CN1025879C - High-strength sintered composite ceramic body having excellent toughness and errosion resistance and process for preparation thereof - Google Patents
High-strength sintered composite ceramic body having excellent toughness and errosion resistance and process for preparation thereof Download PDFInfo
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- CN1025879C CN1025879C CN91102293A CN91102293A CN1025879C CN 1025879 C CN1025879 C CN 1025879C CN 91102293 A CN91102293 A CN 91102293A CN 91102293 A CN91102293 A CN 91102293A CN 1025879 C CN1025879 C CN 1025879C
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
To obtain the titled sintered material having high stability and excellent high-temperature strength and toughness and useful as a valve for high- pressure fluid, by arranging a ceramic layer at the surface and a specific composite layer at the inner side, forming the arranged material and sintering the product in an oxygen-free atmosphere with a hot press etc. A simple ceramic layer (A) composed of a matrix phase 1 of a ceramic and having a working surface thickness (t) of 1-40% of the total thickness (T) is prepared from a compound selected from SiC, Si3N4, sialon, ZrO2 and Al2O3. An inner composite layer (B) is produced by dispersing a dispersoid 2 selected from one or more kinds of particles and one or more kinds of whiskers or fibers of simple metal, metal carbide, metal nitride, metal silicide and metal boride in a ceramic same as the matrix of the layer A. The layers A and B are arranged, formed and sintered in an oxygen-free atmosphere under heating to obtain a high-strength sintered composite ceramic material having excellent corrosion resistance and exhibiting high toughness even if cracks 3 are generated.
Description
The present invention is that application number is CN88104561.4, and the applying date is on July 23rd, 88, and the invention exercise question is divided an application for the patent application of " a kind of high strength sintering composite ceramic body and preparation process thereof with excellent in toughness and high corrosion resistance ".
The present invention relates to the high strength sintering composite ceramic body with excellent in toughness and corrosion resistance and the preparation process thereof of a kind of water turbine and preparation water turbine, be particularly related to a kind of sintering composite ceramic body, this ceramic body can be used as the manufacturing turbine blade, or is used to make and suffers the parts (as water wheels) that serious flow cavitation corrodes and the preparation process of this ceramic body probably.
Up to the present, all use the high-temperature structural material of heat resisting alloy as turbine blade or the like.Yet these heat resisting alloy can not bear the desired higher temperature of modern large steam turbine.Therefore, in order to obtain more large steam turbine, need to use the material more heat-resisting recently than these alloys.Now, have the stupalith such as the SiC of excellent heat resistance and oxidative stability, Si
3N
4And Si-Al-ON(Si
6-ZAl
ZO
ZN
8-Z, 0＜Z＜4.2 wherein), as a kind of high-temperature structural material that can replace above-mentioned heat resisting alloy, attract much attention.
On the other hand, these stupaliths resemble this class of water wheels rotor low temperature structure material of part in addition as being suitable for making, and also attract much attention, and this rotor is easy to suffer liquid stream cavitation corrasion, or increase the wearing and tearing that cause because of dirt in the water or mud and sand content.Yet these stupaliths are very crisp as everyone knows is its shortcoming (seeing the open communique No61-192860 of Japanese I special permission).Therefore, these stupaliths never obtain practical application.
Generally have two kinds of methods to improve the toughness of stupalith: first method is the particulate of disperse metal or metallic compound in this stupalith, for example metal carbide, metal nitride, metal silicide and metal boride; Second method is the fiber or the whisker of disperse metal or metallic compound in this stupalith.These two kinds of methods can be improved toughness under the room temperature, but at high temperature, also have the bad problem of oxidative stability, because be exposed in certain atmosphere at the metal or the metallic compound of this ceramic material surfaces.Therefore, this ceramic component life-span is too short and can't practical application.So, recently ceramic particle, fiber and/or whisker to be gone in disperse in the composite ceramic body and carried out a lot of researchs, this ceramic body at high temperature may have good oxidative stability.Yet the method that has proposed can obviously be improved toughness though comprise described first kind and second method, but can not obtain lasting toughness.In other words, aspect toughness, be unsettled with the resulting product of method that has proposed.
