CN105014769A - 3D printing preparation method based on nanosecond-picosecond-femtosecond laser compound technology for NOx sensor - Google Patents
3D printing preparation method based on nanosecond-picosecond-femtosecond laser compound technology for NOx sensor Download PDFInfo
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- CN105014769A CN105014769A CN201510356921.6A CN201510356921A CN105014769A CN 105014769 A CN105014769 A CN 105014769A CN 201510356921 A CN201510356921 A CN 201510356921A CN 105014769 A CN105014769 A CN 105014769A
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- nanosecond
- femtosecond laser
- sensor
- psec
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B17/00—Details of, or accessories for, apparatus for shaping the material; Auxiliary measures taken in connection with such shaping
- B28B17/0063—Control arrangements
- B28B17/0081—Process control
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
Abstract
The invention discloses a 3D printing preparation method based on the nanosecond-picosecond-femtosecond laser compound technology for a NOx sensor and belongs to the field of NOx sensors. The 3D printing preparation method comprises the following steps: (1) laying raw material powder on a working platform and pre-heating; (2) adopting nanosecond laser to sinter and melt the raw material on the working platform, and meanwhile, adopting a real-time monitoring system to detect the precisions of all printing layer structures of a sensor; and (3) sequentially repeating the steps (1) and (2) till preparation of the NOx sensor is completed. The 3D printing preparation method has the advantages that the complex problems of powder blowing, high residual stress and the like in the conventional laser sintering process are effectively solved, and a compensation step is omitted; and more accurate size control and resistance value control are realized, the process is simpler, follow-up trimming is not needed, and better consistency is achieved.
Description
Technical field
The present invention relates to NO
xsensor field, is specifically related to a kind of NO
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique.
Background technology
In recent years, along with surging of world car consumption, automobile exhaust pollution problem is on the rise.Nitrogen oxide NO in vehicle exhaust
x(NO
2+ NO) discharge can damage the ozone layer, cause acid rain and photochemical fog, to the existence of the mankind with healthyly constitute serious threat.Based on the mixed potential type NO that zirconia is solid electrolyte
xsensor is a kind of new chemical class NO grown up gradually in recent years
xsensor.In more than ten years in the past, zirconia base mixed potential type NO
xsensor obtains and develops rapidly, and researcher conducts extensive research report from the aspect such as electrode material, structure, working mechanism of sensor to sensors with auxiliary electrode.But, NO
xpreparation technology's more complicated of sensor, generally through flow casting molding, cutting, screen printing electrode and insulating barrier slurry, dry, cut into base and sintering process, so many technique often makes the impact being subject to many factors in manufacturing process, causes NO
xthe production efficiency of sensor, precision, uniformity and reliability are not very high, and sintering process can cause higher residual stress to occur, at present, can produce in batches and commercial NO
xsensor only have Japanese NGK mono-.
3D printing technique is that a kind of dusty material that uses successively piles up by selective laser sintering or fusing the increasing material manufacture method to manufacture a product.Relative traditional manufacturing technology, it can produce complexity, the highly difficult product that conventional art is difficult to produce like a cork.But, the piece surface that 3D impact system is prepared often show intensity not high, blow the shortcomings such as the high and rough surface of powder, nodularization, residual stress is high, need to remove the gred and polishing to forming part.Be only utilize vision monitoring to carry out controlling dimension in current 3D print procedure, do not have the real-time monitoring equipment of microstructure and composition, we are unable to find out the microstructure of parts, also just can not control better its mechanical performance.
In recent years, short-pulse laser (as nanosecond laser, picosecond laser and femtosecond laser) due to heat affecting little, machining accuracy is high, thus receives much concern in Precision Machining field.The pulse width of nanosecond laser is nanosecond (10
-9second) level, its repetition rate is generally hundreds of kHz, reaches as high as 10MHz, therefore can reach very high working (machining) efficiency.Psec (10
-12second) laser is enough to avoid energy generation thermal diffusion and reaches these melt peak energy denisty required for critical process, higher mean power (10 W) and good beam quality (M2 < 1.5) can be provided, one 10 μm or less luminous point can be become at effective working distance inner focusing.Femtosecond laser (10
-15second) within the duration of each laser pulse and matter interaction, avoid the existence of thermal diffusion, be similar to the impact and fire damage that the multiple effect such as melting zone, heat affected area, shock wave in long pulse process causes adjacent material fundamentally eliminating, spatial dimension involved by process is reduced greatly, thus improve order of accuarcy, within its beam diameter can focus on 1um, within its precision can reach 100nm, preferably 0.1nm can be reached.
