CN104163625A - Scandium oxide and neodymium oxide composite stabilized titanium oxide-based multi-element nano-composite ceramic die - Google Patents
Scandium oxide and neodymium oxide composite stabilized titanium oxide-based multi-element nano-composite ceramic die Download PDFInfo
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- CN104163625A CN104163625A CN201410381863.8A CN201410381863A CN104163625A CN 104163625 A CN104163625 A CN 104163625A CN 201410381863 A CN201410381863 A CN 201410381863A CN 104163625 A CN104163625 A CN 104163625A
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Abstract
The invention discloses a scandium oxide and neodymium oxide composite stabilized titanium oxide-based multi-element nano-composite ceramic die. The die comprises the following raw materials in parts by weight: 60-80 parts of titanium oxide, 10-20 parts of silicon carbide, 15-25 parts of aluminium oxide, 2-6 parts of scandium oxide, 4-8 parts of neodymium oxide, 2-4 parts of chromium and 1-3 parts of cobalt, wherein nanoscale powder of all the raw materials is adopted; the grain size of titanium oxide is 10-100 nanometers; the grain sizes of silicon carbide and aluminium oxide are 1-10 nanometers; the grain sizes of the other raw materials are 1-100 nanometers. A preparation method is characterized by using titanium oxide as the matrix, adding silicon carbide and aluminium oxide as reinforcing phases, scandium oxide and neodymium oxide as stabilizing agents and chromium and cobalt as sintering aids and carrying out hot pressed sintering on the materials, thus preparing the die. The die has strong ageing and defect resistance, good comprehensive mechanical properties and excellent antifriction and wear resistance properties.
Description
Technical field
The present invention relates to a kind of ceramic die material, specifically the titania based polynary nanometer composite ceramic die of a kind of Scium trioxide and Neodymium trioxide stable composition.
Background technology
Sintex has high hardness and wear resistance, in the time of high speed cutting and dry cutting, shows excellent cutting ability, is the cutter material that a class has 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 awaits further raising.According to Hall-petch relation: grain-size is less, and the intensity of stupalith is higher.Therefore, the research and development of nano modification, nano-micrometre composite ceramic tool material will be one of main direction of 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
0.7n
0.3) 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 TiO
2pottery is the report of the nano composite ceramic cutter material of matrix.
On the other hand, thermostability and the wear resistance of stupalith are splendid, are the ideal materials of manufacturing shaping dies, have very much development prospect, but its toughness are very poor, therefore also aspect mould industry, are not used widely.From domestic and international present situation, the research of ceramic die is still in the research and development stage, and little, the applicable mould applications of kind of stupalith that is applied to 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 moulds 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 obtained good effect.
Can find out 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 range of application all await further expanding and improving.
Summary of the invention
The object of the present invention is to provide the titania based polynary nanometer composite ceramic die of a kind of Scium trioxide and Neodymium trioxide stable composition, this mould resistance to deterioration and defect are strong to ability, have good comprehensive mechanical property and good properties of antifriction and wear resistance.
For achieving the above object, the invention provides following technical scheme:
A kind of Scium trioxide and the titania based polynary nanometer composite ceramic die of Neodymium trioxide stable composition, according to the raw material of weight part be: titanium oxide 60-80 part, silicon carbide 10-20 part, aluminum oxide 15-25 part, Scium trioxide 2-6 part, Neodymium trioxide 4-8 part, chromium 2-4 part, cobalt 1-3 part; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of titanium oxide is 10-100 nanometer, and the footpath grain size of silicon carbide and aluminum oxide is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method is taking titanium oxide as matrix, adds silicon carbide and aluminum oxide as wild phase, taking Scium trioxide and Neodymium trioxide as stablizer, using chromium and cobalt as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step 1: take above-mentioned all raw materials according to weight part;
Step 2: titanium oxide, silicon carbide and aluminum oxide are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic dispersion 20-30 minute, obtains the first suspension simultaneously;
Step 3: Scium trioxide, Neodymium trioxide, chromium and cobalt are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic dispersion 20-30 minute, obtains the second suspension simultaneously;
Step 4: the first suspension and second is suspended and mixed, then fully stir, ultrasonic dispersion 10-20 minute, obtains total mixture suspension simultaneously;
Step 5: total mixture suspension is poured in ball grinder, and taking rare gas element as protective atmosphere, taking dehydrated alcohol as medium, the iron ball that diameter is 1-2mm is mill ball, under the microwave environment of 2450MHz, ball milling 12-24 hour, filters and obtains 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, in hot pressing furnace by the mixed powder pressing mold sinter molding of step 6 gained and get final product.
