CN101164963A - Micro-nano composite ceramic die material and preparation method thereof - Google Patents
Micro-nano composite ceramic die material and preparation method thereof Download PDFInfo
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Abstract
This invention relates to the micron nanometer composite ceramic die material, and its preparation method. In this invention, micron grade Al2O3 ceramic is used as basic material, added are nanometer grade Ti (C,N) ceramic hard granules as dispersing material, Mo, Ni and MgO as agglutinant assistant. The preparation steps are: the powder of Al2O3 and Ti(C,N) are dispersed in the unified dispersing medium, then being proceeded the ball-milling, drying and hot-pressing sintering. This invention method benefits the dispersing effect of the powder with advantages of: simple operation and low cost. This product can be used for making compressing die or drawing die and the like with its comprehensive mechanical properties and abradability being better than that of prior art ceramic die material.
Description
Technical field
The present invention relates to a kind of ceramic die material and preparation method thereof, particularly a kind of nano-carbon titanium nitride (Ti (C
7N
3)) toughened and reinforced micrometer alumina (Al
2O
3) micro-nano composite ceramic die material and preparation method thereof.
Background technology
The thermostability and the wear resistance of stupalith are splendid, are the ideal materials of making shaping dies, have very much development prospect, but its toughness are very poor, therefore also are not used widely aspect mould industry.Costing an arm and a leg of stupalith, and be used for producing and also lack experience, but along with the improvement of science and technology development, manufacturing process and the increase of consumption, cost must descend, and using also will be extensive day by day.In the long term, should set about carrying out the research and development of advanced ceramics moulding stock.
At present, the applied research report of stupalith in all kinds of moulds is confined to the micron order composite ceramic material mostly.Aspect the research of oxide ceramics moulding stock, ZrO
2Toughness reinforcing Al
2O
3Base composite ceramic ZTA can be used for making wortle.As a kind of novel moulding stock, on some performance, be better than rapid steel, Wimet, its fracture toughness property and bending strength reach about 7.2MPam respectively
1/2And 740MPa.Referring to Xu Yufen etc., ZTA 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 Ce-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 KIC 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): 4143.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 the nitride ceramics moulding stock, Si
3N
4Stupalith can be used as a kind of potential moulding stock, and its bending strength and hardness are respectively 200MPa and 82-87GPa.Referring to Liang Jinsheng etc., the research of reaction sintering silicon nitride ceramic die material, Chinese pottery industry, 2000,7 (3): 9-11.Adopt the β '-Sialon ceramic die material of isostatic cool pressing, the preparation of pressureless sintering method, its fracture toughness property and bending strength reach 9.55MPam respectively
1/2And 682MPa, and the bending strength in the time of 1000 ℃ reaches 814MPa especially, so this material has good mechanical behavior under high temperature.Referring to Liu Jun etc., the applied research of Sialon pottery hot extruding die, Chinese mechanical engineering, 1995,6 (3): 57-58.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 ceramics 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 ℃.
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 pottery etc.Just present research and the general status of using, the kind of ceramic die material, performance and range of application all await further enlarging and raising.
Summary of the invention
In order to overcome the weak point of prior art, the invention provides a kind of micro-nano composite ceramic die material, be the micro-nano composite ceramic die material of the toughened and reinforced micrometer alumina base of nano-carbon titanium nitride.The present invention also provides the preparation method of this micro-nano composite ceramic die material.
Micro-nano composite ceramic die material of the present invention is 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 metal molybdenum (Mo), nickel (Ni) and magnesium oxide (MgO) as disperse phase to add nano level Ti.Component is as follows: (C is 5～35% N) to Ti, and Mo is 1～5%, and Ni is 1～5%, and MgO is 0.2～1%, and all the other are Al
2O
3, be volume percent.
It is further preferred,
Described dispersed phase Ti (C, volume percent N) is 10～20%,
The volume percent of described sintering aid Mo is 1.5～4%,
The volume percent of described sintering aid Ni is 1.5～4%,
The volume percent of described sintering aid MgO is 0.3～0.7%.
