CN101798216B - Zirconium oxide-based nano ceramic tool and die material added with titanium boride and preparation method thereof - Google Patents
Zirconium oxide-based nano ceramic tool and die material added with titanium boride and preparation method thereof Download PDFInfo
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- CN101798216B CN101798216B CN201010129537XA CN201010129537A CN101798216B CN 101798216 B CN101798216 B CN 101798216B CN 201010129537X A CN201010129537X A CN 201010129537XA CN 201010129537 A CN201010129537 A CN 201010129537A CN 101798216 B CN101798216 B CN 101798216B
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Abstract
The invention relates to a nano ceramic tool and die material and a preparation method thereof. The ceramic tool and die material is sintered from yttrium stabilized nano ZrO2 serving as matrix, added micro TiB2 and micro alpha-Al2O3 serving as enhancing phases and micro molybdenum, nickel and magnesium oxide serving as sintering aids. The preparation method comprises the following steps: dispersing the nano ZrO2, micro TiB2 and micro alpha-Al2O3 powder respectively, ball-mixing and drying the power to obtain a powdery material, and sintering the powdery material by adopting a hot-pressing method. The method is favorable for improving the mechanical property of the material, and has the advantages of simple preparation, convenient operation and the like. The obtained nano ceramic tool and die material has good comprehensive mechanical property, friction reduction and abrasion resistance, and can be used for manufacturing cutting tools, dies and other abrasion and corrosion resistant parts.
Description
Technical field
The present invention relates to a kind of potter's moulding stock and preparation method thereof, particularly a kind of Zirconium oxide-based nano ceramic tool die material that adds titanium boride and preparation method thereof.
Background technology
The thermostability and the wear resistance of stupalith are splendid, are the ideal materials of making tool and moulds such as cutter and mould.CN1332262A provides a kind of cermet mold material, and chemical ingredients (weight %) is: w10-60%, Cr38.5-80%, Al
2O
31-30%, La
2O
30-15%, any or any two above sum is 0.5-20% among Ni, Co, the Fe.Said material red hardness height, Heat stability is good, oxidation-resistance and high abrasion resistance, good toughness, anti-rapid heat cycle excellent performance.
The ceramic cutting tool material of using at present is confined to a micron composite ceramics mostly, and the mechanical property of material especially intensity, toughness still awaits further raising.Therefore, the research and development of nano modification, nano-micrometre composite ceramic tool material are one of main directions of cutter material development from now on.
Nano composite ceramic cutter material mainly comprises Si
3N
4/ TiNn, Si
3N
4/ TiCn, Si
3N
4-Al
2O
3n-TiC-Y
2O
3, Al
2O
3/ TiC/SiCn, Al
2O
3/ TiCn, Al
2O
3/ Al
2O
3n/ SiC
n, Al
2O
3/ Ti (C
0.7N
0.3)
n/ SiC
n, Al
2O
3/ SiC/SiC
n, Al
2O
3/ TiC/TiN
nDeng, all have than better mechanical property of micron composite ceramic tool material and cutting ability.
From domestic and international present situation, be applied to mould industry stupalith kind seldom, applicable mould applications is very narrow.At present, the applied research of stupalith in all kinds of moulds is confined to a micron composite ceramic material mostly, like ZrO
2Toughness reinforcing Al
2O
3Base composite ceramic ZTA wortle, TZP/TiC/Al
2O
3, Al
2O
3/ TiC composite ceramics wortle, (Ce-TZP)-Al
2O
3Hot-extrusion mold, 3Y-TZP-Al
2O
3Pottery drawing die, PSZ pottery hot extruding die, Al
2O
3/ Cr
3C
2/ (W, Ti) C etc.
CN101164963A provides a kind of micro-nano composite ceramic die material and preparation method thereof with micron order Al
2O
3Pottery is a matrix, and (C, N) the ceramic hard particle forms as the sintering aid hot pressed sintering with Mo, Ni and MgO as disperse phase to add nano level Ti.The stupalith sample of gained carries out cutting processing and records mechanical property parameters and be: bending strength 743-789MPa, fracture toughness property 7.4-8.2MPam
1/2, hardness 19.5-20.4GPa (embodiment 1-3).
