CN110015899A - A kind of aluminium oxide-titanium carbon oxygen solid solution composite ceramics and preparation method thereof - Google Patents

A kind of aluminium oxide-titanium carbon oxygen solid solution composite ceramics and preparation method thereof Download PDF

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CN110015899A
CN110015899A CN201910325941.5A CN201910325941A CN110015899A CN 110015899 A CN110015899 A CN 110015899A CN 201910325941 A CN201910325941 A CN 201910325941A CN 110015899 A CN110015899 A CN 110015899A
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aluminium oxide
solid solution
ball milling
carbon oxygen
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秦家千
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Suqian Mstar Technology Ltd Deeter
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Suqian Mstar Technology Ltd Deeter
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Abstract

The present invention relates to ceramic material science and technology field, in particular to a kind of aluminium oxide-titanium carbon oxygen solid solution composite ceramic material and preparation method thereof.Technical solution of the present invention is by TiC powder and TiO2/ TiO powder mixes in molar ratio, ball milling 3 hours in high energy ball mill, and the powder after ball milling passes through drying, is put into high temperature furnace after compression moulding and handles under protection of argon gas, then cools to room temperature；Sintered block is after broken, ball milling, then by aluminium oxide and TiCxO1‑xPowder and sintering aid appropriate, raw material mix 5~20 hours through physical mechanical method；It is fitted into cold moudling in graphite jig after mixed powder is dry, is sintered in discharge plasma sintering furnace, then cools to room temperature with the furnace, Al can be prepared2O3‑TiCxO1‑xComposite ceramics.

