CN103992100A - Process for preparing layered silicon nitride ceramic with high strength and high toughness by utilizing component gradient design - Google Patents
Process for preparing layered silicon nitride ceramic with high strength and high toughness by utilizing component gradient design Download PDFInfo
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- CN103992100A CN103992100A CN201410252064.0A CN201410252064A CN103992100A CN 103992100 A CN103992100 A CN 103992100A CN 201410252064 A CN201410252064 A CN 201410252064A CN 103992100 A CN103992100 A CN 103992100A
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Abstract
The invention aims to provide a process for preparing layered silicon nitride ceramic with high strength and high toughness by utilizing component gradient design, which comprises the following steps: (1), selecting alpha-Al2O3 and Y2O3 as sintering aids; (2), burdening, respectively weighing commercially available alpha-Si3N4, alpha-Al2O3 and Y2O3 powder according to the proportion of a burden sheet, taking absolute ethyl alcohol as a dispersion medium and a silicon nitride ball with the diameter of 2-3 mm as a grinding medium, ball-milling and uniformly mixing in a nylon tank, and controlling the granularity of a mixed material at about D50=0.2 mu m; (3), forming, adding a 5-9 wt% of polyving akohol (PVA) solution with the concentration of 3 wt% as a temporary binder into the mixed powder, adding various materials with corresponding numbers according to the charging sequence in the picture 1, pressing into blocky structures by using an isostatic pressing machine below 100 MPa, and controlling the thickness of each layer after being pressed at about 2 mm; and (4), sintering.
Description
Technical field
The present invention relates to a kind of technique of utilizing composition gradient design to prepare high-strength and high-ductility layered nitride silicon pottery, belong to field of new.
Background technology
Silicon nitride ceramics has good room temperature and high-temperature mechanical property, intensity is high, density is little, erosion resistant, thermal shock resistance is strong, resist chemical, low thermal coefficient of expansion, being research structured material the most extensively and profoundly in structural ceramics, is also the main candidate material of ceramic engine and other thermal structure part, cutting tool, wearing piece etc.It is the study hotspot of structural ceramic material always.But, because of the fragility defect of silicon nitride ceramics, being improved thoroughly always, this has limited its practical ranges greatly.The toughness that how to improve silicon nitride ceramics is still Si
3n
4the focus of ceramic research.Being engaged at present the scholar of silicon nitride ceramics research in order to improve the toughness of silicon nitride ceramics, is mainly to have proposed a lot of Si from Microstructure Design and two aspects of crystal boundary composition design
3n
4the method for toughening of pottery.Such as from Microstructure Design angle, there are yttria stabilizator, whisker or fiber reinforced, ZrO
2transformation toughening and utilize column β-Si
3n
4crystal grain from toughness reinforcing etc.; From crystal boundary, form design angle, design the crystal boundary of mechanics excellent performance in conjunction with equating.But the toughening effect that these approach obtain is still limited, Chinese scholars can produce larger toughness from the laminate structure of shell and gains enlightenment in recent years, has proposed ceramic laminate structure composite toughening.Mainly between ceramic layer, to design the relatively weak interface layer of " soft " of one deck, such as graphite, boron nitride etc.This strong-laminate structure of weak interface alternate combinations in, the crack propagation on strong interface is during to weak interface layer, crackle will deflect, energy is partially absorbed, thus generation toughening effect.This strong-that weak interface knot is studied in ceramic laminate structure toughening mechanisms is more, and successfully prepares many oxide and non-oxidized substance layered composite ceramic material, for example, aspect silicon nitride ceramic material, existing people has prepared Si
3n
