CN104311035A - A zirconium carbide-based multi-component nanometer composite ceramic mould material and a preparing method thereof - Google Patents
A zirconium carbide-based multi-component nanometer composite ceramic mould material and a preparing method thereof Download PDFInfo
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- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
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- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract
The invention discloses a zirconium carbide-based multi-component nanometer composite ceramic mould material and a preparing method thereof. The material comprises following raw materials by weight: 60-80 parts of zirconium carbide, 10-20 parts of aluminium oxide, 15-25 parts of silicon nitride, 2-6 parts of europium oxide, 4-8 parts of neodymium oxide, 2-4 parts of chromium and 1-3 parts of molybdenum. All the raw materials adopt nanometer powder, wherein the particle size of the zirconium carbide is 10-100 nm, the particle sizes of the aluminium oxide and the silicon nitride are 1-10 nm, and the particle sizes of other raw materials is 1-100 nm. According to the preparing method, the zirconium carbide is adopted as a substrate, the aluminium oxide and the silicon nitride are added and adopted as a reinforcement phase, the europium oxide and the neodymium oxide are adopted as stabilizing agents, the molybdenum and the chromium are adopted as sintering auxiliary agents, and the composite ceramic mould material is obtained by hot pressing and sintering. A mould has high ageing resistance and flaw resisting capability, and has good comprehensive mechanical performance and excellent antifriction wear-resisting performance.
Description
Technical field
The present invention relates to a kind of ceramic die material, specifically a kind of zirconium carbide Quito unit nano composite ceramic mould material and preparation method thereof.
Background technology
Sintex has high hardness and wear resistance, and showing excellent cutting ability when high speed cutting and dry cutting, is the cutter material that a class has development prospect.But the ceramic cutting tool material of application is at present confined to a micron composite ceramics mostly, and especially intensity, toughness still await further raising to the mechanical property of material.According to Hall-petch relation: grain-size is less, the intensity of stupalith is higher.Therefore, the research and development of nano modification, nano-micrometre composite ceramic tool material one of the Main way that will be cutter material development from now on.
Current nano composite ceramic cutter material after deliberation mainly comprises Si
3n
4/ TiNn, Si
3n
4/ TiCn, Si
3n
4-Ai
2o
3n-TiC-Y
2o
3, Al
2o
3/ TiC/SiCn, Al
2o
3/ TiCn, Al
2o
3/ Al
2o
3n/SiCn, Al
2o
3/ Ti (C
07n
03) n/SiCn, Al
2o
3/ SiC/SiCn, Al
2o
3/ TiC/TiNn, etc., all have than the better mechanical property of micron composite ceramic tool material and cutting ability.But up to the present, not yet find with zirconium carbide ceramics the report of the nano composite ceramic cutter material being matrix.
On the other hand, thermostability and the wear resistance of stupalith are splendid, are the ideal materials manufacturing shaping dies, have development prospect very much, but its toughness are very poor, are not therefore also used widely in mould industry.From status both at home and abroad, the research of ceramic die is still in the research and development stage, and little, the applicable mould applications of kind being applied to the stupalith of mould industry is very narrow, and the report of this respect is also few.At present, the applied research of stupalith in all kinds of mould is confined to a micron composite ceramic material, mostly as ZrO
2toughness reinforcing Al
2o
3base composite ceramic ZTA wortle, TZP/TiC/Al
2o
3, Al
2o
3/ TiC composite ceramics wortle, (Ce-TZP)-Al
2o
3hot-extrusion mold, 3Y-TZP-Al
2o
3pottery drawing die, PSZ pottery hot extruding die, Al
2o
3/ Cr
3c
2/ (W, Ti) C etc.Although nano composite ceramic is less in the research of moulding stock application aspect, as compound UP ceramic die, Al
2o
3/ Ti (C, N) etc., but also achieve good effect.
As can be seen from existing research, performance, the price advantage of nano combined especially nano-micron compound pottery could not be not fully exerted in mould applications.With regard to current general status, the kind of ceramic die material, performance and application scope all await expanding further and improving.
Summary of the invention
The object of the present invention is to provide a kind of zirconium carbide Quito unit nano composite ceramic mould material and preparation method thereof, this mould resistance to deterioration 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 invention provides following technical scheme:
A kind of zirconium carbide Quito unit nano composite ceramic mould material, according to the raw material of weight part is: zirconium carbide 60-80 part, aluminum oxide 10-20 part, silicon nitride 15-25 part, europium sesquioxide 2-6 part, Neodymium trioxide 4-8 part, chromium 2-4 part, molybdenum 1-3 part; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium carbide is 10-100 nanometer, and the footpath grain size of aluminum oxide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer.
