CN103058662B - Titanium diboride-based composite self-lubricating ceramic tool material and preparation method thereof - Google Patents
Titanium diboride-based composite self-lubricating ceramic tool material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a titanium diboride-based composite self-lubricating ceramic tool material and a preparation method thereof. The ceramic tool material is formed by using nanometer TiB2 and micro TiB2 as matrix, adding micron WC (Wolfram Carbide) as a wild phase, using micro h-BN (Boron Nitride) as solid lubricant and using micro Mo and micro Ni as sintering aids through hot-pressing and sintering. The preparation method comprises the following steps of: dispersing the nanometer TiB2, the micro TiB2, the micro WC and the micro h-BN powder, respectively, adding micro Mo and micro Ni; carrying out ball-milling and drying on the materials to obtain the powder material; and sintering the powder material by a hot-pressing method. The self-lubricating ceramic tool material obtained by the preparation method disclosed by the invention has good comprehensive mechanical properties and antifriction and wearable performances, and can be used for manufacturing tools, moulds and other antifriction and wearable components.
Description
Technical field
The invention belongs to the ceramic cutting tool material research field, particularly a kind of nano combined self-lubrication ceramic cutter material and preparation method thereof.
Background technology
Ceramic cutting tool material has very high hardness, wear resisting property and good resistance to elevated temperatures.Frictional behaviour to adding self-lubrication ceramic cutter material prepared by solid lubricant in stupalith and can effectively improve ceramic cutting tool material, make ceramic cutting tool material possess self-lubricating function.But solid lubricant has dual character to the impact of ceramic cutting tool material performance: solid lubricant can drag to apply at friction surface and form lubricant film on the one hand, can improve the frictional behaviour of ceramic cutting tool material; Can reduce the mechanical property of ceramic cutting tool material and add on the other hand solid lubricant in ceramic cutting tool material, thereby cause its wear resistance decrease.This is the difficult problem that current self-lubrication ceramic cutter antifriction performance and wear resisting property can not rationally be taken into account.
Nano composite ceramic cutter material is by add nano material in ceramic matrix, utilizes the characteristic of nano material, and the mechanical property of material is greatly improved.CN101265079A provides a kind of nano composite ceramic cutter material and preparation method thereof.This nano composite ceramic cutter material by volume per-cent comprises 54%～64% micron Al
2o
3, 21%～40.5% nano TiC, 3.5%～18% micron WC, 0.5% micron MgO and 0.5% micron NiO.The present invention passes through to micron order Al
2o
3middle interpolation nano level TiC particle and micron order WC particle, and the volume content of control nano level TiC particle and micron order WC particle, using MgO and NiO as sintering aid and grain growth inhibitor, prepares the strong mechanical performance nano composite ceramic cutter material.Although such cutter material mechanical property improves significantly than the micron order cutter material, cutter because frictional coefficient is higher, causes cutting temperature higher in working angles, and tool wear is very fast, and the raising of cutter life is limited.
Summary of the invention
For antifriction performance and the wear resisting property of taking into account the self-lubrication ceramic cutter material, the invention provides nano combined self-lubrication ceramic cutter material of a kind of TiB2 base and preparation method thereof.
Term explanation: h-BN, hexagonal boron nitride.Laminate structure with similar graphite, in the present invention as solid lubricant.
Technical scheme of the present invention is as follows:
The nano combined self-lubrication ceramic cutter material of a kind of TiB2 base, the feed composition volume percent is:
Nanometer TiB
210-40%, micron WC5-15%, micron h-BN6-12%, micron Mo1-3%, micron Ni2-5%, all the other are micron TiB
2; Wherein,
Described nanometer TiB
2median size is 40 ~ 80nm, micron TiB
2median size is 1-5 μ m;
Described micron WC, micron h-BN median size are 1 ~ 1.5 μ m;
Described micron Mo, micron Ni median size are 25 ~ 45 μ m;
Through hot pressed sintering, form.