Nano composite ceramic is used like multiple platform TZP ceramic die, Al at moulding stock
2O
3(C N) etc., obtains certain good result to/Ti.Can find out that from existing research the performance advantage of nano composite ceramic still fails to be not fully exerted in tool and mould fields such as cutter and moulds.With regard to present general status, the kind of potter's moulding stock, performance and range of application all await further enlarging and improving.
Summary of the invention
In order to overcome the weak point of prior art, the present invention provides the better Zirconium oxide-based nano ceramic tool and mould of a kind of comprehensive mechanical property matrix material and preparation method thereof.
Composite ceramic material of the present invention is a kind ofly to strengthen nano zirconium oxide based potter's moulding stock through adding micron titanium boride and micrometer alumina.Technical scheme of the present invention is following:
A kind of nano ceramics tool die material is with yttrium stabilized nano ZrO
2Be matrix, add micron TiB
2With micron α-Al
2O
3As wild phase, as sintering aid, form through hot pressed sintering with micron molybdenum (Mo), micron nickel (Ni) and micron Natural manganese dioxide (MgO); The feed composition volume percent is: TiB
25-20%, α-Al
2O
35-20%, Mo 0.5-2%, Ni 1-3%, MgO 0.5-1.5%, all the other are yttrium stabilized nano ZrO
2Described yttrium stabilized nano ZrO
2Be 4-6mol% yttrium stabilized nano ZrO
2
Preferably, described yttrium stabilized nano ZrO
2Be 5mol% yttrium stabilized nano zirconium white, below be abbreviated as 5Y-ZrO
2, use 5Y-ZrO
2The comprehensive mechanical property of gained moulding stock is best.
Preferably, said TiB
2Volume percent be 5-15%.
Preferably, said α-Al
2O
3Volume percent be 5-15%, further preferred 6-10%.Use α-Al
2O
3Al than other crystal formations
2O
3The mechanical property of gained tool die material is best.
Preferably, the volume percent of said Mo is 1-1.5%.The volume percent of said Ni is 1.5-2.5%.The volume percent of said MgO is 0.8-1.2%.
Preferably, in above-mentioned each component, used raw material is the commercially available prod, wherein the stable ZrO of yttrium
2Nanometer powder, micron α-Al
2O
3Powder and micron TiB
2The powder median size is respectively 39nm, 1 μ m and 1.5 μ m, and purity is all greater than 99%.
Most preferred, the feed composition volume percent of nano ceramics tool die material of the present invention is following:
5Y-ZrO
2?81％，TiB
2?8％，α-Al
2O
3?7％，Mo?1.1％，Ni?1.9％，MgO?1％。
The preparation method of nano ceramics tool die material of the present invention, feed composition ratio comprise that step is following as stated:
(1) takes by weighing the stable ZrO of yttrium in proportion
2Nanometer powder is that 4000 polyoxyethylene glycol (PEG4000) is a dispersion agent with molecular weight, with the stable ZrO of yttrium
2The nanometer powder quality is the radix meter, and the addition of dispersion agent is 0.2-1.0wt%; With an amount of absolute ethyl alcohol is dispersion medium, is made into the stable ZrO of yttrium
2Suspension-s, with whisking appliance fully stir, ultra-sonic dispersion 20-30min, use HCl, NH again
4OH regulates the pH value of suspension-s to 3-4;
(2) with TiB
2And α-Al
2O
3Powder independent ball milling 60-80 hour respectively, successive drying under 110-120 ℃ of temperature in the electric vacunm drying case sieves in inert gas flow behind the complete drying then, seals subsequent use.
