CN104163632B - A kind of aluminum-nitride-based polynary nanometer composite ceramic die material and preparation method thereof - Google Patents

A kind of aluminum-nitride-based polynary nanometer composite ceramic die material and preparation method thereof Download PDF

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CN104163632B
CN104163632B CN201410381907.7A CN201410381907A CN104163632B CN 104163632 B CN104163632 B CN 104163632B CN 201410381907 A CN201410381907 A CN 201410381907A CN 104163632 B CN104163632 B CN 104163632B
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nitride
aluminum
suspension
aluminium
composite ceramic
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CN104163632A (en
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韩巧
李孝君
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YUYAO QIAODI ELECTRIC FACTORY
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Abstract

The invention discloses a kind of aluminum-nitride-based polynary nanometer composite ceramic die material and preparation method thereof, this material according to the raw material of weight portion is: aluminium nitride 60 80 parts, aluminium carbide 10 20 parts, silicon boride 15 25 parts, Scia 26 parts, Dineodymium trioxide 48 parts, chromium 24 parts, 13 parts of tungsten, 13 parts of nickel;Above-mentioned all raw materials all use nanometer grade powder, and wherein the footpath grain size that footpath grain size is 10 100 nanometers, aluminium carbide and silicon boride of aluminium nitride is 1 10 nanometers, and other footpath grain size is 1 100 nanometers;Its preparation method is with aluminium nitride as matrix, adds aluminium carbide and silicon boride as strengthening phase, with Scia and Dineodymium trioxide as stabilizer, using chromium, tungsten and nickel as sintering aid, forms through hot pressed sintering.This mould ageing resistance and defect support ability by force, have good comprehensive mechanical property and excellent properties of antifriction and wear resistance.

Description

A kind of aluminum-nitride-based polynary nanometer composite ceramic die material and preparation method thereof
Technical field
The present invention relates to a kind of ceramic die material, a kind of aluminum-nitride-based polynary nanometer composite ceramic die material and Preparation method.
Background technology
Sintex has high hardness and wearability, shows the cutting ability of excellence when high-speed cutting and dry cutting, is The cutter material of one class great development prospect.But, the ceramic cutting tool material of application is confined to a micron composite ceramics mostly at present, The mechanical property of material especially intensity, toughness still await improving further.According to Hall-petch relation: crystallite dimension The least, the intensity of ceramic material is the highest.Therefore, nano modification, the research and development of nano-micrometre composite ceramic tool material It will be one of the Main way of cutter material development from now on.
Nano composite ceramic cutter material the most after deliberation mainly includes Si3N4/ TiNn, Si3N4/ TiCn, Si3N4-Ai2O3n-TiC-Y2O3, Al2O3/ TiC/SiCn, Al2O3/ TiCn, Al2O3/Al2O3N/SiCn, Al2O3/Ti (C07N0.3) n/SiCn, Al2O3/ SiC/SiCn, Al2O3/ TiC/TiNn, etc., it is respectively provided with ratio micron composite ceramic tool material Preferably mechanical property and cutting ability.But up to the present, not yet find the nano combined pottery with aluminium nitride ceramics as matrix The report of porcelain cutter material.
On the other hand, heat stability and the wearability of ceramic material are splendid, are the ideal materials manufacturing shaping dies, have very much Development prospect, but its toughness is very poor, is not used widely in terms of mould industry.From the point of view of status both at home and abroad, The research of ceramic die is still in the research and development stage, and the kind of the ceramic material being applied to mould industry is little, applicable Mould applications is the narrowest, and the report of this respect is the most few.At present, ceramic material applied research in all kinds of moulds limits to mostly In micron composite ceramic material, such as ZrO2Toughness reinforcing Al2O3Base composite ceramic ZTA wire drawing die, TZP/TiC/Al2O3, Al2O3/ TiC composite ceramics wire drawing die, (Ce-TZP)-Al2O3Hot-extrusion mold, 3Y-TZP-Al2O3Pottery drawing die, PSZ Pottery hot extruding die, Al2O3/Cr3C2/ (W, Ti) C etc..Although nano composite ceramic is in the research of mold materials application aspect Less, such as compound UP ceramic die, Al2O3/ Ti (C, N) etc., but also achieve good effect.
From existing research it can be seen that nano combined especially nano-micron compound pottery performance, price advantage could not be at mould Tool field is not fully exerted.From the point of view of current general status, the kind of ceramic die material, performance and range of application are equal Await expanding further and improving.
