CN101767989A - ZrO2/Ti (C, N) nano composite ceramic mold material and its prepn - Google Patents
ZrO2/Ti (C, N) nano composite ceramic mold material and its prepn Download PDFInfo
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- CN101767989A CN101767989A CN200910229440A CN200910229440A CN101767989A CN 101767989 A CN101767989 A CN 101767989A CN 200910229440 A CN200910229440 A CN 200910229440A CN 200910229440 A CN200910229440 A CN 200910229440A CN 101767989 A CN101767989 A CN 101767989A
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Abstract
The invention relates to a nano composite ceramic mould material and a preparation method thereof. The nano composite ceramic mould material is prepared by adopting a nano-nano compositing method, using nano 4-6Y-ZrO2 as a base body, adding nano Ti(C, N) as a reinforced phase and using nano alpha-Al2O3 and micron molybdenum, nickel and magnesium oxide as sintering aids for hot pressed sintering. The preparation method comprises the following steps of: firstly respectively dispersing nano 4-6Y-ZrO2 and Ti(C, N) or alpha-Al2O3 powder into a dispersion medium; and ball-milling and drying to obtain powder. The invention is beneficial to improving the mechanical property of the material by carrying out the hot pressed sintering by adopting temperature sectional type hot pressing process, and has simple preparation method and convenient operation; and in addition, the obtained nano composite ceramic mould material has good comprehensive mechanical property and abrasion resistance and can be used for manufacturing an extrusion mould, a drawing mould, a cutting tool, an abrasion and corrosion resistant part, and the like.
Description
Technical field
The present invention relates to a kind of ceramic die material and preparation method thereof, (Ti (C, N)) strengthens nano zircite (ZrO to particularly a kind of nano-carbon titanium nitride
2) nano composite ceramic mould material and preparation method thereof.
Background technology
The thermostability and the wear resistance of stupalith are splendid, be the ideal material of making shaping dies, but its toughness are relatively poor, therefore also are not used widely in the mould industry field.
At present, the applied research of stupalith in all kinds of moulds is confined to a micron composite ceramic material mostly.Wherein, ZrO
2Toughness reinforcing Al
2O
3Base composite ceramic ZTA can be used for making wortle, as a kind of novel moulding stock, is better than rapid steel, Wimet on some performance, and its fracture toughness property and bending strength reach about 7.2MPam respectively
1/2And 740MPa.Referring to Xu Yufen etc., TA high technology ceramics wortle draws the research of tungsten filament, HeFei University of Technology's journal (natural science edition), 1996,19 (4): 29-34.Other discovers, adopts TZP and the common toughness reinforcing Al of TiC
2O
3Can significantly improve TZP/TiC/Al
2O
3The mechanical property of composite ceramics, intensity and fracture toughness property can be brought up to 1106MPa and 11.86MPam respectively
1/2Referring to Yin Longwei etc., TZP-TiC-Al
2O
3The application of ceramic composite in mould, powder metallurgy technology, 1997,15 (4): 274-277.Employing pressure sinterings such as Yang Xuefeng are prepared Al
2O
3/ TiC composite ceramics wortle material, this material has good comprehensive mechanical properties, and bending strength is 850MPa, and fracture toughness property is 4.9MPam
1/2Referring to Yang Xuefeng, Al
2O
3The friction and abrasion of/TiC composite ceramics wortle material, silicate journal, 2005,33 (12): 1522-1526.Select better (the Cc-TZP)-Al of high-temperature behavior for use
2O
3Complex phase ceramic is made hot-extrusion mold, its bending strength 892MPa, fracture toughness property 14.3MPam
1/2, Vickers' hardness 10.9GPa allows 650 ℃ of working temperatures.This material has the excellent high-temperature mechanical property, is the suitable material of making copper, aluminium hot-extrusion mold.Referring to Liu Jun etc., hot extruding die is with the performance and the applied research of stupalith, Rare Metals Materials and engineering, 2003,32 (3): 232-235.Other has employing 3Y-TZP-Al
2O
3Stupalith is successfully developed TZP pottery drawing die.This material has higher intensity, hardness and toughness, and especially its fracture toughness property surpasses 10MPam
1/2, bending strength reaches 1450-1490MPa, and microhardness reaches 15-16.5GPa.Referring to Luo Junming etc., 3Y-TZP-Al
2O
3Pottery drawing die material and applied research, diamond and grinding materials and grinding tool engineering 2002, (2): 41-43.The TZP that Yang Gang etc. developed (3Y-8Ce-TZP) ceramic die material, fracture toughness property, bending strength and hardness are respectively 10MPam
1/2, 1335MPa and 15GPa, referring to Yang Gang etc., the exploitation of TZP ceramic bull block and application, mould industry, 2001, (9): 36-38.Shen Hui etc., the preparation and the applied research of PSZ pottery hot extruding die, the Jiangsu pottery, 1996,29 (2): fracture toughness property, bending strength and the hardness of the disclosed PSZ complex phase ceramic of 10-12 reach 10-14MPam respectively
1/2, 650-850MPa and greater than 90HRA, all can satisfy the service requirements of moulding stock preferably.In addition, the stupalith Al that succeeds in developing
2O
3/ Cr
3C
2/ (W, Ti) C has good comprehensive mechanical properties, also is the good material of preparation ceramic die.Referring to Sun Deming etc., Al
2O
3/ Cr
3C
2/ (W, Ti) C ceramic die material research, powder metallurgy technology, 2005,23 (5): 343-346.