(3) take by weighing the TiB that step (2) makes in proportion
2Powder adds absolute ethyl alcohol and is made into TiB
2Suspension-s, fully stirring, ultra-sonic dispersion 20-30min;
(4) take by weighing α-Al that step (2) makes in proportion
2O
3Powder adds absolute ethyl alcohol and is made into α-Al
2O
3Suspension-s, fully stirring, ultra-sonic dispersion 20-30min;
(5) with the stable ZrO of above gained yttrium
2Suspension-s, TiB
2Suspension-s and α-Al
2O
3Suspension-s mixes, and obtains complex phase suspension-s, adds sintering aid Mo, Ni and MgO then in proportion, and ultra-sonic dispersion 20-30min mixes;
(6)) step (5) gained mixture being poured in the ball grinder, is protective atmosphere with the rare gas element, is medium with the absolute ethyl alcohol, and the pellet weight ratio of each component raw material total amount and mill ball is 1: 10-12, ball milling 50-80h; Successive drying under 110-120 ℃ of temperature in the electric vacunm drying case sieves in inert gas flow behind the complete drying then, obtains mixed powder, seals subsequent use;
(7) adopt the pressure sintering sintering, in hot pressing furnace with the powder pressing mold sinter molding of step (6) gained.
Absolute ethyl alcohol described in above-mentioned steps (1), (3) and (4) is as the dispersion medium that is made into suspension-s, and consumption gets final product by conventional selection the in this area, and the present invention does not do special qualification.
Preferably, the mill ball that ball milling is used in step (2) and (6) is a sintered carbide ball.
Preferably, rare gas element is nitrogen or argon gas in step (2) and (6).
Preferably, above-mentioned steps (7) pressure sintering agglomerating operation steps is following:
Earlier with the powder of step (6) the gained graphite jig of packing into, carry out vacuum heating-press sintering then, hot pressing parameters is: holding temperature 1400-1500 ℃; Hot pressing pressure 30-35MPa; Soaking time 40-80min, applies the 100-150min insulation by temperature rise rate 15-25 ℃/min in the time of 1100 ℃.
Excellent results of the present invention is following:
Nano ceramics tool die material of the present invention is through at the stable ZrO of yttrium
2Add micron order hard phase TiB in the nano ceramics matrix
2With micron Al
2O
3Nano combined as the wild phase realization, can form typical intracrystalline/intergranular hybrid architecture at material internal, cause thus along crystalline substance/transcrystalline mixed type fracture mode, highly malleablized mechanism and ZrO that these nano ceramics are exclusive
2Multiple toughened and reinforced mechanism such as transformation toughening, crack deflection, crackle branch, crackle bridging acts synergistically, and improves the mechanical property of material jointly.In addition, to ZrO
2The deficiency that ceramic hardness is on the low side is through TiB
2Adding, can effectively bring into play TiB
2The advantage of high firmness (microhardness reaches more than the 30GPa), thus the hardness performance of matrix material improved.And TiB
2At high temperature can also reduce frictional coefficient, improve the wear resisting property and the antioxidant property of material through the formation of sull.Compare with existing potter's moulding stock; This nano ceramics tool die material has higher intensity, toughness and hardness and good properties of antifriction and wear resistance, can be used for making potter's mould and other wear-resisting and rotten component such as overflow mould, drawing die and cutting tool.
Description of drawings
Fig. 1 is the ZrO that embodiment 1 makes
2The transmission electron microscope of nano ceramics tool die material (TEM) photo, the inner typical intracrystalline of display material/intergranular hybrid architecture.Can see clearly that from figure the nano particle part disperse of size about 100nm is inner in ceramic crystalline grain, part is present in (being the interface of crystal grain and intergranule) on the crystal boundary, has formed typical intracrystalline/intergranular hybrid architecture.
Embodiment
Below in conjunction with embodiment the present invention is further specified.In the feed composition of each embodiment, used 5Y-ZrO
2And 4Y-ZrO
2The nanometer powder median size is 39nm, and purity is greater than 99%; α-Al
2O
3Micron powder and TiB
2Micron powder median size is respectively 1 μ m and 1.5 μ m, and purity is all greater than 99%.Be the commercially available prod.
