CN108503356A - A kind of zirconia oxygen analyzer zirconium pipe and preparation method thereof - Google Patents
A kind of zirconia oxygen analyzer zirconium pipe and preparation method thereof Download PDFInfo
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- CN108503356A CN108503356A CN201810492858.2A CN201810492858A CN108503356A CN 108503356 A CN108503356 A CN 108503356A CN 201810492858 A CN201810492858 A CN 201810492858A CN 108503356 A CN108503356 A CN 108503356A
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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Abstract
The invention belongs to instrument analysis technology field, it is related to a kind of zirconia oxygen analyzer zirconium pipe and preparation method thereof.The zirconium pipe is in addition to mainly containing zirconium oxide, the also yttrium oxide containing molar percentage 3 8%.Using zirconia oxygen analyzer zirconium pipe and preparation method thereof of the present invention, the zirconia oxygen analyzer being prepared can be made to have both good density, intensity, electric conductivity and thermal shock resistance with zirconium pipe.
Description
Technical field
The invention belongs to instrument analysis technology field, it is related to a kind of zirconia oxygen analyzer zirconium pipe and preparation method thereof.
Background technology
Zirconia oxygen analyzer is because of high sensitivity, stability is good, fast response time and simple structure the advantages that due to are extensive
Applied to industries such as petrochemical industry, metallurgy, electric power, light industrys.Wherein zirconia oxygen analyzer is measured by continuous, real-time, dynamic
Oxygen content in Burning Process for Industrial Boiler in discharge gas reaches and improves SO in fuel economy and reduction flue gas2、NOxRow
Purpose high-volume, to realize the energy-saving and emission-reduction of Industrial Boiler.
The critical component of zirconia oxygen analyzer is zirconium pipe, and zirconium pipe is prepared by yttrium oxide stabilized zirconium oxide material.
Since zirconia oxygen analyzer requires in high temperature, there are gas shock and corrosive environment in long-term accurately measure flue gas
Oxygen content, therefore, the zirconium pipe of function admirable not only require good mechanical performance and thermal shock resistance, it is also desirable to have good
Good electric conductivity.
As disclosed in corresponding Chinese patent application, zirconium pipe is the yttria-stabilized zirconia two using 3-8%mol at present
First system is prepared by hot die-casting molding (such as CN101832964) or the method for being injection moulded (such as CN1808109).When
For yttria levels in 8%mol, sintered zirconium oxide is in full cubic phase structure, and electric conductivity is most strong, but flexural strength
Obviously weaken with thermal shock resistance；When yttria levels are 3%mol, flexural strength and thermal shock resistance reach maximum value,
But electric conductivity weakens.
For zirconia material, mechanics, thermodynamics and chemical property are contradictory, to solve this contradiction, are passed through
It is always zirconia material development field focus of attention to improve formula and study new preparation process to improve comprehensive performance.
The forming method of zirconium pipe is another principal element for influencing its density and intensity, and traditional zirconium pipe forming method has heat
Die cast process and injection moulding.The advantages of hot die-casting molding method be small investment, it is simple for process, be suitable for industrialized production；
The disadvantage is that due to, as binder, must first be dewaxed before sintering, such time length, high energy consumption, product are consistent using a large amount of paraffin
Property is poor, zirconium pipe density is low, yield rate is low.The advantages of injection moulding be Automation of Manufacturing Process degree height, green body precision size,
It is easily controllable；The disadvantage is that excluding these using more organic binder (such as polyethylene, epoxy resin), in sintering process has
Machine substance time consumption and energy consumption.And since hot die-casting molding method and injection moulding belong to low pressure molding, while preparation process makes
Use more organic matter as binder, therefore biscuit and sintered zirconium pipe all there is density and intensity is relatively low, thermal shock resistance
The problem of difference.
Invention content
The present invention primary and foremost purpose be to provide a kind of zirconia oxygen analyzer zirconium pipe, with can have both good density,
Intensity, electric conductivity and thermal shock resistance.
In order to achieve this, in the embodiment on basis, the present invention provides a kind of zirconia oxygen analyzer zirconium pipe, institute
The zirconium pipe stated is in addition to mainly containing zirconium oxide, the also yttrium oxide containing molar percentage 3-8%.
In a preferred embodiment, the present invention provides a kind of zirconia oxygen analyzer zirconium pipe, wherein described
Zirconium pipe is in addition to mainly containing zirconium oxide, the also yttrium oxide containing molar percentage 8%.