Wherein, preferred, described nanometer TiB
2with micron TiB
2amount ratio be 1:2 ~ 3 volume ratios.
According to the present invention, preferred, the feed composition volume percent is:
Described nanometer TiB
2volume percent be 15-25%; The volume percent of described micron WC is 8-12%; The volume percent of described micron h-BN is 8-10%; The volume percent of described micron Mo is 1-2%; The volume percent of described micron Ni is 3-4%; Micron TiB
2surplus.
According to the present invention, further preferred, the nano combined self-lubrication ceramic cutter material of described TiB2 base, the feed composition volume percent is: nanometer TiB
220%, micron TiB
255%, micron WC10%, micron h-BN10%, micron Mo2%, micron Ni3%.Wherein, nanometer TiB
2, the micron TiB
2, micron WC and a micron h-BN median size be respectively 50nm, 3-4 μ m, 1 μ m and 1.5 μ m, micron Mo, a micron Ni median size are 38 μ m(400 orders).
In above-mentioned each component, raw material used is commercially available prod, and purity all is greater than 99%.
The preparation method of the nano combined self-lubrication ceramic cutter material of TiB2 base of the present invention, the feed composition ratio as mentioned above, comprises that step is as follows:
(1) take in proportion nanometer TiB
2powder, the polyoxyethylene glycol (PEG4000) that the molecular weight of take is 4000 is dispersion agent, appropriate dehydrated alcohol is dispersion medium, is made into TiB
2suspension, with agitator fully stir, ultrasonic dispersion 20-30min;
(2) take in proportion a micron TiB
2powder, micron WC powder, micron h-BN powder be take respectively appropriate dehydrated alcohol as dispersion medium, are made into TiB
2suspension, WC suspension, h-BN suspension, more respectively with agitator fully stir, ultrasonic dispersion 15-30min;
(3) by above gained TiB
2suspension, WC suspension and h-BN suspension mix, and obtain complex phase suspension, then add in proportion micron Mo and micron Ni as sintering aid, and ultrasonic dispersion 15-30min, mix;
(4) step (3) gained mixture is poured in ball grinder, under protective atmosphere, be take dehydrated alcohol as medium, the pellet weight ratio of each component raw material total amount and mill ball is 1:10-12, ball milling 48-72h; Then successive drying 36-48h at 110-120 ℃ of temperature in the electric vacunm drying case then sieves in protective atmosphere, obtains mixed powder, seals standby;
(5) powder of step (4) gained is packed into graphite jig, then carry out vacuum heating-press sintering, and hot pressing parameters is: holding temperature 1600-1700 ℃, hot pressing pressure 25-35MPa, soaking time 20-40min, temperature rise rate 10-15 ℃/min.
Dehydrated alcohol described in above-mentioned steps (1), (2) is as the dispersion medium that is made into suspension, and consumption gets final product by conventional selection the in this area, and the present invention does not do and is particularly limited.
The method according to this invention, preferred, the described TiB of step (1)
2in suspension, the content of polyoxyethylene glycol PEG4000 is 3-5.5g/L.
The method according to this invention, preferred, the described protective atmosphere of step (4) is nitrogen or argon gas.
The method according to this invention, preferred, the mill ball that in step (4), ball milling is used is sintered carbide ball YG6 or YG8.Also claim the wolfram steel ball, market can be purchased.
The nano combined self-lubrication ceramic cutter material of TiB2 base of the present invention is with nano titanium diboride (TiB
2) and micron TiB2 (TiB
2) be matrix, the nano combined self-lubrication ceramic cutter material that micron hexagonal boron nitride (h-BN) is solid lubricant.
