CN110183229A - A kind of Ti with low-temperature cracks self-healing capability2Al(1-x)SnxC ceramics repair phase raw powder's production technology - Google Patents
A kind of Ti with low-temperature cracks self-healing capability2Al(1-x)SnxC ceramics repair phase raw powder's production technology Download PDFInfo
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Abstract
The invention discloses a kind of low temperature self-healing ceramics to repair phase raw powder's production technology, comprising: presses Ti:Al:Sn:TiC=1:(1-x): the molar ratio ingredient of x:0.9, the step of mixing, be pressed into briquetting after ball milling；Briquetting is placed in high temperature furnace, under vacuum or argon atmosphere, furnace temperature is risen to 1200~1400 DEG C, keeps the temperature the step of 5~60min obtains sintered body；And the step of sintered body is crushed, is milled to obtain the reparation phase powder.The invention also discloses the low temperature self-healing ceramics as made from the preparation method to repair phase powder and block materials.Low temperature self-healing ceramics obtained of the invention repair phase powder, have lower healing temperature and healing time.
Description
Technical field
The present invention relates to advanced ceramics technical fields, and in particular to a kind of with low-temperature cracks self-healing capability
Ti2Al(1-x)SnxC ceramic material and preparation method thereof.
Background technique
Advanced ceramics material is due to its fine structure composition and high intensity, high rigidity, high temperature resistant, anticorrosive, wear-resisting etc.
A series of good characteristics are widely used in the every field such as aerospace, electronics, machinery, biomedicine.And in structural ceramics
Preparation, in processing and use process, the appearance of crackle is very common, and the decaying of intensity caused by crackle and reliability reduce etc.
Problem significantly limits the practical application of material.Therefore, improve the brittleness of ceramic material, increase intensity to improve it in reality
Reliability in use, becoming it being capable of widely applied key.Around the brittleness for improving ceramic material and intensity is improved, at present
Two methods are concentrated mainly on, one is by increasing fiber, particle etc. plays the toughness of increase ceramic material, another method
It is exactly to manufacture and design the ceramic material with self-healing performance.
About the research and development of self-healing ceramic material, just start to be concentrated mainly on UO2,Al2O3Equal ceramics, but heal condition
Compare harsh, the temperature of healing is at 1400 DEG C or more, and close to the fusing point of such oxide ceramics, main healing mechanism is with reheating
It ties similar.Simultaneously because healing temperature is higher, there are problems that crystal grain is seriously grown up, greatly reduce the property of ceramic material
Energy.In recent years, the researchers such as Japan Kotoji have found, SiC or Si3N4This kind of material passes through oxidation reaction, the oxygen of formation
Change product SiO2Crackle, the crackle in repair materials can effectively be filled up.It is also possible to be added to Al as phase is repaired2O3, not
Come in the oxide ceramics such as stone, repairs oxide ceramics, so that the temperature of healing decreases, but still at 1200-1400 DEG C
Within high temperature range；And work as temperature and be lower than 1200 DEG C, then need tens hours even several hundred hours to carry out healed cracks.How into one
Step reduces healing temperature and reduces healing time, and it is extremely urgent to develop the new reparation particle with self-healing function.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation sides that a kind of low-temperature cracks self-healing ceramics repair phase powder
Method, compared with prior art, when repairing phase powder by the ceramics that this method is prepared has lower healing temperature and healing
Between, it can crackle in (< 1000 DEG C) reparations ceramics at low temperature.
Another object of the present invention is to provide the low-temperature cracks self-healing ceramics reparations that aforementioned preparation process is prepared
Phase powder.
Another object of the present invention is to provide a kind of low temperature self-healing ceramic block material.
In order to solve the above-mentioned technical problems, the present invention provides low temperature self-healing ceramics to repair phase raw powder's production technology,
Include:
By Ti:Al:Sn:TiC=1:(1-x): the molar ratio ingredient of x:0.9, mixing, are pressed into the step of briquetting at ball milling；
Briquetting is placed in high temperature furnace, under vacuum or argon atmosphere, furnace temperature is risen to 1200~1400 DEG C, heat preservation
5~60min obtains the step of sintered body；And
The step of sintered body is crushed, is milled to obtain the reparation phase powder；
Wherein: 0≤x≤1.