But, also do not occur at present using nanosecond/the 3D print sensor product of psec/femtosecond laser complex technique.
Summary of the invention
The present invention is directed to existing NO
xthe defect such as the not high and material interface residual stress of the complex process existed in sensor manufacturing process, precision is wayward, R. concomitans nanosecond-psec-femtosecond laser complex technique, provide a kind of NO
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique.
Object of the present invention is realized by following technical scheme:
A kind of NO
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, comprise the steps:
(1) on workbench, raw material powder is laid and preheating;
(2) adopt nanosecond laser to carry out sintering fusing to the raw material on workbench, adopt the precision of each printable layer structure of real-time monitoring system detecting sensor simultaneously;
(3) step (1) and (2) are repeatedly repeated successively, until complete NO
xthe preparation of sensor.
Also comprise in above-mentioned steps (2) and adopt integrated optical fiber laser to provide picosecond laser or femtosecond laser to carry out fine finishining to sensor.
Optical fiber laser provide the most I machining feature size of laser within 1um, precision, within 100nm, preferably can reach 0.1nm.
Described NO
xsensor comprises zirconia base, and the upper surface of described zirconia base is provided with external electrode, and zirconia base inside is provided with chamber layer, air duct and heater from top to bottom successively; Described chamber layer comprises the first chamber, the second chamber and the 3rd chamber, is provided with the first barrier layer between the first chamber and the second chamber, is provided with the second barrier layer between the second chamber and the 3rd chamber, and the 3rd chamber is semiclosed; The top of described first chamber is provided with the first pump oxygen electrode, and bottom is provided with test electrode, and the top of the second chamber is provided with the second pump oxygen electrode; The top of described air duct is provided with reference electrode.
Described zirconia base material is the stable zirconia of YSZ(yttrium).
The material of described first pump oxygen electrode and the second pump oxygen electrode is platinum, ruthenium-oxide or molybdenum oxide.
The material of described test electrode is platinum, ruthenium-oxide or molybdenum oxide.
The material of described heater is platinum.
Described real-time monitoring system comprises one or more in infrared video camera, ESEM, X-ray diffractometer.
Described NO
xthe order that prints of 3D be from top to bottom or from top to bottom.
Of the present invention nanosecond-psec-femtosecond laser complex technique, it is characterized in that sintering fusing by the multi-wavelength integrated fiber lasers of nanosecond laser, picosecond laser and femtosecond laser can be provided first to carry out nanometer laser, then according to the detection and control of real-time monitoring system, picosecond laser or femtosecond laser is used to carry out retrofit adjustment to characteristic size.Real-time monitoring system has multiple both macro and micro detection means, as infrared video camera, ESEM, X-ray diffractometer etc., can use wherein one or more, depend on the precision of sensor processing needs.
NOx sensor provided by the present invention, comprises zirconia base, the first chamber, the second chamber, barrier layer, external electrode, pump oxygen electrode, test electrode, reference electrode, air duct, heater and conductive pin, it is characterized in that:
Described zirconia base is as NO
xthe solid electrolyte of sensor, serves the effect of pump oxygen, namely realizes the electric conductivity of oxonium ion, and its material is the stable zirconia of YSZ(yttrium); Described first chamber and the second chamber are positioned at the top of zirconia base, are respectively used to the gas holding gas to be measured and low oxygen concentration process; Described barrier layer lays respectively at the outside of first, second chamber, enters the first and second chambers for making gas to be measured by the form of diffusion; Described external electrode is positioned at the topmost of zirconia base, described pump oxygen electrode has two, lay respectively at the top of the first and second chambers, external electrode coordinates the voltage or current value that gather zirconia base with pump oxygen electrode, and material can be platinum, ruthenium-oxide, molybdenum oxide etc.; Described test electrode is positioned at the bottom of the second chamber, described reference electrode is positioned at the internal air passageway top of zirconia base, combine with test electrode, for gathering the voltage or current value that the oxygen that pumps from the second chamber produces, material can be platinum, ruthenium-oxide, molybdenum oxide etc.; Be positioned at the below of two chambers during described air duct, the gas pumped into by the second chamber enters air by air duct; Described heater is positioned at the below of air duct, is generally metal platinum; Described conductive pin is positioned at the below of NOx sensor, and multiple conductive pin is connected respectively at above-mentioned each electrode, carries out measurement processing for the signal of telecommunication being drawn out to sensor external.
