CN1317223C - Rare earth reinforced alumina ceramic composite materials and production method thereof - Google Patents
Rare earth reinforced alumina ceramic composite materials and production method thereof Download PDFInfo
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- CN1317223C CN1317223C CNB2004100240849A CN200410024084A CN1317223C CN 1317223 C CN1317223 C CN 1317223C CN B2004100240849 A CNB2004100240849 A CN B2004100240849A CN 200410024084 A CN200410024084 A CN 200410024084A CN 1317223 C CN1317223 C CN 1317223C
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- rare earth
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Abstract
The present invention relates to aluminum oxide ceramic composite material reinforced by rare earth, and a production method thereof. The rare earth reinforcing aluminum oxide ceramic composite material of the present invention is composed of the components of the following proportion by volume: 88.5 to 55 % of alpha-Al2 O3, 10 to 45 % of Ti (C, N), 0.5 to 5% of Mo, 0.5 to 5% of Ni, 0.3 to 2 % of Y2 O3 and O0.2 to 0.8% of Mg. Compared with the existing invention, the mechanical property, particularly the bending resistance of the composite material of the present invention is greatly enhanced than that of corresponding ceramic material without containing rare earth oxide and other existing aluminum oxide ceramic material containing rare earth elements. The production method of the present invention has the advantages of simple operation and high product mechanical property.
Description
(1) technical field under
The present invention relates to a kind of alumina series stupalith and production method thereof, particularly a kind of alumina series ceramic composite and production method thereof with the rare earth reinforcement.
(2) background technology
Rare earth element is meant lanthanon in the periodic table of elements and the scandium close with lanthanon character and yttrium totally 17 kinds of elements.Because the rare earth element atom has special electron structure (4f
x5d
0-16s
2), having many advantages such as electricity price height, atomic radius is big, chemical is active simultaneously, the thermostability of its oxide compound, fusing point and boiling point are all higher.Therefore, can control corresponding character, produce new material behavior by selecting different rare earth elements.
APPLICATION OF RARE-EARTH ELEMENTS just began as far back as the thirties in ceramic industry.To the seventies, the total consumption of rare earth in stupalith reaches 70 tons/year, accounts for 2～3% of national total amount of rare earth.Rare earth element is at Si
3N
4, the application in nitride ceramics such as Sialon and AlN and oxygen, carbon and the borides all possesses some special knowledge.At present, the research in the alumina series composite ceramic material mainly concentrates on Al for rare earth element both at home and abroad
2O
3/ TiC, Al
2O
3/ TiN/ZrO
2, Al
2O
3/ NbC, Al
2O
3/ (W, Ti) components system such as C.
Wherein, to Al
2O
3Studies show that of/TiC pressureless sintering ceramic composite added a small amount of Y
2O
3Very effective to the sintered density that improves material.But it is to Al
2O
3The matrix grain size has no effect, and unfavorable to the mechanical property of material.Afterwards, in the research of Chae etc., the liquid phase that occurs in the sintering process in process of cooling with YAG (Y
3Al
5O
12) the form crystallization separate out, thereby make the fracture toughness property of material reach 4.6～4.8MPam
1/2
Nineteen ninety, Zhuzhou Hard Alloy Plant is succeeded in developing the new ceramics cutter material that adds rare earth oxide.Its major ingredient is Al
2O
3/ TiN/ZrO
2/ RO also has part TiC and AlN in addition.Its hardness 〉=93.5HRA, bending strength is 700MPa.With Al
2O
3/ TiC ceramic cutting tool material is compared, and has identical wear resistance, higher toughness and heat-shock resistance.Its processing object is identical with general ceramic cutting tool material, also can be used for simultaneously under the impact condition cutting, strip off the skin, in the rough turn and even milling.Here, the rare earth oxide that is added is mainly as cubic phase ZrO
2Stablizer.
People such as Acchar and Pasotti is to Al
2O
3/ NbC studies show that, Y
2O
3Be added with the raising that helps the material relative density in right amount, and under the heat pressing process condition, make the hardness of material and fracture toughness property reach 19.7GPa and 4.5MPam respectively
1/2
The author had also once studied pure rare earth element Y, Sm and Ce to Al
2O
3/ (find: an amount of interpolation of three kinds of rare earth elements all can make moderate progress to the bending strength and the fracture toughness property of material for W, the Ti) influence of C ceramic cutting tool material mechanical property.Wherein, the bending strength that contains the stupalith of Rare Earth Y is up to 853MPa, and fracture toughness property reaches 6.0MPam
1/2, improve about 10% and 16% than the corresponding material that does not contain rare earth element respectively.But the hardness of this ceramic cutting tool material is subjected to the influence of the kind of rare earth element and content smaller, and in the scope of being tested, its hardness all remains on about 19GPa.
