CN101239814A - Aluminum oxide-titanium carbide nitride-titanium nickel composite material and preparation method thereof - Google Patents

Aluminum oxide-titanium carbide nitride-titanium nickel composite material and preparation method thereof Download PDF

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CN101239814A
CN101239814A CNA2008100106481A CN200810010648A CN101239814A CN 101239814 A CN101239814 A CN 101239814A CN A2008100106481 A CNA2008100106481 A CN A2008100106481A CN 200810010648 A CN200810010648 A CN 200810010648A CN 101239814 A CN101239814 A CN 101239814A
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powder
ball
titanium
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aluminum oxide
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CN100586896C (en
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修稚萌
孙旭东
李晓东
霍地
李继光
李乾
王亚蓉
茹红强
左良
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Northeastern University China
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Abstract

The present invention relates to an aluminum oxide-carbon titanium nitride-titanium-nickle composite material and the preparing method thereof, the volume percentage of the composite material combination is as follows: Al2O3:60-94, Ti(C, N): 5-35, Ti+Ni: 1-12; the preparation technique process comprises the following two steps of: a first step of raw material mixing and drying: (1) mixing the raw material Al2O3 powder, TiCN powder, ball-grinding medium and surfactant, ball grinding and drying; (2) mixing the raw material Ti powder, Ni powder and ball-grinding medium, and ball-grinding, the ratio of titanium and nickel atom is 1:1-1:4; (3) adding ball-grinding medium into the powder which is mixed and dried in the procedure (1) and (2), ball-grinding and drying, the adding amount of Ti and Ni powder is 1-12vol%, the second step is powder molding and sintering: the mixed powder processed in the procedure (3) is added into the hot pressing stove and is hot pressed for molding in the argon atmosphere, temperature of 1400-1700DGE C and pressure of 25-35MPa. The material of the invention has the following advantages: evident increased material combined properties of hardness, strength and toughness, and the material is more suitable for the cutter material used in the mechanical industry.

