite powder are micron or submicron powder, its purity is all greater than 99%, and mean particle size is all less than 1.5 microns.
4, the preparation method of each described nano WC-Co composite powder modified Ti (CN) based ceramic metal in a kind of claim 1～3 comprises following processing step: the drying of the ball mill crushing of raw material powder, the dispersion of nano WC-Co composite powder, the Ball milling that is mixed in proportion each raw material powder, raw material powder, ball milling slurry, accurate compacting, pre-burning and vacuum sintering or many atmosphere sinterings or high temperature pressure sintering successively;
In the described Ball milling process, as grinding medium, as grinding element, add the dispersion agent of raw material powder gross weight 0.3～1% and 4～5% binding agent with dehydrated alcohol or methyl alcohol with Wimet, ratio of grinding media to material is 1: 6～12, and the Ball milling time is 20～90 hours; The drying of described ball milling slurry is to adopt the spraying drying mode or adopt the vacuum-drying mode, and drying temperature is 80～95 ℃, 90～150 minutes time of drying; The temperature of described pre-burning is 200～500 ℃, and the time is 2～4 hours; The sintering temperature of described vacuum sintering or many atmosphere sinterings is 1400～1470 ℃, and soaking time is 50～90 minutes; Described high temperature pressure agglomerating sintering temperature is 1390～1440 ℃, and pressure is 45～70 standard atmospheric pressures, and soaking time is 40～60 minutes.
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| CN114713827A (en) * | 2022-04-20 | 2022-07-08 | 赣南师范大学 | Hard alloy/metal ceramic powder for 3D printing and preparation method thereof |
| CN114713827B (en) * | 2022-04-20 | 2024-01-30 | 赣南师范大学 | Cemented carbide/metal ceramic powder for 3D printing and preparation method thereof |
| CN115418542A (en) * | 2022-07-12 | 2022-12-02 | 杭州巨星科技股份有限公司 | Nano modified metal ceramic cutter material and preparation method thereof |
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