CN104177088A - Ti-Si-N nanocrystalline-amorphous composite ceramic material and preparation method thereof - Google Patents
Ti-Si-N nanocrystalline-amorphous composite ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Ti-Si-N nanocrystalline-amorphous composite ceramic material and a preparation method thereof. The Ti-Si-N nanocrystalline-amorphous composite ceramic material is characterized in that high-purity TiN nanopowder and silicon nitride nanopowder are taken as raw materials, and then, a discharge plasma sintering technology is adopted to sinter Ti-Si-N block materials, and sintering parameters are controlled to sinter out the Ti-Si-N blocky composite material with grain size of 5-200 nanometers. The preparation method comprises the following steps: sufficiently stirring and mixing the high-purity TiN nano powder and the silicon nitride nanopowder in a powder mixer, pressing and molding, and sintering at a certain temperature under a certain pressure in discharge plasma equipment, and controlling the sintering time, thereby obtaining the Ti-Si-N blocky composite material after the sintering is finished. The Ti-Si-N nanocrystalline-amorphous composite ceramic material has the characteristics of high temperature resistance, abrasion resistance and corrosion resistance, and has a very good application prospect in the field of high-temperature mechanical components and cutting tools.
Description
Technical field
This patent belongs to new material technology field, relates in particular to a kind of Ti-Si-N nanocrystalline and amorphous composite ceramic material and synthetic method thereof.
Background technology
Quality of the height of machining productivity and cutter life, number, working accuracy and the machined surface quality of tooling cost etc., depends on the choose reasonable of cutter material to a great extent.The cutter material of application mainly contains diamond, cubic boron nitride, pottery, sintering metal, Wimet, rapid steel and various coated cutting tool at present.They respectively have feature separately, adapt to different workpiece materials and different cutting speed scopes.As far back as 20 beginnings of the century, Germany and Britain have started to adopt sintex to replace traditional carbon tool steel cutter, but because brittleness of ceramics is at that time larger, so its application is limited to.How to overcome the fragility of ceramic cutting tool material, improve its toughness, become the major subjects of ceramic cutting tool material research in the last hundred years.
The high material of hardness often intensity and toughness low, want to improve toughness often with the cost that drops to of hardness.Contradiction between this Hardness and toughness of ceramic cutting tool material makes research have pottery that high rigidity has again high strength, high tenacity simultaneously becomes the focus of ceramic cutting tool material research.The development of superfine crystal particle technology and the research of nano composite material are that ceramic development has increased new vitality.According to Hall-petch relation, hardness and the intensity of the less stupalith of grain-size are higher, and when grain-size is little when the 100nm left and right, intensity and hardness can improve a lot.Nano modification, the nano combined abnormal growth problem that has successfully solved crystal grain, nanometer particle pinning or enter dislocation district and make to form subgrain boundary in matrix grain, causes matrix grain refinement.But the activity of nano powder is very large, surface reaction intensity of activation is lower, in sintering process, very easily grows up, although add inhibitor, effect is still undesirable, and nanometer scale ceramics cutter material is still in triturating at present, and the sintex product of developing is relatively less.Nano modification, research and development nano combined and superfine crystal particle ceramic cutting tool material will be the main direction that ceramic cutting tool material develops from now on.
The features such as TiN material has that hardness is high, wear resistance and good corrosion resistance, obtain a wide range of applications, but temperature tolerance are poor as cutting tool coating material.In TiN, add the Ti-Si-N matrix material that silicon addition prepares and not only have the hardness higher than TiN, and wear resisting property also improves a lot, particularly r has very big raising.Ti-Si-N material is mainly coated material at present, after being successfully prepared, obtain both at home and abroad research widely from nineteen ninety-five Germany scientist Veprek1995, it is typical nanocrystalline and amorphous matrix material, has superhard and heatproof feature, but does not see synthetic Ti-Si-N block crystal report.