Description

Aluminum oxide-titanium carbonitride-titanium nickel composite material and preparation method thereof
Technical field
The present invention relates to a kind of ceramic composite and preparation method thereof, be specifically related to a kind of aluminum oxide-titanium carbonitride-titanium nickel composite material and preparation method thereof.
Background technology
Along with development high, new technology, mechanical industry has proposed more strict and harsh requirement to cutter material.For example the material that workhardness is higher, higher stock-removing efficiency, precision work and realization is unattended etc., this just requires to improve the intensity, toughness of cutter material, wear-resisting and resistance to sudden heating etc.Alumina ceramic material has characteristics such as high-melting-point, high compression-strength and erosion resistance, but because Al 2O 3Stupalith is crisp greatly, tensile strength is low and impact resistance is poor, so as cutter material, widespread use in practice, the necessary mechanical property that improves material.Various countries propose multiple toughened and reinforced method and advanced Technology in succession for many years.In stupalith, add wild phase as: TiN, Ti (C, N), TiB 2, SiC, (W, Ti) C, WC, Mo 2C, ZrO 2, Y 2O 3Deng composition, utilize second phase, third phase material to carry out the performance that dispersed particle-strengthened, fibrous reinforcement, crystal whisker toughened, transformation toughening or coordination plasticizing reinforcement improve stupalith.Chinese patent CN1911856A (open day on February 14th, 2007) provides a kind of chromium carbide and dispersion consolidatedization of titanium carbonitride alumina matrix composite and preparation method thereof.The volume percent of its component is: 5~30%Cr 3C 2, 5~30%Ti (C, N), 0.2~2%Y 2O 3, 0.2~1%MgO, all the other are Al 2O 3Purpose is to pass through Cr 3C 2And Ti (C, effect N) improves the hardness of material simultaneously.
Summary of the invention
The present invention seeks at aluminum oxide/titanium carbonitride (Al 2O 3/ Ti (C, N)) defective of matrix material existence is developed a kind of aluminum oxide-titanium carbonitride-titanium nickel composite material and preparation method thereof, improves the over-all properties of ceramic composite, hardness, intensity and toughness further provide a kind of cutter material that mechanical industry is used that is more suitable for.
Aluminum oxide-titanium carbonitride-titanium nickel composite material component the percent by volume of the present invention's development is: Al 2O 3: 60~94, and Ti (C, N): 5~35, Ti+Ni:1~12.The over-all properties of matrix material is 20~21GPa for hardness HV, and intensity is 600~800MPa, fracture toughness property 7~9MPam 1/2
The preparation method of the above-mentioned matrix material of the present invention, carry out as follows:
Raw material mixes and is dry:
(1) with raw material A l 2O 3Powder and TiCN powder mixes are called the A mixed powder, mix with ball-milling medium, tensio-active agent, ball milling, and its proportioning raw materials is: Al 2O 3Powder is 60~94vol%, Ti (C 1-XN X) powder is 5~35vol%, X=0.3~0.7 wherein, the surfactant add-on is raw material A l 2O 30~3vol% of powder and TiCN powder total amount, the ball milling time is 12~24 hours; Material behind the ball milling adds baking oven, is under 60 ℃ or 120 ℃ in temperature, dry 24~48 hours;
(2) raw material Ti powder and Ni powder mixes are called the B mixed powder mixes with ball-milling medium, ball milling, titanium and nickle atom proportioning be 1: 1~1: 4,12~24 hours ball milling time, put into vacuum drying oven then, temperature be 60 ℃ dry 24~48 hours down;
(3) with the powder behind step (1) and (2) combination drying, behind the adding ball-milling medium mixing, ball milling 12~24 hours, put into vacuum drying oven then, 60 ℃ of dryings 24~48 hours, B mixed powder add-on was 1~12vol% of A and two kinds of mixed powder total amounts of B, and surplus is the A mixed powder;
Powder forming and sintering:
Mixed powder after step (3) handled is in hot pressing furnace, and under argon shield, temperature is 1400~1700 ℃, and pressure is hot pressing 5~30 minutes under 25~35MPa.
The raw material that the present invention adopts: Al 2O 3Powder: granularity d 50Be 0.1~10 μ m, purity Al 2O 3Content>99.9%; Ti (C 1-XN X): granularity d 50Be 0.1~10 μ m, content>99.9%, wherein X=0.3~0.7; Ti powder: granularity d 50Be 0.1~10 μ m, purity Ti content>99.9%; Ni powder: granularity d 50Be 0.1~10 μ m, purity content>99.9%.
Described tensio-active agent is selected poly carboxylic acid second fat for use, and ball-milling medium is selected dehydrated alcohol or deionized water for use.
Powder in above-mentioned steps (2) or the step (3) behind mixing, the ball milling is put into baking oven vacuum-drying, and vacuum tightness is 1 * 10 -1MPa.
The advantage that the present invention has and the positively effect of generation are: the present invention is Al with aluminum oxide/titanium carbide 2O 3(C, N) matrix material is a matrix to/Ti, is characteristics of the present invention by the intensity and the toughness of adding NiTi raising cutter material.Add Ni and Ti in pottery, metal can improve toughness of material by the particulate reinforcement mode, and Ni and Ti will generate intermetallic compound NiTi, Ti under certain condition 2Ni and TiNi 3And in sintering, form liquid phase, and this is to reducing the sintering temperature of matrix material, and (C, the sintering densification of decomposition N), promotion material is very useful to Ti when suppressing high temperature sintering.The present invention also adds tensio-active agent poly carboxylic acid second fat and can improve Al effectively in the powder mixes process in addition 2O 3(C, the N) homogeneity of powder mixes reduce the reunion of powder to/Ti, improve the density and the mechanical property of material.