In the present invention, Ti, Al, Sn, TiC as raw material are granular material.
As a preferred embodiment of the present invention, that raw material is mixed on ball mill dry-mixed 1~4 after ingredient is small
When.
As a preferred embodiment of the present invention, using agate ball as abrasive media when ball milling.
As a preferred embodiment of the present invention, the mixture after ball milling is pressed under 10~100MPa pressure
Block.
As a preferred embodiment of the present invention, the heating rate of high temperature furnace is 15~40 DEG C/min.
The present invention also provides the low temperature self-healing ceramics being prepared by aforementioned preparation process to repair phase powder, synthesis
Ti2Al(1-x)SnxC powder is that tiny plate is brilliant, and the partial size of powder is less than 10 μm.The powder body material can be added to other potteries
In porcelain, such as aluminium oxide (Al2O3), zirconium oxide (ZrO2) etc., as the reparative factor of the oxide ceramics, so that it has low temperature
Self-repair function.
It is to repair phase powder by ceramics above-mentioned to cause the present invention also provides a kind of low temperature self-healing ceramic block material
Densification and obtain.Wherein, densification can be used this field and disclose known any means progress, for example, sintering, pressure
System, hot isostatic pressing, isostatic cool pressing.
The beneficial effects of the present invention are:
1. raw materials are at low cost.Raw materials are titanium valve (Ti), aluminium powder (Al), glass putty (Sn) and carbonized titanium powder
(TiC), there is sale in the market, it is cheap.
2. preparation process is simple, the period is short.Process flow of the invention is simple, in conventional vacuum drying oven, in vacuum gas
Under atmosphere or argon atmosphere, in the short time, at a temperature of 1200-1400 DEG C synthesize high-purity MAX powder, reduce energy consumption and
The preparation cost of powder.
3. product purity is high.Referring to Fig. 1, there is Ti in XRD diffracting spectrum2Al(1-x)SnxThe diffraction maximum of C, it was demonstrated that
Ti2Al(1-x)SnxThe presence of C phase；Exist in diffracting spectrum without impurity phases such as TiC, shows that the product purity obtained is high.And it obtains
The particle fine uniform obtained.
4. the Sn element of low melting point can be added in selfreparing powder of the invention, so that the associative key in MAX phase weakens, add
Its fast oxygenolysis fills repair crack so as to form oxide under conditions of being lower than 1000 DEG C.Referring to fig. 2, with
The increase of Sn content, Ti2Al(1-x)SnxThe main reaction temperature of C powder is reduced to 680 DEG C or so from 900 DEG C.
5. selfreparing powder of the invention both can be used as other ceramics such as aluminium oxide (Al2O3), zirconium oxide (ZrO2) etc.
The reparative factor of oxide ceramics can also directly densify into block materials, repair splitting for ceramic material by oxidizing thermal treatment
Line and other defects.
Detailed description of the invention
Fig. 1 is the XRD powder diffraction pattern of the reparation phase powder synthesized in embodiment 1-3；
Fig. 2 is Ti2AlxSn(1-x)The differential thermal analysis curve that C powder aoxidizes in air；
Fig. 3 (a) is the Ti synthesized in embodiment 12The SEM picture of AlC powder body material；
Fig. 3 (b) is Ti prepared by embodiment 12AlC block materials are heat-treated the SEM after 3 h at 900 DEG C in air
Photo；
Fig. 4 (a) is the Ti synthesized in embodiment 32Al0.2Sn0.8The SEM photograph of C powder body material；
Fig. 4 (b) is the Ti for preparing embodiment 32Al0.2Sn0.8C powder is added to Al as reparative factor2O3In matrix
(Ti2Al0.2Sn0.8The volume content of C phase is 20%), to be heat-treated the SEM photograph after 48h at 700 DEG C in air；
Wherein: dotted line indicates to lead to Ti due to the solid solution of Sn in figure (1)2The offset of AlC diffraction maximum.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can be with
It more fully understands the present invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
All publications, patent application, patent and the other bibliography that this specification is mentioned all draw in this for reference.