In a word, rare earth element has obtained in the structural ceramic material field using widely at present.By improving the microtexture of material, greatly improved the physical and mechanical property and the use properties of material, thereby wide application prospect has been arranged.But with regard to present research, rare earth is applied to Si more
3N
4, Sialon and ZrO
2Be in the pottery, and at Al
2O
3Use less in the system.And from the application point of view consideration, structural ceramic material still awaits further raising at aspects such as kind, mechanical property and use propertieies.
(3) summary of the invention
The object of the present invention is to provide a kind of alumina series ceramic composite with rare earth reinforcement of good comprehensive mechanical properties, and the production method of above-mentioned stupalith.
The present invention realizes by following measure:
Rare earth reinforced alumina of the present invention is a ceramic composite, is made up of following components in percentage by volume: α-Al
2O
388.5～55%, Ti (C, N) 20～35%, Mo0.5～5%, Ni0.5～5%, Y
2O
30.3～2%, MgO0.2～0.8%.
(C, the mol ratio of C N), N element is 0.3～0.7: 0.7～0.3 to above-mentioned Ti.
In order to realize optimum mechanical properties, the purity of above-mentioned each component should be greater than 99%, and mean diameter is not more than 1 μ m.
The production method of above-mentioned ceramic composite may further comprise the steps, and each component raw material is mixed in proportion, with N
2Gas is protective atmosphere, wet ball-milling 30-100h, and drying is at N
2Sieve in the air-flow, last Thermocompressed sintering and forming, hot pressing parameters is: hot pressing pressure 30～35MPa, 1650 ℃～1800 ℃ of hot pressing temperatures, soaking time is 5～45min.
Above-mentioned production method, during its Thermocompressed sintering and forming, best temperature rise rate is that 0.5～1.0 ℃/s, rate of temperature fall are 0.3～0.75 ℃/s.
Above-mentioned production method is in order to improve purity, described α-Al
2O
3(C N) before the powder mixes, all adopts rare HNO for powder and Ti
3With dilute NaOH solution heated wash 10-30min.
In the above-mentioned matrix material,, play the effect of bonding phase, can improve the intensity of matrix material by adding metal-powder Mo and Ni.
In the above-mentioned matrix material, add Y
2O
3Powder mainly is by clean interface, improves interface bond strength, helps the agglomerating mechanism of action, improves the mechanical property of material.
The present invention is with ceramic raw material Al
2O
3(C, N) hot pressing is compound, thereby forms Al with Ti
2O
3Base Ti (C, N) matrix material.This matrix material has good mechanical performance and high temperature resistant, corrosion-resistant, antioxidant property, can be used for making engineering materialss such as cutter, mould.
Stupalith of the present invention, its test result shows: the rare earth reinforcement Al that is developed
2O
3/ Ti (C, N) bending strength of composite ceramic material is up to 980MPa, and fracture toughness property reaches 6.0MPam
1/2, respectively than pure Al
2O
3Stupalith improves 96% and 57%, improves about 16% times and 15% than the corresponding stupalith that does not contain rare earth oxide.The hardness of material reaches 19.2GPa, is subjected to the influence of rare earth oxide little.
Compare with existing invention, main characteristic of the present invention is by at Al
2O
3(C N) adds rare earth oxide Y to/Ti in the composite ceramics
2O
3, succeed in developing rare earth reinforcement Al
2O
3(its mechanical property especially more corresponding stupalith and other the existing alumina series stupaliths that contains rare earth element that does not contain rare earth oxide of bending strength has a more substantial increase base Ti for C, N) matrix material.
Production method of the present invention has simple to operate, the advantage that the goods mechanical property is high.
(4) embodiment
Embodiment 1
The ceramic composite of present embodiment, its volume percent of respectively forming component is: α-Al
2O
385%, Ti (C, N) 10%, Mo2%, Ni2%, Y
2O
30.5%, MgO0.5%.