In a preferred embodiment, the present invention provides a kind of zirconia oxygen analyzer zirconium pipe, wherein described
Al of the zirconium pipe also containing molar percentage 0.5-3%2O3。
Second object of the present invention is to provide a kind of preparation method of zirconia oxygen analyzer zirconium pipe as described above, with
The zirconia oxygen analyzer being prepared can be made to have both good density, intensity, electric conductivity and thermal shock resistance with zirconium pipe.
In order to achieve this, in the embodiment on basis, the present invention provides a kind of zirconia oxygen analyzer as described above
With the preparation method of zirconium pipe, the preparation method includes the following steps：
(1) prepared by powder：By Y2O3With hot nitric acid dissolve after with ZrOCl2With Al (NO3)3Solution is uniformly mixed, and precipitation is added
Agent ammonium hydroxide, gained sediment is washed, is calcined after dry, grinding, and calcined product adds binder grinding and is granulated；
(2) vibration feeding：The powder that grinding is granulated is fitted under the vibrations of vibrations equipment in rubber mold；
(3) biscuit is suppressed：The rubber mold for filling powder is put into cold isostatic press, zirconium Guan Su is obtained through hydrostatic profile
Base；
(4) pre-burning is processed：By zirconium pipe biscuit arrangement (preferably Open Side Down arranges) in Muffle furnace, heating pre-burning postcooling is simultaneously
It is machined, to reach design size requirement；
(5) high temperature sintering：Zirconium pipe biscuit arrangement (preferably Open Side Down arranges) after pre-burning is processed is in corundum sagger
It is put into high temperature furnace, heating is sintered, and zirconia oxygen analyzer zirconium pipe is obtained after cooling.
In a preferred embodiment, the present invention provides a kind of system of zirconia oxygen analyzer zirconium pipe as described above
In Preparation Method, wherein step (1), the Y2O3、ZrOCl2、Al(NO3)3Mixing molar ratio be 8:89:6-8:91.5:1.
In a preferred embodiment, the present invention provides a kind of system of zirconia oxygen analyzer zirconium pipe as described above
In Preparation Method, wherein step (1), the washing is that deionized water and ethanol solution wash；The drying is freeze-drying.
In a preferred embodiment, the present invention provides a kind of system of zirconia oxygen analyzer zirconium pipe as described above
In Preparation Method, wherein step (1), the calcination temperature is 700-900 DEG C, time 1-3h.
In a preferred embodiment, the present invention provides a kind of system of zirconia oxygen analyzer zirconium pipe as described above
In Preparation Method, wherein step (2), the vibration frequency of the vibrations equipment is 25-30Hz.
In a preferred embodiment, the present invention provides a kind of system of zirconia oxygen analyzer zirconium pipe as described above
In Preparation Method, wherein step (3), the pressure of the hydrostatic profile is 180-200MPa.
In a preferred embodiment, the present invention provides a kind of system of zirconia oxygen analyzer zirconium pipe as described above
In Preparation Method, wherein step (4), the pre-burning is to be warming up to 800-1000 DEG C with the heating rate of 1-3 DEG C/min to carry out in advance
It burns.
In a preferred embodiment, the present invention provides a kind of system of zirconia oxygen analyzer zirconium pipe as described above
In Preparation Method, wherein step (5), the program for the sintering that heats up is：
It is warming up to 800-1000 DEG C of heat preservation 1-2h with the heating rate of 3-5 DEG C/min, later with same heating rate liter
Temperature to 1350-1500 DEG C heat preservation 2-4h.
The beneficial effects of the present invention are utilize zirconia oxygen analyzer zirconium pipe and preparation method thereof of the present invention, energy
The zirconia oxygen analyzer being prepared enough is set to have both good density, intensity, electric conductivity and thermal shock resistance with zirconium pipe.
In the present invention, appropriate Al is adulterated in yttrium oxide fully stabilized zirconia 8YSZ2O3, sintered zirconium Guan Bao can be made
While demonstrate,proving electric conductivity, bending resistance and thermal shock resistance greatly improve.Moreover, the preparation method of the present invention：
(1) appropriate Al is added2O3It is also beneficial to reduce sintering temperature and improves sintered density；
(2) it feeds under the vibration frequency of 25-30Hz, the filling of powder is uniformly closely knit, and forming of green body is good；
(3) isostatic pressing belongs to super-pressure (180-200MPa) molding, molding biscuit density height, isotropism, finished product
Rate is high；
(4) medium temperature pre-sinter process can increase biscuit intensity to be machined, and reach the accurate control of zirconium pipe size；
(5) zirconia sintered body grain size is uniform after high temperature sintering, crystal boundary is apparent, and consistency is high, is conducive to enhance zirconium
The intensity and chemical property of pipe；
(6) entire molding and sintering process stablize easily-controllable, energy- and time-economizing.