4/ BN stratified composite, makes the toughness of silicon nitride obtain larger raising.But the laminate structure composite toughening approach of stupalith except above-mentioned strong-weak interface replaces the structure of combination, can also be designed in theory strong-strong interfacial bond.This strong-toughening mechanism of strong interface laminate structure is the difference between the thermal expansivity utilizing between each layer, on interfacial layer, produce stress effect, when crack propagation is during to interface, first to overcome stress, and then continue to expand, these stress that design are in advance the energy of energy additional absorbent crack propagation just, thereby plays toughening effect.Utilize this machine-processed recent years abroad to have people to carry out trial and obtained comparatively significant toughening effect preparing zirconium white/alumina composite material.But aspect silicon nitride material both at home and abroad all nobody carry out this strong-the toughness reinforcing research of strong interface layer.Because on the one hand, this design based on interfacial layer stress need to be adjusted the thermal expansivity of each bed interface, if the thermal expansion coefficient difference of interface two boundary layers is too greatly, easily cause interface peel, the too little stress of difference DeGrain, toughening effect is also just undesirable.On the other hand, also to avoid excessive because of each layer of composition gradient, cause sintering temperature difference too large, burn till and control difficulty.The two the difference of average coefficient of expansion of zirconium white and aluminum oxide is relatively little, refer to table 1, when controlling the mean thermal expansion coefficients of each layer with composition gradient, relatively easy, the splitting causing thus is also easier to avoid, and it is unanimously also relatively easy to control the firing temperature of each layer;
The mean thermal expansion coefficients of the various materials of table 1 (25 ℃-700 ℃)
| Material category | Mean thermal expansion coefficients, * 10 -6/℃ |
| Silicon nitride | 2.7 |
| Aluminum oxide | 7.8 |
| 3mol% yttrium stable zirconium oxide | 9.6 |
| Yttrium oxide | 7.0 |
| Magnesium oxide | 13 |
And utilize nitride silicon based ceramic layered of this mechanism preparation, at this, need to overcome more difficulty aspect two.Because the thermal expansivity of silicon nitride is smaller, be about 2.7 * 10
-6/ ℃, silicon nitride often selects the oxide compounds such as aluminum oxide, zirconium white, yttrium oxide, magnesium oxide, rare earth oxide as sintering aid when sintering, and the relative silicon nitride of the thermal expansivity of these oxide compounds differs greatly, and refers to table 1.This larger thermal expansion coefficient difference, in the laminate structure of strong-strong interface, easily produces and peels off layering at interlayer, and the sintering temperature difference of composition gradient layer is also relatively large simultaneously.Therefore, if prepare strong-strong interface layered nitride silicon stupalith, adjustment that need to be to the design of the selection of sintering aid, each layer of coefficient of expansion, calcining system, these aspects act on simultaneously, could between interfacial layer, produce stress effect, avoid occurring that stress is excessive, inhomogeneous peeling off of causing simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of technique of utilizing composition gradient design to prepare high-strength and high-ductility layered nitride silicon pottery.Its technical scheme is: the selection of (1) sintering aid.Consider that firing temperature controls and avoid the reason of splitting, select the close α-Al of mean thermal expansion coefficients
2o
3and Y
2o
3proper as sintering aid; While making prepare by force-strong interface stratiform flexible silicon nitride ceramic of sintering aid with yttrium stable zirconium oxide, because zirconic volume change is relatively large in burning till, at interlayer, more easily produces and peel off.(2) batching.By commercially available α-Si
3n
4, α-Al
2o
3, Y
2o
3powder according to the proportioning of table 2, is done dispersion medium with dehydrated alcohol respectively, and the silicon nitride ball of diameter 2-3mm is made grinding medium, ball milling in nylon tank, and the granularity of controlling material is D50=0.2 μ m left and right;
Table 2 allocation sheet (%)
| Numbering | α-Si 3N 4 | α-Al 2O 3 | Y 2O 3 |
| 0# | 82-85 | 7-10 | 6-10 |
| 1# | 85-88 | 7-10 | 6-10 |
| 2# | 89-92 | 4-9 | 4-9 |
(3) moulding.In above-mentioned mixed powder, add the polyvinyl alcohol that 5wt%-9wt% concentration is 3wt% (PVA) solution as interim bonding agent.According to the loading sequence in schematic diagram 1, add material corresponding to various numberings, with being pressed into bulk under isostatic pressing machine 100MPa, after the pressure of every one deck, thickness need be controlled the left and right into 2mm.(4) burn till.The sample suppressing is put into gas pressure sintering stove gas pressure sintering, and system is: RT-600 ℃, 40min, vacuum; 600 ℃-1030 ℃, 40min, N
2pressure 0.5MPa; 1030 ℃-1400 ℃, 45min, N
2pressure 0.5MPa; 1400 ℃-1400 ℃, 30min, N
2pressure 0.5MPa; 1400-1600 ℃, 60min, N
2pressure 1.5MPa; 1600 ℃, 30min, N
2pressure 1.5MPa; 1600 ℃-1690 ℃, 45min, N
2pressure 6MPa; 1690 ℃-1690 ℃, 40min, N
2pressure 6MPa; 1690 ℃-1750 ℃, 30min, N
2pressure 7MPa; 1750 ℃-1750 ℃, 60min, N
2pressure 7Mpa; Then naturally cooling, can obtain the layered nitride silicon stupalith of high-strength and high-ductility.