Production method is as follows: get in proportion purity greater than 99%, mean particle size is less than above-mentioned each raw material of 1 μ m, and each raw material is mixed, compound is medium with the dehydrated alcohol, with N
2Gas is protective atmosphere, wet ball-milling 70h, and material ball ratio (weight ratio) is 1: 10.Wet feed behind the ball milling is through vacuum-drying 32 hours, at N
2Sieve in the air-flow, last hot pressed sintering is made sample.Hot pressing parameters is: hot pressing pressure 30MPa, and 1800 ℃ of hot pressing temperatures, soaking time are 10min, and temperature rise rate is 0.5～1.0 ℃/s, and rate of temperature fall is 0.3～0.75 ℃/s.
The ceramic composite of preparation, its performance is: bending strength is 812MPa, and fracture toughness property reaches 5.3MPam
1/2, the hardness of material is 19.0GPa.
Embodiment 2
The ceramic composite of present embodiment, its volume percent of respectively forming component is: α-Al
2O
359%, Ti (C, N) 35%, Mo1%, Ni4%, Y
2O
30.8%, MgO0.2%.
Production method is as follows: adopt analytical pure Al (OH)
3Decompose preparation α-Al
2O
3, decomposition temperature is 1200 ℃, the time is 2 hours, obtain purity greater than 99%, mean diameter is less than α-Al of 1 μ m
2O
3Powder.The Ti that is adopted (C, N) powder purity is greater than 99%, and particle diameter is 1 μ m.α-Al
2O
3And Ti (C N) all adopts rare HNO before use
3With dilute NaOH solution heated wash 10-30min, to reduce foreign matter content.Mo and Ni metal-powder particle diameter are 200 orders, Y
2O
3Be analytical pure, median size is less than 1 μ m.Each component raw material is mixed according to the above ratio, and compound is medium with the dehydrated alcohol, with N
2Gas is protective atmosphere, wet ball-milling 40h, and material ball ratio (weight ratio) is 1: 6.Wet feed behind the ball milling is through vacuum-drying 24 hours, at N
2Sieve in the air-flow, last hot pressed sintering is made sample.Hot pressing parameters is: hot pressing pressure 35MPa, and 1750 ℃ of hot pressing temperatures, soaking time are 20min, and temperature rise rate is 0.5～1.0 ℃/s, and rate of temperature fall is 0.3～0.75 ℃/s.
The ceramic composite of preparation, its performance is: bending strength is 954MPa, and fracture toughness property reaches 5.9MPam
1/2, the hardness of material is 19.2GPa.
Embodiment 3
The ceramic composite of present embodiment, its volume percent of respectively forming component is: α-Al
2O
370%, Ti (C, N) 20%, Mo4%, Ni4%, Y
2O
31.5%, MgO0.5%.
Production method is as follows: adopt analytical pure Al (OH)
3Decompose preparation α-Al
2O
3, decomposition temperature is 1200 ℃, the time is 1.5 hours, obtain purity greater than 99%, mean diameter is less than α-Al of 1 μ m
2O
3Powder.The Ti that is adopted (C, N) powder purity is greater than 99%, and particle diameter is 1 μ m.Adopt rare HNO before use
3With dilute NaOH solution heated wash 20min, to reduce foreign matter content.Mo and Ni metal-powder particle diameter are 200 orders.Y
2O
3Be analytical pure, median size is less than 1 μ m.Each component raw material is mixed according to the above ratio, and compound is medium with the dehydrated alcohol, with N
2Gas is protective atmosphere, wet ball-milling 60h, and material ball ratio (weight ratio) is 1: 8.Wet feed behind the ball milling is through vacuum-drying 48 hours, at N
2Sieve in the air-flow, last hot pressed sintering is made sample.Hot pressing parameters is: hot pressing pressure 33MPa, 1700 ℃ of hot pressing temperatures, soaking time are 40min.
The ceramic composite of preparation, its performance is: bending strength is 895MPa, and fracture toughness property reaches 6.0MPam
1/2, the hardness of material is 18.8GPa.
Claims (6)
1. a rare earth reinforced alumina is a ceramic composite, it is characterized in that: be made of α-Al following components in percentage by volume
2O
388.5～55%, Ti (C, N) 20～35%, Mo0.5～5%, Ni0.5～5%, Y
2O
30.3～2%, MgO0.2～0.8%.
2. ceramic composite according to claim 1 is characterized in that: (C, the mol ratio of C N), N element is 0.3～0.7: 0.7～0.3 to described Ti.
3. ceramic composite according to claim 1 and 2 is characterized in that: the purity of described component is greater than 99%, and mean diameter is not more than 1 μ m.
