CN102818832B - A kind of porous diffusion barrier limit-current type oxygen sensor and manufacture method thereof - Google Patents
A kind of porous diffusion barrier limit-current type oxygen sensor and manufacture method thereof Download PDFInfo
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- CN102818832B CN102818832B CN201210290833.7A CN201210290833A CN102818832B CN 102818832 B CN102818832 B CN 102818832B CN 201210290833 A CN201210290833 A CN 201210290833A CN 102818832 B CN102818832 B CN 102818832B
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Abstract
The invention discloses a kind of porous diffusion barrier limit-current type oxygen sensor, comprise oxygen pump layer and porous diffusion barrier layer, oxygen pump layer is for adopting La
1-xsr
xga
1-ymg
yo
3- δthe potsherd that material is made, the upper and lower surface of oxygen pump layer is shaped with positive electrode layer and positive electrode layer respectively, and positive and negative electrode layer leads to positive electrode lead and negative electrode lead respectively, and porous diffusion barrier layer is for adopting Al
2o
3the round ceramic thin slice of material sintering, this porous diffusion barrier layer concentric is integrally connected to the lower surface of positive electrode layer, be formed with plane in exposed annular between the porous diffusion upper surface of barrier layer and the connection of positive electrode layer, this annular is sealed with encapsulated layer in plane and on the outer circumference surface of oxygen pump layer, positive electrode layer and positive electrode layer.Its manufacture method comprises blank preparation, high temperature sintering, an electrode layer printing, secondary high-temperature sinters, finished product reburns the steps such as knot.Manufacturing process of the present invention is simple, and stable performance, measurement range are wide, have accuracy of detection high, the feature of response time short and long service life.
Description
Technical field
The present invention relates to a kind of lambda sensor, a kind of limit-current type oxygen sensor that in particularly adopting, warm solid oxygen ion conductor material makes, specifically a kind of porous diffusion barrier limit-current type oxygen sensor and manufacture method thereof.
Background technology
Lambda sensor can be divided into concentration potential type and limit-current type by principle, and limit-current type oxygen sensor can be divided into hole diffusion barrier-type and fine and close diffused.Limit-current type oxygen sensor is high with its measuring accuracy, scope is wide, the response time needs the advantages such as reference gas to obtain applying more and more widely in fields such as metallurgical, food and oxygen techniques soon and not.At present, the exhausted majority of solid electrolyte of limit-current type oxygen sensor is YSZ material, because this material only just has higher oxygen ionic conductivity when temperature is greater than 800 DEG C, this just causes the working temperature of sensor must be greater than 800 DEG C, hot operation brings a series of problem, such as produce at three phase boundary place objectionable impurities, electrode material be difficult to coupling and energy ezpenditure large etc.In order to address these problems, just in the urgent need to reducing the working temperature of sensor, and one of approach finds a kind of solid electrolyte of material substitution YSZ as lambda sensor just in mesophilic range with higher oxygen ionic conductivity.
At present, the middle temperature solid oxygen ion conductor material had been found that in prior art mainly contains δ-Bi
2o
3, CeO
2and La
1-xsr
xga
1-ymg
yo
3-δthree kinds of materials.But due to δ-Bi
2o
3the structural instability of material, can change along with the change of temperature; CeO
2ce in reducing atmosphere
4+easily be reduced into Ce
3+and produce electronic conduction phenomenon, this bi-material is limited by very large when applying.And La
1-xsr
xga
1-ymg
yo
3-δconductivity under equal conditions much superior than YSZ material, and within the scope of very wide partial pressure of oxygen and in reducing atmosphere, there is good stability, therefore this material is considered to most possibly to replace YSZ as middle temperature solid oxygen ion conductor material.
Summary of the invention
Technical matters to be solved by this invention is for above-mentioned prior art present situation, and to be provided in temperature be namely occur good limiting current platform within the scope of 600 DEG C ~ 700 DEG C, and the good a kind of porous diffusion barrier limit-current type oxygen sensor of stable performance, physical strength and manufacture method thereof.This sensor manufacturing process is simple, easy to use, and have oxygen concentration testing scope wide, precision is high, the feature of response time short and long service life.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of porous diffusion barrier limit-current type oxygen sensor, and comprise oxygen pump layer and porous diffusion barrier layer, oxygen pump layer is for adopting La
1-xsr
xga
1-ymg
yo
3-
δ material sinters the round ceramic lamellar body made, and the upper surface of oxygen pump layer and lower surface adopt screen printing technique to be shaped with positive electrode layer and positive electrode layer respectively, positive electrode layer leads to positive electrode lead, and positive electrode layer leads to negative electrode lead, and porous diffusion barrier layer is for adopting Al
2o
3the diameter of material sintering is greater than oxygen pump layer and has the round ceramic thin slice of porous structure, this porous diffusion barrier layer concentric is integrally connected to the lower surface of positive electrode layer, be formed with plane in exposed annular between the porous diffusion upper surface of barrier layer and the connection of positive electrode layer, this annular is sealed with encapsulated layer in plane and on the outer circumference surface of oxygen pump layer, positive electrode layer and positive electrode layer.