As the further scheme of the present invention: the titania based polynary nanometer composite ceramic die of described Scium trioxide and Neodymium trioxide stable composition, according to the raw material of weight part is: titanium oxide 65-75 part, silicon carbide 14-16 part, aluminum oxide 18-22 part, Scium trioxide 3-5 part, Neodymium trioxide 5-7 part, chromium 2.5-3.5 part, cobalt 1.5-2.5 part.
As the further scheme of the present invention: the volume ratio of dehydrated alcohol and polyoxyethylene glycol described in step 2 and step 3 is 1: 0.5-2.
As the further scheme of the present invention: rare gas element 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, holding temperature 1400-1600 DEG C, hot pressing pressure 30-40MPa, soaking time 40-60min, is 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 nanometer silicon carbide and nano aluminium oxide is realized the nano combined of different-grain diameter as wild phase in nano-titanium oxide matrix, add adding of nanometer silicon carbide and nano aluminium oxide, can form typical intracrystalline/intergranular hybrid architecture with nano-titanium oxide, cause thus along crystalline substance/transcrystalline mixed-mode crack pattern, the multiple toughened and reinforced mechanism synergies such as these highly malleablized mechanism and titanium oxide transformation toughening, jointly improve mechanical property and the use properties of material, and research shows: Scium trioxide and Neodymium trioxide are as the compound interpolation of stablizer, not only make material there is quite high resistance to deterioration and defect resistivity, and crystal grain phase transformation critical size is larger, lower to material fineness requirement, thus make material there is good over-all properties.Finally, utilize the little abrading-ball of metallic, what after metal is subject to microwave exposure, occur is dissipated in whole reaction system micro-wave reflection and refraction, has played 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 good 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, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
A kind of Scium trioxide and the titania based polynary nanometer composite ceramic die of Neodymium trioxide stable composition, according to the raw material of weight part be: 60 parts of titanium oxide, 10 parts, silicon carbide, 15 parts, aluminum oxide, 2 parts of Scium trioxides, 4 parts of Neodymium trioxide, 2 parts of chromium, 1 part of cobalt; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of titanium oxide is 10-100 nanometer, and the footpath grain size of silicon carbide and aluminum oxide is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method is taking titanium oxide as matrix, adds silicon carbide and aluminum oxide as wild phase, taking Scium trioxide and Neodymium trioxide as stablizer, using chromium and cobalt as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step 1: take above-mentioned all raw materials according to weight part;
Step 2: titanium oxide, silicon carbide and aluminum oxide are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic dispersion simultaneously 20 minutes, obtains the first suspension; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 0.5;
Step 3: Scium trioxide, Neodymium trioxide, chromium and cobalt are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic dispersion simultaneously 20 minutes, obtains the second suspension; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 0.5;
Step 4: the first suspension and second is suspended and mixed, then fully stir, ultrasonic dispersion simultaneously 10 minutes, obtains total mixture suspension;
Step 5: total mixture suspension is poured in ball grinder, and taking nitrogen as protective atmosphere, taking dehydrated alcohol as medium, the iron ball that diameter is 1mm is mill ball, under the microwave environment of 2450MHz, ball milling 12 hours, filters and obtains 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, in hot pressing furnace by the mixed powder pressing mold sinter molding of step 6 gained and get final product; The processing parameter of pressure sintering sintering: heating-up time 20min, 1400 DEG C of holding temperatures, hot pressing pressure 30MPa, soaking time 40min, is then cooled to room temperature.