Accompanying drawing explanation
Accompanying drawing 1 title: the layered nitride silicon stupalith schematic diagram based on composition gradient design; In figure, be numbered 0#, 1#, 2# each layer of corresponding raw material proportion of composing should with allocation sheet in ratio be mapped.
Embodiment
Embodiment 1:
Step 1: by commercially available α-Si
3n
4, α-Al
2o
3, Y
2o
3powder according to the proportioning of table 3, is done dispersion medium with dehydrated alcohol respectively, and the silicon nitride ball that diameter is 2-3mm is made grinding medium, ball milling in nylon tank, and the granularity of controlling material is D50=0.2 μ m left and right;
Table 3 allocation sheet (%)
| Numbering | α-Si 3N 4 | α-Al 2O 3 | Y 2O 3 |
| 0# | 85 | 8 | 7 |
| 1# | 87 | 7 | 6 |
| 2# | 90 | 6 | 4 |
Step 2: will add the polyvinyl alcohol that 5wt% concentration is 3wt% (PVA) solution in above-mentioned three kinds of material that mix as interim bonding agent.According to the loading sequence in schematic diagram 1, add material corresponding to various numberings, with being pressed into bulk under isostatic pressing machine 100MPa, after the pressure of every one deck, thickness need be controlled the left and right into 2mm;
Step 3: the sample suppressing is put into gas pressure sintering stove gas pressure sintering, and system is: RT-600 ℃, 40min, vacuum; 600 ℃-1030 ℃, 40min, N
2pressure 0.5MPa; 1030 ℃-1400 ℃, 45min, N
2pressure 0.5MPa; 1400 ℃-1400 ℃, 30min, N
2pressure 0.5MPa; 1400-1600 ℃, 60min, N
2pressure 1.5MPa; 1600 ℃, 30min, N
2pressure 1.5MPa; 1600 ℃-1690 ℃, 45min, N
2pressure 6MPa; 1690 ℃-1690 ℃, 40min, N
2pressure 6MPa; 1690 ℃-1750 ℃, 30min, N
2pressure 7MPa; 1750 ℃-1750 ℃, 60min, N
2pressure 7MPa; Then naturally cooling, can obtain the layered nitride silicon stupalith of high-strength and high-ductility.
Embodiment 2:
Step 1: by commercially available α-Si
3n
4, α-Al
2o
3, Y
2o
3powder according to the proportioning of table 4, is done dispersion medium with dehydrated alcohol respectively, and the silicon nitride ball that diameter is 2-3mm is made grinding medium, ball milling in nylon tank, and the granularity of controlling material is D50=0.2 μ m left and right;
Table 4 allocation sheet (%)
| Numbering | α-Si 3N 4 | α-Al 2O 3 | Y 2O 3 |
| 0# | 82 | 10 | 8 |
| 1# | 85 | 8 | 7 |
| 2# | 89 | 6 | 5 |
Step 2: will add the polyvinyl alcohol that 6wt% concentration is 3wt% (PVA) solution in above-mentioned three kinds of material that mix as interim bonding agent.According to the loading sequence in schematic diagram 1, add material corresponding to various numberings, with being pressed into bulk under isostatic pressing machine 100MPa, after the pressure of every one deck, thickness need be controlled the left and right into 2mm;
Step 3: the sample suppressing is put into gas pressure sintering stove gas pressure sintering, and system is: RT-600 ℃, 40min, vacuum; 600 ℃-1030 ℃, 40min, N
2pressure 0.5MPa; 1030 ℃-1400 ℃, 45min, N
2pressure 0.5MPa; 1400 ℃-1400 ℃, 30min, N
2pressure 0.5MPa; 1400-1600 ℃, 60min, N
2pressure 1.5MPa; 1600 ℃, 30min, N
2pressure 1.5MPa; 1600 ℃-1690 ℃, 45min, N
2pressure 6MPa; 1690 ℃-1690 ℃, 40min, N
2pressure 6MPa; 1690 ℃-1750 ℃, 30min, N
2pressure 7MPa; 1750 ℃-1750 ℃, 60min, N
2pressure 7MPa; Then naturally cooling, can obtain the layered nitride silicon stupalith of high-strength and high-ductility.