Nano combined self-lubrication ceramic cutter material of the present invention is with nano titanium diboride (TiB
2) and micron TiB2 (TiB
2) be matrix, add micron tungsten carbide (WC) as wild phase, micron hexagonal boron nitride (h-BN) is solid lubricant, usings micron molybdenum (Mo) and micron nickel (Ni) as sintering aid, through hot pressed sintering, forms.Excellent results is as follows:
1, by adding nanometer TiB
2as body material, can form typical intracrystalline/intergranular type structure at material internal, cause thus along crystalline substance/transcrystalline mixed-mode crack pattern.Due to nanometer TiB
2material has small-size effect, surface-interface effect and quantum size effect, can suppress the growth of matrix grain, by controlling the coupling that each feed composition size is suitable, utilizes its synergy, realizes the target of the mechanical property of raising material.
2, make solid lubricant by adding h-BN, can in working angles, at the composite ceramics wear surface, form one deck and contain B
2o
3, SiO
2and Fe
2o
3friction film, significantly reduce the frictional coefficient of cutter material, improve the friction and wear behavior of material.Due to the laminate structure of h-BN, can suppress the growth of material internal crystal grain; The multiple mechanism such as crack deflection, crackle branch, crackle bridging acts synergistically, and jointly improves the fracture toughness property of material.In addition, its high temperature oxidation resistance of h-BN is better, can be until still have good self-lubricating property in the temperature range of 900 ℃.
3, with the micron self-lubrication ceramic cutter material of prior art, compare, this nano combined self-lubrication ceramic cutter material has higher mechanical property, can be used for making cutting tool, mould and other abrasion-proof corrosion-proof component.
The accompanying drawing explanation
Fig. 1-4 are respectively scanning electronic microscope (SEM) photo of the nano combined self-lubrication ceramic cutter material of TiB2 base that makes of embodiment 1-4 successively, and the fracture mode of display material is along crystalline substance/transcrystalline mixed type.
Fig. 5 is high power scanning electronic microscope (SEM) photo of the nano combined self-lubrication ceramic cutter material of TiB2 base that makes of embodiment 2, the inner typical intracrystalline of display material/intergranular type structure.
Embodiment
Below in conjunction with embodiment, the invention will be further described.In the feed composition of each embodiment, nanometer TiB
2, the micron TiB
2, micron WC and a micron h-BN median size be respectively 50nm, 3-4 μ m, 1 μ m and 1.5 μ m, micron Mo, a micron Ni are 400 orders; Purity all is greater than 99%, is commercially available prod.Mill ball in embodiment is sintered carbide ball YG8.
Embodiment 1
Nano combined self-lubrication ceramic cutter material, the volume percent of feed composition is: nanometer TiB
220%, micron TiB
255%, micron WC10%, micron h-BN10%, micron Mo2%, micron Ni3%.The preparation method is as follows:
Take in proportion nanometer TiB
2powder, take PEG4000 as dispersion agent, and appropriate dehydrated alcohol is dispersion medium, is made into TiB
2suspension (PEG4000 content is 3g/L suspension), with agitator fully stir, ultrasonic wave is disperseed 25min; Take in proportion a micron TiB
2powder, add dehydrated alcohol and be made into mixing suspension, fully stirring, ultrasonic dispersion 20min; Take in proportion a micron WC powder and add dehydrated alcohol and be made into mixing suspension, fully stir, ultrasonic dispersion 20min; Take in proportion a micron h-BN powder and add dehydrated alcohol and be made into mixing suspension, fully stir, ultrasonic dispersion 15min; By gained TiB
2, WC and h-BN suspension mixes, and obtains complex phase suspension, then adds in proportion sintering aid Mo and Ni, through ultrasonic dispersion 25min, mix; Mixture is poured in ball grinder, be take rare gas element as protective atmosphere, take dehydrated alcohol as medium, take sintered carbide ball as grinding element, the pellet weight ratio is 1:11, ball milling 54h; Then in the electric vacunm drying case at 110 ℃ of lower successive drying 42h of design temperature, after complete drying, in inert gas flow, sieve, the graphite jig of then powder being packed into, carry out vacuum heating-press sintering.Hot pressing parameters is: 1650 ℃ of holding temperatures, hot pressing pressure 35MPa, soaking time 30min, 10 ℃/min of temperature rise rate.Obtain nano combined self-lubrication ceramic cutter material.