For optimizing technique scheme, the measure taked also comprises:
Above-mentioned encapsulated layer is elevated-temperature seal glass glaze; Oxygen pump layer is fine and close La
1-xsr
xga
1-ymg
yo
3-δceramic disks, diameter is about 7.5mm, and thickness is about 0.6mm; Porous diffusion barrier layer is the Al with porous structure
2o
3ceramic disks, diameter is approximately 10.5mm, and thickness is about 0.7mm.
Above-mentioned positive electrode lead and negative electrode lead are respectively used to the both positive and negative polarity being connected power supply.
Above-mentioned La
1-xsr
xga
1-ymg
yo
3-δin material, wherein the span of x and y is respectively 0.1≤x≤0.2 and 0.1≤y≤0.2.
The material of above-mentioned positive electrode layer and positive electrode layer and positive electrode lead and negative electrode lead is platinum.
Above-mentioned positive electrode layer and the thickness of positive electrode layer are 20um.
Present invention also offers a kind of manufacture method of porous diffusion barrier limit-current type oxygen sensor, the method comprises the following steps:
Prepared by blank: first use mould and oil press by La
1-xsr
xga
1-ymg
yo
3-δpowder and Al
2o
3powder is pressed into the porous diffusion barrier layer blank that oxygen pump layer blank that diameter is 10mm and diameter are 13mm respectively;
A high temperature sintering: the porous diffusion barrier layer potsherd above-mentioned oxygen pump layer blank and porous diffusion barrier layer blank being sent into respectively the obtained fine and close oxygen pump layer potsherd of sintering in high temperature sintering furnace and porous structure;
Electrode layer prints: adopt high-precision silk screen printing machine to print positive electrode layer and positive electrode layer respectively at the upper and lower surface of above-mentioned oxygen pump layer potsherd, and draw positive electrode lead and negative electrode lead respectively from positive electrode layer and positive electrode layer simultaneously;
Secondary high-temperature sinters: the one side adopting the mode of platinum slurry adhesion oxygen pump layer potsherd to be had a positive electrode layer and above-mentioned porous spread barrier layer potsherd couple together and together with send in high temperature sintering furnace the lambda sensor blank sintering and obtain integrative-structure;
Finished product sinters again: above-mentioned lambda sensor blank is coated glass glaze after cooling naturally on the outer peripheral face of the porous exposed upper plane of diffusion barrier layer and positive electrode layer, oxygen pump layer, positive electrode layer and again sends into this product obtained of sintering in high temperature sintering furnace.
The time that in an above-mentioned high temperature sintering, oxygen pump layer blank sinters in high temperature sintering furnace is 2h to 6h, and furnace temperature is 1350 DEG C ~ 1500 DEG C; The time that porous diffusion barrier layer blank sinters in high temperature sintering furnace is 3h to 6h, and furnace temperature is 1500 DEG C ~ 1550 DEG C.
In above-mentioned secondary high-temperature sintering, the sintering temperature of high temperature sintering furnace is 900 DEG C ~ 1000 DEG C, and the time is 1h.
During above-mentioned finished product sinters again, the sintering temperature of high temperature sintering furnace is 900 DEG C, and the time is 1h ~ 3h.
Compared with prior art, the oxygen pump layer of lambda sensor of the present invention adopts the conductivity under equal conditions La of larger than YSZ material 2 times to 4 times
1-xsr
xga
1-ymg
yo
3-δmaterial makes, and porous diffusion barrier layer is the Al with porous structure
2o
3potsherd, thus product just can present good performance in mesophilic range, occurs good limiting current platform, and the scope can measuring oxygen concentration is 0 ~ 80%, and the response time is within the scope of 10s ~ 15s.Significantly reduce the situation that conventional oxygen sensor need work under 800 DEG C of hot environments, improve the serviceable life of lambda sensor.Manufacturing process of the present invention is simple, and stable performance, measurement range extensively, have accuracy of detection high, the feature that the response time is short.Can be widely used in fields such as metallurgy, food and oxygens.
Accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment of the present invention;
Fig. 2 is the present invention at the I-V curve map of 650 DEG C;
Fig. 3 is the graph of a relation of limiting current value of the present invention and oxygen concentration;
Fig. 4 is response time curve map of the present invention.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are described in further detail.
Reference numeral is wherein: oxygen pump layer 1; Porous diffusion barrier layer 2; Positive electrode layer 3; Positive electrode layer 4; Encapsulated layer 5; Positive electrode lead 6; Negative electrode lead 7; Power supply 8; Reometer 9.
Shown in Fig. 1, a kind of porous diffusion barrier limit-current type oxygen sensor of the present invention, comprise oxygen pump layer 1 and porous diffusion barrier layer 2, oxygen pump layer 1 is for adopting La
1-xsr
xga
1-ymg
yo
3-δmaterial sinters the round ceramic lamellar body made, and the upper surface of oxygen pump layer 1 and lower surface adopt screen printing technique to be shaped with positive electrode layer 3 and positive electrode layer 4 respectively, positive electrode layer 3 leads to positive electrode lead 6, and positive electrode layer 4 leads to negative electrode lead 7, and porous diffusion barrier layer 2 is for adopting Al
2o
3the diameter of material sintering is greater than oxygen pump layer 1 and has the round ceramic thin slice of porous structure, this porous diffusion barrier layer 2 concentric is integrally connected to the lower surface of positive electrode layer 4, be formed with plane in exposed annular between the porous diffusion upper surface of barrier layer 2 and the connection of positive electrode layer 4, this annular is sealed with encapsulated layer 5 in plane and on the outer circumference surface of oxygen pump layer 1, positive electrode layer 3 and positive electrode layer 41.Oxygen pump layer 1 of the present invention adopts La
1-xsr
xga
1-ymg
yo
3-δmaterial makes, and instead of traditional YSZ material, La
1-xsr
xga
1-ymg
yo
3-δthe conductivity of material is 2 times of YSZ material under equal conditions to 4 times, and has good stability within the scope of very wide partial pressure of oxygen and in reducing atmosphere, is therefore as optimal material in middle temperature solid oxygen ion conductor material.Porous diffusion barrier layer 2 is Al
2o
3material is through sintering the ceramic sheet with porous structure made, and the oxygen molecule therefore in environment can pass through its free diffusing.Product of the present invention is stable work in work at 600 DEG C ~ 700 DEG C, there is good limiting current platform, the scope can measuring oxygen concentration is 0 ~ 80%, response time is within the scope of 10s ~ 15s, there is stable performance, measurement range is wide, accuracy of detection is high, the response time short and feature of long service life.As can see from Figure 1, the present invention operationally can set up reometer 9 in the line.
Encapsulated layer 5 of the present invention is elevated-temperature seal glass glaze.
In embodiment, positive electrode lead 6 and negative electrode lead 7 are respectively used to the both positive and negative polarity being connected power supply 8.
La of the present invention
1-xsr
xga
1-ymg
yo
3-δin material, wherein the span of x and y is respectively 0.1≤x≤0.2 and 0.1≤y≤0.2.
The material of positive electrode layer 3 of the present invention and positive electrode layer 4 and positive electrode lead 6 and negative electrode lead 7 is platinum.
The thickness of positive electrode layer 3 of the present invention and positive electrode layer 4 is 20um.
Oxygen pump layer 1 of the present invention and porous diffusion barrier layer 2 make ceramic disks through sintering, and after sintering, the diameter of oxygen pump layer 1 is about 7.5mm, and thickness is about 0.6mm, and the diameter of porous diffusion barrier layer 2 is approximately 10.5mm, and thickness is about 0.7mm.
Present invention also offers a kind of manufacture method of porous diffusion barrier limit-current type oxygen sensor, the method comprises the following steps:
Prepared by blank: first use mould and oil press by La
1-xsr
xga
1-ymg
yo
3-δpowder and Al
2o
3powder is pressed into the porous diffusion barrier layer blank that oxygen pump layer blank that diameter is 10mm and diameter are 13mm respectively;
A high temperature sintering: the porous diffusion barrier layer potsherd above-mentioned oxygen pump layer blank and porous diffusion barrier layer blank being sent into respectively the obtained fine and close oxygen pump layer potsherd of sintering in high temperature sintering furnace and porous structure;
Electrode layer prints: adopt high-precision silk screen printing machine to print positive electrode layer and positive electrode layer respectively at the upper and lower surface of above-mentioned oxygen pump layer potsherd, and draw positive electrode lead and negative electrode lead respectively from positive electrode layer and positive electrode layer simultaneously;
Secondary high-temperature sinters: the one side adopting the mode of platinum slurry adhesion oxygen pump layer potsherd to be had a positive electrode layer and above-mentioned porous spread barrier layer potsherd couple together and together with send in high temperature sintering furnace the lambda sensor blank sintering and obtain integrative-structure;
Finished product sinters again: above-mentioned lambda sensor blank is coated glass glaze after cooling naturally on the outer peripheral face of the porous exposed upper plane of diffusion barrier layer and positive electrode layer, oxygen pump layer, positive electrode layer and again sends into this product obtained of sintering in high temperature sintering furnace.