Preferably, in above-mentioned each component, used Al
2O
3By calcining Al (OH)
3Make α-Al
2O
3Powder, its purity are all greater than 99%, and mean particle size is 0.5 μ m～1.5 μ m; (C N) is commercial powder to used Ti, and purity is greater than 98%, and mean particle size is 60-100nm.
The preparation method of micro-nano composite ceramic die material of the present invention, component ratio as mentioned above, preparation process is as follows:
(1) with Al
2O
3Powder is 2000 polyoxyethylene glycol (PEG with molecular weight
2000) be dispersion agent, be dispersion medium with an amount of dehydrated alcohol, be made into Al
2O
3Suspension, with agitator fully stir, ultra-sonic dispersion, use HCl and NH again
4OH regulates pH value to 2.5～3.5 of suspension; With Al
2O
3Powder quality is that the dosage of radix score powder is 0.5-2wt%;
(2) with Ti (C, N) powder are that 2000 polyoxyethylene glycol (PEG) is a dispersion agent with molecular weight, are dispersion medium with an amount of dehydrated alcohol, be made into Ti (C, N) suspension, with agitator fully stir, ultra-sonic dispersion, use HCl and NH again
4OH regulates pH value to 2.5～3.5 of suspension; With Ti (C, N) powder quality is that the dosage of radix score powder is 0.5-2wt%;
(3) with step (1) gained Al
2O
3Suspension and step (2) gained Ti (C, N) suspension mixes, and obtains complex phase suspension, and this complex phase suspension is regulated its pH value to 2.5～3.5 once more through behind the ultra-sonic dispersion, adds Mo, Ni and MgO sintering aid then in proportion, mixes;
(4) with step (3) gained mixture, being protective atmosphere with the rare gas element, is medium with the dehydrated alcohol, is grinding element with the sintered carbide ball, ball milling 30～80h; Dry in vacuum drying oven then, in inert gas flow, sieve behind the complete drying, obtain powder, seal standby;
(5) adopt the pressure sintering sintering, in hot pressing furnace with the powder pressing mold sinter molding of step (4) gained.
Preferably, the pellet weight ratio of each component raw material and sintered carbide ball is 1: 8～10 in the step (4).
Preferably, rare gas element is one of nitrogen, argon gas in the step (4).
Preferably, the operation of above-mentioned steps (5) pressure sintering agglomerating is as follows:
The graphite jig of earlier powder of step (3) gained being packed into carries out vacuum heating-press sintering then; Hot pressing parameters is: hot pressing pressure 28～32MPa, 1600 ℃～1700 ℃ of hot pressing temperatures, soaking time 10～20min.Get the toughened and reinforced micrometer alumina based micro-nano of product nano-carbon titanium nitride composite ceramic die material.
Micro-nano composite ceramic die material of the present invention, by add nanometer Ti (C, N) hard particles can improve intensity, toughness and the hardness of material simultaneously as disperse phase, significantly improve the mechanical property and the use properties of material, and have simple, the lower-cost advantage of preparation method.And from the dispersing technology aspect of nano ceramics, the many waters of present research are dispersion medium, are that the Ball milling medium is inconsistent with adopting dehydrated alcohol in the later stage real material preparation process, thereby cause dispersion effect to reduce.Method of the present invention mainly is that the preparation method with single powder dispersing technology and mixed powder interrelates, and adopts unified dispersion medium, more helps improving the dispersion effect of powder.Compare with existing ceramic die material, this composite ceramic die 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 other cutters, 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, used Al
2O
3Be by calcining Al (OH)
3Make α-Al
2O
3Powder, its purity are all greater than 99%, and mean particle size is 1 μ m; (C N) is commercial powder to used Ti, and purity is greater than 98%, and mean particle size is 80nm.