The nano combined self-lubrication ceramic cutter material sample made is carried out to the line cutting processing, and thick fine grinding, grinding, polishing record its mechanical property parameters and are: bending strength 750MPa, fracture toughness property 5.0MPam
1/2, Vickers' hardness 15.5GPa.Frictional coefficient is 0.29.
Embodiment 2
Nano combined self-lubrication ceramic cutter material, the volume percent of feed composition is: nanometer TiB
210%, micron TiB
265%, WC8%, micron h-BN12%, micron Mo2.5%, micron Ni2.5%.The preparation method is as follows:
Take in proportion nanometer TiB
2powder, appropriate dehydrated alcohol is dispersion medium, and the polyoxyethylene glycol (PEG4000) that the interpolation molecular weight is 4000 is dispersion agent, and dispersion agent PEG4000 content is 4.5g/L suspension, is made into TiB
2suspension.With agitator fully stir, ultrasonic wave is disperseed 20min; Take in proportion a micron TiB
2powder, add dehydrated alcohol and be made into mixing suspension, fully stirring, ultrasonic dispersion 15min; Take in proportion a micron WC powder and add dehydrated alcohol and be made into mixing suspension, fully stir, ultrasonic dispersion 15min; Take in proportion a micron h-BN powder and add dehydrated alcohol and be made into mixing suspension, fully stir, ultrasonic dispersion 20min; By gained TiB
2, WC and h-BN suspension mixes, and obtains complex phase suspension, then adds in proportion sintering aid micron Mo and a micron Ni, through ultrasonic dispersion 20min, mix; Mixture is poured in ball grinder, be take nitrogen as protective atmosphere, take dehydrated alcohol as medium, take sintered carbide ball as grinding element, the pellet weight ratio is 1:10, ball milling 48h; Then in the electric vacunm drying case at 110 ℃ of lower successive drying 48h of design temperature, after complete drying, in inert gas flow, sieve, the graphite jig of then powder being packed into, carry out vacuum heating-press sintering.Hot pressing parameters is: 1600 ℃ of holding temperatures, hot pressing pressure 28MPa, soaking time 40min, 10 ℃/min of temperature rise rate.Obtain nano combined self-lubrication ceramic cutter material.
The nano combined self-lubrication ceramic cutter material sample made is carried out to the line cutting processing, and thick fine grinding, grinding, polishing record its mechanical property parameters and are: bending strength 690MPa, fracture toughness property 4.9MPam
1/2, Vickers' hardness 15.6GPa.Frictional coefficient is 0.3.
Embodiment 3
Nano combined self-lubrication ceramic cutter material, the volume percent of feed composition is: nanometer TiB
230%, micron TiB
245%, micron WC12%, micron h-BN8%, micron Mo3%, micron Ni2%.The preparation method is as follows:
Take in proportion nanometer TiB
2powder, take PEG4000 as dispersion agent (content is 3.5g/L suspension), and appropriate dehydrated alcohol is dispersion medium, is made into TiB
2suspension, with agitator fully stir, ultrasonic wave is disperseed 30min; Take in proportion a micron TiB
2powder, add dehydrated alcohol and be made into mixing suspension, fully stirring, ultrasonic dispersion 15min; Take in proportion a micron WC powder and add dehydrated alcohol and be made into mixing suspension, fully stir, ultrasonic dispersion 25min; Take in proportion a micron h-BN powder and add dehydrated alcohol and be made into mixing suspension, fully stir, ultrasonic dispersion 20min; By gained TiB
2, WC and h-BN suspension mixes, and obtains complex phase suspension, then adds in proportion sintering aid Mo and Ni, through ultrasonic dispersion 30min, mix; Mixture is poured in ball grinder, be take rare gas element as protective atmosphere, take dehydrated alcohol as medium, take sintered carbide ball as grinding element, the pellet weight ratio is 1:12, ball milling 60h; Then in the electric vacunm drying case at 120 ℃ of lower successive drying 36h of design temperature, after complete drying, in inert gas flow, sieve, the graphite jig of then powder being packed into, carry out vacuum heating-press sintering.Hot pressing parameters is: 1680 ℃ of holding temperatures, hot pressing pressure 32MPa, soaking time 25min, 14 ℃/min of temperature rise rate.Obtain nano combined self-lubrication ceramic cutter material.
