CN104163626B - A kind of zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die - Google Patents
A kind of zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die Download PDFInfo
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Abstract
The invention discloses a kind of zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, according to the raw material of weight portion be: titanium oxide 60 80 parts, zirconium carbide 10 20 parts, zirconium oxide 15 25 parts, praseodymium oxide 26 parts, dysprosia 48 parts, 24 parts of nickel, cobalt 13 parts, magnesium oxide 13 parts；Above-mentioned all raw materials all use nanometer grade powder, and wherein the footpath grain size of titanium oxide is 10 100 nanometers, and zirconium carbide and zirconic footpath grain size are 1 10 nanometers, and other footpath grain size is 1 100 nanometers；Its preparation method is with titanium oxide as matrix, adds zirconium carbide and zirconium oxide as strengthening phase, with praseodymium oxide and dysprosia as stabilizer, using nickel, cobalt and magnesium oxide 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
Technical field
The present invention relates to a kind of ceramic die material, specifically a kind of zirconium oxide is titania based with zirconium carbide composite strengthening polynary to be received
Nano-scale composite ceramics mould.
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
(C0.7N03) 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 with TiO2Pottery is the nano composite ceramic of matrix
The report of 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 zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic ceramic former
Tool, this mould 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 zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, according to the raw material of weight portion
For: titanium oxide 60-80 part, zirconium carbide 10-20 part, zirconium oxide 15-25 part, praseodymium oxide 2-6 part, dysprosia 4-8 part,
Nickel 2-4 part, cobalt 1-3 part, magnesium oxide 1-3 part；Above-mentioned all raw materials all use nanometer grade powder, the wherein footpath of titanium oxide
Grain size is 10-100 nanometer, and zirconium carbide and zirconic footpath grain size are 1-10 nanometer, and other footpath grain size is 1-100
Nanometer；Its preparation method is with titanium oxide as matrix, and interpolation zirconium carbide and zirconium oxide are as strengthening phase, with praseodymium oxide and oxidation
Dysprosium is stabilizer, using nickel, cobalt and magnesium oxide as sintering aid, forms through hot pressed sintering；Concrete preparation process is as follows:
Step one: weigh above-mentioned all raw materials according to weight portion；
Step 2: titanium oxide, zirconium carbide and zirconium oxide 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: praseodymium oxide, dysprosia, nickel, cobalt and magnesium oxide are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol,
Then it is sufficiently stirred for, simultaneously ultrasonic disperse 20-30 minute, obtains 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: described zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramics
Mould, according to the raw material of weight portion be: titanium oxide 65-75 part, zirconium carbide 14-16 part, zirconium oxide 18-22 part, oxidation
Praseodymium 3-5 part, dysprosia 5-7 part, nickel 2.5-3.5 part, cobalt 1.5-2.5 part.
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
Titanium oxide matrix adds nano-zirconium carbide and realizes the nano combined of different-grain diameter, nano-sized carbon with nano zircite mutually as strengthening
Change zirconium and the addition of nano zircite, typical intracrystalline/intergranular hybrid architecture can be defined with nano-titanium oxide, thus
Cause along multiple toughening and strengthening such as crystalline substance/transcrystalline mixed-mode crack pattern, these strengthened mechanism and titanium oxide transformation toughenings
Synergism, improves mechanical property and the serviceability of material jointly；And study and show: praseodymium oxide and dysprosia are as surely
Determine the compound interpolation of agent, not only make material have at a relatively high ageing resistance and defect resistivity, and crystal grain phase transformation is critical
Size is bigger, requires relatively low, so that material has preferable combination property to material fineness.Finally, metallic is utilized
Little abrading-ball, the reflection to microwave occurred after metal is by microwave exposure and refraction are dissipated in whole reaction system, rise
Arrive the effect of microwave heating, reaction can have been accelerated and carry out.Compared with existing ceramic die material, this polynary nanometer composite ceramics
Mold materials has more preferable comprehensive mechanical property and excellent properties of antifriction and wear resistance, can be used for make extrusion die, drawing die with
And potter's mould such as 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 zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, according to the raw material of weight portion
For: titanium oxide 60 parts, zirconium carbide 10 parts, zirconium oxide 15 parts, praseodymium oxide 2 parts, dysprosia 4 parts, 2 parts of nickel, cobalt 1
Part, magnesium oxide 1 part；Above-mentioned all raw materials all use nanometer grade powder, and wherein the footpath grain size of titanium oxide is that 10-100 receives