The above-mentioned composite material combination property of producing through the present invention reaches: hardness Hv is 20~21GPa, and intensity is 600~800MPa, and fracture toughness property is 7~10MPam 1/2, can satisfy the performance requriements of machining tool material fully.
Embodiment
Embodiment 1 (Al 2O 3-5vol%TiC 0.5N 0.5The preparation and the performance of)-1vol% (Ti+Ni) matrix material
At Al 2O 3Powder (granularity d 50Be 0.1 μ m, purity>99.90%) adds the volume percentage in and is 5 TiC 0.5N 0.5Powder (granularity d 50Be 0.1 μ m, purity>99.90%), be ball-milling medium with the dehydrated alcohol, alumina balls are abrading-ball, ball milling 12 hours was put into 60 ℃ of baking oven inner dryings 24 hours then, obtained Al 2O 3-5vol%TiC 0.5N 0.5Mixed powder.Ti powder and Ni powder are pressed 1: 1 mixed of atomic ratio, are ball-milling medium with the dehydrated alcohol, and Stainless Steel Ball is an abrading-ball, and ball milling 12 hours was put into 60 ℃ of vacuum oven 48 hours then, and vacuum tightness is 1 * 10 -1MPa obtains the Ti-Ni mixed powder.The Al that is mixing 2O 3-5vol%TiC 0.5N 0.5Adding volume percentage is 1 the Ti-Ni mixed powder that mixes in the mixed powder, is ball-milling medium with the dehydrated alcohol, and Stainless Steel Ball is an abrading-ball, and ball milling 12 hours was put into 60 ℃ of vacuum oven 24 hours then, and vacuum tightness is 1 * 10 -1MPa.With the powder hot pressing in hot pressing furnace that mixes.Hot pressing temperature is that 1700 ℃, sintering pressure are 35MPa hot pressing time 30min, and hot pressing atmosphere is argon gas.Adopt Vickers penetration hardness method to measure material hardness (Hv); Adopt the three-point bending strength test to detect the intensity of material; Adopt monolateral breach beam method (SENB) to detect the fracture toughness property of material; Adopt scanning electron microscope (SEM) to detect the microstructure and the fracture of material.The detected result of material property is: hardness (Hv) 20GPa, three-point bending resistance intensity 600MPa, fracture toughness property 7.1MPam 1/2
Embodiment 2
The component of present embodiment alumina matrix composite is (Al 2O 3-25vol%TiC 0.3N 0.7)-8vol% (Ti+Ni) is at Al 2O 3Powder (granularity d 50Be 0.5 μ m, purity>99.9%) adds the volume percentage in and is 25 TiC 0.3N 0.7Powder (granularity d 50Be 0.3 μ m, purity>99.9%), be ball-milling medium with the deionized water, alumina balls are abrading-ball, ball milling 20 hours was put into 120 ℃ of baking oven inner dryings 48 hours then, obtained Al 2O 3-5vol%TiC 0.5N 0.5Mixed powder.With Ti powder (granularity d 50Be 0.5 μ m, purity>99.9%) and Ni powder (granularity d 50Be 0.5 μ m, purity>99.9%) press 1: 2 mixed of atomic ratio, with the dehydrated alcohol ball-milling medium, Stainless Steel Ball is an abrading-ball, and ball milling 24 hours was put into 60 ℃ of vacuum oven 24 hours then, and vacuum tightness is 1 * 10 -1MPa obtains the Ti-Ni mixed powder.The Al that is mixing 2O 3-25vol%TiC 0.5N 0.5Adding volume percentage is 8 the Ti-Ni mixed powder that mixes in the mixed powder, is ball-milling medium with the dehydrated alcohol, and Stainless Steel Ball is an abrading-ball, and ball milling 24 hours was put into 60 ℃ of vacuum oven 36 hours then.With the powder hot pressing in hot pressing furnace that mixes.Hot pressing temperature is that 1500 ℃, sintering pressure are 30MPa hot pressing time 15min, and hot pressing atmosphere is argon gas.The detected result of material property is after the hot pressing: hardness (Hv) 20GPa, three-point bending resistance intensity 716MPa, fracture toughness property 9.1MPam 1/2
Embodiment 3
The component of present embodiment alumina matrix composite is (Al 2O 3-35vol%TiC 0.3N 0.7)-12vol% (Ti+Ni) is at Al 2O 3Powder (granularity d 50Be 3 μ m, purity>99.9%) adds the volume percentage in and is 35 TiC 0.5N 0.5Powder (granularity d 50Be 3 μ m, purity>99.9%), Al 2O 3-35vol%TiC 0.3N 0.7The preparation of powder mix is as described in the example 1.With Ti powder (granularity d 50Be 2 μ m, purity>99.9%) and Ni powder (granularity d 50Be 2 μ m, purity>99.9%) press 1: 4 mixed of atomic ratio, the preparation of powder mix is as described in the example 1.The Al that is mixing 2O 3-35vol%TiC 0.3N 0.7Adding volume percentage is 12 the Ti-Ni mixed powder that mixes in the mixed powder, is ball-milling medium with the dehydrated alcohol, and Stainless Steel Ball is an abrading-ball, and ball milling 18 hours was put into 60 ℃ of vacuum oven 24 hours then, and vacuum tightness is 1 * 10 -1MPa.With the powder hot pressing in hot pressing furnace that mixes.Hot pressing temperature is that 1550 ℃, sintering pressure are 30MPa hot pressing time 10min, and hot pressing atmosphere is argon gas.The detected result of material property is after the hot pressing: hardness (Hv) 21GPa, three-point bending resistance intensity 816MPa, fracture toughness property 9.8MPam 1/2
Embodiment 4
The component of present embodiment alumina matrix composite is (Al 2O 3-25vol%TiC 0.3N 0.7)-10vol% (Ti+Ni) is at Al 2O 3Powder (granularity d 5010 μ m, purity>99.9%) adds the volume percentage in and is 25 TiC 0.3N 0.7Powder (granularity d 508 μ m, purity>99.9%), Al 2O 3-25vol%TiC 0.3N 0.7The preparation of powder mix is as described in the example 2.With Ti powder (granularity d 50Be 8 μ m, purity>99.9%) and Ni powder (granularity d 50Be 8 μ m, purity>99.9%) press 1: 3 mixed of atomic ratio, the preparation of powder mix is as described in the example 1.The Al that is mixing 2O 3-25vol%TiC 0.3N 0.7Adding volume percentage is 10 the Ti-Ni mixed powder that mixes in the mixed powder, is ball-milling medium with the dehydrated alcohol, and Stainless Steel Ball is an abrading-ball, and ball milling 24 hours was put into 60 ℃ of vacuum oven 48 hours then, and vacuum tightness is 1 * 10 -1MPa.With the powder hot pressing in hot pressing furnace that mixes.Hot pressing temperature is that 1400 ℃, sintering pressure are 25MPa hot pressing time 5min, and hot pressing atmosphere is argon gas.The detected result of material property is after the hot pressing: hardness (Hv) 21GPa, three-point bending resistance intensity 806MPa, fracture toughness property 8.8MPam 1/2

