CN106747448A - A kind of tungsten carbide-base polynary nanometer composite ceramic die material and preparation method thereof - Google Patents
A kind of tungsten carbide-base polynary nanometer composite ceramic die material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of tungsten carbide-base polynary nanometer composite ceramic die material and preparation method thereof, the material is according to the raw material of weight portion：60 80 parts of tungsten carbide, 10 20 parts of zirconium oxide, 15 25 parts of titanium nitride, 26 parts of manganese oxide, 48 parts of neodymia, 24 parts of chromium, 13 parts of manganese；Above-mentioned all raw materials use nanometer grade powder, and the footpath grain size of wherein tungsten carbide is 10 100 nanometers, and the footpath grain size of zirconium oxide and titanium nitride is 1 10 nanometers, and other footpath grain sizes are 1 100 nanometers；Its preparation method is that, with tungsten carbide as matrix, addition zirconium oxide and titanium nitride, with manganese oxide and neodymia as stabilizer, using chromium and manganese as sintering aid, are formed as enhancing phase through hot pressed sintering.The mould ageing resistance and defect support ability by force, with 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 tungsten carbide-base polynary nanometer composite ceramic die material
And preparation method thereof.
Background technology
Sintex has hardness and wearability high, and excellent machinability is shown in high-speed cutting and dry cutting
Can, it is the cutter material of the great development prospect of a class.But, the ceramic cutting tool material applied at present is confined to micron and is combined mostly
Ceramics, especially intensity, toughness still await further raising to the mechanical property of material.According to Hall-petch relations：Crystal grain
Size is smaller, and the intensity of ceramic material is higher.Therefore, nano modification, the research of nano-micrometre composite ceramic tool material and open
Hair will be one of Main way of cutter material development from now on.
The nano composite ceramic cutter material studied at present mainly includes Si3N4/ TiNn, Si3N4/ TiCn, Si3N4-
Ai2O3n-TiC-Y2O3, Al2O3/ TiC/SiCn, Al2O3/ TiCn, Al2O3/Al2O3N/SiCn, Al2O3/Ti (C0.7N0.3)n/
SiCn, Al2O3/ SiC/SiCn, Al2O3/ TiC/TiNn, etc. being respectively provided with mechanical property more more preferable than micron composite ceramic tool material
Energy and cutting ability.But up to the present, not yet find nano composite ceramic cutter material with tungsten carbide ceramics as matrix
Report.
On the other hand, the heat endurance and wearability of ceramic material are splendid, are the ideal materials for manufacturing shaping dies, have very much
It is promising, but its toughness is very poor, therefore be not used widely in terms of mould industry also.Come from status both at home and abroad
See, the research of ceramic die is still in the research and development stage, be applied to mould industry ceramic material species seldom, can apply
Mould applications it is very narrow, the report of this respect is also few.At present, application study of the ceramic material in all kinds of moulds is limited to mostly
In micron composite ceramic material, such as ZrO2Toughness reinforcing A12O3Base composite ceramic ZTA wire drawing dies, TZP/TiC/A12O3, A12O3/TiC
Composite ceramics wire drawing die, (Ce-TZP)-A12O3Hot-extrusion mold, 3Y-TZP-A12O3Ceramic drawing die, PSZ ceramics hot extrusions
Mould, A12O3/Cr3C2/ (W, Ti) C etc..Nano composite ceramic is although less in the research of mold materials application aspect, such as compound
UP ceramic dies, A12O3/ Ti (C, N) etc., but also achieve good effect.
The performance of nano combined especially nano-micron compound ceramics is can be seen that from existing research, price advantage could not
It is not fully exerted in mould applications.From the point of view of current general status, the species of ceramic die material, performance and range of application
Await further expanding and improving.
The content of the invention
It is an object of the invention to provide a kind of tungsten carbide-base polynary nanometer composite ceramic die material and preparation method thereof,
The mould ageing resistance and defect support ability by force, with good comprehensive mechanical property and excellent properties of antifriction and wear resistance.