Embodiment 1
The nano ceramics tool die material, the volume percent of feed composition is: 81%5Y-ZrO
2, 8%TiB
2, 7% α-Al
2O
3, 1.1%Mo, 1.9%Ni, 1%MgO.The preparation method is following:
Take by weighing 5Y-ZrO in proportion
2Nanometer powder is that 4000 polyoxyethylene glycol (PEG4000) is a dispersion agent with molecular weight, with 5Y-ZrO
2The nanometer powder quality is the radix meter, and the addition of dispersion agent is 0.6wt%; With an amount of absolute ethyl alcohol is dispersion medium, is made into 5Y-ZrO
2Suspension-s, with whisking appliance fully stir, ultra-sonic dispersion 25min, use HCl and NH again
4OH regulates the pH value to 3 of suspension-s; With raw material TiB
2And α-Al
2O
3Powder is independent ball milling 70 hours respectively, and successive drying under 110 ℃ of temperature in the electric vacunm drying case sieves in inert gas flow behind the complete drying then, seals subsequent use.Take by weighing the TiB that makes in proportion
2Powder adds absolute ethyl alcohol and is made into TiB
2Suspension-s, fully stirring, ultra-sonic dispersion 25min; Take by weighing the α-Al that makes in proportion
2O
3Powder adds absolute ethyl alcohol and is made into α-Al
2O
3Suspension-s, fully stirring, ultra-sonic dispersion 25min; With gained 5Y-ZrO
2, TiB
2And α-Al
2O
3Suspension-s mixes, and obtains complex phase suspension-s, adds sintering aid Mo, Ni and MgO then in proportion, through ultra-sonic dispersion 30min, mixes; Mixture is poured in the ball grinder, is protective atmosphere with the rare gas element, is medium with the absolute ethyl alcohol, is grinding element with the sintered carbide ball, and the pellet weight ratio is 1: 10, ball milling 60h; Then in the electric vacunm drying case at 110 ℃ of following successive dryings of design temperature, in inert gas flow, sieve behind the complete drying, with the powder graphite jig of packing into, carry out vacuum heating-press sintering then.Hot pressing parameters is: 1430 ℃ of holding temperatures, and hot pressing pressure 35MPa, soaking time 60min, 20 ℃/min of temperature rise rate applies the 120min insulation in the time of 1100 ℃.The stupalith sample that makes is carried out cutting processing, record its mechanical property parameters and be: bending strength 1055MPa, fracture toughness property 10.57MPam
1/2, Vickers' hardness 13.59GPa.
Embodiment 2
The nano ceramics tool die material, the volume percent of feed composition is: 86.7%5Y-ZrO
2, 5%TiB
2, 5% α-Al
2O
3, 1%Mo, 1.5%Ni, 0.8%MgO.The preparation method is following:
Take by weighing 5Y-ZrO in proportion
2Nanometer powder is that 4000 polyoxyethylene glycol (PEG4000) is a dispersion agent with molecular weight, with 5Y-ZrO
2The nanometer powder quality is the radix meter, and the addition of dispersion agent is 0.3wt%; With an amount of absolute ethyl alcohol is dispersion medium, is made into 5Y-ZrO
2Suspension-s, with whisking appliance fully stir, ultra-sonic dispersion 20min, use HCl and NH again
4OH regulates the pH value to 4 of suspension-s; With TiB
2And α-Al
2O
3Powder is independent ball milling 60 hours respectively, and successive drying under 120 ℃ of temperature in the electric vacunm drying case sieves in inert gas flow behind the complete drying then, seals subsequent use.Take by weighing the TiB that makes in proportion
2Powder adds absolute ethyl alcohol and is made into TiB
2Suspension-s, fully stirring, ultra-sonic dispersion 20min; Take by weighing the α-Al that makes in proportion
2O
3Powder adds absolute ethyl alcohol and is made into α-Al
2O
3Suspension-s, fully stirring, ultra-sonic dispersion 20min; With gained 5Y-ZrO
2, TiB
2And α-Al
2O
3Suspension-s mixes, and obtains complex phase suspension-s, adds sintering aid Mo, Ni and MgO then in proportion, through ultra-sonic dispersion 20min, mixes; Mixture is poured in the ball grinder, is protective atmosphere with the rare gas element, is medium with the absolute ethyl alcohol, is grinding element with the sintered carbide ball, and the pellet weight ratio is 1: 11, ball milling 50h; Then in the electric vacunm drying case at 120 ℃ of following successive dryings of design temperature, in inert gas flow, sieve behind the complete drying, with the powder graphite jig of packing into, carry out vacuum heating-press sintering then.Hot pressing parameters is: 1410 ℃ of holding temperatures, and hot pressing pressure 30MPa, soaking time 50min, 15 ℃/min of temperature rise rate applies the 100min insulation in the time of 1100 ℃.The stupalith sample that makes is carried out cutting processing, record its mechanical property parameters and be: bending strength 986MPa, fracture toughness property 9.7MPam
1/2, Vickers' hardness 12.66GPa.