Unless otherwise defined, all technical and scientific terms used herein all has what those skilled in the art routinely understood to contain
Justice.In case of conflict, it is subject to the definition of this specification.
When this specification with prefix " well known to those skilled in the art ", " prior art " or its export material similar to term
Whens material, substance, method, step, device or component etc., object derived from the prefix is covered this field when the application proposes and is routinely made
Those of with, but also include also being of little use at present, it will but become art-recognized for suitable for those of similar purpose.
In the context of the present specification, other than the content clearly stated, any matters or item that do not mention are equal
It is directly applicable in those of known in the art without carrying out any change.Moreover, any embodiment described herein can be with
It is freely combined with one or more other embodiments described herein, the technical solution or technical idea formed therefrom regards
For the original disclosure of the present invention or a part of original description, and be not considered as not disclosing or be expected herein it is new in
Hold, unless those skilled in the art think that the combination is obvious unreasonable.
Embodiment 1
By Ti powder: Al powder: the molar ratio of C powder is that 2:1:0.9 ingredient is mixed in the ball mill using agate ball as abrasive media
Material 2 hours.Then mixture is placed in mold, the pressure through 50MPa is pressed into block.Then block is put into high temperature furnace,
Under vacuum atmosphere, furnace temperature is risen to 1400 DEG C with the heating rate of 25 DEG C/min, keeps the temperature 60 minutes；Then it is crushed, ball milling,
Obtain Ti2AlC powder body material, then by the Ti of synthesis2AlC powder is densified into block materials.
Fig. 3 (b) is referred to, manufactures crackle on block materials using vickers hardness tester, then in air atmosphere, by band
There are the block materials of crackle to be heat-treated 3 hours at a temperature of 900 DEG C, observes that whole crackles are repaired.
Embodiment 2
By Ti powder: Al powder: Sn powder: the molar ratio of TiC powder is 1:0.8:0.2:0.9 ingredient, using agate ball as abrasive media,
Mixing 2 hours in the ball mill.Then mixture is placed in mold, the pressure through 50MPa is pressed into block.Then by block
It is put into high temperature furnace, under vacuum atmosphere, furnace temperature is risen to 1350 DEG C with the heating rate of 15 DEG C/min, keeps the temperature 30 minutes；So
By broken, ball milling, Ti is obtained2Al0.8Sn0.2C powder body material.
Embodiment 3
By Ti powder: Al powder: Sn powder: the molar ratio of TiC powder is 1:0.2:0.8:0.9 ingredient, using agate ball as abrasive media,
Mixing 2 hours in the ball mill.Then mixture is placed in mold, the pressure through 50MPa is pressed into block.Then by block
It is put into high temperature furnace, under vacuum atmosphere, furnace temperature is risen to 1350 DEG C with the heating rate of 15 DEG C/min, keeps the temperature 30 minutes.So
By broken, ball milling, Ti is obtained2Al0.2Sn0.8The powder body material of C.
Fig. 4 (b) is referred to, by the Ti of synthesis2Al0.2Sn0.8C powder, which is added in alumina substrate, prepares composite material,
It is then in air atmosphere heat-treated 48 hours, is observed at 700 DEG C in sample surfaces manufacture crackle using vickers hardness tester
It is repaired to whole crackles.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, protection model of the invention
It encloses without being limited thereto.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in the present invention
Protection scope within.Protection scope of the present invention is subject to claims.
Claims (9)
1. low temperature self-healing ceramics repair phase raw powder's production technology characterized by comprising
By Ti:Al:Sn:TiC=1:(1-x): the molar ratio ingredient of x:0.9, the step of mixing, be pressed into briquetting after ball milling；
Briquetting is placed in high temperature furnace, under vacuum or argon atmosphere, furnace temperature is risen to 1200~1400 DEG C, heat preservation 5~
60min obtains the step of sintered body；And
The step of sintered body is crushed, is milled to obtain the reparation phase powder；
Wherein: 0≤x≤1.