To achieve the above object, the present invention provides following technical scheme：
A kind of tungsten carbide-base polynary nanometer composite ceramic die material, be according to the raw material of weight portion：Tungsten carbide 60-80 parts, oxygen
Change 10-20 parts, titanium nitride 15-25 parts, manganese oxide 2-6 parts, neodymia 4-8 parts, chromium 2-4 parts, manganese 1-3 parts of zirconium；Above-mentioned all originals
Material uses nanometer grade powder, and the footpath grain size of wherein tungsten carbide is 10-100 nanometers, the footpath grain size of zirconium oxide and titanium nitride
It it is 1-10 nanometers, other footpath grain sizes are 1-100 nanometers.
As further scheme of the invention：The tungsten carbide-base polynary nanometer composite ceramic die material and its preparation side
Method, be according to the raw material of weight portion：Tungsten carbide 65-75 parts, zirconium oxide 14-16 parts, titanium nitride 18-22 parts, manganese oxide 3-5 parts,
Neodymia 5-7 parts, chromium 2.5-3.5 parts, manganese 1.5-2.5 parts.
The preparation method of described tungsten carbide-base polynary nanometer composite ceramic die material, with tungsten carbide as matrix, addition
Zirconium oxide and titanium nitride as enhancing phase, with manganese oxide and neodymia as stabilizer, using chromium and manganese as sintering aid, through hot pressing
Sintering is formed；Specific preparation process is as follows：
Step one：Above-mentioned all raw materials are weighed according to weight portion；
Step 2：Tungsten carbide, zirconium oxide and titanium nitride are added in the mixed solution of absolute ethyl alcohol and polyethylene glycol, then fully
Stirring, while ultrasonic disperse 20-30 minutes, obtain the first suspension；
Step 3：Manganese oxide, neodymia, chromium and manganese are added in the mixed solution of absolute ethyl alcohol and polyethylene glycol, then fully
Stirring, while ultrasonic disperse 20-30 minutes, obtain the second suspension；
Step 4：First suspension and second are suspended and is mixed, be then sufficiently stirred for, while ultrasonic disperse 10-20 minutes, obtain
Total mixture suspension；
Step 5：Total mixture suspension is poured into ball grinder, is Jie with absolute ethyl alcohol with inert gas as protective atmosphere
Matter, the iron ball of a diameter of 1-2mm is mill ball, under the microwave environment of 2450MHz, ball milling 12-24 hours, is filtrated to get grinding
Liquid；The gross weight of all raw materials is 1 with the weight ratio of mill ball:10-20；
Step 6：Lapping liquid is vacuum dried at a temperature of 110-120 DEG C, is sieved in inert gas flow after being completely dried,
Mixed powder is obtained, is sealed standby；
Step 7：Sintered using pressure sintering, obtain final product the mixed powder pressing mold sinter molding obtained by step 6 in hot pressing furnace.
As further scheme of the invention：The volume ratio of absolute ethyl alcohol described in step 2 and step 3 and polyethylene glycol
It is 1:0.5-2.
As further scheme of the invention：Inert gas described in step 5 and step 6 is nitrogen or rare gas.
As further scheme of the invention：Pressure sintering sintering process parameter is in step 7：Heating-up time 20-30min,
1400-1600 DEG C of holding temperature, hot pressing pressure 30-40MPa, soaking time 40-60min, is then cooled to room temperature.
Compared with prior art, the beneficial effects of the invention are as follows：Polynary nanometer composite ceramic die of the present invention, by receiving
Nano zircite is added in rice tungsten carbide matrix and mutually realize the nano combined of different-grain diameter as enhancing with Nano titanium nitride, add
The addition of nano zircite and Nano titanium nitride, can form typical transgranular/intergranular hybrid architecture with nanometer tungsten carbide,
Thus cause along crystalline substance/transcrystalline mixed-mode crack pattern, these strengthened mechanisms are various with tungsten carbide transformation toughening etc. toughened and reinforced
Mechanism acts synergistically, the common mechanical property and performance for improving material；And research shows：Manganese oxide and neodymia conduct
The compound addition of stabilizer, not only makes material have at a relatively high ageing resistance and defect resistivity, and crystal grain phase transformation is faced
Ungraduated ruler cun is relatively low to material fineness requirement than larger, so that material has preferable combination property.Finally, using metallic
Small abrading-ball, the reflection and refraction to microwave occurred after metal is subject to microwave irradiation is dissipated in whole reaction system, is risen
The effect of heating using microwave is arrived, reaction can be accelerated to carry out.Compared with existing ceramic die material, the polynary nanometer composite ceramic ceramic former
Tool material there is more preferable comprehensive mechanical property and excellent properties of antifriction and wear resistance, can be used for make extrusion die, drawing die and
The ceramics tool and mould such as cutting tool.