4. the production method of the described ceramic composite of claim 1; it is characterized in that: may further comprise the steps; each component raw material is mixed in proportion, and is protective atmosphere with the rare gas element, wet ball-milling 30-100h; dry; sieve, last Thermocompressed sintering and forming, hot pressing parameters is: hot pressing pressure 30～35MPa; 1650 ℃～1800 ℃ of hot pressing temperatures, soaking time is 5～45min.
5. production method according to claim 4 is characterized in that: during described Thermocompressed sintering and forming, its temperature rise rate is 0.5～1.0 ℃/s, and rate of temperature fall is 0.3～0.75 ℃/s.
6. according to claim 4 or 5 described production methods, it is characterized in that: described α-Al
2O
3(C N) before the powder mixes, all adopts rare HNO for powder and Ti
3With dilute NaOH solution heated wash 10-30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100240849A CN1317223C (en) | 2004-05-11 | 2004-05-11 | Rare earth reinforced alumina ceramic composite materials and production method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100240849A CN1317223C (en) | 2004-05-11 | 2004-05-11 | Rare earth reinforced alumina ceramic composite materials and production method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1569732A CN1569732A (en) | 2005-01-26 |
| CN1317223C true CN1317223C (en) | 2007-05-23 |
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ID=34480481
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| CNB2004100240849A Expired - Fee Related CN1317223C (en) | 2004-05-11 | 2004-05-11 | Rare earth reinforced alumina ceramic composite materials and production method thereof |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100355695C (en) * | 2006-09-01 | 2007-12-19 | 山东轻工业学院 | Chromium carbide and carbon titanium nitride particle dispersion consolidated aluminium oxide base ceramic composite material and its preparation method |
| CN101063187B (en) * | 2007-05-23 | 2010-10-13 | 济南钢铁股份有限公司 | Preparation method of ceramic-metal composite material |
| CN101857438A (en) * | 2010-05-25 | 2010-10-13 | 山东大学 | Method for preparing aluminum oxide-titanium carbide-zirconium oxide nanocomposite ceramic material |
| CN103242032A (en) * | 2013-04-25 | 2013-08-14 | 安徽三丁光伏节能电器有限公司 | Rare-earth composite ceramic material applied to illumination industry and manufacturing method thereof |
| CN104131208A (en) * | 2014-08-06 | 2014-11-05 | 南京理工大学 | Aluminium oxide-titanium carbide micron composite ceramic cutter material and microwave sintering method thereof |
| CN106631035B (en) * | 2016-12-29 | 2020-08-11 | 广东工业大学 | Composite ceramic and preparation method thereof |
| CN112521132B (en) * | 2020-12-07 | 2022-03-01 | 山东大学 | Bionic ceramic tool preparation method and prepared bionic ceramic tool |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56114864A (en) * | 1980-02-07 | 1981-09-09 | Mitsubishi Metal Corp | High strength alumina sintered ceramics |
| US5213731A (en) * | 1990-02-24 | 1993-05-25 | Ssangyong Cement Industrial Co., Ltd. | Method for manufacture of a sintered body of Al2 O3 -Tic system useful as a cutting tool |
| JPH0624837A (en) * | 1992-07-03 | 1994-02-01 | Denki Kagaku Kogyo Kk | Parts for rotary compressor |
| JP2000103667A (en) * | 1998-09-30 | 2000-04-11 | Kyocera Corp | Al2O3-TiC-BASED SINTERED PRODUCT AND SUBSTRATE FOR THIN FILM MAGNETIC HEAD USING THE SAME ii |
-
2004
- 2004-05-11 CN CNB2004100240849A patent/CN1317223C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56114864A (en) * | 1980-02-07 | 1981-09-09 | Mitsubishi Metal Corp | High strength alumina sintered ceramics |
| US5213731A (en) * | 1990-02-24 | 1993-05-25 | Ssangyong Cement Industrial Co., Ltd. | Method for manufacture of a sintered body of Al2 O3 -Tic system useful as a cutting tool |
| JPH0624837A (en) * | 1992-07-03 | 1994-02-01 | Denki Kagaku Kogyo Kk | Parts for rotary compressor |
| JP2000103667A (en) * | 1998-09-30 | 2000-04-11 | Kyocera Corp | Al2O3-TiC-BASED SINTERED PRODUCT AND SUBSTRATE FOR THIN FILM MAGNETIC HEAD USING THE SAME ii |
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|---|---|
| CN1569732A (en) | 2005-01-26 |
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