Discharge plasma sintering technique (Spark Plasma Sintering or SPS) also claims plasma activated sintering (Plasma Activated Sintering or PAS), claim again electromagnetism assisted sintering technique, come from the pulse electric current sintering principle that the thirties in 20th century, American scientist proposed.To the end of the sixties, Japanology the similar but more advanced sintering technology-electric spark sintering of principle, and obtained license.Owing to failing at that time to solve the problems such as this technology production efficiency is low, SPS technology could not be widely applied.Until 1988, Japanese aboveground Research Institute goes out First SPS device, just in novel material research field, applies.After the nineties, Japan has carried out a large amount of research and development work to aspects such as SPS equipment, technology and fabrication of new materials, has released and can be used for industrial SPS third generation product.Realize the sintering pressure of 10-100t and the pulse sintering electric current of 5000-8000A, developed again recently pressure and reach 500t, pulsed current and reach the large-scale SPS device of 25000A.More than 200 dissimilar SPS equipment has been equipped by current worldwide university, industrial research institutes and enterprise, and wherein Japan has accounted for 90 %.Sumitomo Shi Tan Co., Ltd. of Japan has successfully set up SPS industrial production line; large-scale production advanced ceramics material, function-graded material, electronic material, diamond cutter material and superfine crystal particle high-abrasive material are realized; because it has increased substantially performance in reducing costs, thereby cause the very big concern of investigation of materials circle and industrial community.Meanwhile, the state such as the U.S., Europe, Singapore, Korea S, China has also carried out the research and development of SPS new technology and novel material in succession.
SPS sintering technology, after the eighties in last century technical research maturation, has been widely used in the preparation process of the material such as pottery, Wimet at present, and in world wide, major part is studied colleges and universities in one's power and is all furnished with SPS plasma sintering equipment.This sintering technology has that many traditional hot pressed sintering modes are a little incomparable, and sintered sample density is high, and mechanical characteristics improves obviously.Then rarer people utilizes SPS plasma sintering technique to prepare Ti-Si-N matrix material.This experiment utilizes the plurality of advantages of SPS sintering technology, attempts preparing Ti-Si-N nanocrystalline and amorphous composite block material by new preparation method, can be directly formed to cutter and use, and has broad application prospects and important scientific research value.
Summary of the invention
The object of the present invention is to provide a kind of Ti-Si-N nanocrystalline and amorphous composite ceramics block material and preparation method thereof, this nanocomposite stupalith not only has high rigidity, high-temperature resistant and unreactiveness characteristic, has good toughness because special nanocrystalline and amorphous structure makes material simultaneously.
Its concrete technical scheme is as follows:
A kind of Ti-Si-N nanocrystalline and amorphous composite ceramic material, it is characterized in that: described composite ceramic material is composited by nanocrystalline TiN and nanocrystalline silicon nitride, nanocrystalline TiN is embedded in the silicon nitride of amorphous, the nanocrystalline granularity of TiN is 5-200 nanometer, and crystal boundary silicon nitride thickness is 0.5-50 nanometer.
In described composite ceramic material, silicon nitride content molar percentage is 1-20.%.
The preparation method of above-mentioned Ti-Si-N nanocrystalline and amorphous composite ceramic material is: step is as follows:
(1) take respectively nanocrystalline TiN and nanocrystalline silicon nitride, then both are mixed;
(2) be 10-60MPa at sintering pressure, sintering temperature is 1000-1500 DEG C, under nitrogen environment, the nanocrystalline TiN mixing and nanocrystalline silicon nitride is carried out to SPS sintering, and sintering time is controlled at 3-10 minute.
The purity that described nanocrystalline TiN and nanocrystalline silicon nitride are is greater than 99.9%.
In described composite ceramic material, the molar percentage of silicon nitride content is 1-20%.
In the present invention, due to the restriction of silicon nitride to TiN nanocrystal, make TiN crystal grain growth rate in the time of high temperature slack-off, can obtain less crystal grain.According to Hall-petch relation, hardness and the intensity of the less stupalith of grain-size are higher, and when grain-size is little during to 100 nm and following yardstick, intensity and hardness can improve a lot.Nanometer scale ceramics cutter material is still in triturating at present, and the nanocrystalline ceramics cutter material of developing is relatively less.Nanocomposite ceramic cutting tool material is the main direction developing in the future.In addition in the present invention, on the crystal boundary of TiN nanocrystalline material, add the mode that adopts superhard and low-friction coefficient combination, reach good result of use.Adopt the cutting tool that the present invention manufactures can process most difficult-to-machine material for this reason, there is good conformability and good market application foreground.
