CN101148351A - High-purity compact aluminum oxide ceramic supporting element and manufacturing method thereof - Google Patents
High-purity compact aluminum oxide ceramic supporting element and manufacturing method thereof Download PDFInfo
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- CN101148351A CN101148351A CNA2007100460378A CN200710046037A CN101148351A CN 101148351 A CN101148351 A CN 101148351A CN A2007100460378 A CNA2007100460378 A CN A2007100460378A CN 200710046037 A CN200710046037 A CN 200710046037A CN 101148351 A CN101148351 A CN 101148351A
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Abstract
The present invention relates to support member of high purity compact alumina ceramic and its making process. The support member consists of Al2O3 99.6-99.98 wt%, MgO 0.01-0.3 wt% and composite additive 0.01-0.3 wt%. It has high compactness, high mechanical strength, high hardness, excellent micro structure, precise shape and size and comprehensive performance meeting the requirement for use in precise navigation engineering instrument, and is one structure with fine through holes or ultra thin wall in high size precision and locating precision.
Description
Technical field
The present invention relates to a kind of insulated support and manufacture method thereof, especially relate to high-purity compact aluminum oxide ceramic supporting element and manufacture method thereof.
Background technology
High-purity compact aluminum oxide ceramic supporting element is the key part of precision navigation Engineering Control instrument, for guaranteeing that precision navigation Engineering Control instrument has high precision and reliability, require precision navigation Engineering Control instrument to reach the superior performance standard with insulativity, density, physical strength and the hardness of ceramic component, microstructure of products, dimensional precision etc.The high-insulativity of high-purity compact aluminum oxide ceramic, high physical and chemical stability and dimensional stability etc. can satisfy the requirement of precision navigation Engineering Control instrument.But the over-all properties of the alumina-ceramic spare of Xiao Shouing but is difficult to meet the demands in the market.For example: CN 1730596A discloses a kind of " high purity aluminum oxide seal ring and manufacture method thereof ", and its volume density and physical strength are too low; CN 1412148A discloses a kind of " transparent alumina goods and manufacture method thereof ", this document relates to the manufacture method of a kind of injection moulding or hot injection molding transparent alumina goods, can be made into complex-shaped, accurate in size polycrystal alumina goods, but the fine and close transparent alumina of being mentioned degreasing at a slow speed at low temperatures, sintering temperature is preferably in 1750~1850 ℃ carrying out, complex process not only, and be unfavorable for the refinement of stupalith crystal grain and the raising of density, be difficult to adapt to preparation with support electrode goods thick than heavy wall.
Summary of the invention
Purpose of the present invention is exactly high-purity compact aluminum oxide ceramic supporting element and the manufacture method thereof that a kind of high-compactness, high mechanical strength and hardness are provided for the defective that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions: high-purity compact aluminum oxide ceramic supporting element is characterized in that the composition of this strut member is: Al
2O
399.6wt%~99.98wt%, MgO0.01wt%~0.3wt%, composite additive 0.01wt%~0.3wt%.
The technical performance index of this strut member is as follows: Al
2O
3Content is 99.6wt%~99.98wt%, and volume density is 3.95~3.97g/cm
3, hardness (Hv) is 18GPa, folding strength is greater than 400MPa.
Described composite additive is selected from La
2O
3, Nd
2O
5, Y
2O
3, Yb
2O
3, ZrO
2In one or more.
Described strut member comprises heavy wall strut member or thin-walled strut member, the wall thickness of described heavy wall strut member greater than 6mm, have the pore of 1~9 or more a plurality of perforations, the wall thickness of described thin-walled strut member is 0.2~0.5mm.
The manufacture method of high-purity compact aluminum oxide ceramic supporting element is characterized in that, this method may further comprise the steps:
(1) with content more than or equal to 99.99wt%Al
2O
3High purity aluminium oxide powder 99.6wt%~99.98wt%, contain magnesian soluble salt 0.01wt%~0.3wt%, soluble salt 0.01wt%~0.3wt% of containing the composite additive component carries out weighing respectively;
(2) powder and the soluble salt with weighing in the step (1) places the mill jar, and the volume by 1: 2~2.8 adds pure water, and mixed grinding 4~8 hours is pressed 0.4wt%~1.2wt% again and added the moulding wedding agent, obtains alumina slurry;
(3) with alumina slurry oven dry, granulation, obtain the granulation powder;
(4) the granulation powder is placed be pressed into predetermined shape in the grinding tool, impose 180~220Mpa pressure again, CIP (isostatic cool pressing) moulding obtains the blank of moulding;
(5) blank to moulding carries out machining, and preprocessing becomes needed blank shape and size;
(6) place in the high temperature sintering furnace, 800~1150 ℃ of following pre-burnings 1~4 hour;
(7) 1580~1700 ℃ of following high temperature sinterings 1~4 hour, obtain high-purity compact aluminum oxide ceramic supporting element.