Specific embodiment
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,
Obviously, described embodiment is only a part of embodiment of the 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 the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of tungsten carbide-base polynary nanometer composite ceramic die material, be according to the raw material of weight portion：60 parts of tungsten carbide, zirconium oxide
10 parts, 15 parts of titanium nitride, 2 parts of manganese oxide, 4 parts of neodymia, 2 parts of chromium, 1 part of manganese；Above-mentioned all raw materials use nanometer grade powder,
The footpath grain size of wherein tungsten carbide is 10-100 nanometers, and the footpath grain size of zirconium oxide and titanium nitride is 1-10 nanometers, other footpaths
Grain size is 1-100 nanometers；Its preparation method be with tungsten carbide as matrix, addition zirconium oxide and titanium nitride as enhancing phase, with
Manganese oxide and neodymia are stabilizer, using chromium and manganese as sintering aid, are formed through hot pressed sintering；Specific preparation process is as follows：
Step one：Above-mentioned all raw materials are weighed according to weight portion；
Step 2：Tungsten carbide, zirconium oxide and titanium nitride are added in the mixed solution of absolute ethyl alcohol and polyethylene glycol, then fully
Stirring, while ultrasonic disperse 20 minutes, obtains the first suspension；The absolute ethyl alcohol is 1 with the volume ratio of polyethylene glycol:0.5；
Step 3：Manganese oxide, neodymia, chromium and manganese are added in the mixed solution of absolute ethyl alcohol and polyethylene glycol, then fully
Stirring, while ultrasonic disperse 20 minutes, obtains the second suspension；The absolute ethyl alcohol is 1 with the volume ratio of polyethylene glycol:0.5；
Step 4：First suspension and second are suspended mixing, is then sufficiently stirred for, while ultrasonic disperse 10 minutes, obtains total
Mixture suspension；
Step 5：Total mixture suspension is poured into ball grinder, with nitrogen as protective atmosphere, with absolute ethyl alcohol as medium, directly
Footpath is mill ball for the iron ball of 1mm, and under the microwave environment of 2450MHz, ball milling 12 hours is filtrated to get lapping liquid；All originals
The gross weight of material is 1 with the weight ratio of mill ball:10；
Step 6：Lapping liquid is vacuum dried at a temperature of 110 DEG C, is sieved in stream of nitrogen gas after being completely dried, mixed
Powder, seals standby；
Step 7：Sintered using pressure sintering, obtain final product the mixed powder pressing mold sinter molding obtained by step 6 in hot pressing furnace；Heat
The technological parameter of platen press sintering：Heating-up time 20min, 1400 DEG C of holding temperature, hot pressing pressure 30MPa, soaking time 40min,
Then it is cooled to room temperature.