Nano composite ceramic is also less in the research of moulding stock application facet.Adopt chemical coprecipitation to make the 3Y-TZP nano powder that median size is 20nm.With the compound 3Y-TZP micro mist of the 3Y-TZP nano powder of 3-10%, adopt isostatic pressing and sintering to prepare high performance compound TZP ceramic die, referring to good page or leaf recklessly etc., the development of nano combined TZP ceramic die, Foshan pottery, 2002, (6): 8-9.In addition, pass through to strengthen ZrO with a spot of 3Y-TZP nano powder
2Phase transformation enhancing and nanometer strengthen, and can significantly improve TZP ceramic die intensity, hardness, and firing temperature is reduced to 1480 ℃ from 1540 ℃.C.H.Xu etc., Preparation of an Advanced Al
2O
3BasedNanocomposite Ceramic Die Material, Materials Science Forum, 2009,628-629:465-470 has studied a kind of micro-nano composite ceramic die material Al
2O
3(C N), has also obtained good effect to/Ti.
From existing ceramic die research as can be seen, premium propertiess such as the hardness that stupalith is high, thermotolerance, wear resistance are brought into play far away because of its relatively poor obdurability, can only be used to not have or seldom have the mould of shock load and tensile stress, former mostly is static load equipment such as extrusion machine or hydropress, and mold shape is generally comparatively simple, and material only limits to ZTA, TZP, Sialon, Al
2O
3Pottery etc., and be limited to a micron composite ceramics more, the nano combined especially Na-performance advantage of Na composite ceramics fails to be applied in mould applications.With regard to present general status, the kind of ceramic die material, 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 invention provides a kind of Na-Na composite ceramic die material, be that nano-carbon titanium nitride strengthens the nano zircite nano composite ceramic mould material.The present invention also provides the preparation method of this nano composite ceramic mould material.
Nano composite ceramic mould material of the present invention is with yttrium stabilized nano ZrO
2Be matrix, (C is N) as wild phase, with nanometer α-Al to add nanometer Ti
2O
3, micron molybdenum (Mo), nickel (Ni) and magnesium oxide (MgO) forms as the sintering aid hot pressed sintering.The feed composition volume percent is as follows:: (C N) is 10-25%, α-Al to Ti
2O
3Be 5-15%, Mo is 1-5%, and Ni is 3-6%, and MgO is 0.5-1.5%, and 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
2Comprehensive mechanical property the best of gained moulding stock.
Preferably, described wild phase Ti (C, volume percent N) is 10-20%,
Preferably, described sintering aid α-Al
2O
3Volume percent be 8-15%, use α-Al
2O
3Al than other crystal formations
2O
3The mechanical property of gained moulding stock is best.
Preferably, the volume percent of described sintering aid Mo is 2-4%,
Preferably, the volume percent of described sintering aid Ni is 3-5%,
Preferably, the volume percent of described sintering aid MgO is 0.5-1.2%.
Preferably, in above-mentioned each component, used yttrium stabilized nano ZrO
2With nanometer α-Al
2O
3Powder is commercially available, and median size is respectively 39nm and 40nm, and purity is greater than 99%; (C N) is commercial powder to used Ti, and purity is greater than 98%, and median size is 80nm.