The content of the Alpha-alumina of described high purity aluminium oxide powder is more than or equal to 99.99wt%, and one time grain fineness number is less than or equal to 1 μ m.
Described soluble salt comprises nitrate.
Described pure water comprises the deionization pure water.
Described moulding wedding agent comprises PVA.
The furnace atmosphere of described high temperature sintering furnace comprises oxidizing atmosphere, reducing atmosphere, inert atmosphere or the vacuum condition under the normal atmosphere.
The invention solves the gordian technique difficult point of high-purity compact aluminum oxide ceramic supporting element, compare with existing alumina-ceramic spare, the purity of alumina-ceramic spare of the present invention (alumina content) is brought up to 99.7wt%~99.98wt% from 99.5wt%, and volume density is from 3.85~3.93g/cm
3Bring up to 3.95~3.97g/cm
3, bending strength is brought up to 400~430MPa from 360~370MPa, and hardness (Hv) reaches 18~18.2GPa, and grain-size is 3~5 μ m; The strut member heavy wall connects pore and is of a size of 0.30~2.80mm greater than 6mm, and dimensional precision reaches ± 0.005mm, and the location dimension precision that connects pore reaches 0.05mm.
The present invention also is applicable to the support frame of producing high-precision ultra-thin-wall, and the wall thickness of support frame reaches 0.2mm ± 0.02mm, can guarantee high technology ceramics support frame high-insulativity, high physical and chemical stability and dimensional stability.
Compared with prior art, alumina-supported part of the present invention has high-compactness, high mechanical strength and hardness, good microstructure, accurate shape and size, over-all properties can satisfy the requirement of precision navigation Engineering Control instrument, have a plurality of perforation pores or ultra-thin-wall structure, pore size and pore location are accurately.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
A kind of manufacture method of high-purity compact aluminum oxide ceramic supporting element, at first with high purity aluminium oxide powder (content of Alpha-alumina is that 99.99wt%, a grain fineness number are 1 μ m) 99.7wt%~99.75wt%, contain magnesium oxide (MgO) nitrate 0.15wt%~0.2wt%, contain lanthanum trioxide (La
2O
3) nitrate 0.05wt%~0.1wt% carry out weighing respectively, the powder and the nitrate of weighing are placed the mill jar, add the deionization pure water by 1: 2.2 volume, mixed grinding 6 hours, press 0.8wt% again and add PVA, obtain alumina slurry, alumina slurry is dried, granulation, obtain the granulation powder, the granulation powder placed be pressed into predetermined shape in the grinding tool, CIP under 200Mpa pressure (cold all press) moulding obtains the blank of moulding, blank to moulding carries out machining, preprocessing becomes to have 3 shapes that connect the strut member blank of pore, size placed in the vacuum high-temperature sintering stove, 1000 ℃ of pre-burnings 2 hours, 1650 ℃ of high temperature sinterings 2 hours, obtain high-purity compact aluminum oxide ceramic supporting element again; This strut member composition is: Al
2O
399.7wt%, MgO 0.2wt%, La
2O
30.1wt%.
The high-purity compact aluminum oxide ceramic supporting element that obtains is carried out Performance Detection: volume density is 3.96g/cm
3, hardness (Hv) is 18GPa, and bending strength is 406MPa, and average grain size is 4.5 μ m, and 3 sizes that connect pores are respectively 0.30,0.7,1.5mm, and precision be ± 0.005mm that the location dimension precision of perforation pore is 0.05mm.