Therefore, the zirconium pipe even compact, flexural strength of preparation method of the invention preparation are high, have good electric conductivity
Energy and thermal shock resistance.
Specific implementation mode
The specific implementation mode of the present invention is further illustrated with reference to embodiments.
Embodiment 1：The preparation (one) of zirconia oxygen analyzer zirconium pipe
By Y2O3With hot nitric acid dissolve after with ZrOCl2With Al (NO3)3Solution is uniformly mixed, and the molar ratio of three is 8:
91.5:1.Precipitating reagent ammonium hydroxide is added, gained sediment carries out after deionized water and ethanol solution washing, freeze-drying, grinding
Calcining (temperature is 700 DEG C, time 3h), calcined product adds binder grinding and is granulated.The powder that grinding is granulated is being shaken
Dynamic frequency is to be packed into design size in the shock platforms (0.5 type of ZP-0.5 X, the first vibrating machine factory of Xinxiang City) of 25Hz
Ram-jolt is filled in rubber mold.Then the rubber mold for filling Zirconium powder is put into cold isostatic press (LDJ200/1000-
300 types, Chuan Xi Machines Plants), in the case where pressure is 180MPa, isostatic pressing obtains zirconium pipe biscuit.Then by the zirconium pipe biscuit of acquisition
It is placed in Muffle furnace (KSS-1400 DEG C of type, Luoyang Lu Wei kilns Co., Ltd), 800 is warming up to the heating rate of 1 DEG C/min
Then natural cooling after DEG C is machined to reach design size.Finally by the zirconium pipe biscuit after mechanical processing be open to
Under be arranged in corundum sagger and be put into high temperature furnace (KSS-1700 DEG C of type, Luoyang Lu Wei kilns Co., Ltd), with heating rate 3
DEG C/min be warming up to 800 DEG C heat preservation 2h, later with same heating rate be warming up to 1350 DEG C heat preservation 4h after furnace cooling, you can
Obtain boiler oxygen analysis instrument zirconium pipe.The zirconium pipe contains 0.5%molAl2O3With the yttrium oxide of 8mol%.
Embodiment 2：The preparation (two) of zirconia oxygen analyzer zirconium pipe
By Y2O3With hot nitric acid dissolve after with ZrOCl2With Al (NO3)3Solution is uniformly mixed, and the molar ratio of three is 8:
90.5:3.Precipitating reagent ammonium hydroxide is added, gained sediment carries out after deionized water and ethanol solution washing, freeze-drying, grinding
Calcining (temperature is 800 DEG C, time 2h), calcined product adds binder grinding and is granulated.The powder that grinding is granulated is being shaken
Dynamic frequency is to be packed into design size in the vibrations equipment (0.5 type of ZP-0.5 X, the first vibrating machine factory of Xinxiang City) of 28Hz
Ram-jolt is filled in rubber mold.Then the rubber mold for filling Zirconium powder is put into cold isostatic press (LDJ200/1000-
300 types, Chuan Xi Machines Plants), in the case where pressure is 190MPa, isostatic pressing obtains zirconium pipe biscuit.Then by the zirconium pipe biscuit of acquisition
It is placed in Muffle furnace (KSS-1400 DEG C of type, Luoyang Lu Wei kilns Co., Ltd), 900 is warming up to the heating rate of 2 DEG C/min
Then natural cooling after DEG C is machined to reach design size.Finally by the zirconium pipe biscuit after mechanical processing be open to
Under be arranged in corundum sagger and be put into high temperature furnace (KSS-1700 DEG C of type, Luoyang Lu Wei kilns Co., Ltd), with heating rate 4
DEG C/min be warming up to 900 DEG C heat preservation 2h, later with same heating rate be warming up to 1400 DEG C heat preservation 3h after furnace cooling, you can
Obtain boiler oxygen analysis instrument zirconium pipe.The zirconium pipe contains 1.5%molAl2O3With the yttrium oxide of 8mol%.