Rice, zirconium carbide and zirconic footpath grain size are 1-10 nanometer, and other footpath grain size is 1-100 nanometer: its preparation side
Method is with titanium oxide as matrix, adds zirconium carbide and zirconium oxide as strengthening phase, with praseodymium oxide and dysprosia as stabilizer, with
Nickel, cobalt and magnesium oxide, 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: titanium oxide, zirconium carbide and zirconium oxide 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: praseodymium oxide, dysprosia, nickel, cobalt and magnesium oxide are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol,
Then it is sufficiently stirred for, simultaneously ultrasonic disperse 20 minutes, obtains the second suspension；Described dehydrated alcohol and the body of Polyethylene Glycol
Long-pending 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 zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, according to the raw material of weight portion
For: titanium oxide 70 parts, zirconium carbide 15 parts, zirconium oxide 20 parts, praseodymium oxide 4 parts, dysprosia 6 parts, 3 parts of nickel, cobalt 2
Part, magnesium oxide 2 parts；Above-mentioned all raw materials all use nanometer grade powder, and wherein the footpath grain size of titanium oxide is that 10-100 receives
Rice, zirconium carbide and zirconic footpath grain size are 1-10 nanometer, and other footpath grain size is 1-100 nanometer；Its preparation side
Method is with titanium oxide as matrix, adds zirconium carbide and zirconium oxide as strengthening phase, with praseodymium oxide and dysprosia as stabilizer, with
Nickel, cobalt and magnesium oxide, 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: titanium oxide, zirconium carbide and zirconium oxide 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: praseodymium oxide, dysprosia, nickel, cobalt and magnesium oxide are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol,
Then it is sufficiently stirred for, simultaneously ultrasonic disperse 25 minutes, obtains the second suspension；Described dehydrated alcohol and the body of Polyethylene Glycol
Long-pending 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 zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, according to the raw material of weight portion
For: titanium oxide 80 parts, zirconium carbide 20 parts, zirconium oxide 25 parts, praseodymium oxide 6 parts, dysprosia 8 parts, 4 parts of nickel, cobalt 3
Part, magnesium oxide 3 parts；Above-mentioned all raw materials all use nanometer grade powder, and wherein the footpath grain size of titanium oxide is that 10-100 receives
Rice, zirconium carbide and zirconic footpath grain size are 1-10 nanometer, and other footpath grain size is 1-100 nanometer；Its preparation side
Method is with titanium oxide as matrix, adds zirconium carbide and zirconium oxide as strengthening phase, with praseodymium oxide and dysprosia as stabilizer, with
Nickel, cobalt and magnesium oxide, 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: titanium oxide, zirconium carbide and zirconium oxide 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: praseodymium oxide, dysprosia, nickel, cobalt and magnesium oxide are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol,
Then it is sufficiently stirred for, simultaneously ultrasonic disperse 30 minutes, obtains the second suspension；Described dehydrated alcohol and the body of Polyethylene Glycol
Long-pending 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 (5)
1. a zirconium oxide and the preparation method of zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, it is characterized in that, described zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, according to the raw material of weight portion be: titanium oxide 60-80 part, zirconium carbide 10-20 part, zirconium oxide 15-25 part, praseodymium oxide 2-6 part, dysprosia 4-8 part, nickel 2-4 part, cobalt 1-3 part, magnesium oxide 1-3 part；Above-mentioned all raw materials all use nanometer grade powder, and wherein the footpath grain size of titanium oxide is 10-100 nanometer, and zirconium carbide and zirconic footpath grain size are 1-10 nanometer, and other footpath grain size is 1-100 nanometer；Its preparation method is with titanium oxide as matrix, adds zirconium carbide and zirconium oxide as strengthening phase, with praseodymium oxide and dysprosia as stabilizer, using nickel, cobalt and magnesium oxide as sintering aid, forms through hot pressed sintering；Concrete preparation process is as follows:
Step one: weigh above-mentioned all raw materials according to weight portion；
Step 2: titanium oxide, zirconium carbide and zirconium oxide are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, are then sufficiently stirred for, simultaneously ultrasonic disperse 20-30 minute, obtain the first suspension；
Step 3: praseodymium oxide, dysprosia, nickel, cobalt and magnesium oxide are added in the mixed solution of dehydrated alcohol and Polyethylene Glycol, are then sufficiently stirred for, simultaneously ultrasonic disperse 20-30 minute, obtain 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, obtains 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, ball milling 12-24 hour, it is filtrated to get lapping liquid；The gross weight of all raw materials and the weight ratio of mill ball are 1: 10-20；
Step 6: be vacuum dried at a temperature of 110-120 DEG C by lapping liquid, sieve after being completely dried in inert gas flow, obtain mixed powder, seals 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.