Embodiment 2
A kind of manufacture method of high-purity compact aluminum oxide ceramic supporting element, at first with high purity aluminium oxide powder (content of Alpha-alumina is that 99.99wt%, a grain fineness number are 1 μ m) 99.75wt%~99.80wt%, contain magnesium oxide (MgO) nitrate 0.1wt%~0.2wt%, contain lanthanum trioxide (La
2O
3) nitrate, ytterbium oxide (Yb
2O
3) nitrate and Neodymium trioxide (Nd
2O
5) nitrate 0.01wt%~0.1wt% carry out weighing respectively, the powder and the nitrate of weighing are placed the mill jar, add the deionization pure water by 1: 2.4 volume, mixed grinding 5 hours, press 1.0wt% again and add PVA, obtain alumina slurry, alumina slurry is dried, granulation, obtain the granulation powder, the granulation powder placed be pressed into predetermined shape in the grinding tool, CIP moulding under 210Mpa pressure obtains the blank of moulding, blank to moulding carries out machining, preprocessing becomes to have 5 shapes that connect the strut member blank of pore, size places in the interior high temperature sintering furnace for the oxidizing atmosphere under the normal atmosphere of stove, 900 ℃ of pre-burnings 3 hours, 1640 ℃ of high temperature sinterings 2.5 hours, obtain high-purity compact aluminum oxide ceramic supporting element again; This strut member composition is: Al
2O
399.75wt%, MgO0.15wt%, La
2O
3+ Yb
2O
3+ Nd
2O
50.1wt%.
The high-purity compact aluminum oxide ceramic supporting element that obtains is carried out Performance Detection: volume density is 3.97g/cm
3, hardness (Hv) is 18.2GPa, and bending strength is 430MPa, and average grain size is 3.8 μ m, and 5 connect that pore is of a size of 0.30,0.7,1.0,1.5,2.0mm, and precision be ± 0.005mm that the location dimension precision of perforation pore is 0.05mm.
Embodiment 3
A kind of manufacture method of high-purity compact aluminum oxide ceramic supporting element, at first with high purity aluminium oxide powder (content of Alpha-alumina is that 99.99wt%, a grain fineness number are 1 μ m) 99.7wt%~99.98wt%, contain magnesium oxide (MgO) nitrate 0.01wt%~0.2wt%, contain yttrium oxide (Y
2O
3) nitrate and zirconium white (ZrO
2) nitrate 0.01wt%~0.2wt% carry out weighing respectively, the powder and the nitrate of weighing are placed the mill jar, add the deionization pure water by 1: 2.6 volume, mixed grinding 7 hours, press 0.6wt% again and add PVA, obtain alumina slurry, alumina slurry is dried, granulation, obtain the granulation powder, the granulation powder placed be pressed into predetermined shape in the grinding tool, CIP moulding under 190Mpa pressure obtains the blank of moulding, blank to moulding carries out machining, preprocessing becomes to have 7 shapes that connect the strut member blank of pore, size places in the interior high temperature sintering furnace for the reducing atmosphere under the normal atmosphere of stove, 1100 ℃ of pre-burnings 1.5 hours, 1700 ℃ of high temperature sinterings 1 hour, obtain high-purity compact aluminum oxide ceramic supporting element again; The composition of this strut member is: Al
2O
399.8wt%, MgO 0.05wt%, Y
2O
3+ ZrO
20.15wt%.
The high-purity compact aluminum oxide ceramic supporting element that obtains is carried out Performance Detection: volume density is 3.95g/cm
3, hardness (Hv) is 18GPa, bending strength is 400MPa, average grain size is 4.8 μ m, 7 connect that pore is of a size of 0.30,0.7,1.0,1.5,1.7,2.0,2.7mm, and precision be ± 0.005mm that the location dimension precision of perforation pore is 0.05mm.
Embodiment 4
A kind of manufacture method of high-purity compact aluminum oxide ceramic supporting element, at first with high purity aluminium oxide powder (content of Alpha-alumina is that 99.99wt%, a grain fineness number are 1 μ m) 99.6wt%~99.7wt%, contain magnesium oxide (MgO) nitrate 0.2wt%~0.3wt%, contain lanthanum trioxide (La
2O
3) nitrate and yttrium oxide (Y
2O
3) nitrate 0.01wt%~0.1wt% carry out weighing (La wherein respectively
2O
3With Y
2O
3Ratio be 1: 1), the powder and the nitrate of weighing are placed the mill jar, add the deionization pure water by 1: 2 volume, mixed grinding 4 hours, press 0.4wt% again and add PVA, obtain alumina slurry, alumina slurry is dried, granulation, obtain the granulation powder, the granulation powder placed be pressed into predetermined shape in the grinding tool, CIP moulding under 180Mpa pressure obtains the blank of moulding, blank to moulding carries out machining, preprocessing becomes to have 9 shapes that connect the strut member blank of pore, size places in the interior high temperature sintering furnace for the inert atmosphere under the normal atmosphere of stove, 1150 ℃ of pre-burnings 1 hour, 1580 ℃ of high temperature sinterings 4 hours, obtain high-purity compact aluminum oxide ceramic supporting element again; The composition of this strut member is: Al
2O
399.6wt%, MgO 0.3wt%, La
2O
3+ Y
2O
30.1wt%.