Embodiment 3:
Step 1: by commercially available α-Si
3n
4, α-Al
2o
3, Y
2o
3powder according to the proportioning of table 5, is done dispersion medium with dehydrated alcohol respectively, and the silicon nitride ball that diameter is 2-3mm is made grinding medium, ball milling in nylon tank, and the granularity of controlling material is D50=0.2 μ m left and right;
Table 5 allocation sheet (%)
| Numbering | α-Si 3N 4 | α-Al 2O 3 | Y 2O 3 |
| 0# | 84 | 9 | 7 |
| 1# | 88 | 7 | 5 |
| 2# | 92 | 4 | 4 |
Step 2: will add the polyvinyl alcohol that 7wt% concentration is 3wt% (PVA) solution in above-mentioned three kinds of material that mix as interim bonding agent.According to the loading sequence in schematic diagram 1, add material corresponding to various numberings, with being pressed into bulk under isostatic pressing machine 100MPa, after the pressure of every one deck, thickness need be controlled the left and right into 2mm;
Step 3: the sample suppressing is put into gas pressure sintering stove gas pressure sintering, and system is: RT-600 ℃, 40min, vacuum; 600 ℃-1030 ℃, 40min, N
2pressure 0.5MPa; 1030 ℃-1400 ℃, 45min, N
2pressure 0.5MPa; 1400 ℃-1400 ℃, 30min, N
2pressure 0.5MPa; 1400-1600 ℃, 60min, N
2pressure 1.5MPa; 1600 ℃, 30min, N
2pressure 1.5MPa; 1600 ℃-1690 ℃, 45min, N
2pressure 6MPa; 1690 ℃-1690 ℃, 40min, N
2pressure 6MPa; 1690 ℃-1750 ℃, 30min, N
2pressure 7MPa; 1750 ℃-1750 ℃, 60min, N
2pressure 7MPa; Then naturally cooling, can obtain the layered nitride silicon stupalith of high-strength and high-ductility.
Claims (5)
1. a technique of utilizing composition gradient design to prepare high-strength and high-ductility layered nitride silicon pottery, it is characterized in that adopting following steps: the selection of (1) sintering aid, consider that firing temperature controls and avoid the reason of splitting, select the close α-Al of mean thermal expansion coefficients
2o
3and Y
2o
3proper as sintering aid; While making prepare by force-strong interface stratiform flexible silicon nitride ceramic of sintering aid with yttrium stable zirconium oxide, because zirconic volume change is relatively large in burning till, at interlayer, more easily produces and peel off; (2) batching, by commercially available α-Si
3n
4, α-Al
2o
3, Y
2o
3powder according to the proportioning of table 2, is done dispersion medium with dehydrated alcohol respectively, and the silicon nitride ball of diameter 2-3mm is made grinding medium, ball milling in nylon tank, and the granularity of controlling material is D50=0.2 μ m left and right; (3) moulding, in above-mentioned mixed powder, add the polyvinyl alcohol that 5wt%-9wt% concentration is 3wt% (PVA) solution as interim bonding agent, according to the loading sequence in Fig. 1, add material corresponding to various numberings, with being pressed into bulk under isostatic pressing machine 100MPa, after the pressure of every one deck, thickness need be controlled the left and right into 2mm; (4) burn till, the sample suppressing is put into gas pressure sintering stove gas pressure sintering, and system is: RT-600 ℃, 40min, vacuum; 600 ℃-1030 ℃, 40min, N
2pressure 0.5MPa; 1030 ℃-1400 ℃, 45min, N
2pressure 0.5MPa; 1400 ℃-1400 ℃, 30min, N
2pressure 0.5MPa; 1400-1600 ℃, 60min, N
2pressure 1.5MPa; 1600 ℃, 30min, N
2pressure 1.5MPa; 1600 ℃-1690 ℃, 45min, N
2pressure 6MPa; 1690 ℃-1690 ℃, 40min, N
2pressure 6MPa; 1690 ℃-1750 ℃, 30min, N
2pressure 7MPa; 1750 ℃-1750 ℃, 60min, N
2pressure 7MPa, naturally cooling then, can obtain the layered nitride silicon stupalith of high-strength and high-ductility.
2. the technique of utilizing composition gradient design to prepare high-strength and high-ductility layered nitride silicon pottery according to claim 1, it is characterized in that: the proportion scale of each raw material in (2) in table 2, need be according to the ratio control in table, such ratio has guaranteed that the mean thermal expansion coefficients between each layer keeps a rational gradient each other, guarantees that the firing temperature of each layer can not fluctuate too large simultaneously.
3. the technique of utilizing composition gradient design to prepare high-strength and high-ductility layered nitride silicon pottery according to claim 1, it is characterized in that: in (3), say the design of mentioning Fig. 1 laminate structure, it is the key that forms stress interfacial layer, and what must be outer field mean thermal expansion coefficients compared with internal layer be little, and stack design only in this way could guarantee to produce the toughness reinforcing effect of significant stress.