Embodiment 3
The nano ceramics tool die material, the volume percent of feed composition is: 72.8%5Y-ZrO
2, 12%TiB
2, 10% α-Al
2O
3, 1.5%Mo, 2.5%Ni, 1.2%MgO.The preparation method is following:
Take by weighing 5Y-ZrO in proportion
2Nanometer powder is that 4000 polyoxyethylene glycol (PEG4000) is a dispersion agent with molecular weight, with 5Y-ZrO
2The nanometer powder quality is the radix meter, and the addition of dispersion agent is 0.8wt%; With an amount of absolute ethyl alcohol is dispersion medium, is made into 5Y-ZrO
2Suspension-s, with whisking appliance fully stir, ultra-sonic dispersion 30min, use HCl and NH again
4OH regulates the pH value to 3 of suspension-s; With TiB
2And α-Al
2O
3Powder is independent ball milling 80 hours respectively, and successive drying under 110 ℃ of temperature in the electric vacunm drying case sieves in inert gas flow behind the complete drying then, seals subsequent use.Take by weighing the TiB that makes in proportion
2Powder adds absolute ethyl alcohol and is made into TiB
2Suspension-s, fully stirring, ultra-sonic dispersion 30min; Take by weighing the α-Al that makes in proportion
2O
3Powder adds absolute ethyl alcohol and is made into α-Al
2O
3Suspension-s, fully stirring, ultra-sonic dispersion 30min; With gained 5Y-ZrO
2, TiB
2And α-Al
2O
3Suspension-s mixes, and obtains complex phase suspension-s, adds sintering aid Mo, Ni and MgO then in proportion, through ultra-sonic dispersion 25min, mixes; Mixture is poured in the ball grinder, is protective atmosphere with the rare gas element, is medium with the absolute ethyl alcohol, is grinding element with the sintered carbide ball, and the pellet weight ratio is 1: 12, ball milling 80h; Then in the electric vacunm drying case at 110 ℃ of following successive dryings of design temperature, in inert gas flow, sieve behind the complete drying, with the powder graphite jig of packing into, carry out vacuum heating-press sintering then.Hot pressing parameters is: 1470 ℃ of holding temperatures, and hot pressing pressure 32MPa, soaking time 80min, 25 ℃/min of temperature rise rate applies the 140min insulation in the time of 1100 ℃.The stupalith sample that makes is carried out cutting processing, record its mechanical property parameters and be: bending strength 913MPa, fracture toughness property 9.42MPam
1/2, Vickers' hardness 13.28GPa.
Embodiment 4
Of embodiment 1, different is to use 4Y-ZrO
2Replace 5Y-ZrO
2, the volume percent of feed composition is: 80%4Y-ZrO
2, 8%TiB
2, 8% α-Al
2O
3, 1.1%Mo, 1.9%Ni, 1%MgO.The stupalith sample that makes is carried out cutting processing, record its mechanical property parameters and be: bending strength 979MPa, fracture toughness property 9.94MPam
1/2, Vickers' hardness 13.37GPa.
Claims (9)
1. a nano ceramics tool die material is with yttrium stabilized nano ZrO
2Be matrix, add micron TiB
2With micron α-Al
2O
3As wild phase, as sintering aid, form through hot pressed sintering with micron molybdenum, micron nickel and micron Natural manganese dioxide; The feed composition volume percent is: TiB
25-20%, α-Al
2O
35-20%, Mo 0.5-2%, Ni 1-3%, MgO 0.5-1.5%, all the other are yttrium stabilized nano ZrO
2Described yttrium stabilized nano ZrO
2Be 4-6mol% yttrium stabilized nano ZrO
2
2. nano ceramics tool die material according to claim 1 is characterized in that, described yttrium stabilized nano ZrO
2It is 5mol% yttrium stabilized nano zirconium white.