As the further scheme of the present invention: described zirconium carbide Quito unit nano composite ceramic mould material and preparation method thereof, according to the raw material of weight part is: zirconium carbide 65-75 part, aluminum oxide 14-16 part, silicon nitride 18-22 part, europium sesquioxide 3-5 part, Neodymium trioxide 5-7 part, chromium 2.5-3.5 part, molybdenum 1.5-2.5 part.
The preparation method of described zirconium carbide Quito unit nano composite ceramic mould material take zirconium carbide as matrix, adds aluminum oxide and silicon nitride as wild phase, with europium sesquioxide and Neodymium trioxide for stablizer, using chromium and molybdenum as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step one: take above-mentioned all raw materials according to weight part;
Step 2: zirconium carbide, aluminum oxide and silicon nitride are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20-30 minute, obtains the first suspension simultaneously;
Step 3: europium sesquioxide, Neodymium trioxide, chromium and molybdenum are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20-30 minute, obtains the second suspension simultaneously;
Step 4: suspend the first suspension and second mixing, and then fully stir, ultrasonic disperse 10-20 minute, obtains total mixture suspension simultaneously;
Step 5: pour in ball grinder by total mixture suspension is protective atmosphere with rare gas element, take dehydrated alcohol as medium, and diameter is the iron ball of 1-2mm is mill ball, and under the microwave environment of 2450MHz, ball milling 12-24 hour, filters and obtain lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 10-20;
Step 6: by lapping liquid vacuum-drying at 110-120 DEG C of temperature, sieve in inert gas flow after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt 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 in step 2 and step 3, the volume ratio of dehydrated alcohol and polyoxyethylene glycol is 1: 0.5-2.
As the further scheme of the present invention: described in step 5 and step 6, rare gas element 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, holding temperature 1400-1600 DEG C, hot pressing pressure 30-40MPa, soaking time 40-60min, be then 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 adding nano aluminium oxide and nano-silicon nitride realizes the nano combined of different-grain diameter as wild phase in nano-zirconium carbide matrix, add adding of nano aluminium oxide and nano-silicon nitride, typical intracrystalline/intergranular hybrid architecture can be defined with nano-zirconium carbide, cause along crystalline substance/transcrystalline mixed-mode crack pattern thus, the multiple toughening and strengthening such as these strengthened mechanism and zirconium carbide transformation toughening act synergistically, common mechanical property and the use properties improving material, and research shows: europium sesquioxide and Neodymium trioxide add as the compound of stablizer, material is not only made to have quite high resistance to deterioration and defect resistivity, and crystal grain phase transformation critical size is larger, requires lower to material fineness, thus make material have good over-all properties.Finally, utilize the little abrading-ball of metallic, what occur after metal is subject to microwave exposure is dissipated in whole reaction system micro-wave reflection and refraction, serves the effect of microwave heating, can accelerated reaction carry out.Compared with existing ceramic die material, this polynary nanometer composite ceramic die material has better comprehensive mechanical property and excellent properties of antifriction and wear resistance, can be used for making potter's moulds such as overflow mould, drawing die and cutting tool.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A kind of zirconium carbide Quito unit nano composite ceramic mould material, according to the raw material of weight part is: zirconium carbide 60 parts, 10 parts, aluminum oxide, silicon nitride 15 parts, europium sesquioxide 2 parts, Neodymium trioxide 4 parts, chromium 2 parts, molybdenum 1 part; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium carbide is 10-100 nanometer, and the footpath grain size of aluminum oxide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method take zirconium carbide as matrix, adds aluminum oxide and silicon nitride as wild phase, with europium sesquioxide and Neodymium trioxide for stablizer, using chromium and molybdenum as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step one: take above-mentioned all raw materials according to weight part;
Step 2: zirconium carbide, aluminum oxide and silicon nitride are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20 minutes, obtains the first suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 0.5;
Step 3: europium sesquioxide, Neodymium trioxide, chromium and molybdenum are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20 minutes, obtains the second suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 0.5;
Step 4: suspend the first suspension and second mixing, and then fully stir, ultrasonic disperse 10 minutes, obtains total mixture suspension simultaneously;
Step 5: pour in ball grinder by total mixture suspension is protective atmosphere with nitrogen, take dehydrated alcohol as medium, and diameter is the iron ball of 1mm is mill ball, and under the microwave environment of 2450MHz, ball milling 12 hours, filters and obtain lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 10;
Step 6: by lapping liquid vacuum-drying at 110 DEG C of temperature, sieve in stream of nitrogen gas after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace; The processing parameter of pressure sintering sintering: heating-up time 20min, holding temperature 1400 DEG C, hot pressing pressure 30MPa, soaking time 40min, be then cooled to room temperature.