Embodiment 3：The preparation (three) of zirconia oxygen analyzer zirconium pipe
By Y2O3With hot nitric acid dissolve after with ZrOCl2With Al (NO3)3Solution is uniformly mixed, and the molar ratio of three is 8:89:
6.Precipitating reagent ammonium hydroxide is added, gained sediment is calcined after deionized water and ethanol solution washing, freeze-drying, grinding
(temperature is 900 DEG C, time 1h), calcined product adds binder grinding and is granulated.The powder that grinding is granulated is in vibrations frequency
Rate is that the rubber for designing size is packed into the shock platforms (0.5 type of ZP-0.5 X, the first vibrating machine factory of Xinxiang City) of 30Hz
Ram-jolt is filled in mold.Then the rubber mold for filling Zirconium powder is put into cold isostatic press (LDJ200/1000-300
Type, Chuan Xi Machines Plants), in the case where pressure is 200MPa, isostatic pressing obtains zirconium pipe biscuit.Then the zirconium pipe biscuit of acquisition is set
In Muffle furnace (KSS-1400 DEG C of type, Luoyang Lu Wei kilns Co., Ltd), 1000 DEG C are warming up to the heating rate of 3 DEG C/min
Then natural cooling afterwards is machined to reach design size.Finally by the zirconium pipe biscuit after mechanical processing, Open Side Down
Be arranged in corundum sagger and be put into high temperature furnace (KSS-1700 DEG C of type, Luoyang Lu Wei kilns Co., Ltd), with 5 DEG C of heating rate/
Min be warming up to 1000 DEG C heat preservation 1h, later with same heating rate be warming up to 1500 DEG C heat preservation 2h after furnace cooling, you can obtain
Obtain boiler oxygen analysis instrument zirconium pipe.The zirconium pipe contains 3%molAl2O3With the yttrium oxide of 8mol%.
Embodiment 4：The detection of zirconia oxygen analyzer zirconium pipe is prepared
The zirconia oxygen analyzer that embodiment 1-3 is prepared carried out respectively with zirconium pipe relative density, flexural strength,
The detection of thermal shock number and conductivity, acquired results are as shown in table 1 below.
Wherein：
Relative density is actual density and theoretical density (6.27g/cm3) ratio.Actual density is measured using drainage,
Its method is to weigh zirconium pipe respectively in air and the weight G that is completely immersed in water with one thousandth balance1And G2, then practical close
Degree is G1/(G1-G2)。
Flexural strength using three-point bending method (method referring to：GB6569-2006 fine ceramics bending strength test side
Method) it measures, instrument is the Japanese all-round experimental machine of Shimadzu AG-2000A types refractory ceramics.
The test method of thermal shock number is：Zirconium pipe is quickly put into from room temperature state in 800 DEG C of high temperature Muffle furnace, and
5min is kept the temperature, is then quickly moved in air, after sample is completely cooling, and is put into 800 DEG C of high temperature Muffle furnace, this mistake
Journey is a cycle, repeatedly.
It is Shanghai Huachen instrument company CHI660A electrochemistry that the detection of conductivity, which uses AC impedance spectrometry, instrument,
Work station.
The testing result for the zirconia oxygen analyzer zirconium pipe that 1 embodiment 1-3 of table is prepared
By above-mentioned detection and analysis result it is found that nationality had both by the zirconium pipe that is prepared of preparation method of the present invention it is good close
Degree, intensity, electric conductivity and thermal shock resistance.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.If in this way, belonging to the model of the claims in the present invention and its equivalent technology to these modifications and changes of the present invention
Within enclosing, then the present invention is also intended to include these modifications and variations.Above-described embodiment or embodiment are only to the present invention
For example, the present invention can also be implemented with other ad hoc fashions or other particular form, without departing from the present invention's
Main idea or substantive characteristics.Therefore, it is regarded as from the point of view of the embodiment of description is in terms of any illustrative and non-limiting.This
The range of invention should be illustrated that any variation equivalent with the intention and range of claim also should include by appended claims
Within the scope of the invention.
Claims (10)
1. a kind of zirconia oxygen analyzer zirconium pipe, it is characterised in that：The zirconium pipe also contains in addition to mainly containing zirconium oxide
The yttrium oxide of molar percentage 3-8%.