Claims (5)

1, a kind of aluminum oxide-titanium carbonitride-titanium nickel composite material is characterized in that the moiety percent by volume is: Al 2O 3: 60~94, and Ti (C, N): 5~35, Ti+Ni:1~12.
2,, it is characterized in that processing step is as follows according to the preparation method of the described aluminum oxide-titanium carbonitride of claim 1-titanium nickel composite material:
Raw material mixes and is dry:
(1) with raw material A l 2O 3Powder and TiCN powder mixes are called the A mixed powder, mix with ball-milling medium, tensio-active agent, ball milling, and its proportioning raw materials is: Al 2O 3Powder is 60~94vol%, Ti (C 1-XN X) powder is 5~35vol%, X=0.3~0.7 wherein, the surfactant add-on is raw material A l 2O 30~3vol% of powder and TiCN powder total amount, the ball milling time is 12~24 hours; Material behind the ball milling adds baking oven, is under 60 ℃ or 120 ℃ in temperature, dry 24~48 hours;
(2) raw material Ti powder and Ni powder mixes are called the B mixed powder mixes with ball-milling medium, ball milling, titanium and nickle atom proportioning be 1: 1~1: 4,12~24 hours ball milling time, put into vacuum drying oven then, temperature be 60 ℃ dry 24~48 hours down;
(3) with the powder behind step (1) and (2) combination drying, behind the adding ball-milling medium mixing, ball milling 12~24 hours, put into vacuum drying oven then, 60 ℃ of dryings 24~48 hours, B mixed powder add-on was 1~12vol% of A and two kinds of mixed powder total amounts of B, and surplus is the A mixed powder;
Powder forming and sintering:
Mixed powder after step (3) handled adds in the hot pressing furnace, and under argon shield, temperature is 1400~1700 ℃, and pressure is hot pressing 5~30 minutes under 25~35MPa.
3, according to the preparation method of the described aluminum oxide-titanium carbonitride of claim 2-titanium nickel composite material, it is characterized in that described tensio-active agent selects poly carboxylic acid second fat for use, ball-milling medium is selected dehydrated alcohol or deionized water for use.
4, according to the preparation method of the described aluminum oxide-titanium carbonitride of claim 2-titanium nickel composite material, it is characterized in that mixed powder is put into drying under the baking oven vacuum in step (2) or the step (3), vacuum tightness is 1 * 10 -1MPa.
5, according to the preparation method of the described aluminum oxide-titanium carbonitride of claim 2-titanium nickel composite material, it is characterized in that raw material A l 2O 3Powder: granularity d 50Be 0.1~10 μ m, purity Al 2O 3Content>99.9%; Ti (C 1-XN X): granularity d 50Be 0.1~10 μ m, content>99.9%, wherein X=0.3~0.7; Ti powder: granularity d 50Be 0.1~10 μ m, purity Ti content>99.9%; Ni powder: granularity d 50Be 0.1~10 μ m, purity content>99.9%.
CN200810010648A 2008-03-14 2008-03-14 Aluminum oxide-titanium carbonitride-titanium nickel composite material and preparation method thereof Expired - Fee Related CN100586896C (en)