Embodiment 1
Micro-nano composite ceramic die material, the volume percent of each component is: α-Al
2O
379.5%, Ti (C, N) 15%, Mo2.5%, Ni2.5%, MgO0.5%.The preparation method is as follows:
With Al
2O
3, (C, N) single-phase powder are that 2000 polyoxyethylene glycol is a dispersion agent with molecular weight respectively, with α-Al to Ti
2O
3Or Ti (C, N) quality is that radix score powder addition is respectively 1wt%, is dispersion medium with an amount of dehydrated alcohol, is made into corresponding α-Al respectively
2O
3Or Ti (C, N) single-phase suspension, respectively with agitator fully stir, ultra-sonic dispersion, use HCl and NH respectively
4OH regulates the pH value to 3.0 of suspension.Then with gained α-Al
2O
3And Ti (C, N) suspension of two kinds of powders mixes, and obtains complex phase suspension.Mixed complex phase suspension is regulated its pH value to 3.0 once more through behind the ultra-sonic dispersion.Add sintering aids such as Mo, Ni and MgO afterwards.After each component raw material mixing; with nitrogen is protective atmosphere; with the dehydrated alcohol is medium; with the sintered carbide ball is grinding element, and the pellet weight ratio is 1: 10, ball milling 50h; dry in vacuum drying oven then; sieve in nitrogen gas stream 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, 1650 ℃ of hot pressing temperatures, soaking time 15min.Then the stupalith sample that makes is carried out cutting processing, record its mechanical property parameters and be: bending strength is 789MPa, and fracture toughness property is 8.1MPam
1/2, hardness is 20.4GPa.
Embodiment 2
Micro-nano composite ceramic die material, the volume percent of its each component is: α-Al
2O
384.3%, Ti (C, N) 10%, Mo1.5%, Ni3.5%, MgO0.7%.The preparation method is as follows:
With Al
2O
3, (C, N) single-phase powder are that 2000 polyoxyethylene glycol is a dispersion agent with molecular weight respectively, with α-Al to Ti
2O
3Or Ti (C, N) quality is that radix score powder addition is respectively 1.5wt%, is dispersion medium with an amount of dehydrated alcohol, is made into corresponding α-Al respectively
2O
3Or Ti (C, N) single-phase suspension, respectively with agitator fully stir, ultra-sonic dispersion, use HCl and NH respectively
4OH regulates the pH value to 2.9 of suspension.Then with α-Al
2O
3And Ti (C, N) suspension of two kinds of powders mixes, and obtains complex phase suspension.Mixed complex phase suspension is regulated its pH value to 2.9 once more through behind the ultra-sonic dispersion.Add sintering aids such as Mo, Ni and MgO afterwards.After each component raw material mixing; with the argon gas is protective atmosphere; with the dehydrated alcohol is medium; with the sintered carbide ball is grinding element, and the pellet weight ratio is 1: 8, ball milling 80h; dry in vacuum drying oven then; sieve in argon gas stream 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 28MPa, 1620 ℃ of hot pressing temperatures, soaking time 18min.Then the stupalith sample that makes is carried out cutting processing, record its mechanical property parameters and be: bending strength is 743MPa, and fracture toughness property is 7.4MPam
1/2, hardness is 19.5GPa.
Embodiment 3
Micro-nano composite ceramic die material, the volume percent of its each component is: α-Al
2O
374.1%, Ti (C, N) 20%, Mo4%, Ni1.5%, MgO0.4%.The preparation method is as follows:
With Al
2O
3, (C, N) single-phase powder are that 2000 polyoxyethylene glycol is a dispersion agent with molecular weight respectively, with α-Al to Ti
2O
3Or Ti (C, N) quality is that radix score powder addition is respectively 0.8wt%, is dispersion medium with an amount of dehydrated alcohol, is made into corresponding α-Al respectively
2O
3Or Ti (C, N) single-phase suspension, with agitator fully stir, ultra-sonic dispersion, with HCl and NH
4OH regulates the pH value to 3.2 of suspension.Then with α-Al
2O
3And Ti (C, N) suspension of two kinds of powders mixes, and obtains complex phase suspension.Mixed complex phase suspension is regulated its pH value to 3.2 once more through behind the ultra-sonic dispersion.Add sintering aids such as Mo, Ni and MgO afterwards.After each component raw material mixing; with nitrogen is protective atmosphere; with the dehydrated alcohol is medium; with the sintered carbide ball is grinding element, and the pellet weight ratio is 1: 10, ball milling 40h; dry in vacuum drying oven then; sieve in nitrogen gas stream 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 32MPa, 1680 ℃ of hot pressing temperatures, soaking time 12min.Then the stupalith sample that makes is carried out cutting processing, record its mechanical property parameters and be: bending strength is 772MPa, and fracture toughness property is 8.2MPam
1/2, hardness is 20.1GPa.