The high-purity compact aluminum oxide ceramic supporting element that obtains is carried out Performance Detection: volume density is 3.95g/cm
3Hardness (Hv) is 18.0GPa, bending strength is 402MPa, average grain size is 3 μ m, wall thickness is 7mm, 9 sizes that connect pores are respectively 0.30,0.7,1.0,1.1,1.5,2.0,2.3,2.5,2.8mm, and precision be ± 0.005mm that the location dimension precision of perforation pore is 0.05mm.
Embodiment 5
A kind of manufacture method of high-purity compact aluminum oxide ceramic supporting element, at first with high purity aluminium oxide powder (content of Alpha-alumina is that 99.99wt%, a grain fineness number are 1 μ m) 99.94wt%~99.98wt%, contain magnesium oxide (MgO) nitrate 0.01wt%~0.05wt%, contain lanthanum trioxide (La
2O
3) nitrate 0.01wt%~0.05wt% carry out weighing respectively, the powder and the nitrate of weighing are placed the mill jar, add the deionization pure water by 1: 2.8 volume, mixed grinding 8 hours, press 1.2wt% again and add PVA, obtain alumina slurry, alumina slurry is dried, granulation, obtain the granulation powder, the granulation powder placed be pressed into predetermined shape in the grinding tool, CIP moulding under 220Mpa pressure obtains the blank of moulding, blank to moulding carries out machining, preprocessing becomes to have 1 shape that connects the toroidal support blank of pore, size placed in the vacuum high-temperature sintering stove, 800 ℃ of pre-burnings 4 hours, 1680 ℃ of high temperature sinterings 1.5 hours, obtain high-purity compact aluminum oxide ceramic supporting element again; The composition of this strut member is: Al
2O
399.98wt%, MgO 0.01wt%, La
2O
30.01wt%.
The high-purity compact aluminum oxide ceramic supporting element that obtains is carried out Performance Detection: volume density is 3.96g/cm
3, hardness (Hv) is 18GPa, and bending strength is 406MPa, and average grain size is 4.2 μ m, and the toroidal support wall thickness is 0.5mm, 1 connects pore size is 12.7mm.
Embodiment 6
A kind of manufacture method of high-purity compact aluminum oxide ceramic supporting element, at first with high purity aluminium oxide powder (content of Alpha-alumina is that 99.99wt%, a grain fineness number are 1 μ m) 99.6wt%~99.7wt%, contain magnesium oxide (MgO) nitrate 0.1wt%~0.2wt%, contain lanthanum trioxide (La
2O
3) nitrate, yttrium oxide (Y
2O
3) nitrate and zirconium white (ZrO
2) nitrate 0.2wt%~0.3wt% carry out weighing (La wherein respectively
2O
3, Y
2O
3, ZrO
2Ratio be 2: 1: 1), the powder and the nitrate of weighing are placed the mill jar, add the deionization pure water by 1: 2.2 volume, mixed grinding 6 hours, press 0.8wt% again and add PVA, obtain alumina slurry, alumina slurry is dried, granulation, obtain the granulation powder, the granulation powder placed be pressed into predetermined shape in the grinding tool, CIP moulding under 200Mpa pressure obtains the blank of moulding, blank to moulding carries out machining, preprocessing becomes to have 5 shapes that connect the strut member blank of pore, size places in the interior high temperature sintering furnace for the oxidizing atmosphere under the normal atmosphere of stove, 1000 ℃ of pre-burnings 2 hours, 1650 ℃ of high temperature sinterings 2 hours, obtain high-purity compact aluminum oxide ceramic supporting element again; The composition of this strut member is: Al
2O
399.6wt%, MgO 0.1wt%, La
2O
3+ Y
2O
3+ ZrO
20.3wt%.
The high-purity compact aluminum oxide ceramic supporting element that obtains is carried out Performance Detection: volume density is 3.97g/cm
3, hardness (Hv) is 18.2GPa, bending strength is 430MPa, average grain size is 4 μ m, and wall thickness is 6.5mm, and 5 connect that pore is of a size of 0.30,0.7,1.0,1.5,2.0mm, precision is ± 0.005mm that the location dimension precision that connects pore is 0.05mm.