Embodiment 2
A kind of tungsten carbide-base polynary nanometer composite ceramic die material, be according to the raw material of weight portion：70 parts of tungsten carbide, zirconium oxide
15 parts, 20 parts of titanium nitride, 4 parts of manganese oxide, 6 parts of neodymia, 3 parts of chromium, 2 parts of manganese；Above-mentioned all raw materials use nanometer grade powder,
The footpath grain size of wherein tungsten carbide is 10-100 nanometers, and the footpath grain size of zirconium oxide and titanium nitride is 1-10 nanometers, other footpaths
Grain size is 1-100 nanometers；Its preparation method be with tungsten carbide as matrix, addition zirconium oxide and titanium nitride as enhancing phase, with
Manganese oxide and neodymia are stabilizer, using chromium and manganese as sintering aid, are formed through hot pressed sintering；Specific preparation process is as follows：
Step one：Above-mentioned all raw materials are weighed according to weight portion；
Step 2：Tungsten carbide, zirconium oxide and titanium nitride are added in the mixed solution of absolute ethyl alcohol and polyethylene glycol, then fully
Stirring, while ultrasonic disperse 25 minutes, obtains the first suspension；The absolute ethyl alcohol is 1 with the volume ratio of polyethylene glycol:1；
Step 3：Manganese oxide, neodymia, chromium and manganese are added in the mixed solution of absolute ethyl alcohol and polyethylene glycol, then fully
Stirring, while ultrasonic disperse 25 minutes, obtains the second suspension；The absolute ethyl alcohol is 1 with the volume ratio of polyethylene glycol:1；
Step 4：First suspension and second are suspended mixing, is then sufficiently stirred for, while ultrasonic disperse 15 minutes, obtains total
Mixture suspension；
Step 5：Total mixture suspension is poured into ball grinder, with nitrogen as protective atmosphere, with absolute ethyl alcohol as medium, directly
Footpath is mill ball for the iron ball of 1.5mm, and under the microwave environment of 2450MHz, ball milling 18 hours is filtrated to get lapping liquid；It is all
The gross weight of raw material is 1 with the weight ratio of mill ball:15；
Step 6：Lapping liquid is vacuum dried at a temperature of 115 DEG C, is sieved in stream of nitrogen gas after being completely dried, mixed
Powder, seals standby；
Step 7：Sintered using pressure sintering, obtain final product the mixed powder pressing mold sinter molding obtained by step 6 in hot pressing furnace；Heat
The technological parameter of platen press sintering：Heating-up time 25min, 1500 DEG C of holding temperature, hot pressing pressure 35MPa, soaking time 50min,
Then it is cooled to room temperature.
Embodiment 3
A kind of tungsten carbide-base polynary nanometer composite ceramic die material, be according to the raw material of weight portion：80 parts of tungsten carbide, zirconium oxide
20 parts, 25 parts of titanium nitride, 6 parts of manganese oxide, 8 parts of neodymia, 4 parts of chromium, 3 parts of manganese；Above-mentioned all raw materials use nanometer grade powder,
The footpath grain size of wherein tungsten carbide is 10-100 nanometers, and the footpath grain size of zirconium oxide and titanium nitride is 1-10 nanometers, other footpaths
Grain size is 1-100 nanometers；Its preparation method be with tungsten carbide as matrix, addition zirconium oxide and titanium nitride as enhancing phase, with
Manganese oxide and neodymia are stabilizer, using chromium and manganese as sintering aid, are formed through hot pressed sintering；Specific preparation process is as follows：
Step one：Above-mentioned all raw materials are weighed according to weight portion；
Step 2：Tungsten carbide, zirconium oxide and titanium nitride are added in the mixed solution of absolute ethyl alcohol and polyethylene glycol, then fully
Stirring, while ultrasonic disperse 30 minutes, obtains the first suspension；The absolute ethyl alcohol is 1 with the volume ratio of polyethylene glycol:2；
Step 3：Manganese oxide, neodymia, chromium and manganese are added in the mixed solution of absolute ethyl alcohol and polyethylene glycol, then fully
Stirring, while ultrasonic disperse 30 minutes, obtains the second suspension；The absolute ethyl alcohol is 1 with the volume ratio of polyethylene glycol:2；
Step 4：First suspension and second are suspended mixing, is then sufficiently stirred for, while ultrasonic disperse 20 minutes, obtains total
Mixture suspension；
Step 5：Total mixture suspension is poured into ball grinder, with argon gas as protective atmosphere, with absolute ethyl alcohol as medium, directly
Footpath is mill ball for the iron ball of 2mm, and under the microwave environment of 2450MHz, ball milling 24 hours is filtrated to get lapping liquid；All originals
The gross weight of material is 1 with the weight ratio of mill ball:20；
Step 6：Lapping liquid is vacuum dried at a temperature of 120 DEG C, is sieved in an argon stream after being completely dried, mixed
Powder, seals standby；
Step 7：Sintered using pressure sintering, obtain final product the mixed powder pressing mold sinter molding obtained by step 6 in hot pressing furnace；Heat
The technological parameter of platen press sintering：Heating-up time 30min, 1600 DEG C of holding temperature, hot pressing pressure 40MPa, soaking time 60min,
Then it is 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, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be in other specific forms realized.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires to be limited rather than described above, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each implementation method is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should
Specification an as entirety, the technical scheme in each embodiment can also be formed into those skilled in the art through appropriately combined
May be appreciated other embodiment.