2. low temperature self-healing ceramics as described in claim 1 repair phase raw powder's production technology, which is characterized in that will after ingredient
Raw material is mixed on ball mill dry-mixed 1~4 hour.
3. low temperature self-healing ceramics as described in claim 1 repair phase raw powder's production technology, which is characterized in that when ball milling with
Agate ball is abrasive media.
4. low temperature self-healing ceramics as described in claim 1 repair phase raw powder's production technology, which is characterized in that after ball milling
Mixture briquet under 10~100MPa pressure.
5. low temperature self-healing ceramics as described in claim 1 repair phase raw powder's production technology, which is characterized in that high temperature furnace
Heating rate is 15~40 DEG C/min.
6. the low temperature self-healing ceramics that preparation method according to claim 1-5 is prepared repair phase powder.
7. low temperature self-healing ceramics as claimed in claim 6 repair phase powder, which is characterized in that the partial size of the powder is less than
10μm。
8. a kind of low temperature self-healing ceramic block material, which is characterized in that repair phase powder by ceramics as claimed in claim 6 and cause
Densification and obtain.
9. a kind of low temperature self-healing ceramic block material, which is characterized in that repair phase powder by ceramics as claimed in claim 7 and cause
Densification and obtain.
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| CN201810594262.3A CN110183229A (en) | 2018-06-11 | 2018-06-11 | A kind of Ti with low-temperature cracks self-healing capability2Al(1-x)SnxC ceramics repair phase raw powder's production technology |
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| CN201810594262.3A CN110183229A (en) | 2018-06-11 | 2018-06-11 | A kind of Ti with low-temperature cracks self-healing capability2Al(1-x)SnxC ceramics repair phase raw powder's production technology |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116211A (en) * | 2019-12-27 | 2020-05-08 | 中铭瓷(苏州)纳米粉体技术有限公司 | Preparation method of ternary nano lamellar MAX phase powder and product thereof |
| CN115504790A (en) * | 2022-09-23 | 2022-12-23 | 哈尔滨师范大学 | Preparation of Ti by combining combustion synthesis with hot-pressing sintering 2 AlC ceramic and method for preparing composite material thereof |
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| CN1724467A (en) * | 2005-06-15 | 2006-01-25 | 北京交通大学 | Process for synthesizing tin titanium carbide ceramic powder under atmospheric pressure |
| US20100009143A1 (en) * | 2006-10-17 | 2010-01-14 | Snecma Propulsion Solide | Process for manufacturing a part made of a ceramic matrix composite containing matrix phases for healing and deflecting cracks |
| CN102633505A (en) * | 2012-03-14 | 2012-08-15 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-purity MAX-phase ceramic powder |
| CN106083117A (en) * | 2016-06-21 | 2016-11-09 | 中国科学院宁波材料技术与工程研究所 | There is fiber reinforced ceramic matric composite of ternary layered MAX phase boundary surface layer and preparation method thereof |
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2018
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| CN1724467A (en) * | 2005-06-15 | 2006-01-25 | 北京交通大学 | Process for synthesizing tin titanium carbide ceramic powder under atmospheric pressure |
| US20100009143A1 (en) * | 2006-10-17 | 2010-01-14 | Snecma Propulsion Solide | Process for manufacturing a part made of a ceramic matrix composite containing matrix phases for healing and deflecting cracks |
| CN102633505A (en) * | 2012-03-14 | 2012-08-15 | 中国科学院宁波材料技术与工程研究所 | Method for preparing high-purity MAX-phase ceramic powder |
| CN106083117A (en) * | 2016-06-21 | 2016-11-09 | 中国科学院宁波材料技术与工程研究所 | There is fiber reinforced ceramic matric composite of ternary layered MAX phase boundary surface layer and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116211A (en) * | 2019-12-27 | 2020-05-08 | 中铭瓷(苏州)纳米粉体技术有限公司 | Preparation method of ternary nano lamellar MAX phase powder and product thereof |
| CN115504790A (en) * | 2022-09-23 | 2022-12-23 | 哈尔滨师范大学 | Preparation of Ti by combining combustion synthesis with hot-pressing sintering 2 AlC ceramic and method for preparing composite material thereof |
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