The preparation method of nano composite ceramic mould material of the present invention, component ratio as mentioned above, preparation process is as follows:
(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 dehydrated alcohol is dispersion medium, is made into the stable ZrO of yttrium
2Suspension, with agitator fully stir, ultra-sonic dispersion 20-30min, use HCl and NH again
4OH regulates the pH value of suspension to 3-4;
(2) take by weighing in proportion nanometer Ti (C, N) powder are that 4000 polyoxyethylene glycol (PEG4000) is a dispersion agent with molecular weight, with Ti (C, N) powder quality is the radix meter, the addition of dispersion agent is 0.2-1.0wt%; With an amount of dehydrated alcohol is dispersion medium, be made into Ti (C, N) suspension, with agitator fully stir, ultra-sonic dispersion 20-30min, use HCl and NH again
4OH regulates the pH value of suspension to 3-4;
(3) take by weighing nanometer α-Al in proportion
2O
3Powder is that 4000 polyoxyethylene glycol (PEG4000) is a dispersion agent with molecular weight, with α-Al
2O
3Powder quality is the radix meter, and the addition of dispersion agent is 0.2-1.0wt%; With an amount of dehydrated alcohol is dispersion medium, is made into α-Al
2O
3Suspension, with agitator fully stir, ultra-sonic dispersion 20-30min, use HCl and NH again
4OH regulates the pH value of suspension to 3-4;
(4) with step (1)-stable ZrO of (3) gained yttrium
2, Ti (C, N) and α-Al
2O
3Suspension mixes, and obtains complex phase suspension, and this complex phase suspension is regulated its pH value to 3-4 once more through ultra-sonic dispersion 10-20min, adds Mo, Ni and MgO sintering aid then in proportion, mixes;
(5) step (4) gained mixture being poured in the ball grinder, is protective atmosphere with the rare gas element, is medium with the dehydrated alcohol, is grinding element with the sintered carbide ball, ball milling 30-60h; Then in the electric vacunm drying case under design temperature successive drying, in inert gas flow, sieve behind the complete drying, obtain mixed powder, seal standby;
(6) adopt the pressure sintering sintering, in hot pressing furnace with the powder pressing mold sinter molding of step (5) gained.
Preferably, the pellet weight ratio of each component raw material total amount and sintered carbide ball is 1 in the step (5): 10-12.
Preferably, rare gas element is nitrogen or argon gas in the step (5).
Preferably, electric vacunm drying case design temperature is 110-120 ℃ in the step (5).
Preferably, above-mentioned steps (6) pressure sintering agglomerating operation steps is as follows:
The graphite jig of earlier powder of step (5) gained being packed into carries out vacuum heating-press sintering then; Hot pressing parameters is: heating-up time 30-40min, and holding temperature 1400-1550 ℃, hot pressing pressure 30-35MPa, soaking time 30-50min is cooled to room temperature then.
Further preferably take temperature section formula heat pressing process:
When i. heating up before temperature reaches 1000 ℃ little exert pressure, little pressure is 5-10MPa, when temperature reaches 1000 ℃ pressure is transferred to 20MPa, temperature is added to hot pressing pressure 30-35MPa gradually when reaching holding temperature 1400-1550 ℃;
Reduce moulding pressure by a small margin when ii. insulation finishes the back cooling, pressure regulation power was to 20MPa when promptly temperature dropped to 1100 ℃, and pressure regulation power is to 10MPa in the time of 950 ℃, and pressure regulation power is 0 in the time of 850 ℃; (Ti (C, N)) strengthens nano zircite (ZrO finally to obtain the product nano-carbon titanium nitride
2) nano composite ceramic mould material; In the temperature-fall period more than 850 ℃ the time cooling rate be 10-20 ℃/min, 20-30 ℃/min is up to room temperature in the time of below 850 ℃.
The hot pressing of above temperature section formula is to consider ZrO
2The phase transformation of pottery in temperature changing process and the volume change that thereupon produces are to guarantee ZrO
2The transformation toughening effect of pottery.Take temperature section formula heat pressing process, promptly in different temperature stage control hot pressing parameters differences.