Embodiment 2
A kind of zirconium carbide Quito unit nano composite ceramic mould material, according to the raw material of weight part is: zirconium carbide 70 parts, 15 parts, aluminum oxide, silicon nitride 20 parts, europium sesquioxide 4 parts, Neodymium trioxide 6 parts, chromium 3 parts, molybdenum 2 parts; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium carbide is 10-100 nanometer, and the footpath grain size of aluminum oxide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method take zirconium carbide as matrix, adds aluminum oxide and silicon nitride as wild phase, with europium sesquioxide and Neodymium trioxide for stablizer, using chromium and molybdenum as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step one: take above-mentioned all raw materials according to weight part;
Step 2: zirconium carbide, aluminum oxide and silicon nitride are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 25 minutes, obtains the first suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 1;
Step 3: europium sesquioxide, Neodymium trioxide, chromium and molybdenum are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 25 minutes, obtains the second suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 1;
Step 4: suspend the first suspension and second mixing, and then fully stir, ultrasonic disperse 15 minutes, obtains total mixture suspension simultaneously;
Step 5: pour in ball grinder by total mixture suspension is protective atmosphere with nitrogen, take dehydrated alcohol as medium, and diameter is the iron ball of 1.5mm is mill ball, and under the microwave environment of 2450MHz, ball milling 18 hours, filters and obtain lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 15;
Step 6: by lapping liquid vacuum-drying at 115 DEG C of temperature, sieve in stream of nitrogen gas after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace; The processing parameter of pressure sintering sintering: heating-up time 25min, holding temperature 1500 DEG C, hot pressing pressure 35MPa, soaking time 50min, be then cooled to room temperature.
Embodiment 3
A kind of zirconium carbide Quito unit nano composite ceramic mould material, according to the raw material of weight part is: zirconium carbide 80 parts, 20 parts, aluminum oxide, silicon nitride 25 parts, europium sesquioxide 6 parts, Neodymium trioxide 8 parts, chromium 4 parts, molybdenum 3 parts; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium carbide is 10-100 nanometer, and the footpath grain size of aluminum oxide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method take zirconium carbide as matrix, adds aluminum oxide and silicon nitride as wild phase, with europium sesquioxide and Neodymium trioxide for stablizer, using chromium and molybdenum as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step one: take above-mentioned all raw materials according to weight part;
Step 2: zirconium carbide, aluminum oxide and silicon nitride are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 30 minutes, obtains the first suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 2;
Step 3: europium sesquioxide, Neodymium trioxide, chromium and aluminium are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 30 minutes, obtains the second suspension simultaneously; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 2;
Step 4: suspend the first suspension and second mixing, and then fully stir, ultrasonic disperse 20 minutes, obtains total mixture suspension simultaneously;
Step 5: pour in ball grinder by total mixture suspension is protective atmosphere with argon gas, take dehydrated alcohol as medium, and diameter is the iron ball of 2mm is mill ball, and under the microwave environment of 2450MHz, ball milling 24 hours, filters and obtain lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 20;
Step 6: by lapping liquid vacuum-drying at 120 DEG C of temperature, sieve in an argon stream after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace: the processing parameter of pressure sintering sintering: heating-up time 30min, holding temperature 1600 DEG C, hot pressing pressure 40MPa, soaking time 60min, is then cooled to room temperature.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (6)
1. zirconium carbide Quito unit nano composite ceramic mould material, is characterized in that, according to the raw material of weight part be: zirconium carbide 60-80 part, aluminum oxide 10-20 part, silicon nitride 15-25 part, europium sesquioxide 2-6 part, Neodymium trioxide 4-8 part, chromium 2-4 part, molybdenum 1-3 part; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of zirconium carbide is 10-100 nanometer, and the footpath grain size of aluminum oxide and silicon nitride is 1-10 nanometer, and other footpath grain size is 1-100 nanometer.