Summary of the invention
It is an object of the invention to provide a kind of aluminum-nitride-based polynary nanometer composite ceramic die material and preparation method thereof, this mould Tool ageing resistance and defect support ability by force, have good comprehensive mechanical property and excellent properties of antifriction and wear resistance.
For achieving the above object, the present invention provides following technical scheme:
A kind of aluminum-nitride-based polynary nanometer composite ceramic die material, according to the raw material of weight portion be: aluminium nitride 60-80 part, Aluminium carbide 10-20 part, silicon boride 15-25 part, Scia 2-6 part, Dineodymium trioxide 4-8 part, chromium 2-4 part, tungsten 1-3 part, Nickel 1-3 part;Above-mentioned all raw materials all use nanometer grade powder, and wherein the footpath grain size of aluminium nitride is 10-100 nanometer, carbon The footpath grain size changing aluminum and silicon boride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer.
As the further scheme of the present invention: described aluminum-nitride-based polynary nanometer composite ceramic die material and preparation method thereof, According to the raw material of weight portion it is: aluminium nitride 65-75 part, aluminium carbide 14-16 part, silicon boride 18-22 part, Scia 3-5 Part, Dineodymium trioxide 5-7 part, chromium 2.5-3.5 part, tungsten 1.5-2.5 part, nickel 1-3 part.
The preparation method of described aluminum-nitride-based polynary nanometer composite ceramic die material, with aluminium nitride as matrix, adds carbonization Aluminum and silicon boride are as strengthening phase, with Scia and Dineodymium trioxide as stabilizer, using chromium, tungsten and nickel as sintering aid, through heat Pressure sintering forms;Concrete preparation process is as follows:
Step one: weigh above-mentioned all raw materials according to weight portion;
Step 2: aluminium nitride, aluminium carbide and silicon boride are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, then fill Divide stirring, ultrasonic disperse 20-30 minute simultaneously, obtain the first suspension;
Step 3: Scia, Dineodymium trioxide, chromium, tungsten and nickel are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, so After be sufficiently stirred for, ultrasonic disperse 20-30 minute simultaneously, obtain the second suspension;
Step 4: suspend mixing by the first suspension and second, is then sufficiently stirred for, simultaneously ultrasonic disperse 10-20 minute, Obtain total mixture suspension;
Step 5: pour in ball grinder by total mixture suspension, with noble gas as protective atmosphere, with dehydrated alcohol for being situated between Matter, the iron ball of a diameter of 1-2mm is mill ball, under the microwave environment of 2450MHz, ball milling 12-24 hour, filters To lapping liquid;The gross weight of all raw materials and the weight ratio of mill ball are 1: 10-20;
Step 6: lapping liquid is vacuum dried at a temperature of 110-120 DEG C, sieves in inert gas flow after being completely dried, Obtain mixed powder, seal standby;
Step 7: use pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace.
As the further scheme of the present invention: dehydrated alcohol described in step 2 and step 3 with the volume ratio of Polyethylene Glycol is 1∶0.5-2。
As the further scheme of the present invention: noble gas described in step 5 and step 6 is nitrogen or rare gas.
As the further scheme of the present invention: in step 7, pressure sintering sintering process parameter is: heating-up time 20-30min, protect Temperature temperature 1400-1600 DEG C, hot pressing pressure 30-40MPa, temperature retention time 40-60min, then it is cooled to room temperature.
Compared with prior art, the invention has the beneficial effects as follows: polynary nanometer composite ceramic die of the present invention, by nanometer Adding nano silicon carbide aluminum in aluminium nitride matrix and realize the nano combined of different-grain diameter with nanometer silicon boride mutually as strengthening, interpolation is received Rice aluminium carbide and the addition of nanometer silicon boride, can define typical intracrystalline/intergranular hybrid architecture with nano aluminum nitride, Thus causing along crystalline substance/transcrystalline mixed-mode crack pattern, these strengthened mechanism are multiple toughened and reinforced with aluminium nitride transformation toughening etc. Mechanism synergism, improves mechanical property and the serviceability of material jointly;And study and show: Scia and Dineodymium trioxide are made For the compound interpolation of stabilizer, material is not only made to have at a relatively high ageing resistance and a defect resistivity, and crystal grain phase transformation Critical dimension is bigger, requires relatively low, so that material has preferable combination property to material fineness.Finally, gold is utilized Belonging to the little abrading-ball of matter, the reflection to microwave and the refraction that are occurred after metal is by microwave exposure are dissipated to whole reaction system In, serve the effect of microwave heating, reaction can be accelerated and carry out.Compared with existing ceramic die material, this polynary nanometer is multiple Close ceramic die material and there is more preferable comprehensive mechanical property and excellent properties of antifriction and wear resistance, can be used for making extrusion die, drawing Potter's mould such as withdrawing pattern and cutting tool.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, aobvious So, described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based in the present invention Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, all Belong to the scope of protection of the invention.