Nano composite ceramic mould material of the present invention, (C N) realizes that as wild phase Na-Na is compound, can improve intensity, toughness and the hardness of material simultaneously by adding nanometer Ti, significantly improve the mechanical property and the use properties of material, and have simple, the easy to operate advantage of preparation method.Especially aspect preparation technology, consider ZrO
2The phase transformation of pottery in temperature changing process and the volume change that thereupon produces are to guarantee ZrO
2The transformation toughening effect of pottery, the present invention has taked temperature section formula heat pressing process especially, promptly takes different hot pressing parameterses in the different temperature stages, more helps improving the mechanical property of material.Compare with existing ceramic die material, this nano composite ceramic mould material has improved comprehensive mechanical performance and good abrasion resistance properties, can be used for making ceramic dies such as overflow mould, drawing die and cutting tool, wear-and corrosion-resistant component etc.
Embodiment
The present invention will be further described below in conjunction with embodiment.In the component of each embodiment, the ZrO that used yttrium is stable
2Nanometer powder and nanometer α-Al
2O
3Powder is commercially available, and median size is respectively 39nm and 40nm, and purity is greater than 99%; (C N) is commercial powder to used Ti, and purity is greater than 98%, and median size is 80nm.
Embodiment 1
Nano composite ceramic mould material, the volume percent of feed composition is: 63%5Y-ZrO
2, 16.5%Ti (C, N), 12% α-Al
2O
3, 4.5%Ni, 3%Mo, 1%MgO.The preparation method is as follows:
Take by weighing 5Y-ZrO in proportion respectively
2, Ti (C, N) and α-Al
2O
3Nanometer powder is that 4000 polyoxyethylene glycol is a dispersion agent with molecular weight, respectively with 5Y-ZrO
2, Ti (C, N) and α-Al
2O
3Powder quality is the radix meter, the addition 0.4wt% of dispersion agent; With an amount of dehydrated alcohol is dispersion medium, is made into 5Y-ZrO respectively
2, Ti (C, N) and α-Al
2O
3Powder suspension, with agitator fully stir, ultra-sonic dispersion 30min, use HCl and NH again
4OH regulates the pH value to 3.5 of suspension.With gained 5Y-ZrO
2, Ti (C, N) and α-Al
2O
3Suspension mixes, and obtains complex phase suspension, behind this complex phase suspension process ultra-sonic dispersion 20min, regulates its pH value to 3.5 once more, adds Mo, Ni and MgO sintering aid then in proportion, mixes; Mixture is poured in the ball grinder, is protective atmosphere with the rare gas element, is medium with the dehydrated 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 120 ℃ of following successive dryings of design temperature, in inert gas flow, sieve behind the complete drying, the graphite jig of then powder being packed into carries out vacuum heating-press sintering.Hot pressing parameters is: hot pressing pressure 30MPa, 1500 ℃ of holding temperatures, heating-up time 30min, soaking time 30min.Take temperature section formula heat pressing process: little pressure 5MPa pressurization before 1000 ℃ during intensification, in the time of 1000 ℃ pressure is transferred to 20MPa, be added to hot pressing pressure 30MPa during near 1500 ℃ of holding temperatures gradually; Insulation reduces moulding pressure after finishing by a small margin, is transferred to 20MPa during 1100 ℃ of left and right sides, is transferred to 10MPa in the time of 950 ℃, is transferred to 0 in the time of 850 ℃.In the temperature-fall period more than 850 ℃ the time cooling rate be 10 ℃/min, 20 ℃/min is up to room temperature in the time of below 850 ℃; Then the stupalith sample that makes is carried out cutting processing, record its mechanical property parameters and be: bending strength 958MPa, fracture toughness property 7.48MPam
1/2, Vickers' hardness 13.09GPa.