2. zirconium carbide Quito unit according to claim 1 nano composite ceramic mould material, it is characterized in that, described zirconium carbide Quito unit nano composite ceramic mould material and preparation method thereof, according to the raw material of weight part is: zirconium carbide 65-75 part, aluminum oxide 14-16 part, silicon nitride 18-22 part, europium sesquioxide 3-5 part, Neodymium trioxide 5-7 part, chromium 2.5-3.5 part, molybdenum 1.5-2.5 part.
3. the preparation method of zirconium carbide Quito unit as claimed in claim 1 or 2 nano composite ceramic mould material, it is characterized in that, take zirconium carbide as matrix, interpolation aluminum oxide and silicon nitride are as wild phase, with europium sesquioxide and Neodymium trioxide for stablizer, using chromium and molybdenum as sintering aid, form through hot pressed sintering; Concrete preparation process is as follows:
Step one: take above-mentioned all raw materials according to weight part;
Step 2: zirconium carbide, aluminum oxide and silicon nitride are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20-30 minute, obtains the first suspension simultaneously;
Step 3: europium sesquioxide, Neodymium trioxide, chromium and molybdenum are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic disperse 20-30 minute, obtains the second suspension simultaneously;
Step 4: suspend the first suspension and second mixing, and then fully stir, ultrasonic disperse 10-20 minute, obtains total mixture suspension simultaneously;
Step 5: pour in ball grinder by total mixture suspension is protective atmosphere with rare gas element, take dehydrated alcohol as medium, and diameter is the iron ball of 1-2mm is mill ball, and under the microwave environment of 2450MHz, ball milling 12-24 hour, filters and obtain lapping liquid; The gross weight of all raw materials and the weight ratio of mill ball are 1: 10-20;
Step 6: by lapping liquid vacuum-drying at 110-120 DEG C of temperature, sieve in inert gas flow after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt pressure sintering sintering, by the mixed powder pressing mold sinter molding of step 6 gained and get final product in hot pressing furnace.
4. the preparation method of zirconium carbide Quito according to claim 3 unit nano composite ceramic mould material, is characterized in that, described in step 2 and step 3, the volume ratio of dehydrated alcohol and polyoxyethylene glycol is 1: 0.5-2.
5. the preparation method of zirconium carbide Quito according to claim 1 unit nano composite ceramic mould material, is characterized in that, described in step 5 and step 6, rare gas element is nitrogen or rare gas.
6. the preparation method of zirconium carbide Quito unit according to claim 1 nano composite ceramic mould material, 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, soaking time 40-60min, is then cooled to room temperature.
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Cited By (4)
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| CN104987048A (en) * | 2015-07-14 | 2015-10-21 | 苏州恒辉科技有限公司 | Ceramic material for nanometer aluminum oxide mold and preparation method of ceramic material |
| CN105016732A (en) * | 2015-08-03 | 2015-11-04 | 佛山蓝途科技有限公司 | High-strength and good-abrasion-resistance zirconium carbide ceramic material and preparing method thereof |
| CN106222513A (en) * | 2016-07-29 | 2016-12-14 | 余姚市巧迪电器厂 | A kind of ceramic die of high intensity and preparation method thereof |
| CN106747448A (en) * | 2016-12-09 | 2017-05-31 | 姚旭 | A kind of tungsten carbide-base polynary nanometer composite ceramic die material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104987048A (en) * | 2015-07-14 | 2015-10-21 | 苏州恒辉科技有限公司 | Ceramic material for nanometer aluminum oxide mold and preparation method of ceramic material |
| CN105016732A (en) * | 2015-08-03 | 2015-11-04 | 佛山蓝途科技有限公司 | High-strength and good-abrasion-resistance zirconium carbide ceramic material and preparing method thereof |
| CN105016732B (en) * | 2015-08-03 | 2017-12-05 | 长乐品苑建材科技有限公司 | Good zirconium carbide ceramic material of a kind of intensity high-wearing feature and preparation method thereof |
| CN106222513A (en) * | 2016-07-29 | 2016-12-14 | 余姚市巧迪电器厂 | A kind of ceramic die of high intensity and preparation method thereof |
| CN106747448A (en) * | 2016-12-09 | 2017-05-31 | 姚旭 | A kind of tungsten carbide-base polynary nanometer composite ceramic die material and preparation method thereof |
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Application publication date: 20150128 |