As mentioned above, the known method that whisker, fiber and/or particulate are permeated in the stupalith can be improved its toughness.Yet the fact on the other hand is that this disperse reduces the intensity of stupalith.In other words, usually, when the toughness of stupalith increased, its intensity reduced; And when the intensity of stupalith increased, its toughness reduced.So, under the situation of some loss of intensity, improve and carried out a lot of research work aspect the toughness.On the other hand, also have some problems like this, promptly wherein disperse the stupalith of metal or metallic compound at high temperature can not use because its metallic region can be oxidized.
The objective of the invention is to solve some above-mentioned problems.
Another object of the present invention provides the high strength sintering composite ceramic body of a kind of silicon carbide that improves toughness, silicon nitride or SiAlON, and this ceramic body at high temperature and is stable and can uses also have good corrosion resistance at low temperatures.
Further object of the present invention provides the technology of the above-mentioned high strength sintering composite ceramic body of preparation.
The invention provides a kind of high strength sintering composite ceramic body, it is characterized in that it constitutes as the sinter skin of single stupalith working surface and the sintering internal layer of a composite ceramic material that contains suitable disperse material by one with excellent in toughness and corrosion resistance; The ceramic layer of single stupalith and the internal layer of composite ceramic material combine in sintering body, and the shape of disperse material is a kind of in particulate, whisker and the fiber at least.
In addition, according to the present invention, coating one deck single ceramic material surfaces layer is forming a base substrate, and with this base substrate hot pressed sintering or do not have pressure sintering and prepare above-mentioned high strength sintering composite ceramic body on the internal layer composite ceramic material.
Accompanying drawing is briefly described as follows:
Fig. 1 (A), 1(B) and 1(C) be one group of sectional schematic diagram, be used to illustrate the fracture mechanism of sintered ceramic body.
Fig. 2 (A) and 2(B) be one group of sectional schematic diagram, be used to illustrate another fracture mechanism of sintered ceramic body.
Fig. 3 shows the diagram relatively of different materials resistance to flexure.
Fig. 4 shows the diagram relatively of different materials fracture toughness.
Fig. 5 is the anti-liquid stream of a surperficial different materials cavitation corrasion ability plotted curve relatively.
Fig. 6 shows resistance to flexure and fracture toughness and according to the surface layer thickness of sintering composite ceramic body of the present invention plotted curve to the integral thickness ratio.
Fig. 7 is the axial streaming water wheels sketch that is used for embodiment 5.
Of the present invention being described in detail as follows:
Pottery has metal or the more not available superior functions of plastics. Yet pottery also has a weakness, is exactly that it is very crisp. According to the present invention, have the characteristic of pottery as the superficial layer of working face, even when ceramic body produces the crack, can also keep on the whole higher fracture toughness. And, there is earlier the ceramic body acid resistance that contains metal particle, whisker or fiber of technology sintering poor, still, ceramic body of the present invention has good acid resistance.
One of result of study of present inventor is, their find to have earlier quantity and the size of the unstable tiny flaw that produces with the mixture that is exposed to surface of ceramic body of the ceramic body toughness of technology sintering relevant.
Based on above-mentioned discovery, the characteristic (being heat resistance, corrosion resistance and intensity) that the present invention attempts to improve the disadvantage (being that toughness is bad) of pottery and don't reduces pottery.