The nano combined self-lubrication ceramic cutter material sample made is carried out to the line cutting processing, and thick fine grinding, grinding, polishing record its mechanical property parameters and are: bending strength 678MPa, fracture toughness property 5.1MPam
1/2, Vickers' hardness 15.4GPa; Frictional coefficient is 0.31.
Embodiment 4
Nano combined self-lubrication ceramic cutter material, the volume percent of feed composition is: nanometer TiB
240%, micron TiB
235%, micron WC10%, micron h-BN9%, micron Mo1.5%, micron Ni4.5%.The preparation method is as follows:
Take in proportion nanometer TiB
2powder, take PEG4000 as dispersion agent (PEG4000 content is 4g/L suspension), and appropriate dehydrated alcohol is dispersion medium, is made into TiB
2suspension, with agitator fully stir, ultrasonic wave is disperseed 30min; Take in proportion a micron TiB
2powder, add dehydrated alcohol and be made into mixing suspension, fully stirring, ultrasonic dispersion 20min; Take in proportion a micron WC powder and add dehydrated alcohol and be made into mixing suspension, fully stir, ultrasonic dispersion 25min; Take in proportion a micron h-BN powder and add dehydrated alcohol and be made into mixing suspension, fully stir, ultrasonic dispersion 25min; By gained TiB
2, WC and h-BN suspension mixes, and obtains complex phase suspension, then adds in proportion sintering aid Mo and Ni, through ultrasonic dispersion 20min, mix; Mixture is poured in ball grinder, be take rare gas element as protective atmosphere, take dehydrated alcohol as medium, take sintered carbide ball as grinding element, the pellet weight ratio is 1:10, ball milling 66h; Then in the electric vacunm drying case at 110 ℃ of lower successive drying 40h of design temperature, after complete drying, in inert gas flow, sieve, the graphite jig of then powder being packed into, carry out vacuum heating-press sintering.Hot pressing parameters is: 1620 ℃ of holding temperatures, hot pressing pressure 30MPa, soaking time 35min, 12 ℃/min of temperature rise rate.Obtain nano combined self-lubrication ceramic cutter material.
The nano combined self-lubrication ceramic cutter material sample made is carried out to the line cutting processing, and thick fine grinding, grinding, polishing record its mechanical property parameters and are: bending strength 659MPa, fracture toughness property 5.2MPam
1/2, Vickers' hardness 15.1GPa; Frictional coefficient is 0.32.
Claims (1)
1. the preparation method of the nano combined self-lubrication ceramic cutter material of TiB2 base, the feed composition volume percent is:
Nanometer TiB
210-40%, micron WC 5-15%, micron h-BN 6-12%, micron Mo 1-3%, micron Ni 2-5%, all the other are micron TiB
2; Wherein,
Described nanometer TiB
2median size is 40 ~ 80nm, micron TiB
2median size is 1-5 μ m;
Described micron WC, micron h-BN median size are 1 ~ 1.5 μ m;
Described micron Mo, micron Ni median size are 25 ~ 45 μ m;
Preparation process is as follows:
(1) take in proportion nanometer TiB
2powder, the polyoxyethylene glycol that the molecular weight of take is 4000 is dispersion agent, appropriate dehydrated alcohol is dispersion medium, is made into nanometer TiB
2suspension, with agitator fully stir, ultrasonic dispersion 20-30min;
(2) take in proportion a micron TiB
2powder, micron WC powder, micron h-BN powder be take respectively appropriate dehydrated alcohol as dispersion medium, are made into a micron TiB
2suspension, WC suspension, h-BN suspension, more respectively with agitator fully stir, ultrasonic dispersion 15-30min;
(3) by above gained nanometer TiB
2suspension, micron TiB
2suspension, WC suspension and h-BN suspension mix, and obtain complex phase suspension, then add in proportion micron Mo and micron Ni as sintering aid, and ultrasonic dispersion 15-30min, mix;
(4) step (3) gained mixture is poured in ball grinder, under protective atmosphere, be take dehydrated alcohol as medium, the pellet weight ratio of each component raw material total amount and mill ball is 1:10-12, ball milling 48-72h; Then successive drying 36-48h at 110-120 ℃ of temperature in the electric vacunm drying case then sieves in protective atmosphere, obtains mixed powder, seals standby;
(5) powder of step (4) gained is packed into graphite jig, then carry out vacuum heating-press sintering, and hot pressing parameters is: holding temperature 1600-1700 ℃, hot pressing pressure 25-35MPa, soaking time 20-40min, temperature rise rate 10-15 ℃/min.