Embodiment 2
A kind of Scium trioxide and the titania based polynary nanometer composite ceramic die of Neodymium trioxide stable composition, according to the raw material of weight part be: 70 parts of titanium oxide, 15 parts, silicon carbide, 20 parts, aluminum oxide, 4 parts of Scium trioxides, 6 parts of Neodymium trioxide, 3 parts of chromium, 2 parts of cobalts; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of titanium oxide is 10-100 nanometer, and the footpath grain size of silicon carbide and aluminum oxide is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method is taking titanium oxide as matrix, adds silicon carbide and aluminum oxide as wild phase, taking Scium trioxide and Neodymium trioxide as stablizer, using chromium and cobalt as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step 1: take above-mentioned all raw materials according to weight part;
Step 2: titanium oxide, silicon carbide and aluminum oxide are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic dispersion simultaneously 25 minutes, obtains the first suspension; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 1;
Step 3: Scium trioxide, Neodymium trioxide, chromium and cobalt are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic dispersion simultaneously 25 minutes, obtains the second suspension; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 1;
Step 4: the first suspension and second is suspended and mixed, then fully stir, ultrasonic dispersion simultaneously 15 minutes, obtains total mixture suspension;
Step 5: total mixture suspension is poured in ball grinder, and taking nitrogen as protective atmosphere, taking dehydrated alcohol as medium, the iron ball that diameter is 1.5mm is mill ball, under the microwave environment of 2450MHz, ball milling 18 hours, filters and obtains 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, in hot pressing furnace by the mixed powder pressing mold sinter molding of step 6 gained and get final product; The processing parameter of pressure sintering sintering: heating-up time 25min, 1500 DEG C of holding temperatures, hot pressing pressure 35MPa, soaking time 50min, is then cooled to room temperature.
Embodiment 3
A kind of Scium trioxide and the titania based polynary nanometer composite ceramic die of Neodymium trioxide stable composition, according to the raw material of weight part be: 80 parts of titanium oxide, 20 parts, silicon carbide, 25 parts, aluminum oxide, 6 parts of Scium trioxides, 8 parts of Neodymium trioxide, 4 parts of chromium, 3 parts of cobalts; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of titanium oxide is 10-100 nanometer, and the footpath grain size of silicon carbide and aluminum oxide is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method is taking titanium oxide as matrix, adds silicon carbide and aluminum oxide as wild phase, taking Scium trioxide and Neodymium trioxide as stablizer, using chromium and cobalt as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step 1: take above-mentioned all raw materials according to weight part;
Step 2: titanium oxide, silicon carbide and aluminum oxide are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic dispersion simultaneously 30 minutes, obtains the first suspension; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 2;
Step 3: Scium trioxide, Neodymium trioxide, chromium and cobalt are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic dispersion simultaneously 30 minutes, obtains the second suspension; The volume ratio of described dehydrated alcohol and polyoxyethylene glycol is 1: 2;
Step 4: the first suspension and second is suspended and mixed, then fully stir, ultrasonic dispersion simultaneously 20 minutes, obtains total mixture suspension;
Step 5: total mixture suspension is poured in ball grinder, and taking argon gas as protective atmosphere, taking dehydrated alcohol as medium, the iron ball that diameter is 2mm is mill ball, under the microwave environment of 2450MHz, ball milling 24 hours, filters and obtains 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 argon stream after complete drying, obtain mixed powder, seal for subsequent use;
Step 7: adopt pressure sintering sintering, in hot pressing furnace by the mixed powder pressing mold sinter molding of step 6 gained and get final product; The processing parameter of pressure sintering sintering: heating-up time 30min, 1600 DEG C of holding temperatures, 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 example embodiment, and in the situation that not deviating from spirit of the present invention or essential characteristic, can realize the present invention with other specific form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, is therefore intended to all changes that drop in the implication and the scope that are equal to important document of claim to include in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but be not that 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 make specification sheets as a whole, and the technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (5)