Usually, produce the crack in ceramic body, it ruptures immediately. When some particulates of disperse in the matrix of hybrid ceramic body, just can improve the toughness of hybrid ceramic body, because the difference of physical property can absorb the energy of crack end points between these particulates and matrix. Yet the intensity of this ceramic body has but descended on the other hand. The inventor has studied the reason that this intensity descends. Found that the disperse particulate that is exposed on the surface of ceramic body makes between particulate and the ceramic matrix produces the gap and produces stress at this place concentrated, and very easily crack, even stress value very little also be like this. The result is that intensity significantly reduces. On the other hand, do at this hybrid ceramic body of use in the situation of other part of water wheels that is subject to liquid stream cavitation corrasion, this ceramic body can be subjected to water erosion on a lot of interfaces of particulate on the working face and matrix, and working surface can come off by sheet, and water wheels can't be used. In addition, well-known, the result is owing to gap between particulate and matrix has been eliminated in the reaction of particulate and matrix, and toughness can not improve so.
Fig. 1 (A), 1(B) and 1(C) be one group of sectional schematic diagram, be respectively applied for the single ceramic body of explanation, earlier the composite ceramic body of technology and the fracture mechanism of composite ceramic body of the present invention arranged.
At Fig. 1 (A), 1(B) and 1(C) in, reference numerals 1 expression ceramic matrix, 2 dispersions (herein being microgranular), 3 cracks.In other words, in the single ceramic body of Fig. 1 (A), under higher stress, produced crack 3, and this ceramic body breaks immediately.Therefore, the fracture toughness (K of single ceramic body
JC) be low.Having earlier in the technology composite ceramic body of Fig. 1 (B), the disperse material exposes, and is applied to the weak part that stress on the working surface concentrates on interface between dispersion and the matrix.Therefore, under lower stress, the ceramic body among Fig. 1 (B) breaks, so its intensity is low.But the ceramic body among Fig. 1 (B) has higher fracture toughness than the single ceramic body among Fig. 1 (A), because crack 3 expands to and walk around dispersion 2, and its expansion energy is weakened.The characteristic that has two kinds of ceramic bodies among Fig. 1 (A) and Fig. 1 (B) according to the composite ceramic body among Fig. 1 of the present invention (C).In other words, this composite ceramic body is to be that the worksheet surface layer of single stupalith (matrix 1) of t and the hybrid ceramic material internal layer with dispersion 2 constitute by thickness.In other words, the incipient crack only produces under higher stress, and the internal layer dispersion has stoped fracture propagation then, has therefore improved fracture toughness.In Fig. 1 (C), T represents the total thickness of this ceramic body.
Fig. 2 (A) expression dispersion 2 is situations about being made of fiber, and Fig. 2 (B) expression dispersion 2 is situations about being made of whisker (monocrystal).The same with the ceramic body shown in Fig. 1 (C), it is the worksheet surface layer of single stupalith (matrix 1) of t and the internal layer of a composite ceramic material that the ceramic body of Fig. 2 (A) and Fig. 2 (B) also has a thickness.Therefore, the ceramic body of Fig. 2 (B) also and the ceramic body of Fig. 1 (C) same advantage is arranged.
According to the present invention, dispersion can be a metal or alloy, because sintered ceramic body of the present invention has a full wafer stupalith or is the worksheet surface layer of single stupalith, thereby does not have the internal layer dispersion and exposes.Therefore, sintered ceramic physical efficiency of the present invention is at high temperature used, and under the situation that does not reduce its resistance to flexure, has improved fracture toughness, and good anti-liquid stream cavitation corrasion ability is arranged.Therefore, sintering composite ceramic body of the present invention can be used in valve or the water wheels that contact with the current of high speed, high pressure.