2. the preparation method of the nano combined self-lubrication ceramic cutter material of TiB2 base according to claim 1, is characterized in that described nanometer TiB
2with micron TiB
2amount ratio be 1:2 ~ 3 volume ratios.
3. the preparation method of the nano combined self-lubrication ceramic cutter material of TiB2 base according to claim 1, is characterized in that, the feed composition volume percent is:
Described nanometer TiB
2volume percent be 15-25%; The volume percent of described micron WC is 8-12%; The volume percent of described micron h-BN is 8-10%; The volume percent of described micron Mo is 1-2%; The volume percent of described micron Ni is 3-4%; Micron TiB
2surplus.
4. the preparation method of the nano combined self-lubrication ceramic cutter material of TiB2 base according to claim 1, is characterized in that, described feed composition volume percent is: nanometer TiB
220%, micron TiB
255%, micron WC 10%, micron h-BN 10%, micron Mo 2%, micron Ni 3%; Wherein, nanometer TiB
2, the micron TiB
2, micron WC and a micron h-BN median size be respectively 50nm, 3-4 μ m, 1 μ m and 1.5 μ m, micron Mo, a micron Ni median size are 38 μ m.
5. the preparation method of the nano combined self-lubrication ceramic cutter material of TiB2 base according to claim 1, is characterized in that, the described nanometer TiB of step (1)
2in suspension, the content of polyoxyethylene glycol PEG4000 is 3-5.5g/L.
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| CN104355649A (en) * | 2014-10-29 | 2015-02-18 | 安徽省皖捷液压科技有限公司 | Special ceramics for nozzle and preparation method for special ceramics |
| CN104355650A (en) * | 2014-10-29 | 2015-02-18 | 安徽省皖捷液压科技有限公司 | Cracking-resistant ceramic for nozzles and preparation method of crack-resisting ceramic |
| CN105819863A (en) * | 2016-03-10 | 2016-08-03 | 湘潭大学 | High-performance in situ reaction self-lubricating ceramic cutter material and preparation method thereof |
| CN106242575A (en) * | 2016-07-30 | 2016-12-21 | 余姚市巧迪电器厂 | A kind of chromium boride base composite ceramic mold materials and preparation method thereof |
| CN106278279A (en) * | 2016-07-30 | 2017-01-04 | 余姚市巧迪电器厂 | A kind of titanium boride base composite ceramic mold materials and preparation method thereof |
| CN106994039A (en) * | 2017-05-23 | 2017-08-01 | 南通大学附属医院 | A kind of preparation method of new Sagittal condylar fracture replacement and fixation pincers and its binding clip |
| CN109437915A (en) * | 2018-11-19 | 2019-03-08 | 广东工业大学 | A kind of transition metal boride hard ceramic material and its preparation method and application |
| CN110157998B (en) * | 2019-05-27 | 2021-02-02 | 太原理工大学 | Superhard self-lubricating cutter material and preparation method thereof |
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