Embodiment 2
Nano composite ceramic mould material, the volume percent of each component is: 70.5%5Y-ZrO
2, 10%Ti (C, N), 10% α-Al
2O
3, 51%Ni, 4%Mo, 0.5%MgO.The preparation method is as follows:
Take by weighing 5Y-ZrO in proportion respectively
2, Ti (C, N) and α-Al
2O
3Nanometer powder is that 4000 polyoxyethylene glycol is a dispersion agent with molecular weight, respectively with 5Y-ZrO
2, Ti (C, N) and Al
2O
3Powder quality is the radix meter, the addition 1.0wt% of dispersion agent; With an amount of dehydrated alcohol is dispersion medium, is made into 5Y-ZrO respectively
2, Ti (C, N) and α-Al
2O
3Powder suspension, with agitator fully stir, ultra-sonic dispersion 30min, use HCl and NH again
4OH regulates the pH value to 3 of suspension.With gained 5Y-ZrO
2, Ti (C, N) and α-Al
2O
3Suspension mixes, and obtains complex phase suspension, behind this complex phase suspension process ultra-sonic dispersion 15min, regulates its pH value to 3 once more, adds Mo, Ni and MgO sintering aid then in proportion, mixes; Mixture is poured in the ball grinder, is protective atmosphere with the rare gas element, is medium with the dehydrated 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 110 ℃ of following successive dryings of design temperature, in inert gas flow, sieve behind the complete drying, the graphite jig of then powder being packed into carries out vacuum heating-press sintering.Hot pressing parameters is: hot pressing pressure 35MPa, 1460 ℃ of holding temperatures, heating-up time 40min, soaking time 50min.Take temperature section formula heat pressing process: little pressure 10MPa pressurization before 1000 ℃ during intensification, in the time of 1000 ℃ pressure is transferred to 20MPa, be added to hot pressing pressure 35MPa during near 1460 ℃ of holding temperatures gradually; Insulation reduces moulding pressure after finishing by a small margin, is transferred to 20MPa during 1100 ℃ of left and right sides, is transferred to 10MPa in the time of 950 ℃, is transferred to 0 in the time of 850 ℃.In the temperature-fall period more than 850 ℃ the time cooling rate be 15 ℃/min, 30 ℃/min is up to room temperature in the time of below 850 ℃; Then the stupalith sample that makes is carried out cutting processing, record its mechanical property parameters and be: bending strength 1152MPa, fracture toughness property 6.66MPam
1/2, Vickers' hardness 12.52GPa.
Embodiment 3
Nano composite ceramic mould material, the volume percent of each component is: 54.2%5Y-ZrO
2, 22%Ti (C, N), 15% α-Al
2O
3, 5%Ni, 3%Mo, 0.8%MgO.The preparation method is as follows:
Take by weighing 5Y-ZrO in proportion respectively
2, Ti (C, N) and α-Al
2O
3Nanometer powder is that 4000 polyoxyethylene glycol is a dispersion agent with molecular weight, respectively with 5Y-ZrO
2, Ti (C, N) and α-Al
2O
3Powder quality is the radix meter, the addition 0.4wt% of dispersion agent; With an amount of dehydrated alcohol is dispersion medium, is made into 5Y-ZrO respectively
2, Ti (C, N) and α-Al
2O
3Powder suspension, with agitator fully stir, ultra-sonic dispersion 25min, use HCl and NH again
4OH regulates the pH value to 4 of suspension.With gained 5Y-ZrO
2, Ti (C, N) and α-Al
2O
3Suspension mixes, and obtains complex phase suspension, behind this complex phase suspension process ultra-sonic dispersion 20min, regulates its pH value to 4 once more, adds Mo, Ni and MgO sintering aid then in proportion, mixes; Mixture is poured in the ball grinder, is protective atmosphere with the rare gas element, is medium with the dehydrated alcohol, is grinding element with the sintered carbide ball, and the pellet weight ratio is 1: 12, ball milling 40h; 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, the graphite jig of then powder being packed into carries out vacuum heating-press sintering.Hot pressing parameters is: hot pressing pressure 30MPa, 1540 ℃ of holding temperatures, heating-up time 40min, soaking time 40min.Take temperature section formula heat pressing process: little pressure 8MPa pressurization before 1000 ℃ during intensification, in the time of 1000 ℃ pressure is transferred to 20MPa, be added to hot pressing pressure 30MPa during near 1540 ℃ of holding temperatures gradually; Insulation reduces moulding pressure after finishing by a small margin, is transferred to 20MPa during 1100 ℃ of left and right sides, is transferred to 10MPa in the time of 950 ℃, is transferred to 0 in the time of 850 ℃.In the temperature-fall period more than 850 ℃ the time cooling rate be 10 ℃/min, 25 ℃/min is up to room temperature in the time of below 850 ℃; Then the stupalith sample that makes is carried out cutting processing, record its mechanical property parameters and be: bending strength 832MPa, fracture toughness property 8.42MPam
1/2, Vickers' hardness 12.67GPa.