For achieving the above object, technical scheme provided by the invention is: the nano TiN of certain ingredients ratio and nano-silicon nitride are mixed, then in SPS equipment, carry out sintering, utilize high-energy and the hot properties of SPS technology, control sintering parameter and material composition, the Ti-Si-N nano bulk material of synthetic high rigidity low-friction coefficient, applies it to processing characteristics and the working durability of in cutting tool, improving cutter.
The present invention also provides above-mentioned Ti-Si-N nano block and preparation method thereof, it is characterized in that: under 10-60MPa, 1000-1500 DEG C, nitrogen environment, the nanocrystalline TiN mixing and nanocrystalline silicon nitride are carried out to sintering, sintering technology adopts discharge plasma sintering, and sintering time is controlled at 3-10 minute; After sintering, the nanocrystalline size control of TiN is in 5-200 nanometer, and silicon nitride forms amorphous.Crystal boundary silicon nitride thickness is 0.5-50 nanometer.Coating hardness is controlled at 20-40GPa, and frictional coefficient is controlled at 0.3-0.7.After naturally cooling, obtain Ti-Si-N nanocrystalline and amorphous composite ceramics block material, be processed into the shape of tool needing, obtain nanocrystalline superhard low-friction coefficient cutting tool.
The present invention utilizes the high temperature high energy characteristic of discharge plasma and nanocrystalline and amorphous complex effect to carry out the Ti-Si-N nano bulk material of synthesizing superhard low-friction coefficient as shown from the above technical solution.Conventional arc-over and medium frequency magnetron sputtering technology are the technologies of preparing of the Ti-Si-N coated material that is most widely used at present, general arc ion plating has high ionization level, easily obtain good coating adhesion, but its most fatal defect is exactly to have larger particle contamination, in addition easily form large styloid, cause the resistance to corrosion of coating poor.Magnetron sputtering has coating densification, and the feature of polluting without macrobead, has good anti-corrosion capability.But it is low that the problem of magnetron sputtering maximum is exactly ionization level, the bonding force of coating is poor.In tool sharpening process, have larger stress and friction process, conventional magnetron sputtering use properties in the time preparing superhard coating is poor for this reason.Because coated material is generally less than 10 microns, in the Tool in Cutting course of processing, will soon wear and tear, the processing life-span is limited.
The present invention takes into full account shortcoming prepared by existing Ti-Si-N material, change conventional thought, no longer using superhard low-friction coefficient Ti-Si-N material as coatings applications to cutter, but synthesize overall TiSiN block materials and apply it in solid tool, change the history without nanocrystalline and amorphous stupalith in current cutter block materials.According to Hall-petch relation, hardness and the intensity of the less stupalith of grain-size are higher, and when grain-size is little to below 100nm time, intensity and hardness can improve a lot.The activity of common nano powder is very large, and surface reaction intensity of activation is lower, in sintering process, very easily grows up, although add inhibitor, effect is still undesirable, and nanometer scale ceramics cutter material is still in triturating at present, and the sintex product of developing is relatively less.In SPS sintering process, the discharge plasma that when electrode passes into DC pulse current, moment produces, makes that sintered compact is inner respectively evengranularly self to be produced joule heating and make particle surface activation.Similar with conducting self-heating reaction synthesis method (SHS) and microwave sintering method, SPS effectively utilizes the self-heating effect of powder inside and carries out sintering.SPS sintering process can be regarded as the result of particle electric discharge, conduction heating and pressurization comprehensive action.In the present invention, utilize the high-temperature stability that silicon nitride is good, the TiN material of itself and high rigidity is carried out to combination, in sintering process, because thermodynamic process silicon nitride is diffused on the crystal boundary of TiN, hinder growing up of TiN crystal grain.Form nanocrystallinely, solve the abnormal growth problem of TiN crystal grain.
The present invention is by nanocrystalline and amorphous complex effect, plasma discharging technology and polynary compounding technology combination, and the synthetic Ti-Si-N nano bulk material with high rigidity low-friction coefficient is mainly from the viewpoint of as follows:
One, TiN is the hard coating material of industrial widespread use, it is the desirable coated material of slow cutting instrument, can alleviate adhering to of cutting edge sapwood material, reduce cutting force, increase the depth of cut, improve working accuracy, maintain the stable of cutting geometry, improve the surface quality of workpiece, be also the desired coating of worn parts simultaneously, particularly because its low adhesion tendency has been widened the application in many Wear System.Therefore be widely used in forming technique tool coating, for example the coating of sheet moulding instrument in automotive industry; Because TiN coating has that hardness is high, corrosion-resistant, viscosity is not good, chemical stability is good and the premium properties such as frictional coefficient is low, greatly improve processing performance and the use properties of tool and mould.Be prepared into block cutter material, can be increased substantially its processing characteristics.