With volume is that 20% Si C powder (medium grain size is 30 μ m) is added to Si
3N
4In the powder (medium grain size is 1.0 μ m).Again in the ratio that accounts for total volume 5% with sintering aid Al
2O
3And Y
2O
3Add in the mixture.Stir and the Keading machine in these pulvis fully mixed obtain powder (a).To pure Si
3N
4The same sintering aid of middle adding obtains powder (b).The granularity of registration powder (a) makes a green briquette with the 200kgf/cm pressurization then.Use the same method and make another green briquette by powder (b).Green briquette as the powder (b) of worksheet surface layer is put on powder (a) green briquette, make the thickness t of powder be comprise powder (a) thickness total thickness T 25%.These green briquettes are put into the hotpress of using the graphite pressing mold, are 1800 ℃ in maximum temperature, and pressure is under the 300kgf/cm, and sintering makes it become sintering body (C) in nitrogen.In this embodiment, carry out hot pressed sintering, and in another embodiment, confirmed that pressureless sintering also can obtain same advantage.For relatively, prepared sintering body (A) and the Si of pure SiN
3N
4The mixed powder sintering body (B) of-20% volume SiC.From these agglomerates, obtain being used for flexuraltest and be of a size of the test piece of 4mmx4mmx4Dmm and be used to measure fracture toughness K
ICOther test pieces.According to JIS R 1610-1981, measure resistance to flexure with 4 bend test methods; When measuring fracture toughness, in any case its method of measurement will accomplish that tensile stress only puts on Si with the SENB method
3N
4Layer.In this method, the width of otch and the degree of depth are respectively 0.1mm and 0.3mm.
Fig. 3 expresses (A), (B) and (C) resistance to flexure that records of every kind of test piece of agglomerate.From Fig. 3 as seen, the resistance to flexure of agglomerate (C) is equal to or greater than the resistance to flexure of agglomerate (A), and is far longer than the resistance to flexure of agglomerate (B), and the resistance to flexure numerical value of agglomerate (B) disperses very much.
Fig. 4 expresses (A), (B) and (C) the fracture toughness K that records of every kind of test piece of agglomerate.Opposite with resistance to flexure value represented among Fig. 3, the fracture toughness of agglomerate (A) presents than low value.The resistance to flexure of sintered combined ceramic block of the present invention (C) and the undiminished trend of fracture toughness both, so it is good.
Resemble the test piece that in embodiment 1, is used to measure resistance to flexure and the same agglomerate of fracture toughness and done the test of anti-liquid stream cavitation corrasion ability.The diameter of these test pieces is 22mm, and thickness is 2mm.Test is carried out under the following conditions: frequency 6.5KHz, amplitude 120 μ m.
This test result is illustrated among Fig. 5.From Fig. 5 as seen, composite ceramic body of the present invention presents the ability of good anti-cavitation corrasion.This means composite ceramic body of the present invention as contact at a high speed, the parts of high-pressure liquid are very favorable.
Embodiment 3
Except changing pure Si
3N
4Beyond the ceramic thickness t, be used in that the same manner has made some test pieces among the embodiment 1.In other words, with changing thickness t to comprising thickness t and Si
3N
4-20% volume SiC hybrid ceramic layer thickness changes thickness t in the method for the ratio of interior total thickness T.The resistance to flexure and the fracture toughness of test piece have been measured.
Its result is illustrated in Fig. 6.From Fig. 6 as seen, when the ratio of t/T greater than 1% the time, resistance to flexure (representing with filled circles) is too low; And when the t/T ratio surpassed 45%, fracture toughness (representing with open circles) was too low.When the t/T ratio in 1～40% scope, preferably in 5～30% scopes, not only higher resistance to flexure, and obtain higher fracture toughness.Also can provide a disperse particulate layer as internal layer, cover this internal layer all surfaces and make sintering composite ceramic body of the present invention with single ceramic layer then.
In this embodiment, dispersion is Si C, but it also can be from pottery, metal, and the oxide of alloy and metal, nitride is chosen one or more and is obtained same advantage in silicon compounds and the boride.In addition, in this embodiment, granularity is 30 μ m, but granularity is all effective in 2.0～200 mu m ranges, and is more effective in 20～100 mu m ranges.
With same quadrat method among the embodiment 1, integral sintered with the composite ceramics internal layer that contains whisker and fiber single ceramic layer as working surface.The resistance to flexure and the fracture toughness of this sintering body have been measured.It the results are shown in the table 1.