Embodiment 4
Nano composite ceramic mould material, the volume percent of each component is: 70.5%4Y-ZrO
2, 10%Ti (C, N), 10% α-Al
2O
3, 51%Ni, 4%Mo, 0.5%MgO.The preparation method is with embodiment 2, and the gained stupalith records its mechanical property parameters and is: bending strength 972MPa, fracture toughness property 6.52MPam
1/2, Vickers' hardness 12.23GPa.
Embodiment 5
Nano composite ceramic mould material, the volume percent of each component is: 63%6Y-ZrO
2, 16.5%Ti (C, N), 12% α-Al
2O
3, 4.5%Ni, 3%Mo, 1%MgO.The preparation method is with embodiment 1, and the gained stupalith records its mechanical property parameters and is: bending strength 869MPa, fracture toughness property 7.31MPam
1/2, Vickers' hardness 12.73GPa.
Claims (9)
1. a nano composite ceramic mould material is with yttrium stabilized nano ZrO
2Be matrix, (C is N) as wild phase, with nanometer α-Al to add nanometer Ti
2O
3, micron molybdenum (Mo), nickel (Ni) and magnesium oxide (MgO) forms as the sintering aid hot pressed sintering; The feed composition volume percent is as follows: (C N) is 10-25%, α-Al to Ti
2O
3Be 5-15%, Mo is 1-5%, and Ni is 3-6%, and MgO is 0.5-1.5%, and all the other are yttrium stabilized nano ZrO
2Pottery; Described yttrium stabilized nano ZrO
2Be 4-6mol% yttrium stabilized nano ZrO
2
2. nano composite ceramic mould material according to claim 1 is characterized in that, described yttrium stabilized nano ZrO
2It is 5mol% yttrium stabilized nano zirconium white.
3. nano composite ceramic mould material according to claim 1 is characterized in that, (C, volume percent N) is 10-20% to described component wild phase Ti.
4. nano composite ceramic mould material according to claim 1 is characterized in that, described sintering aid α-Al
2O
3Volume percent be 8-15%.
5. nano composite ceramic mould material according to claim 1, it is characterized in that, the volume percent of described sintering aid Mo is 2-4%, and the volume percent of described sintering aid Ni is 3-5%, and the volume percent of described sintering aid MgO is 0.5-1.2%.
6. the preparation method of the described nano composite ceramic mould material of claim 1, step is as follows:
(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.Owt%; With an amount of dehydrated alcohol is dispersion medium, is made into the stable ZrO of yttrium
2Suspension, with agitator fully stir, ultra-sonic dispersion 20-30min, use HCl and NH again
4OH regulates the pH value of suspension to 3-4;
(2) take by weighing in proportion nanometer Ti (C, N) powder are that 4000 polyoxyethylene glycol (PEG4000) is a dispersion agent with molecular weight, with Ti (C, N) powder quality is the radix meter, the addition of dispersion agent is 0.2-1.0wt%; With an amount of dehydrated alcohol is dispersion medium, be made into Ti (C, N) suspension, with agitator fully stir, ultra-sonic dispersion 20-30min, use HCl and NH again
4OH regulates the pH value of suspension to 3-4;
(3) take by weighing nanometer α-Al in proportion
2O
3Powder is that 4000 polyoxyethylene glycol (PEG4000) is a dispersion agent with molecular weight, with α-Al
2O
3Powder quality is the radix meter, and the addition of dispersion agent is 0.2-1.0wt%; With an amount of dehydrated alcohol is dispersion medium, is made into α-Al
2O
3Suspension, with agitator fully stir, ultra-sonic dispersion 20-30min, use HCl and NH again
4OH regulates the pH value of suspension to 3-4;
(4) with step (1)-stable ZrO of (3) gained yttrium
2, Ti (C, N) and α-Al
2O
3Suspension mixes, and obtains complex phase suspension, and this complex phase suspension is regulated its pH value to 3-4 once more through ultra-sonic dispersion 10-20min, adds Mo, Ni and MgO sintering aid then in proportion, mixes;
(5) step (4) gained mixture being poured in the ball grinder, is protective atmosphere with the rare gas element, is medium with the dehydrated alcohol, is grinding element with the sintered carbide ball, ball milling 30-60h; Then in the electric vacunm drying case under design temperature successive drying, in inert gas flow, sieve behind the complete drying, obtain mixed powder, seal standby;
(6) adopt the pressure sintering sintering, in hot pressing furnace with the powder pressing mold sinter molding of step (5) gained.