Claims (8)
1. a micro-nano composite ceramic die material is characterized in that: with micron order Al
2O
3Pottery is a matrix, and interpolation nano level Ti (C, N) the ceramic hard particle forms as the sintering aid hot pressed sintering with Mo, Ni and MgO as disperse phase, component is as follows: (C is 5～35% N) to Ti, and Mo is 1～5%, Ni is 1～5%, and MgO is 0.2～1%, and all the other are Al
2O
3, be volume percent.
2. micro-nano composite ceramic die material according to claim 1 is characterized in that, (C, volume percent N) is 10～20% to described dispersed phase Ti.
3. micro-nano composite ceramic die material according to claim 1 is characterized in that, the volume percent of described sintering aid Mo is 1.5～4%.
4. micro-nano composite ceramic die material according to claim 1 is characterized in that, the volume percent of described sintering aid Ni is 1.5～4%.
5. the preparation method of the described micro-nano composite ceramic die material of claim 1, step is as follows:
(1) with Al
2O
3Powder is 2000 polyoxyethylene glycol (PEG with molecular weight
2000) be dispersion agent, with Al
2O
3Powder quality is the radix meter, the dosage 0.5-2wt% of dispersion agent; With an amount of dehydrated alcohol is dispersion medium, is made into Al
2O
3Suspension, with agitator fully stir, ultra-sonic dispersion, use HCl and NH again
4OH regulates pH value to 2.5～3.5 of suspension;
(2) with Ti (C, N) powder, with molecular weight is that 2000 polyoxyethylene glycol (PEG) is a dispersion agent, with Ti (C, N) powder quality is the radix meter, the dosage 0.5-2wt% of dispersion agent, with an amount of dehydrated alcohol is dispersion medium, is made into Ti (C, N) suspension, with agitator fully stir, ultra-sonic dispersion, use HCl and NH again
4OH regulates pH value to 2.5～3.5 of suspension;
(3) with step (1) gained Al
2O
3Suspension and step (2) gained Ti (C, N) suspension mixes, and obtains complex phase suspension, and this complex phase suspension is regulated its pH value to 2.5～3.5 once more through behind the ultra-sonic dispersion, adds Mo, Ni and MgO sintering aid then in proportion, mixes;
(4) with step (3) gained mixture, being protective atmosphere with the rare gas element, is medium with the dehydrated alcohol, is grinding element with the sintered carbide ball, ball milling 30～80h; Dry in vacuum drying oven then, in inert gas flow, sieve behind the complete drying, obtain powder, seal standby;
(5) adopt the pressure sintering sintering, in hot pressing furnace with the powder pressing mold sinter molding of step (4) gained.
6. the preparation method of micro-nano composite ceramic die material according to claim 5 is characterized in that, the pellet weight ratio of raw material and sintered carbide ball is 1: 8～10 in the step (4).
7. the preparation method of micro-nano composite ceramic die material according to claim 5 is characterized in that, rare gas element is one of nitrogen, argon gas described in the step (4).
8. the preparation method of micro-nano composite ceramic die material according to claim 5 is characterized in that, the technology of step (5) is as follows:
The graphite jig of earlier powder of step (4) gained being packed into carries out vacuum heating-press sintering then; Hot pressing parameters is: hot pressing pressure 28～32MPa, and 1600 ℃～1700 ℃ of hot pressing temperatures, soaking time 10～20min gets product.
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