Embodiment 1
A kind of aluminum-nitride-based polynary nanometer composite ceramic die material, according to the raw material of weight portion be: aluminium nitride 60 parts, carbon. Change 10 parts of aluminum, silicon boride 15 parts, Scia 2 parts, Dineodymium trioxide 4 parts, chromium 2 parts, 1 part of tungsten, 1 part of nickel;Above-mentioned institute Raw material is had all to use nanometer grade powder, the wherein footpath that footpath grain size is 10-100 nanometer, aluminium carbide and silicon boride of aluminium nitride Grain size is 1-10 nanometer, and other footpath grain size is 1-100 nanometer;Its preparation method is with aluminium nitride as matrix, adds Add aluminium carbide and silicon boride as strengthening phase, with Scia and Dineodymium trioxide as stabilizer, using chromium, tungsten and nickel as sintering aid, Form through hot pressed sintering;Concrete preparation process is as follows:
Step one: weigh above-mentioned all raw materials according to weight portion;
Step 2: aluminium nitride, aluminium carbide and silicon boride are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, then fill Divide stirring, ultrasonic disperse 20 minutes simultaneously, obtain the first suspension;Described dehydrated alcohol with the volume ratio of Polyethylene Glycol is 1∶0.5;
Step 3: Scia, Dineodymium trioxide, chromium, tungsten and nickel are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, so After be sufficiently stirred for, ultrasonic disperse 20 minutes simultaneously, obtain the second suspension;Described dehydrated alcohol and the volume of Polyethylene Glycol Ratio is 1: 0.5;
Step 4: suspend mixing by the first suspension and second, is then sufficiently stirred for, simultaneously ultrasonic disperse 10 minutes, To total mixture suspension;
Step 5: total mixture suspension is poured in ball grinder, with nitrogen as protective atmosphere, with dehydrated alcohol as medium, The iron ball of a diameter of 1mm is mill ball, under the microwave environment of 2450MHz, and ball milling 12 hours, it is filtrated to get lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 10;
Step 6: lapping liquid is vacuum dried at a temperature of 110 DEG C, sieves in stream of nitrogen gas after being completely dried, mixed Close powder, seal standby;
Step 7: use pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace; The technological parameter of pressure sintering sintering: heating-up time 20min, holding temperature 1400 DEG C, hot pressing pressure 30MPa, temperature retention time 40min, is then cooled to room temperature.
Embodiment 2
A kind of aluminum-nitride-based polynary nanometer composite ceramic die material, according to the raw material of weight portion be: aluminium nitride 70 parts, carbon Change 15 parts of aluminum, silicon boride 20 parts, Scia 4 parts, Dineodymium trioxide 6 parts, chromium 3 parts, 2 parts of tungsten and 2 parts of nickel;Above-mentioned institute Raw material is had all to use nanometer grade powder, the wherein footpath that footpath grain size is 10-100 nanometer, aluminium carbide and silicon boride of aluminium nitride Grain size is 1-10 nanometer, and other footpath grain size is 1-100 nanometer;Its preparation method is with aluminium nitride as matrix, adds Add aluminium carbide and silicon boride as strengthening phase, with Scia and Dineodymium trioxide as stabilizer, using chromium, tungsten and nickel as sintering aid, Form through hot pressed sintering;Concrete preparation process is as follows:
Step one: weigh above-mentioned all raw materials according to weight portion;
Step 2: aluminium nitride, aluminium carbide and silicon boride are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, then fill Divide stirring, ultrasonic disperse 25 minutes simultaneously, obtain the first suspension;Described dehydrated alcohol with the volume ratio of Polyethylene Glycol is 1∶1;
Step 3: Scia, Dineodymium trioxide, chromium, tungsten and nickel are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, so After be sufficiently stirred for, ultrasonic disperse 25 minutes simultaneously, obtain the second suspension;Described dehydrated alcohol and the volume of Polyethylene Glycol Ratio is 1: 1;
Step 4: suspend mixing by the first suspension and second, is then sufficiently stirred for, simultaneously ultrasonic disperse 15 minutes, To total mixture suspension;
Step 5: total mixture suspension is poured in ball grinder, with nitrogen as protective atmosphere, with dehydrated alcohol as medium, The iron ball of a diameter of 1.5mm is mill ball, under the microwave environment of 2450MHz, and ball milling 18 hours, it is filtrated to get grinding Liquid;The gross weight of all raw materials and the weight ratio of mill ball are 1: 15;
Step 6: lapping liquid is vacuum dried at a temperature of 115 DEG C, sieves in stream of nitrogen gas after being completely dried, mixed Close powder, seal standby;
Step 7: use pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace; The technological parameter of pressure sintering sintering: heating-up time 25min, holding temperature 1500 DEG C, hot pressing pressure 35MPa, temperature retention time 50min, is then cooled to room temperature.