Embodiment 7
A kind of manufacture method of high-purity compact aluminum oxide ceramic support frame, adopt and embodiment 2 identical materials prescriptions, powder process, moulding process and parameter, obtain the blank of moulding, blank to moulding carries out machining, preprocessing becomes shape, the size of needed support frame blank, place in the stove in the high temperature sintering furnace for the oxidizing atmosphere under the normal atmosphere, pre-burning and sintering method that employing and embodiment 2 are identical obtain the high-purity compact aluminum oxide ceramic support frame; The composition of this support frame is: Al
2O
399.75wt%, MgO 0.15wt%, La
2O
3+ Yb
2O
3+ Nd
2O
50.1wt%.
The high-purity compact aluminum oxide ceramic support frame that obtains is carried out Performance Detection: volume density is 3.97g/cm
3, hardness (Hv) is 18.2GPa, and bending strength is 430MPa, and average grain size is 3.8 μ m, and wall thickness is 0.2 ± 0.02mm.
Claims (10)
1. high-purity compact aluminum oxide ceramic supporting element is characterized in that, the composition of this strut member is: Al
2O
399.6wt%~99.98wt%, MgO 0.01wt%~0.3wt%, composite additive 0.01wt%~0.3wt%.
2. high-purity compact aluminum oxide ceramic supporting element according to claim 1 is characterized in that the technical performance index of this strut member is as follows: Al
2O
3Content is 99.6wt%~99.98wt%, and volume density is 3.95~3.97g/cm
3, hardness (Hv) is 18GPa, folding strength is greater than 400MPa.
3. high-purity compact aluminum oxide ceramic supporting element according to claim 1 is characterized in that described composite additive is selected from La
2O
3, Nd
2O
5, Y
2O
3, Yb
2O
3, ZrO
2In one or more.
4. high-purity compact aluminum oxide ceramic supporting element according to claim 1, it is characterized in that, described strut member comprises heavy wall strut member or thin-walled strut member, the wall thickness of described heavy wall strut member greater than 6mm, have the pore of 1~9 or more a plurality of perforations, the wall thickness of described thin-walled strut member is 0.2~0.5mm.
5. the manufacture method of high-purity compact aluminum oxide ceramic supporting element is characterized in that, this method may further comprise the steps:
(1) with content more than or equal to 99.99wt%Al
2O
3High purity aluminium oxide powder 99.6wt%~99.98wt%, contain magnesian soluble salt 0.01wt%~0.3wt%, soluble salt 0.01wt%~0.3wt% of containing the composite additive component carries out weighing respectively;
(2) powder and the soluble salt with weighing in the step (1) places the mill jar, and the volume by 1: 2~2.8 adds pure water, and mixed grinding 4~8 hours is pressed 0.4wt%~1.2wt% again and added the moulding wedding agent, obtains alumina slurry;
(3) with alumina slurry oven dry, granulation, obtain the granulation powder;
(4) the granulation powder is placed be pressed into predetermined shape in the grinding tool, impose 180~220Mpa pressure again, CIP (isostatic cool pressing) moulding obtains the blank of moulding;
(5) blank to moulding carries out machining, and preprocessing becomes needed blank shape and size;
(6) place in the high temperature sintering furnace, 800~1150 ℃ of following pre-burnings 1~4 hour;
(7) 1580~1700 ℃ of following high temperature sinterings 1~4 hour, obtain high-purity compact aluminum oxide ceramic supporting element.
6. the manufacture method of high-purity compact aluminum oxide ceramic supporting element according to claim 5 is characterized in that, the content of the Alpha-alumina of described high purity aluminium oxide powder is more than or equal to 99.99wt%, and one time grain fineness number is less than or equal to 1 μ m.
7. the manufacture method of high-purity compact aluminum oxide ceramic supporting element according to claim 5 is characterized in that, described soluble salt comprises nitrate.
8. the manufacture method of high-purity compact aluminum oxide ceramic supporting element according to claim 5 is characterized in that, described pure water comprises the deionization pure water.
9. the manufacture method of high-purity compact aluminum oxide ceramic supporting element according to claim 5 is characterized in that, described moulding wedding agent comprises PVA.
10. the manufacture method of high-purity compact aluminum oxide ceramic supporting element according to claim 5 is characterized in that, the furnace atmosphere of described high temperature sintering furnace comprises oxidizing atmosphere, reducing atmosphere, inert atmosphere or the vacuum condition under the normal atmosphere.
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