Claims (6)
1. a kind of tungsten carbide-base polynary nanometer composite ceramic die material, it is characterised in that the raw material according to weight portion is：Carbonization
Tungsten 60-80 parts, zirconium oxide 10-20 parts, titanium nitride 15-25 parts, manganese oxide 2-6 parts, neodymia 4-8 parts, chromium 2-4 parts, manganese 1-3
Part；Above-mentioned all raw materials use nanometer grade powder, and the footpath grain size of wherein tungsten carbide is 10-100 nanometers, zirconium oxide and nitridation
The footpath grain size of titanium is 1-10 nanometers, and other footpath grain sizes are 1-100 nanometers.
2. tungsten carbide-base polynary nanometer composite ceramic die material according to claim 1, it is characterised in that the carbonization
Tungsten Quito unit nano composite ceramic mould material and preparation method thereof, be according to the raw material of weight portion：Tungsten carbide 65-75 parts, oxygen
Change 14-16 parts, titanium nitride 18-22 parts, manganese oxide 3-5 parts, neodymia 5-7 parts, chromium 2.5-3.5 parts, manganese 1.5-2.5 parts of zirconium.
3. a kind of preparation method of tungsten carbide-base polynary nanometer composite ceramic die material as claimed in claim 1 or 2, it is special
Levy and be, with tungsten carbide as matrix, add zirconium oxide and titanium nitride as enhancing phase, with manganese oxide and neodymia as stabilizer,
Using chromium and manganese as sintering aid, formed through hot pressed sintering；Specific preparation process is as follows：
Step one：Above-mentioned all raw materials are weighed according to weight portion；
Step 2：Tungsten carbide, zirconium oxide and titanium nitride are added in the mixed solution of absolute ethyl alcohol and polyethylene glycol, then fully
Stirring, while ultrasonic disperse 20-30 minutes, obtain the first suspension；
Step 3：Manganese oxide, neodymia, chromium and manganese are added in the mixed solution of absolute ethyl alcohol and polyethylene glycol, then fully
Stirring, while ultrasonic disperse 20-30 minutes, obtain the second suspension；
Step 4：First suspension and second are suspended and is mixed, be then sufficiently stirred for, while ultrasonic disperse 10-20 minutes, obtain
Total mixture suspension；
Step 5：Total mixture suspension is poured into ball grinder, is Jie with absolute ethyl alcohol with inert gas as protective atmosphere
Matter, the iron ball of a diameter of 1-2mm is mill ball, under the microwave environment of 2450MHz, ball milling 12-24 hours, is filtrated to get grinding
Liquid；The gross weight of all raw materials is 1 with the weight ratio of mill ball:10-20；
Step 6：Lapping liquid is vacuum dried at a temperature of 110-120 DEG C, is sieved in inert gas flow after being completely dried,
Mixed powder is obtained, is sealed standby；
Step 7：Sintered using pressure sintering, obtain final product the mixed powder pressing mold sinter molding obtained by step 6 in hot pressing furnace.
4. the preparation method of tungsten carbide-base polynary nanometer composite ceramic die material according to claim 2, its feature exists
In absolute ethyl alcohol described in step 2 and step 3 is 1 with the volume ratio of polyethylene glycol:0.5-2.
5. the preparation method of tungsten carbide-base polynary nanometer composite ceramic die material according to claim 1, its feature exists
In inert gas described in step 5 and step 6 is nitrogen or rare gas.
6. the preparation method of tungsten carbide-base polynary nanometer composite ceramic die material according to claim 1, its feature exists
In pressure sintering sintering process parameter is in step 7：Heating-up time 20-30min, 1400-1600 DEG C of holding temperature, hot pressing pressure
30-40MPa, soaking time 40-60min, is then cooled to room temperature.
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| CN108298990A (en) * | 2017-12-25 | 2018-07-20 | 柳州科瑞科技有限公司 | A kind of ceramic mold and preparation method thereof |
| CN108516843A (en) * | 2018-06-12 | 2018-09-11 | 胡俊旭 | A kind of microwave sintering method and more gas part microwave agglomerating furnaces |
| CN111056852A (en) * | 2019-12-19 | 2020-04-24 | 西安交通大学 | Binding phase-free WC-based hard alloy cutter material and preparation method thereof |
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| 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 |
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