Embodiment 3
A kind of aluminum-nitride-based polynary nanometer composite ceramic die material, according to the raw material of weight portion be: aluminium nitride 80 parts, carbon Change 20 parts of aluminum, silicon boride 25 parts, Scia 6 parts, Dineodymium trioxide 8 parts, chromium 4 parts, 3 parts of tungsten and 3 parts of nickel;Above-mentioned institute Raw material is had all to use nanometer grade powder, the wherein footpath that footpath grain size is 10-100 nanometer, aluminium carbide and silicon boride of aluminium nitride Grain size is 1-10 nanometer, and other footpath grain size is 1-100 nanometer;Its preparation method is with aluminium nitride as matrix, adds Add aluminium carbide and silicon boride as strengthening phase, with Scia and Dineodymium trioxide as stabilizer, using chromium, tungsten and nickel as sintering aid, Form through hot pressed sintering;Concrete preparation process is as follows:
Step one: weigh above-mentioned all raw materials according to weight portion;
Step 2: aluminium nitride, aluminium carbide and silicon boride are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, then fill Divide stirring, ultrasonic disperse 30 minutes simultaneously, obtain the first suspension;Described dehydrated alcohol with the volume ratio of Polyethylene Glycol is 1∶2;
Step 3: Scia, Dineodymium trioxide, chromium, tungsten and nickel are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, so After be sufficiently stirred for, ultrasonic disperse 30 minutes simultaneously, obtain the second suspension;Described dehydrated alcohol and the volume of Polyethylene Glycol Ratio is 1: 2;
Step 4: suspend mixing by the first suspension and second, is then sufficiently stirred for, simultaneously ultrasonic disperse 20 minutes, To total mixture suspension;
Step 5: total mixture suspension is poured in ball grinder, with argon as protective atmosphere, with dehydrated alcohol as medium, The iron ball of a diameter of 2mm is mill ball, under the microwave environment of 2450MHz, and ball milling 24 hours, it is filtrated to get lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 20;
Step 6: lapping liquid is vacuum dried at a temperature of 120 DEG C, sieves in an argon stream after being completely dried, mixed Close powder, seal standby;
Step 7: use pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace; The technological parameter of pressure sintering sintering: heating-up time 30min, holding temperature 1600 DEG C, hot pressing pressure 40MPa, temperature retention time 60min, is then cooled to room temperature.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and do not carrying on the back In the case of the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter from From the point of view of which point, all should regard embodiment as exemplary, and be nonrestrictive, the scope of the present invention is by appended power Profit requires rather than described above limits, it is intended that all by fall in the implication of equivalency and scope of claim Change is included in the present invention.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only comprises One independent technical scheme, this narrating mode of description is only the most for clarity sake, and those skilled in the art should be by Description is as an entirety, and the technical scheme in each embodiment can also be through appropriately combined, and forming those skilled in the art can With other embodiments understood.