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CN101871070A (en) * 2010-06-04 2010-10-27 重庆大学 Novel metal ceramic composite material and preparation method thereof
CN102886942A (en) * 2011-07-19 2013-01-23 东北大学 Layered composite boron carbide ceramic material and its preparation method
CN104480364A (en) * 2014-11-10 2015-04-01 沈阳理工大学 Al2O3-TiCN/Co-Ni metal ceramic die material and preparation method thereof
CN104496429A (en) * 2014-12-24 2015-04-08 东北大学 Al2O3-Ti (C, N)-cBN ceramic cutter material and its preparation method
TWI493061B (en) * 2010-08-19 2015-07-21 Hon Hai Prec Ind Co Ltd Coating, articles coated with the coating, and method for manufacturing the articles
CN108101520A (en) * 2017-12-23 2018-06-01 深圳万佳互动科技有限公司 Alundum (Al2O3)-composite material of silicon carbide and preparation method thereof
CN108439960A (en) * 2018-04-28 2018-08-24 九江职业技术学院 A kind of Al2O3-TiB2- TiN ceramic cutting tool materials and preparation method thereof
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* Cited by examiner, † Cited by third party
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CN101871070A (en) * 2010-06-04 2010-10-27 重庆大学 Novel metal ceramic composite material and preparation method thereof
CN101871070B (en) * 2010-06-04 2012-07-04 重庆大学 Novel metal ceramic composite material and preparation method thereof
TWI493061B (en) * 2010-08-19 2015-07-21 Hon Hai Prec Ind Co Ltd Coating, articles coated with the coating, and method for manufacturing the articles
CN102886942A (en) * 2011-07-19 2013-01-23 东北大学 Layered composite boron carbide ceramic material and its preparation method
CN102886942B (en) * 2011-07-19 2014-11-26 东北大学 Layered composite boron carbide ceramic material and its preparation method
CN104480364A (en) * 2014-11-10 2015-04-01 沈阳理工大学 Al2O3-TiCN/Co-Ni metal ceramic die material and preparation method thereof
CN104496429A (en) * 2014-12-24 2015-04-08 东北大学 Al2O3-Ti (C, N)-cBN ceramic cutter material and its preparation method
CN104496429B (en) * 2014-12-24 2017-03-29 东北大学 Al2O3Ti (C, N) cBN ceramic cutting tool materials and preparation method thereof
CN108101520A (en) * 2017-12-23 2018-06-01 深圳万佳互动科技有限公司 Alundum (Al2O3)-composite material of silicon carbide and preparation method thereof
CN108439960A (en) * 2018-04-28 2018-08-24 九江职业技术学院 A kind of Al2O3-TiB2- TiN ceramic cutting tool materials and preparation method thereof
CN111001818A (en) * 2019-12-31 2020-04-14 南通金源智能技术有限公司 3D printing aluminum oxide titanium cobalt carbonitride nickel powder and preparation method thereof

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