4. the technique of utilizing composition gradient design to prepare high-strength and high-ductility layered nitride silicon pottery according to claim 1, it is characterized in that: in (4) after the pressure of each layer gauge control in about 2mm, the thickness of each layer has impact comparatively significantly to producing the toughness reinforcing effect of stress, experimental result shows, after each lamination, gauge control is in 2mm left and right, and the toughening effect that burns till rear generation is more remarkable.
5. the technique of utilizing composition gradient design to prepare high-strength and high-ductility layered nitride silicon pottery according to claim 1, is characterized in that: the calcining system of the establishment in (5): for: RT-600 ℃, 40min, vacuum; 600 ℃-1030 ℃, 40min, N
2pressure 0.5MPa; 1030 ℃-1400 ℃, 45min, N
2pressure 0.5MPa; 1400 ℃-1400 ℃, 30min, N
2pressure 0.5MPa; 1400-1600 ℃, 60min, N
2pressure 1.5MPa; 1600 ℃, 30min, N
2pressure 1.5MPa; 1600 ℃-1690 ℃, 45min, N
2pressure 6MPa; 1690 ℃-1690 ℃, 40min, N
2pressure 6MPa; 1690 ℃-1750 ℃, 30min, N
2pressure 7MPa; 1750 ℃-1750 ℃, 60min, N
2pressure 7MPa, then naturally cooling; This calcining system has been considered the adjustment to the difference of each layer of calcining system, guarantees that each layer all reached comparatively fine and close sintering degree.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105420474A (en) * | 2015-11-18 | 2016-03-23 | 宁波金鹏高强度紧固件有限公司 | Machining method for long nut |
| CN105459564A (en) * | 2015-11-23 | 2016-04-06 | 哈尔滨工业大学 | Preparation method of interface self-toughening Si3N4/SiC laminar ceramic material |
| CN107337450A (en) * | 2017-06-30 | 2017-11-10 | 广东新秀新材料股份有限公司 | High tenacity ceramics, its preparation method and application |
| CN107954722A (en) * | 2017-12-05 | 2018-04-24 | 广东工业大学 | One kind prepares Si by self-diffusion3N4The method of functionally gradient material (FGM) |
| CN109661384A (en) * | 2016-07-28 | 2019-04-19 | 于利奇研究中心有限公司 | Enhance the method and ceramics of crystalline ceramics |
| CN109851370A (en) * | 2019-03-22 | 2019-06-07 | 常德科锐新材料科技有限公司 | The production method of high-intensitive high thermal conductivity silicon nitride board |
| CN110092645A (en) * | 2019-05-24 | 2019-08-06 | 广东工业大学 | A kind of composite ceramic substrate and preparation method thereof |
| CN110590378A (en) * | 2019-09-19 | 2019-12-20 | 太原科技大学 | Preparation method of homogenized and distributed silicon nitride ceramic material |
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| CN105459564A (en) * | 2015-11-23 | 2016-04-06 | 哈尔滨工业大学 | Preparation method of interface self-toughening Si3N4/SiC laminar ceramic material |
| CN109661384A (en) * | 2016-07-28 | 2019-04-19 | 于利奇研究中心有限公司 | Enhance the method and ceramics of crystalline ceramics |
| CN107337450A (en) * | 2017-06-30 | 2017-11-10 | 广东新秀新材料股份有限公司 | High tenacity ceramics, its preparation method and application |
| CN107954722B (en) * | 2017-12-05 | 2021-05-04 | 广东工业大学 | Method for preparing Si3N4 gradient material through self-diffusion |
| CN107954722A (en) * | 2017-12-05 | 2018-04-24 | 广东工业大学 | One kind prepares Si by self-diffusion3N4The method of functionally gradient material (FGM) |
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| CN110092645A (en) * | 2019-05-24 | 2019-08-06 | 广东工业大学 | A kind of composite ceramic substrate and preparation method thereof |
| CN110092645B (en) * | 2019-05-24 | 2021-07-13 | 广东工业大学 | Composite ceramic substrate and preparation method thereof |
| CN110590378A (en) * | 2019-09-19 | 2019-12-20 | 太原科技大学 | Preparation method of homogenized and distributed silicon nitride ceramic material |
| CN110723988A (en) * | 2019-11-04 | 2020-01-24 | 景德镇陶瓷大学 | Gradient coating prestress reinforced building ceramic product and preparation method thereof |
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