Claims (6)

1. an aluminum-nitride-based polynary nanometer composite ceramic die material, it is characterised in that be according to the raw material of weight portion: nitridation Aluminum 60-80 part, aluminium carbide 10-20 part, silicon boride 15-25 part, Scia 2-6 part, Dineodymium trioxide 4-8 part, chromium 2-4 part, Tungsten 1-3 part, nickel 1-3 part;Above-mentioned all raw materials all use nanometer grade powder, and wherein the footpath grain size of aluminium nitride is that 10-100 receives Rice, the footpath grain size of aluminium carbide and silicon boride is 1-10 nanometer, and the footpath grain size of other raw materials is 1-100 nanometer;
The preparation method of described aluminum-nitride-based polynary nanometer composite ceramic die material is: with aluminium nitride as matrix, adds carbonization Aluminum and silicon boride are as strengthening phase, with Scia and Dineodymium trioxide as stabilizer, using chromium, tungsten and nickel as sintering aid, through hot pressing Sintering forms;Concrete preparation process is as follows:
Step one: weigh above-mentioned all raw materials according to weight portion;
Step 2: aluminium nitride, aluminium carbide and silicon boride are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, the most fully Stirring, ultrasonic disperse 20-30 minute simultaneously, obtain the first suspension;
Step 3: Scia, Dineodymium trioxide, chromium, tungsten, nickel are added in the dehydrated alcohol mixed solution with Polyethylene Glycol, then It is sufficiently stirred for, simultaneously ultrasonic disperse 20-30 minute, obtains the second suspension;
Step 4: the first suspension and the second suspension are mixed, is then sufficiently stirred for, simultaneously ultrasonic disperse 10-20 minute, Obtain total mixture suspension;
Step 5: total mixture suspension is poured in ball grinder, with noble gas as protective atmosphere, with dehydrated alcohol as medium, The iron ball of a diameter of 1-2mm is mill ball, under the microwave environment of 2450MHz, and ball milling 12-24 hour, it is filtrated to get grinding Liquid;The gross weight of all raw materials and the weight ratio of mill ball are 1: 10-20;
Step 6: lapping liquid is vacuum dried at a temperature of 110-120 DEG C, sieves in inert gas flow after being completely dried, Obtain mixed powder, seal standby;
Step 7: use pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace.
Aluminum-nitride-based polynary nanometer composite ceramic die material the most according to claim 1, it is characterised in that described nitridation Aluminum Quito unit nano composite ceramic mould material, according to the raw material of weight portion be: aluminium nitride 65-75 part, aluminium carbide 14-16 part, Silicon boride 18-22 part, Scia 3-5 part, Dineodymium trioxide 5-7 part, chromium 2.5-3.5 part, tungsten 1.5-2.5 part, nickel 1.5-2.5 Part.
3. a preparation method for aluminum-nitride-based polynary nanometer composite ceramic die material as claimed in claim 1 or 2, it is special Levy and be, with aluminium nitride as matrix, add aluminium carbide and silicon boride as strengthening phase, with Scia and Dineodymium trioxide as stabilizer, Using chromium, tungsten and nickel as sintering aid, form through hot pressed sintering;Concrete preparation process is as follows:
Step one: weigh above-mentioned all raw materials according to weight portion;
Step 2: aluminium nitride, aluminium carbide and silicon boride are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, the most fully Stirring, ultrasonic disperse 20-30 minute simultaneously, obtain the first suspension;
Step 3: Scia, Dineodymium trioxide, chromium, tungsten, nickel are added in the dehydrated alcohol mixed solution with Polyethylene Glycol, then It is sufficiently stirred for, simultaneously ultrasonic disperse 20-30 minute, obtains the second suspension;
Step 4: the first suspension and the second suspension are mixed, is then sufficiently stirred for, simultaneously ultrasonic disperse 10-20 minute, Obtain total mixture suspension;
Step 5: total mixture suspension is poured in ball grinder, with noble gas as protective atmosphere, with dehydrated alcohol as medium, The iron ball of a diameter of 1-2mm is mill ball, under the microwave environment of 2450MHz, and ball milling 12-24 hour, it is filtrated to get grinding Liquid;The gross weight of all raw materials and the weight ratio of mill ball are 1: 10-20;
Step 6: lapping liquid is vacuum dried at a temperature of 110-120 DEG C, sieves in inert gas flow after being completely dried, Obtain mixed powder, seal standby;
Step 7: use pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace.
The preparation method of aluminum-nitride-based polynary nanometer composite ceramic die material the most according to claim 3, it is characterised in that Dehydrated alcohol described in step 2 and step 3 is 1: 0.5-2 with the volume ratio of Polyethylene Glycol.
The preparation method of aluminum-nitride-based polynary nanometer composite ceramic die material the most according to claim 3, it is characterised in that Noble gas described in step 5 and step 6 is nitrogen or rare gas.
The preparation method of aluminum-nitride-based polynary nanometer composite ceramic die material the most according to claim 3, it is characterised in that In step 7, pressure sintering sintering process parameter is: heating-up time 20-30min, holding temperature 1400-1600 DEG C, hot pressing pressure 30-40MPa, temperature retention time 40-60min, then it is cooled to room temperature.
CN201410381907.7A 2014-08-04 A kind of aluminum-nitride-based polynary nanometer composite ceramic die material and preparation method thereof Active CN104163632B (en)

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