Description

A kind of aluminium oxide-titanium carbon oxygen solid solution composite ceramics and preparation method thereof
Technical field
The present invention relates to ceramic material science and technology field, in particular to a kind of aluminium oxide-titanium carbon oxygen solid solution composite ceramic Ceramic material and preparation method thereof.
Background technique
Composite ceramic material has many advantages, such as high-melting-point, good wearability, thermo-chemical stability, high rigidity, is suitable for The cutter of production processing difficult-to-machine material.It is right with the high speed in the fields such as China's aerospace, national defence, industry, sustainable development The requirement of material comprehensive performance is higher and higher.Since composite ceramics can further enhance the toughness of pure alumina ceramics, not The hardness and high-temperature behavior of aluminium oxide ceramics are reduced very much, thus is got the attention.Titanium carbide have fusing point it is high, it is anti-oxidant, Intensity is high, thermal conductivity is good, chemical stability is good, good toughness and to the excellent properties such as the chemical inertness of steel metalloid, institute It is mainly used to manufacture cermet, heat-resisting alloy and hard alloy with titanium carbide.Simultaneously because titanium carbide has these formedness Can, titanium carbide is widely used in various composite materials as a kind of reinforced phase for strengthening matrix.As alumina composite is made pottery In porcelain, due to having high intensity, high rigidity, excellent wearability and chemical stability, alumina-titanium carbide system obtains titanium carbide To study and apply extensively.
Pure alumina powder is about in 1750 °C of beginning creeps and sintering.So high sintering temperature, can make kiln resistance to The reduced service life of fiery material, energy consumption is excessive and material firing property is bad etc..Therefore, ceramic post sintering process In sintering aid is added usually to reduce the sintering temperature of high-melting-point ceramics, to realize the reduction of energy consumption and preparation cost.Such as Titanium dioxide, magnesia, yttrium oxide etc..Therefore, agglomeration is helped in order to play sintering aid, sintering aid and main phase requirement Uniformly mixing.Currently, the adding method of prior art ceramic post sintering auxiliary agent generally uses and the common ball milling mixing of main phase substance Mode, however this method is easy mixing non-uniform phenomenon, so how to improve and prepare the composite ceramic material of excellent properties It is extremely urgent.
Summary of the invention
The technical problems to be solved by the invention: for prior art ceramic post sintering auxiliary agent adding method generally use with The mode of the common ball milling mixing of main phase substance, however this method is easy mixing non-uniform phenomenon, provides a kind of aluminium oxide-titanium Carbon oxygen solid solution composite ceramic material and preparation method thereof is utilized with realizing that sintering aid is evenly dispersed in main phase powder Titanium carbide-titanium dioxide (titanium monoxide) forms solid solution at high temperature, can form reinforced phase-sintering aid solid solution, benefit Use Ti-C-O solid solution simultaneously as reinforced phase and sintering aid, raising alumina powder is sintered at a lower temperature and powder The uniformity of sintering, to prepare high hardness high toughness aluminium oxide-oxidation of coal titanium composite ceramics.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of aluminium oxide-titanium carbon oxygen solid solution composite ceramics and preparation method thereof, by weight percentage, by following substance group At:
Aluminium oxide 50~95%
Titanium carbon oxygen solid solution 5~50%
The specific preparation step of titanium carbon oxygen solid solution are as follows:
(1) 8:2,6:4,5:5,4:6,2:8 in molar ratio, TiC powder are mixed with TiO2 or TiO powder, after the completion of mixing, then in height Ball milling 3 hours in energy ball mill；
(2) after the completion of ball milling, powder after ball milling is collected to obtain, is dried and is put into high temperature furnace after compression moulding, Argon atmosphere protection, 1400~1600 DEG C isothermal holding 4 hours, standing is cooled to room temperature；
(3) it after being cooled to room temperature, collects sintered material and to be crushed, ball milling, that is, TiCxO1-x powder is prepared.
The processing step that aluminium oxide-titanium carbon oxygen solid solution composite ceramics are specifically prepared are as follows:
(1) 95:5 ~ 50:50 by weight percentage by aluminium oxide and titanium carbon oxygen solid solution crushing grinding and is mixed, and must be mixed Grain, hybrid particles are placed in ball grinder, make ball-milling medium with dehydrated alcohol, and ball-milling treatment simultaneously collects to obtain slurry, dry, powder processed Obtain ball milling powder；
(2) ball milling powder is added in graphite jig, the compression moulding at 10~20MPa, blank must be suppressed and be placed in electric discharge Vacuum-sintering in plasma sintering furnace, control sintering temperature are 1400~1600 DEG C, and the rate of heat addition is 10~50 DEG C/min, are burnt Knot pressure power is 10~50MPa, 30~120min of heat preservation sintering, and it is compound can be prepared into the aluminium oxide-titanium carbon oxygen solid solution Ceramic material.
The present invention is compared with other methods, and advantageous effects are:
Technical solution of the present invention forms solid solution using titanium carbide-titanium dioxide (titanium monoxide) at high temperature, can form increasing Strong phase-sintering aid solid solution, since the composite solid solution material of preparation is mainly slit-shaped central hole structure, there are part macropores And micropore is not present, architectural characteristic mainly based on loose and porous structure, is added in material as additive use Portion, using Ti-C-O solid solution simultaneously as reinforced phase and sintering aid, improve alumina powder be sintered at a lower temperature and The uniformity of powder sintering, to prepare high hardness high toughness aluminium oxide-oxidation of coal titanium composite ceramics.
Detailed description of the invention