7. the preparation method of nano composite ceramic mould material according to claim 6 is characterized in that, the pellet weight ratio of each component raw material total amount and sintered carbide ball is 1 in the step (5): 10-12.
8. the preparation method of nano composite ceramic mould material according to claim 6 is characterized in that, rare gas element is one of nitrogen, argon gas described in the step (5).
9. the preparation method of nano composite ceramic mould material according to claim 6 is characterized in that, step (6) pressure sintering sintering is:
The graphite jig of earlier powder of step (5) gained being packed into carries out vacuum heating-press sintering then; Hot pressing parameters is: heating-up time 30-40min, and holding temperature 1400-1550 ℃, hot pressing pressure 30-35MPa, soaking time 30-50min is cooled to room temperature then; Take temperature section formula heat pressing process as follows:
When i. heating up before temperature reaches 1000 ℃ little exert pressure, little pressure is 5-10MPa, when temperature reaches 1000 ℃ pressure is transferred to 20MPa, temperature is added to hot pressing pressure 30-35MPa gradually when reaching holding temperature 1400-1550 ℃;
Reduce moulding pressure by a small margin when ii. insulation finishes the back cooling, pressure regulation power was to 20MPa when promptly temperature dropped to 1100 ℃, and pressure regulation power is to 10MPa in the time of 950 ℃, and pressure regulation power is 0 in the time of 850 ℃; (Ti (C, N)) strengthens nano zircite (ZrO finally to obtain the product nano-carbon titanium nitride
2) nano composite ceramic mould material; In the temperature-fall period more than 850 ℃ the time cooling rate be 10-20 ℃/min, 20-30 ℃/min is up to room temperature in the time of below 850 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910229440A CN101767989A (en) | 2009-10-26 | 2009-10-26 | ZrO2/Ti (C, N) nano composite ceramic mold material and its prepn |
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| CN200910229440A CN101767989A (en) | 2009-10-26 | 2009-10-26 | ZrO2/Ti (C, N) nano composite ceramic mold material and its prepn |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101913871A (en) * | 2010-07-15 | 2010-12-15 | 南京信息工程大学 | Abrasion-resistant ceramic composite material and preparation method thereof |
| CN101956117A (en) * | 2010-10-22 | 2011-01-26 | 山东轻工业学院 | Nano zirconia and micron tungsten carbide toughened and enhanced metal ceramic die material and preparation method thereof |
| CN104163630A (en) * | 2014-08-04 | 2014-11-26 | 余姚市巧迪电器厂 | Aluminium oxide, titanium carbide and silicon nitride composite reinforced zirconium boride-based multi-element nano-composite ceramic die |
| CN104163626A (en) * | 2014-08-04 | 2014-11-26 | 余姚市巧迪电器厂 | Zirconium oxide and zirconium carbide composite reinforced titanium oxide-based multi-element nano-composite ceramic die |
| CN104311035A (en) * | 2014-08-04 | 2015-01-28 | 余姚市巧迪电器厂 | A zirconium carbide-based multi-component nanometer composite ceramic mould material and a preparing method thereof |
| CN104446396A (en) * | 2014-12-11 | 2015-03-25 | 中国石油大学(华东) | Preparation method of micro-nano composite aluminum oxide-titanium nitride-zirconium oxide-nickel-molybdenum ceramic material |
| CN105081339A (en) * | 2015-09-29 | 2015-11-25 | 河南科技大学 | Preparing method of tungsten-zirconium-yttrium ternary alloy powder |
| CN105174964A (en) * | 2015-08-21 | 2015-12-23 | 王晶怡 | Colorimetric pool ceramic block material |
| CN106116618A (en) * | 2016-06-23 | 2016-11-16 | 吴迪 | A kind of preparation method of low expansion composite ceramic die material |
| CN106145938A (en) * | 2015-04-27 | 2016-11-23 | 深圳市商德先进陶瓷有限公司 | Zirconia composite ceramics and preparation method thereof |