Two, silicon nitride is a kind of important structural ceramic material.It is a kind of superhard material, itself has oilness, has high strength, resistant to elevated temperatures feature, and in stupalith, its comprehensive mechanical property is best, resistance to thermal shock performance, antioxidant property, abrasion resistance properties, corrosion resisting property are good, are first candidate materials of heat engine parts with pottery.In mechanical industry, silicon nitride ceramics is as bearing ball, roller, ball race, tool and mould, Advanced Ceramic Tool, pump plunger, axle sealing material etc.And it can also resist thermal shock, in air, be heated to more than 1000 DEG C, sharply cooling sharply heating again, can be not cracked yet.Apply it to the lubricity that can increase substantially cutter in cutter material for this reason.
Three, nanocrystalline and amorphous complex intensifying effect is one of widely used technology in thin film technique in recent years, but do not see use in block ceramic is synthetic, it is mainly to utilize the high rigidity of titanium nitride and the low-friction coefficient of silicon nitride that the present invention utilizes this effect that titanium nitride and silicon nitride are carried out compound, in performance, form complementary and strengthen, being expected to the cutter material system that exploitation makes new advances;
Four, discharge plasma sintering process is powder to be packed in the mould that the materials such as graphite make, utilize upper and lower stamping and powered electrode that specific sintering power supply and pressing pressure are put on to sintered powder, through discharge activation, thermoplastic distortion and the cooling a kind of new powder metallurgy sintered technology of producing high performance material that completes.Discharge plasma sintering has the feature of sintering in pressure process, and the pressurization in plasma body and sintering process that pulsed current produces is conducive to reduce the sintering temperature of powder.The feature of low voltage, high electric current, can make the densification of powder Fast Sintering simultaneously.It has the distinguishing features such as heat-up rate is fast, sintering time is short, weave construction is controlled, energy-conserving and environment-protective, can be used to prepare metallic substance, stupalith, matrix material, also can be used to prepare nano bulk material, amorphous block material, gradient material etc.But in cutter material, apply less.It is mainly in order to shorten sintering time that the present invention utilizes this technology, improves sintering temperature, controls the growth of titanium nitride crystal;
Therefore tool of the present invention has the following advantages: the first, and on material structure, compared with conventional TiSiN coating, prepared by the present invention is three-dimensional block materials, can better bring into play the high temperature resistant of TiSiN material and low-friction coefficient characteristic; Two, the present invention makes full use of nanocrystalline and amorphous complex effect formation titanium nitride nano crystalline substance and is embedded in amorphous silicon nitride, have larger difference with conventional cutter material, in the time of machining, cutter material has good hardness and toughness, has given full play to the feature of its tough combination; The 3rd, compared with conventional TiSiN technology of preparing, the present invention adopts plasma discharging technology can help preferably to suppress the growth of titanium nitride crystal grain, and the while can increase substantially again the density of stupalith; The 4th, from material angle, the present invention by the TiN of high rigidity and and the silicon nitride combination of low-friction coefficient, comparatively novel on material composition, do not see relevant document at present and deliver, can reach good result of use.The 5th, the present invention TiSiN is made to block materials and be applied to cutting tool and component of machine in, will increase substantially adaptability and the machinability of cutting tool; The 6th, it is simple that the present invention adopts plasma discharging technology to have device structure, is easy to control, and prospects for commercial application is good;
The superhard low-friction coefficient stupalith of the prepared Ti-Si-N of the present invention has good abrasion-proof and temperature-resistant performance, can ensure cutting tool long-term stable operation, cutting tool processing characteristics is increased substantially, processing quality is stable, working (machining) efficiency improves, and has reduced the production cost of producer.