1. a Scium trioxide and the titania based polynary nanometer composite ceramic die of Neodymium trioxide stable composition, it is characterized in that, according to the raw material of weight part be: titanium oxide 60-80 part, silicon carbide 10-20 part, aluminum oxide 15-25 part, Scium trioxide 2-6 part, Neodymium trioxide 4-8 part, chromium 2-4 part, cobalt 1-3 part; Above-mentioned all raw materials all adopt nanoscale powder, and wherein the footpath grain size of titanium oxide is 10-100 nanometer, and the footpath grain size of silicon carbide and aluminum oxide is 1-10 nanometer, and other footpath grain size is 1-100 nanometer; Its preparation method is taking titanium oxide as matrix, adds silicon carbide and aluminum oxide as wild phase, taking Scium trioxide and Neodymium trioxide as stablizer, using chromium and cobalt as sintering aid, forms through hot pressed sintering; Concrete preparation process is as follows:
Step 1: take above-mentioned all raw materials according to weight part;
Step 2: titanium oxide, silicon carbide and aluminum oxide are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic dispersion 20-30 minute, obtains the first suspension simultaneously;
Step 3: Scium trioxide, Neodymium trioxide, chromium and cobalt are added in the mixing solutions of dehydrated alcohol and polyoxyethylene glycol, then fully stir, ultrasonic dispersion 20-30 minute, obtains the second suspension simultaneously;
Step 4: the first suspension and second is suspended and mixed, then fully stir, ultrasonic dispersion 10-20 minute, obtains total mixture suspension simultaneously;
Step 5: total mixture suspension is poured in ball grinder, and taking rare gas element as protective atmosphere, taking dehydrated alcohol as medium, the iron ball that diameter is 1-2mm is mill ball, under the microwave environment of 2450MHz, ball milling 12-24 hour, filters and obtains 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, in hot pressing furnace by the mixed powder pressing mold sinter molding of step 6 gained and get final product.
2. the titania based polynary nanometer composite ceramic die of Scium trioxide according to claim 1 and Neodymium trioxide stable composition, it is characterized in that, the titania based polynary nanometer composite ceramic die of described Scium trioxide and Neodymium trioxide stable composition, according to the raw material of weight part is: titanium oxide 65-75 part, silicon carbide 14-16 part, aluminum oxide 18-22 part, Scium trioxide 3-5 part, Neodymium trioxide 5-7 part, chromium 2.5-3.5 part, cobalt 1.5-2.5 part.
3. the titania based polynary nanometer composite ceramic die of Scium trioxide according to claim 1 and Neodymium trioxide stable composition, is characterized in that, the volume ratio of dehydrated alcohol and polyoxyethylene glycol described in step 2 and step 3 is 1: 0.5-2.
4. the titania based polynary nanometer composite ceramic die of Scium trioxide according to claim 1 and Neodymium trioxide stable composition, is characterized in that, rare gas element described in step 5 and step 6 is nitrogen or rare gas.
5. the titania based polynary nanometer composite ceramic die of Scium trioxide according to claim 1 and Neodymium trioxide stable composition, 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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| 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 |
| CN108772052A (en) * | 2018-05-30 | 2018-11-09 | 中国科学院宁波材料技术与工程研究所 | A kind of titania-based porous blocks and its preparation method and application |
| CN109354497A (en) * | 2018-12-12 | 2019-02-19 | 中国工程物理研究院化工材料研究所 | The transparent Indium scandium ceramics and preparation method thereof of Ho doping |
| 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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108772052A (en) * | 2018-05-30 | 2018-11-09 | 中国科学院宁波材料技术与工程研究所 | A kind of titania-based porous blocks and its preparation method and application |
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| CN109354497A (en) * | 2018-12-12 | 2019-02-19 | 中国工程物理研究院化工材料研究所 | The transparent Indium scandium ceramics and preparation method thereof of Ho doping |
| CN109354497B (en) * | 2018-12-12 | 2021-06-22 | 中国工程物理研究院化工材料研究所 | Ho-doped transparent scandium oxide ceramic and preparation method thereof |
| 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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| CN104163625B (en) | 2016-02-17 |
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Inventor after: Huang Changping Inventor after: Deng Xuehui Inventor after: Huang Shaoguang Inventor after: Wu Qiucai Inventor after: Huang Xiaotao Inventor after: Su Zhiqiang Inventor after: Yang Yunshan Inventor after: Li Hengheng Inventor before: Han Qiao Inventor before: Li Xiaojun |
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Effective date of registration: 20170407 Address after: 514245 Meizhou, Zhejiang Province, Tai Po Town, ceramics industrial park Patentee after: MEIZHOU SHUNYAUN CERAMICS INDUSTRY 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 |
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