| CN106316391A (en) * | 2016-08-31 | 2017-01-11 | 太仓宏达俊盟新材料有限公司 | Production method of high-temperature-resistant zirconia skateboard |
| CN106747433A (en) * | 2017-02-28 | 2017-05-31 | 安徽拓吉泰新型陶瓷科技有限公司 | Zirconium oxide-based nano ceramic tool die material and preparation method thereof |
| CN107523710A (en) * | 2017-08-24 | 2017-12-29 | 台州学院 | A kind of whisker modified Ti (C, N) based composite metal ceramic preparation of resistance to high temperature oxidation |
| CN109906212A (en) * | 2016-10-17 | 2019-06-18 | 住友电气工业株式会社 | Sintered body and cutting element comprising the sintered body |
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- 2009-10-26 CN CN200910229440A patent/CN101767989A/en active Pending
Non-Patent Citations (1)
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| 张洪波: "氧化锆基纳米陶瓷工模具材料研制及其应用基础研究", 《中国优秀硕士学位论文全文数据库》 * |
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| CN101913871A (en) * | 2010-07-15 | 2010-12-15 | 南京信息工程大学 | Abrasion-resistant ceramic composite material and preparation method thereof |
| CN101956117A (en) * | 2010-10-22 | 2011-01-26 | 山东轻工业学院 | Nano zirconia and micron tungsten carbide toughened and enhanced metal ceramic die material and preparation method thereof |
| CN104163630B (en) * | 2014-08-04 | 2016-01-27 | 余姚市巧迪电器厂 | A kind of aluminum oxide and the first nano composite ceramic mould of titanium carbide and silicon nitride composite strengthening zirconium boride 99.5004323A8ure Quito |
| CN104163626B (en) * | 2014-08-04 | 2016-09-14 | 余姚市巧迪电器厂 | A kind of zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die |
| CN104311035A (en) * | 2014-08-04 | 2015-01-28 | 余姚市巧迪电器厂 | A zirconium carbide-based multi-component nanometer composite ceramic mould material and a preparing method thereof |
| CN104163626A (en) * | 2014-08-04 | 2014-11-26 | 余姚市巧迪电器厂 | Zirconium oxide and zirconium carbide composite reinforced titanium oxide-based multi-element nano-composite ceramic die |
| CN104163630A (en) * | 2014-08-04 | 2014-11-26 | 余姚市巧迪电器厂 | Aluminium oxide, titanium carbide and silicon nitride composite reinforced zirconium boride-based multi-element nano-composite ceramic die |
| CN104446396A (en) * | 2014-12-11 | 2015-03-25 | 中国石油大学(华东) | Preparation method of micro-nano composite aluminum oxide-titanium nitride-zirconium oxide-nickel-molybdenum ceramic material |
| CN106145938A (en) * | 2015-04-27 | 2016-11-23 | 深圳市商德先进陶瓷有限公司 | Zirconia composite ceramics and preparation method thereof |
| CN105174964A (en) * | 2015-08-21 | 2015-12-23 | 王晶怡 | Colorimetric pool ceramic block material |
| CN105081339A (en) * | 2015-09-29 | 2015-11-25 | 河南科技大学 | Preparing method of tungsten-zirconium-yttrium ternary alloy powder |
| CN106116618A (en) * | 2016-06-23 | 2016-11-16 | 吴迪 | A kind of preparation method of low expansion composite ceramic die material |
| CN106116618B (en) * | 2016-06-23 | 2019-05-24 | 北京知淘科技有限责任公司 | A kind of preparation method of low expansion composite ceramic die material |
| CN106316391A (en) * | 2016-08-31 | 2017-01-11 | 太仓宏达俊盟新材料有限公司 | Production method of high-temperature-resistant zirconia skateboard |
| CN109906212A (en) * | 2016-10-17 | 2019-06-18 | 住友电气工业株式会社 | Sintered body and cutting element comprising the sintered body |
| CN109906212B (en) * | 2016-10-17 | 2022-07-19 | 住友电气工业株式会社 | Sintered body and cutting tool comprising same |
| CN106747433A (en) * | 2017-02-28 | 2017-05-31 | 安徽拓吉泰新型陶瓷科技有限公司 | Zirconium oxide-based nano ceramic tool die material and preparation method thereof |
| CN106747433B (en) * | 2017-02-28 | 2020-05-08 | 安徽拓吉泰新型陶瓷科技有限公司 | Zirconia-based nano ceramic tool and die material and preparation method thereof |
| CN107523710A (en) * | 2017-08-24 | 2017-12-29 | 台州学院 | A kind of whisker modified Ti (C, N) based composite metal ceramic preparation of resistance to high temperature oxidation |
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