2. zirconia oxygen analyzer according to claim 1 zirconium pipe, it is characterised in that：The zirconium pipe also contain mole
The Al of percentage 0.5-3%2O3。
3. a kind of preparation method of zirconia oxygen analyzer according to claim 2 zirconium pipe, which is characterized in that described
Preparation method includes the following steps：
(1) prepared by powder：By Y2O3With hot nitric acid dissolve after with ZrOCl2With Al (NO3)3Solution is uniformly mixed, and precipitating reagent is added
Ammonium hydroxide, gained sediment is washed, is calcined after dry, grinding, and calcined product adds binder grinding and is granulated；
(2) vibration feeding：The powder that grinding is granulated is fitted under the vibrations of vibrations equipment in rubber mold；
(3) biscuit is suppressed：The rubber mold for filling powder is put into cold isostatic press, zirconium pipe biscuit is obtained through hydrostatic profile；
(4) pre-burning is processed：Zirconium pipe biscuit is arranged in Muffle furnace, the pre-burning postcooling that heats up simultaneously is machined, and is set to reach
Count size requirement；
(5) high temperature sintering：Zirconium pipe biscuit after pre-burning is processed, which is arranged in corundum sagger, is put into high temperature furnace, and heating is burnt
Knot obtains zirconia oxygen analyzer zirconium pipe after cooling.
4. preparation method according to claim 3, it is characterised in that：In step (1), the Y2O3、ZrOCl2、Al
(NO3)3Mixing molar ratio be 8:89:6-8:91.5:1.
5. preparation method according to claim 3, it is characterised in that：In step (1), the washing be deionized water and
Ethanol solution washs；The drying is freeze-drying.
6. preparation method according to claim 3, it is characterised in that：In step (1), the calcination temperature is 700-
900 DEG C, time 1-3h.
7. preparation method according to claim 3, it is characterised in that：In step (2), the vibrations frequency of the vibrations equipment
Rate is 25-30Hz.
8. preparation method according to claim 3, it is characterised in that：In step (3), the pressure of the hydrostatic profile is
180-200MPa。
9. preparation method according to claim 3, it is characterised in that：In step (4), the pre-burning be with 1-3 DEG C/
The heating rate of min is warming up to 800-1000 DEG C of progress pre-burning.
10. preparation method according to claim 3, it is characterised in that：In step (5), the program for the sintering that heats up is：
It is warming up to 800-1000 DEG C of heat preservation 1-2h with the heating rate of 3-5 DEG C/min, is warming up to later with same heating rate
1350-1500 DEG C of heat preservation 2-4h.
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| CN201810492858.2A CN108503356A (en) | 2018-05-22 | 2018-05-22 | A kind of zirconia oxygen analyzer zirconium pipe and preparation method thereof |
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| CN201810492858.2A CN108503356A (en) | 2018-05-22 | 2018-05-22 | A kind of zirconia oxygen analyzer zirconium pipe and preparation method thereof |
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|---|---|---|---|---|
| CN1249287A (en) * | 1998-09-25 | 2000-04-05 | 重庆渝伦高技术陶瓷有限公司 | Ceramic block gauge material and its making technology |
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| US20180134624A1 (en) * | 2015-04-27 | 2018-05-17 | Suntech Advanced Ceramics (Shenzhen) Co., Ltd. | Zirconium oxide composite ceramic and preparation method therefor |
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2018
- 2018-05-22 CN CN201810492858.2A patent/CN108503356A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1249287A (en) * | 1998-09-25 | 2000-04-05 | 重庆渝伦高技术陶瓷有限公司 | Ceramic block gauge material and its making technology |
| CN101967057A (en) * | 2010-10-14 | 2011-02-09 | 北京科技大学 | Zirconium oxide-based solid electrolyte powder for automobile oxygen sensor and preparation method thereof |
| US20180134624A1 (en) * | 2015-04-27 | 2018-05-17 | Suntech Advanced Ceramics (Shenzhen) Co., Ltd. | Zirconium oxide composite ceramic and preparation method therefor |
| CN106938931A (en) * | 2017-03-13 | 2017-07-11 | 南京云启金锐新材料有限公司 | High purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 周欣燕等: "( ZrO2) 0.96 ( Y2O3) 0.03( Al2O3) 0.01陶瓷的制备及性能研究", 《稀有金属》 * |
| 周欣燕等: "Al2O3掺杂8YSZ固体电解质的烧结及性能研究", 《材料开发与应用》 * |
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