3. nano ceramics tool die material according to claim 1 is characterized in that, said TiB
2Volume percent be 5-15%, said α-Al
2O
3Volume percent be 5-15%.
4. nano ceramics tool die material according to claim 1 is characterized in that, said α-Al
2O
3Volume percent be 6-10%.
5. nano ceramics tool die material according to claim 1 is characterized in that, the volume percent of said Mo is 1-1.5%, and the volume percent of said Ni is 1.5-2.5%, and the volume percent of said MgO is 0.8-1.2%.
6. nano ceramics tool die material according to claim 1 is characterized in that, the feed composition volume percent is following:
5Y-ZrO
2?81％，TiB
2?8％，α-Al
2O
3?7％，Mo?1.1％，Ni?1.9％，MgO?1％。
7. the preparation method of the arbitrary described nano ceramics tool die material of claim 1-6 comprises that step is following:
(1) takes by weighing yttrium stabilized nano ZrO in proportion
2, be that 4000 polyoxyethylene glycol is a dispersion agent with molecular weight, with yttrium stabilized nano ZrO
2Quality is the radix meter, and the addition of dispersion agent is 0.2-1.0wt%; With an amount of absolute ethyl alcohol is dispersion medium, is made into the stable ZrO of yttrium
2Suspension-s, with whisking appliance fully stir, ultra-sonic dispersion 20-30min, with HCl, NH
4OH regulates the pH value of suspension-s to 3-4;
(2) with TiB
2And α-Al
2O
3Powder independent ball milling 60-80 hour respectively, successive drying under 110-120 ℃ of temperature in the electric vacunm drying case sieves in inert gas flow behind the complete drying then, seals subsequent use;
(3) take by weighing the TiB that step (2) makes in proportion
2Powder adds absolute ethyl alcohol and is made into TiB
2Suspension-s, fully stirring, ultra-sonic dispersion 20-30min;
(4) take by weighing α-Al that step (2) makes in proportion
2O
3Powder adds absolute ethyl alcohol and is made into α-Al
2O
3Suspension-s, fully stirring, ultra-sonic dispersion 20-30min;
(5) with the stable ZrO of above gained yttrium
2Suspension-s, TiB
2Suspension-s and α-Al
2O
3Suspension-s mixes, and obtains complex phase suspension-s, adds sintering aid Mo, Ni and MgO then in proportion, and ultra-sonic dispersion 20-30min mixes;
(6) step (5) gained mixture being poured in the ball grinder, is protective atmosphere with the rare gas element, is medium with the absolute ethyl alcohol, and the pellet weight ratio of each component raw material total amount and mill ball is 1: 10-12, ball milling 50-80h; Successive drying under 110-120 ℃ of temperature in the electric vacunm drying case sieves in inert gas flow behind the complete drying then, obtains mixed powder, seals subsequent use;
(7) adopt the pressure sintering sintering, in hot pressing furnace with the powder pressing mold sinter molding of step (6) gained.
8. the preparation method of nano ceramics tool die material according to claim 7 is characterized in that, rare gas element is one of nitrogen, argon gas described in the step (6).
9. the preparation method of nano ceramics tool die material according to claim 7; It is characterized in that; Step (7) pressure sintering sintering process parameter is: holding temperature 1400-1500 ℃, and hot pressing pressure 25-35MPa, soaking time 40-80min; Temperature rise rate 15-25 ℃/min, apply the 100-150min insulation in the time of 1100 ℃.
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| CN104370542B (en) * | 2014-10-27 | 2016-03-02 | 合肥市东庐机械制造有限公司 | A kind of zirconia-based ceramics cutter material and preparation method thereof |
| CN104388792B (en) * | 2014-10-31 | 2016-06-08 | 青岛橡胶谷知识产权有限公司 | A kind of high temperature resistant cermet material and its preparation method |
| CN106518068A (en) * | 2016-11-10 | 2017-03-22 | 佛山蓝途科技有限公司 | High-strength composite ceramic tool and preparation method thereof |
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| CN112266251B (en) * | 2020-10-29 | 2023-09-19 | 齐鲁工业大学 | Preparation method of silicon nitride/titanium carbide ceramic material based on spark plasma sintering |
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