Fig. 1 is aluminium oxide of the present invention-oxidation of coal titanium composite ceramics process flow chart；
Fig. 2 is the obtained composite ceramics scanning electron microscope (SEM) photograph of implementation column 7；
Fig. 3 is the composite ceramics Vickers hardness impression figure being prepared in embodiment 9.
Specific embodiment
The content of present invention is described in further detail below with reference to specific embodiment, without will limit power of the present invention The range of force request protection.
By TiC powder and TiO2,8:2 is mixed in molar ratio, ball milling 3 hours in high energy ball mill；Powder after ball milling passes through It is dry, it is put into after compression moulding in high temperature furnace and handles 4 hours for 1400 degree under protection of argon gas, then cool to room temperature；After sintering Block by broken, ball milling, that is, TiCxO1-x powder is prepared, preparation-obtained TiCxO1-x powder is pressed with alumina powder According to 95:5 weight ratio proportion speed mixing, ball-milling medium is made with dehydrated alcohol, together after ball milling, slurry passes through drying, powder processed；It will Powder after ball milling is fitted into graphite jig, with 10MPa pressure forming, is then placed in vacuum in discharge plasma sintering furnace and is burnt Knot, sintering temperature are as follows: 1600 °C, the rate of heat addition are as follows: 10 °C/min, pressure 50MPa；Heat preservation 120 minutes, after heat preservation, Decrease temperature and pressure and aluminium oxide-oxidation of coal titanium composite ceramics, Vickers hardness 18GPa can successfully be prepared.
By TiC powder and TiO2,2:8 is mixed in molar ratio, ball milling 3 hours in high energy ball mill；Powder after ball milling passes through It is dry, it is put into after compression moulding in high temperature furnace and handles 4 hours for 1600 degree under protection of argon gas, then cool to room temperature；After sintering Block by broken, ball milling, that is, TiCxO1-x powder is prepared, preparation-obtained TiCxO1-x powder is pressed with alumina powder According to 80:20 weight ratio proportion speed mixing, ball-milling medium is made with dehydrated alcohol, together after ball milling, slurry passes through drying, powder processed； Powder after ball milling is fitted into graphite jig, with 20MPa pressure forming, is then placed in vacuum in discharge plasma sintering furnace Sintering, sintering temperature are as follows: 1500 °C, the rate of heat addition are as follows: 50 °C/min, pressure 10MPa；Heat preservation 60 minutes, after heat preservation, Decrease temperature and pressure and aluminium oxide-oxidation of coal titanium composite ceramics, Vickers hardness 17GPa can successfully be prepared.
By TiC powder and TiO powder, 8:2 is mixed in molar ratio, ball milling 3 hours in high energy ball mill；Powder warp after ball milling It crosses and dries, be put into after compression moulding in high temperature furnace and handle 4 hours for 1400 degree under protection of argon gas, then cool to room temperature；Sintering By broken, ball milling TiCxO1-x powder is prepared, by preparation-obtained TiCxO1-x powder and alumina powder in block afterwards According to 50:50 weight ratio proportion speed mixing, ball-milling medium is made with dehydrated alcohol, together after ball milling, slurry passes through drying, system Powder；Powder after ball milling is fitted into graphite jig, with 20MPa pressure forming, is then placed in discharge plasma sintering furnace Vacuum-sintering, sintering temperature are as follows: 1400 °C, the rate of heat addition are as follows: 20 °C/min, pressure 20MPa；Heat preservation 30 minutes, heat preservation knot Shu Hou, decrease temperature and pressure and can successfully be prepared aluminium oxide-oxidation of coal titanium composite ceramics, Vickers hardness 15GPa.
By TiC powder and TiO powder, 5:5 is mixed in molar ratio, ball milling 3 hours in high energy ball mill；Powder warp after ball milling It crosses and dries, be put into after compression moulding in high temperature furnace and handle 4 hours for 1600 degree under protection of argon gas, then cool to room temperature；Sintering By broken, ball milling TiCxO1-x powder is prepared, by preparation-obtained TiCxO1-x powder and alumina powder in block afterwards According to 70:30 weight ratio proportion speed mixing, ball-milling medium is made with dehydrated alcohol, together after ball milling, slurry passes through drying, system Powder；Powder after ball milling is fitted into graphite jig, with 20MPa pressure forming, is then placed in discharge plasma sintering furnace Vacuum-sintering, sintering temperature are as follows: 1500 °C, the rate of heat addition are as follows: 20 °C/min, pressure 30MPa；Heat preservation 60 minutes, heat preservation knot Shu Hou, decrease temperature and pressure and can successfully be prepared aluminium oxide-oxidation of coal titanium composite ceramics, Vickers hardness 17GPa.
By TiC powder and TiO powder, 2:8 is mixed in molar ratio, ball milling 3 hours in high energy ball mill；Powder warp after ball milling It crosses and dries, be put into after compression moulding in high temperature furnace and handle 4 hours for 1500 degree under protection of argon gas, then cool to room temperature；Sintering By broken, ball milling TiCxO1-x powder is prepared, by preparation-obtained TiCxO1-x powder and alumina powder in block afterwards According to 70:30 weight ratio proportion speed mixing, ball-milling medium is made with dehydrated alcohol, together after ball milling, slurry passes through drying, system Powder；Powder after ball milling is fitted into graphite jig, with 20MPa pressure forming, is then placed in discharge plasma sintering furnace Vacuum-sintering, sintering temperature are as follows: 1500 °C, the rate of heat addition are as follows: 20 °C/min, pressure 30MPa；Heat preservation 60 minutes, heat preservation knot Shu Hou, decrease temperature and pressure and can successfully be prepared aluminium oxide-oxidation of coal titanium composite ceramics, Vickers hardness 17GPa.
Performance detection is carried out to the embodiment 1 of technical solution of the present invention preparation, its scanning electron microscope is predominantly detected and Vickers is hard Degree, the specific picture that detects are shown in Figure of description.
As seen from the figure, composite ceramic material prepared by the present invention has excellent mechanical property and architectural characteristic.