Brief description of the drawings
Fig. 1. the nanocrystalline and amorphous structural representation of preparing for the present invention;
Fig. 2. be TiSiN block nanometer stupalith relative density variation diagram in the present invention;
Fig. 3. the TiSiN block nanometer material section pattern of preparing for the present invention;
Fig. 4. the TiSiN block nanometer material XRD figure of preparing for the present invention;
Fig. 5. the TiSiN block nanometer material high resolution pattern of preparing for the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
In the present embodiment, preparation method is: in meal mixer to high-purity Ti N nanometer powder and silicon nitride nanopowder through being fully uniformly mixed, compression moulding, in plasma discharging equipment, carry out subsequently sintering under certain temperature and pressure condition, control sintering time, sintering finishes rear acquisition Ti-Si-N block composite material.
embodiment 1:under 10MPa, 1000 DEG C, nitrogen environment, the nanocrystalline TiN mixing and nanocrystalline silicon nitride are carried out to sintering, sintering time is controlled at 3 minutes; After sintering, the nanocrystalline size control of TiN is in 5 nanometers, and silicon nitride forms amorphous.Crystal boundary silicon nitride thickness is 0.5 nanometer.Material hardness after sintering is controlled at 20GPa, and frictional coefficient is controlled at 0.3.After naturally cooling, obtain Ti-Si-N nanocrystalline and amorphous composite ceramics block material, wherein the molar percentage of crystal boundary silicon nitride is 1%, the molar percentage of nanocrystalline TiN is 99%, is processed into the shape of tool needing, and obtains nanocrystalline and amorphous compounded superhard low-friction coefficient cutting tool.
embodiment 2:under 20MPa, 1200 DEG C, nitrogen environment, the nanocrystalline TiN mixing and nanocrystalline silicon nitride are carried out to sintering, sintering time is controlled at 5 minutes; After sintering, the nanocrystalline size control of TiN is in 10 nanometers, and silicon nitride forms amorphous.Crystal boundary silicon nitride thickness is 2 nanometers.Material hardness after sintering is controlled at 25GPa, and frictional coefficient is controlled at 0.4.After naturally cooling, obtain Ti-Si-N nanocrystalline and amorphous composite ceramics block material, wherein the molar percentage of crystal boundary silicon nitride is 4%, the molar percentage of nanocrystalline TiN is 96%, is processed into the shape of tool needing, and obtains nanocrystalline and amorphous compounded superhard low-friction coefficient cutting tool.
embodiment 3:under 40MPa, 1300 DEG C, nitrogen environment, the nanocrystalline TiN mixing and nanocrystalline silicon nitride are carried out to sintering, sintering time is controlled at 6 minutes; After sintering, the nanocrystalline size control of TiN is in 50 nanometers, and silicon nitride forms amorphous.Crystal boundary silicon nitride thickness is 10 nanometers.Material hardness after sintering is controlled at 40GPa, and frictional coefficient is controlled at 0.45.After naturally cooling, obtain Ti-Si-N nanocrystalline and amorphous composite ceramics block material, wherein the molar percentage of crystal boundary silicon nitride is 8%, the molar percentage of nanocrystalline TiN is 92%, is processed into the shape of tool needing, and obtains nanocrystalline and amorphous compounded superhard low-friction coefficient cutting tool.
embodiment 4:under 60MPa, 1500 DEG C, nitrogen environment, the nanocrystalline TiN mixing and nanocrystalline silicon nitride are carried out to sintering, sintering time is controlled at 10 minutes; After sintering, the nanocrystalline size control of TiN is in 200 nanometers, and silicon nitride forms amorphous.Crystal boundary silicon nitride thickness is 50 nanometers.Material hardness after sintering is controlled at 30GPa, and frictional coefficient is controlled at 0.5.After naturally cooling, obtain Ti-Si-N nanocrystalline and amorphous composite ceramics block material, wherein the molar percentage of crystal boundary silicon nitride is 20%, the molar percentage of nanocrystalline TiN is 80%, is processed into the shape of tool needing, and obtains nanocrystalline and amorphous compounded superhard low-friction coefficient cutting tool.
embodiment 5:under 30MPa, 1400 DEG C, nitrogen environment, the nanocrystalline TiN mixing and nanocrystalline silicon nitride are carried out to sintering, sintering time is controlled at 9 minutes; After sintering, the nanocrystalline size control of TiN is in 200 nanometers, and silicon nitride forms amorphous.Crystal boundary silicon nitride thickness is 50 nanometers.Material hardness after sintering is controlled at 35GPa, and frictional coefficient is controlled at 0.7.After naturally cooling, obtain Ti-Si-N nanocrystalline and amorphous composite ceramics block material, wherein the molar percentage of crystal boundary silicon nitride is 20%, the molar percentage of nanocrystalline TiN is 80%, is processed into the shape of tool needing, and obtains nanocrystalline and amorphous compounded superhard low-friction coefficient cutting tool.