The diameter of fiber and length are respectively 7～10 μ m and are about 1cm or longer.The diameter of whisker and length are respectively 0.5～1 μ m and 20～100 μ m.
Can find out obviously that from table 1 sintering body of the present invention is than good many of single ceramic sintered bodies.(table 1 is seen the literary composition back)
Fig. 7 is the sketch of used in the present embodiment Francis water wheels.These water wheels are made by 13%Cr～5%Ni cast steel.In Fig. 7, reference numerals 1 expression rotor, 2 main shafts, 3 keys, 4 shields, 5 ring seats, 6 top covers, 7 base rings, 8 draft tubes, ceramic fitting, 10 main shaft sealing devices, 11 crowns, 12 times rings, 13 guide vanes, 14 guide vane controlling rods and lining 15.
The flow passage components in the wheel week 11 of these water wheels sintering composite ceramic body member 9 that boning, this ceramic body obtains in embodiment 1, by single Si
3N
4Surface layer and Si
3N
4The composite bed of-SiC whisker constitutes.These water wheels turn round in containing the powerful current of a large amount of mud and sand, abraded quantity only for do not have ceramic component water wheels 1/10th or still less.Being connected of cast steel and sintering composite ceramic body is to utilize mechanical means and resinoid bond to finish.
In the present invention, not only use resin binder, and realize connecting with brazing, mechanical connection or the like.
Ceramic fitting not only can be embedded on wheel week, and can be embedded on other flow passage components (as rotor).
Table 1
Resistance to flexure KiC
Single ceramic layer composite ceramic layer sintering condition
KgS/mm
2MN/m 3/2
Si
3N
469 5.0
Si
3N
4Si
3N
41800 ℃ 67 7.8 of-20% volume SiC whisker
Si
3N
4Si
3N
4-20% volume SiC fiber 300Kg/cm
268 7.8
Si
3N
4Si
3N
4-20% volume W fiber hot pressing 70 8.2
Si
3N
4Si
3N
4-20% volume C fiber 66 7.5
SiC 2100℃ 75 3.5
SiC SiC-20% volume SiC whisker 300Kgf/cm
272 6.0
SiC SiC-20% volume SiC fiber hot pressing 72 5.7
Si
5AlON
770 5.0
Si
5AlON
7Si
5AlON
71750 ℃ 68 7.7 of-20% volume SiC particulate
300Kgf/cm
2
Si
5AlON
7Si
5AlON
7-20% volume SiC whisker hot pressing 67 7.8
ZrO
21500℃ 70.3 7.0
ZrO
2ZrO
2-20% volume Al
2O
3Fiber does not have pressure 69.7 8.5
ZrO
2ZrO
2-20% volume Sic whisker 69.8 8.7
Al
2O
342 2.0
Al
2O
3Al
2O
3-20% volume Al
2O
31500 ℃ 40 3.5 of fiber
Al
2O
3Al
2O
3-20% volume TiC particulate does not have pressure 40 3.7
Claims (1)
1, a kind of water turbine, its flow passage components comprise rotor (1), volute (4), seat ring (5), top cover (6), base ring (7), guide vane (13) and draft tube (8), its rotor (1) is by crown (11), following ring (12) and working blade are formed, and it is characterized in that, coat composite ceramic layer on the surface, position that is subject to cavitation corrosion and abrasion of flow passage components, the agglomerant that this composite ceramic layer is made of single stupalith is done the top layer and is formed by containing the internal layer that disperse material and sintered ceramic material constitute, top layer and internal layer are sintered to one, and described disperse material is a particle, a kind of in whisker and the fiber.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62185266A JPS6428282A (en) | 1987-07-24 | 1987-07-24 | High-strength sintered composite ceramic material having excellent toughness and corrosion resistance and production thereof |