Claims (3)

1. a kind of aluminium oxide-titanium carbon oxygen solid solution composite ceramics and preparation method thereof, it is characterised in that: by weight percentage, By following material composition:
Aluminium oxide 50~95%
Titanium carbon oxygen solid solution 5~50%.
2. a kind of aluminium oxide-titanium carbon oxygen solid solution composite ceramics as described in claim 1 and preparation method thereof, feature exists In: the specific preparation step of titanium carbon oxygen solid solution are as follows:
(1) 8:2,6:4,5:5,4:6,2:8 in molar ratio, by TiC powder and TiO2Or the mixing of TiO powder, after the completion of mixing, then in height Ball milling 3 hours in energy ball mill；
(2) after the completion of ball milling, powder after ball milling is collected to obtain, is dried and is put into high temperature furnace after compression moulding, Argon atmosphere protection, 1400~1600 DEG C isothermal holding 4 hours, standing is cooled to room temperature；
(3) it after being cooled to room temperature, collects sintered material and to be crushed, ball milling, that is, TiCxO1-x powder is prepared.
3. a kind of aluminium oxide-titanium carbon oxygen solid solution composite ceramics as described in claim 1 and preparation method thereof, it is characterised in that The processing step that aluminium oxide-titanium carbon oxygen solid solution composite ceramics are specifically prepared are as follows:
(1) 95:5 ~ 50:50 by weight percentage by aluminium oxide and titanium carbon oxygen solid solution crushing grinding and is mixed, and must be mixed Grain, hybrid particles are placed in ball grinder, make ball-milling medium with dehydrated alcohol, and ball-milling treatment simultaneously collects to obtain slurry, dry, powder processed Obtain ball milling powder；
(2) ball milling powder is added in graphite jig, the compression moulding at 10~20MPa, blank must be suppressed and be placed in electric discharge Vacuum-sintering in plasma sintering furnace, control sintering temperature are 1400~1600 DEG C, and the rate of heat addition is 10~50 DEG C/min, are burnt Knot pressure power is 10~50MPa, 30~120min of heat preservation sintering, and it is compound can be prepared into the aluminium oxide-titanium carbon oxygen solid solution Ceramic material.
CN201910325941.5A 2019-04-23 2019-04-23 A kind of aluminium oxide-titanium carbon oxygen solid solution composite ceramics and preparation method thereof Withdrawn CN110015899A (en)

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US8110516B2 (en) * 2008-11-28 2012-02-07 Tdk Corporation Sintered body and production method thereof
JP5228850B2 (en) * 2008-11-28 2013-07-03 Ｔｄｋ株式会社 Sintered body

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JP5228850B2 (en) * 2008-11-28 2013-07-03 Ｔｄｋ株式会社 Sintered body

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