Fig. 1 is Ti-Si-N nanocrystalline and amorphous composite ceramics block material structure schematic diagram prepared by the present invention, and as can be seen from the figure, TiN Nanocrystals Embedded, in amorphous silicon nitride, because nanocrystalline yardstick is less, can improve the hardness of material.The amorphous silicon nitride of crystal boundary can improve the toughness of material.The nano ceramic material that adopts this kind of structure has good cutting ability during as cutting tool.
Fig. 2 is TiSiN block nanometer stupalith relative density variation diagram prepared by the present invention.Increase with silicon nitride content, the density of nano material declines.
Fig. 3 is TiSiN block nanometer stupalith Cross Section Morphology prepared by the present invention, and as can be seen from the figure material grains yardstick is nano level, compact structure;
Fig. 4 is TiSiN block nanometer stupalith XRD figure prepared by the present invention, and as can be seen from the figure in material, TiN exists with crystalline form, is non-crystal structure after silicon nitride sintering.
Fig. 5 is TiSiN block nanometer stupalith High-Resolution Map prepared by the present invention, on the nanocrystalline crystal boundary of TiN, is as can be seen from the figure amorphous silicon nitride, and material is typical nano-amorphous structure.
Claims (5)
1. a Ti-Si-N nanocrystalline and amorphous composite ceramic material, it is characterized in that: described composite ceramic material is composited by nanocrystalline TiN and nanocrystalline silicon nitride, nanocrystalline TiN is embedded in the silicon nitride of amorphous, the nanocrystalline granularity of TiN is 5-200 nanometer, and crystal boundary silicon nitride thickness is 0.5-50 nanometer.
2. Ti-Si-N nanocrystalline and amorphous composite ceramic material as claimed in claim 1, is characterized in that: in described composite ceramic material, the molar percentage of silicon nitride content is 1-20%.
3. prepare a method for Ti-Si-N nanocrystalline and amorphous composite ceramic material as claimed in claim 1, it is characterized in that: step is as follows: (1) takes respectively nanocrystalline TiN and nanocrystalline silicon nitride, then both is mixed; (2) be 10-60MPa at sintering pressure, sintering temperature is 1000-1500 DEG C, under nitrogen environment, the nanocrystalline TiN mixing and nanocrystalline silicon nitride is carried out to SPS sintering, and sintering time is controlled at 3-10 minute.
4. the preparation method of Ti-Si-N nanocrystalline and amorphous composite ceramic material as claimed in claim 3, is characterized in that: the purity that described nanocrystalline TiN and nanocrystalline silicon nitride are is greater than 99.9%.
5. the preparation method of Ti-Si-N nanocrystalline and amorphous composite ceramic material as claimed in claim 3, is characterized in that: in described composite ceramic material, the molar percentage of silicon nitride content is 1-20%.
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| CN112275597A (en) * | 2020-09-04 | 2021-01-29 | 江苏信轮美合金发展有限公司 | Bicycle rim anticorrosion technology |
| CN113718093A (en) * | 2021-09-03 | 2021-11-30 | 南昌航空大学 | High-speed impact large-area preparation of amorphous/nanocrystalline composite coating and preparation process thereof |
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| CN101508574A (en) * | 2009-03-25 | 2009-08-19 | 王铀 | Ceramic material with amorphous/nanocrystalline structure and method of producing the same |
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| CN107142458A (en) * | 2017-05-05 | 2017-09-08 | 重庆大学 | A kind of nano composite material, aluminum alloy die-casting die surface peening nano-composite coating and its application |
| CN112275597A (en) * | 2020-09-04 | 2021-01-29 | 江苏信轮美合金发展有限公司 | Bicycle rim anticorrosion technology |
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Application publication date: 20141203 |