The time that in an above-mentioned high temperature sintering, oxygen pump layer blank sinters in high temperature sintering furnace is 2h to 6h, and furnace temperature is 1350 DEG C ~ 1500 DEG C; The time that described porous diffusion barrier layer blank sinters in high temperature sintering furnace is 3h to 6h, and furnace temperature is 1500 DEG C ~ 1550 DEG C.
In above-mentioned secondary high-temperature sintering, the sintering temperature of high temperature sintering furnace is 900 DEG C ~ 1000 DEG C, and the time is 1h.
During above-mentioned finished product sinters again, the sintering temperature of high temperature sintering furnace is 900 DEG C, and the time is 1h ~ 3h.
The principle of work of lambda sensor of the present invention is: during working sensor, power supply 8 applies an operating voltage to sensor, electronics is flowed out by its negative pole, positive electrode layer 4 is flowed into by reometer 9 and negative electrode lead 7, under the catalytic action of platinum with near oxygen molecule react, make oxygen molecule change into oxonium ion; Oxonium ion is pumped into rapidly positive electrode layer 3 under the electric potential difference effect of oxygen pump layer 1 both sides, departs from electronics afterwards, again becomes oxygen molecule, get back in environment and go under the catalytic action of platinum; Because porous diffusion barrier layer 2 possesses porous structure, so the oxygen molecule in environment can be freely spread to positive electrode layer 4 place by it, diffusivity is determined by its porosity and extraneous oxygen concentration; And the pump oxygen ability of oxygen pump layer 1 increases along with the increase of voltage, when being greater than the oxygen molecule diffusivity of porous diffusion barrier layer 2, will occur limiting current platform, namely electric current does not increase with the increase of voltage; Therefore the diffusivity of the oxygen molecule of porous diffusion barrier layer 2 determines the size of limiting current, again because the porosity of the porous diffusion barrier layer 2 prepared is definite value, so extraneous oxygen concentration determines its diffusivity; So extraneous oxygen concentration determines limiting current size, the limiting current that namely different oxygen concentrations is corresponding different.Figure 2 shows that the present invention is when temperature 650 DEG C, the I-V curve map recorded, as can be seen from the figure under different oxygen concentration environment, different limiting current platforms has been there is when voltage is 0.6V-1.2V, read the limiting current value of each limiting current platform, find that itself and oxygen concentration present good linear relationship, as shown in Figure 3.So, apply certain voltage to sensor, according to the current value that reometer 9 shows, the oxygen concentration size in environment can be obtained in conjunction with its linear functional relation, thus reach the object measuring oxygen concentration.Meanwhile, at 650 DEG C, oxygen concentration changes back and forth between 1% and 40%, and the response time curve recorded as shown in Figure 4, can draw from figure, and the rising response time is 10s-15s, and the decline response time is 15s-20s, and the Repeatability of sensor is better.