Zirconium oxide the most according to claim 1 and the preparation method of zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, it is characterized in that, described zirconium oxide and zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, according to the raw material of weight portion be: titanium oxide 65-75 part, zirconium carbide 14-16 part, zirconium oxide 18-22 part, praseodymium oxide 3-5 part, dysprosia 5-7 part, nickel 2.5-3.5 part, cobalt 1.5-2.5 part, magnesium oxide 1.5-2.5 part.
Zirconium oxide the most according to claim 1 and the preparation method of zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, 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.
Zirconium oxide the most according to claim 1 and the preparation method of zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, it is characterised in that noble gas described in step 5 and step 6 is nitrogen or rare gas.
Zirconium oxide the most according to claim 1 and the preparation method of zirconium carbide composite strengthening titania based polynary nanometer composite ceramic die, it is characterized 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, is then cooled to room temperature.
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| CN105712718B (en) * | 2016-01-25 | 2018-01-30 | 济南大学 | A kind of stratiform C/ZrC composites and preparation method thereof |
| CN105734381A (en) * | 2016-03-22 | 2016-07-06 | 苏州莱特复合材料有限公司 | Cermet material for high-strength mold and preparation method of cermet material |
| CN107673772B (en) * | 2017-10-17 | 2019-10-29 | 齐鲁工业大学 | A kind of Al adding zirconium oxide whisker2O3/ Ti (C, N) nano composite ceramic cutter material and preparation method thereof |
| CN111875400B (en) * | 2020-08-13 | 2022-12-23 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of high-temperature heat-insulating material containing zirconium carbide |
| CN114749669A (en) * | 2022-03-28 | 2022-07-15 | 江苏电子信息职业学院 | Hot die pressing mold preparation method based on nano material modification |
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| CN101767989A (en) * | 2009-10-26 | 2010-07-07 | 山东轻工业学院 | ZrO2/Ti (C, N) nano composite ceramic mold material and its prepn |
| CN103757513A (en) * | 2013-12-30 | 2014-04-30 | 沈阳理工大学 | A Al2O3/Ti (C, N) nanocomposite cermet mold material and its prepn |
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| CN101767989A (en) * | 2009-10-26 | 2010-07-07 | 山东轻工业学院 | ZrO2/Ti (C, N) nano composite ceramic mold material and its prepn |
| CN103757513A (en) * | 2013-12-30 | 2014-04-30 | 沈阳理工大学 | A Al2O3/Ti (C, N) nanocomposite cermet mold material and its prepn |
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Inventor after: Wu Zeliang Inventor before: Han Qiao Inventor before: Li Xiaojun |
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| TR01 | Transfer of patent right |
Effective date of registration: 20170526 Address after: 521000. The east side of the factory building of Chaozhou Economic Development Experimental Area in Guangdong province (D2-3-1) Patentee after: Chaozhou Jiayu Ceramics Co.,Ltd. Address before: 510000 unit 2414-2416, building, No. five, No. 371, Tianhe District, Guangdong, China Patentee before: GUANGDONG GAOHANG INTELLECTUAL PROPERTY OPERATION Co.,Ltd. Effective date of registration: 20170526 Address after: 510000 unit 2414-2416, building, No. five, No. 371, Tianhe District, Guangdong, China Patentee after: GUANGDONG GAOHANG INTELLECTUAL PROPERTY OPERATION Co.,Ltd. Address before: 315400 Zhejiang province Yuyao City Yangming streets Kang Shan Cun of more than 47-1 Patentee before: YUYAO QIAODI ELECTRIC FACTORY |