| JP185266/87 | 1987-07-24 |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN198888102293A Division CN88102293A (en) | 1987-04-16 | 1988-04-16 | A kind of method of producing granulated fertilizer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1057505A CN1057505A (en) | 1992-01-01 |
| CN1025879C true CN1025879C (en) | 1994-09-07 |
Family
ID=16167818
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN91102293A Expired - Fee Related CN1025879C (en) | 1987-07-24 | 1988-07-23 | High-strength sintered composite ceramic body having excellent toughness and errosion resistance and process for preparation thereof |
| CN88104561A Pending CN1032535A (en) | 1987-07-24 | 1988-07-23 | A kind of high strength sintering composite ceramic body and preparation technology thereof with excellent in toughness and corrosion resistance |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN88104561A Pending CN1032535A (en) | 1987-07-24 | 1988-07-23 | A kind of high strength sintering composite ceramic body and preparation technology thereof with excellent in toughness and corrosion resistance |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JPS6428282A (en) |
| CN (2) | CN1025879C (en) |
| IN (1) | IN169656B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2660346B2 (en) * | 1987-09-17 | 1997-10-08 | 株式会社豊田中央研究所 | Ceramic composite materials |
| CN100439286C (en) * | 2006-08-29 | 2008-12-03 | 中材高新材料股份有限公司 | Method for preparing super high temperature complex phase ceramic ZrB2-ZrC-SiC near to zero ablation |
| CN100400468C (en) * | 2006-09-06 | 2008-07-09 | 哈尔滨工业大学 | Alpha-sialon composite ceramic material and preparation method thereof |
| CN101172877B (en) * | 2006-10-16 | 2010-06-16 | 宁波大学 | Process for manufacturing multicomponent combination toughness reinforcing silicon carbide ceramic including crystal whisker and fibre |
| FR2945458B1 (en) | 2009-05-13 | 2011-06-17 | Sanofi Aventis | HIGH PRESSURE HOMOGENIZATION WITH A SILICON NITRIDE VALVE |
| CN102476494B (en) * | 2011-09-05 | 2013-08-07 | 深圳光启高等理工研究院 | Dielectric substrate manufacturing method |
| PL421648A1 (en) | 2017-05-19 | 2018-12-03 | General Electric Company | Removal of a kevlar wrapper from a fan housing |
| CN107324848B (en) * | 2017-07-21 | 2020-06-26 | 湖南中科光电有限公司 | Water-resistant zirconia ceramics protector and optical fiber ceramic ferrule |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55113680A (en) * | 1979-02-19 | 1980-09-02 | Tokyo Shibaura Electric Co | Manufacture of ceramic fiber having compounded layer |
| JPS5895648A (en) * | 1981-11-30 | 1983-06-07 | トヨタ自動車株式会社 | Manufacture of one-direction reinforced silicon carbide ceramic body |
| JPS59156970A (en) * | 1983-02-23 | 1984-09-06 | 黒崎窯業株式会社 | Refractory brick |
| JPS6246965A (en) * | 1985-08-23 | 1987-02-28 | 黒崎窯業株式会社 | Sic-si3n4 base composite ceramics and manufacture |
| SE8602750D0 (en) * | 1986-06-19 | 1986-06-19 | Sandvik Ab | Laminated ceramic sinter body |
-
1987
- 1987-07-24 JP JP62185266A patent/JPS6428282A/en active Pending
-
1988
- 1988-07-11 IN IN578/CAL/88A patent/IN169656B/en unknown
- 1988-07-23 CN CN91102293A patent/CN1025879C/en not_active Expired - Fee Related
- 1988-07-23 CN CN88104561A patent/CN1032535A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6428282A (en) | 1989-01-30 |
| CN1057505A (en) | 1992-01-01 |
| CN1032535A (en) | 1989-04-26 |
| IN169656B (en) | 1991-11-30 |
| JPH0565470B1 (en) | 1993-09-17 |
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