Claims (1)
1. the manufacture method of a porous diffusion barrier limit-current type oxygen sensor, this porous diffusion barrier limit-current type oxygen sensor comprises oxygen pump layer (1) and porous diffusion barrier layer (2), it is characterized in that: described oxygen pump layer (1) is for adopting La
1-xsr
xga
1-ymg
yo
3-δmaterial sinters the round ceramic lamellar body made, and the upper surface of oxygen pump layer (1) and lower surface adopt screen printing technique to be shaped with positive electrode layer (3) and positive electrode layer (4) respectively, described positive electrode layer (3) leads to positive electrode lead (6), described positive electrode layer (4) leads to negative electrode lead (7), and described porous diffusion barrier layer (2) is for adopting Al
2o
3the diameter of material sintering is greater than oxygen pump layer (1) and has the round ceramic thin slice of porous structure, this porous diffusion barrier layer (2) concentric is integrally connected to the lower surface of positive electrode layer (4), be formed with plane in exposed annular between the upper surface of described porous diffusion barrier layer (2) and the connection of positive electrode layer (4), this annular is sealed with encapsulated layer (5) in plane and on the outer circumference surface of oxygen pump layer (1), positive electrode layer (3) and positive electrode layer (4); Described encapsulated layer (5) is elevated-temperature seal glass glaze; Oxygen pump layer (1) is fine and close La
1-xsr
xga
1-ymg
yo
3-δceramic disks, diameter is 7.5mm, and thickness is 0.6mm; Porous diffusion barrier layer (2) is the Al with porous structure
2o
3ceramic disks, diameter is 10.5mm, and thickness is 0.7mm; Described La
1-xsr
xga
1-ymg
yo
3-δin material, wherein the value of x and y is respectively x=0.2 and y=0.1; Described positive electrode lead (6) is respectively used to negative electrode lead (7) both positive and negative polarity being connected power supply (8); Described positive electrode layer (3) and the material of positive electrode layer (4) and positive electrode lead (6) and negative electrode lead (7) are platinum; Described positive electrode layer (3) and the thickness of positive electrode layer (4) are 20um; Porous diffusion barrier limit-current type oxygen sensor when temperature 650 DEG C, voltage 0.6V-1.2V and oxygen concentration present good linear relationship, occur good limiting current platform, the scope can measuring oxygen concentration is 0 ~ 80%, and the response time is within the scope of 10s ~ 15s; Porous diffusion barrier limit-current type oxygen sensor operationally sets up reometer (9) in the line, and the manufacture method of porous diffusion barrier limit-current type oxygen sensor, comprises the following steps:
Prepared by blank: first use mould and oil press by La
1-xsr
xga
1-ymg
yo
3-δpowder and Al
2o
3powder is pressed into the porous diffusion barrier layer blank that oxygen pump layer blank that diameter is 10mm and diameter are 13mm respectively;
A high temperature sintering: the porous diffusion barrier layer potsherd above-mentioned oxygen pump layer blank and porous diffusion barrier layer blank being sent into respectively the obtained fine and close oxygen pump layer potsherd of sintering in high temperature sintering furnace and porous structure; The time that in a high temperature sintering, oxygen pump layer blank sinters in high temperature sintering furnace is 2h to 6h, and furnace temperature is 1350 DEG C ~ 1500 DEG C; The time that porous diffusion barrier layer blank sinters in high temperature sintering furnace is 3h to 6h, and furnace temperature is 1500 DEG C ~ 1550 DEG C;
Electrode layer prints: adopt high-precision silk screen printing machine to print positive electrode layer and positive electrode layer respectively at the upper and lower surface of above-mentioned oxygen pump layer potsherd, and draw positive electrode lead and negative electrode lead respectively from positive electrode layer and positive electrode layer simultaneously;
Secondary high-temperature sinters: the one side adopting the mode of platinum slurry adhesion oxygen pump layer potsherd to be had a positive electrode layer and above-mentioned porous spread barrier layer potsherd couple together and together with send in high temperature sintering furnace the lambda sensor blank sintering and obtain integrative-structure; In secondary high-temperature sintering, the sintering temperature of high temperature sintering furnace is 900 DEG C ~ 1000 DEG C, and the time is 1h;
Finished product sinters again: above-mentioned lambda sensor blank is coated glass glaze after cooling naturally on the outer peripheral face of the porous exposed upper plane of diffusion barrier layer and positive electrode layer, oxygen pump layer, positive electrode layer and again sends into this product obtained of sintering in high temperature sintering furnace; During finished product sinters again, the sintering temperature of high temperature sintering furnace is 900 DEG C, and the time is 1h ~ 3h.
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| CN202710510U (en) * | 2012-08-16 | 2013-01-30 | 宁波大学 | Porous diffusion barrier limit current type oxygen sensor |
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| JPH07140109A (en) * | 1993-06-23 | 1995-06-02 | Fujikura Ltd | Limit current type oxygen sensor and its manufacture |
| JP3831320B2 (en) * | 2002-08-30 | 2006-10-11 | 矢崎総業株式会社 | Limit current type oxygen sensor |
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| CN202710510U (en) * | 2012-08-16 | 2013-01-30 | 宁波大学 | Porous diffusion barrier limit current type oxygen sensor |
Non-Patent Citations (3)
| Title |
|---|
| 基于La0.9Sr0.1Ga0.8Mg0.2O2.85固体电解质浓差电势型氧传感器的研究;陈康等;《第十六届全国固态离子学学术会议暨下一代能源材料与技术国际研讨会—会议论文摘要集》;20120706;第158页 * |
| 极限电流型氧传感器的多层共烧制备;沈杰等;《传感技术学报》;20091130;第22卷(第11期);第1533-1537页 * |
| 极限电流型氧传感器的研究;武强等;《传感器与微系统》;20061231;第25卷(第6期);第46-48页 * |
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