NO
xthe key step of the 3D printing preparation method of sensor is:
(1) on workbench, raw material powder is laid and preheating;
(2) use nanosecond laser to carry out sintering fusing, use each printable layer structure of real-time monitoring system detecting sensor whether to reach required precision simultaneously, if needed, then use integrated optical fiber laser to provide picosecond laser or femtosecond laser fine finishining;
(3) above-mentioned steps is repeated until complete 3D printing.
According to NO
xthe hierarchy of sensor, the order that 3D prints can be from top to bottom, also can be from top to bottom.
NO
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, use nanosecond laser to carry out sintering fusing, simultaneously in conjunction with real-time monitoring system for the accurately machined part use picosecond laser of needs or femtosecond laser, described NO
xsensor comprises zirconia base, the first chamber, the second chamber, barrier layer, external electrode, pump oxygen electrode, test electrode, reference electrode, air duct, heater and conductive pin, it is characterized in that:
Described nanosecond, psec, femtosecond laser are integrated in a multi-wavelength optical fiber laser, and selection provides one or more in three kinds of laser as required; Described real-time monitoring system comprises infrared video camera, ESEM, X-ray diffractometer etc. can detect NO
xthe instrument of sensor surface pattern and microstructure;
Described NO
xsensor is further characterized in that, the first chamber and the second chamber are positioned at the top of zirconia base, and described barrier layer lays respectively at the outside of first, second chamber; Described external electrode is positioned at the topmost of zirconia base, and described pump oxygen electrode has two, lays respectively at the top of the first and second chambers; Described test electrode is positioned at the bottom of the second chamber, and described reference electrode is positioned at the internal air passageway top of zirconia base; Be positioned at the below of two chambers during described air duct, described heater is positioned at the below of air duct; Described conductive pin is positioned at NO
xthe below of sensor, multiple conductive pin is connected respectively at above-mentioned each electrode;
Described optical fiber laser provide the most I machining feature size of laser within 1um, precision, within 100nm, preferably can reach 0.1nm;
Described nanosecond laser completes NO
xthe sintering fusing of sensor body structure;
Described picosecond laser or femtosecond laser are used for NO
xthe key structure of sensor carries out sintering fusing or fine finishining;
Multiple checkout equipment in described real-time monitoring system can use wherein one or more, depend on the NO that 3D prints
xthe required precision of sensor;
Described zirconia base is the solid electrolyte layer based on zirconia material, and its material is YSZ, the zirconia that namely yttrium is stable;
The material of described external electrode, pump oxygen electrode, test electrode and reference electrode can be all platinum, ruthenium-oxide, molybdenum oxide etc.
The present invention proposes a kind of based on nanosecond-NO of psec-femtosecond laser complex technique
xsensor 3D Method of printing, uses nanosecond laser to carry out sintering fusing, uses picosecond laser or femtosecond laser, NO simultaneously in conjunction with real-time monitoring system for the accurately machined part of needs
xsensor comprises zirconia base, the first chamber, the second chamber, barrier layer, external electrode, pump oxygen electrode, test electrode, reference electrode, air duct, heater and conductive pin.The preparation method that the present invention proposes achieves more accurate size Control and resistance controls, comprise each layer thickness, electrode size etc., technique does not more simply need follow-uply to repair resistance, there is better uniformity, can reach and not do compensation and spendable precision, eliminate conventional 3D and printed the rear required operation such as cleaning, polishing, efficiently solve and blow the problems such as powder, residual stress is high, intensity is low.
The method can the advantage of the aspect such as integrated process velocity, precision and cost, applied to sintering and the micro Process of sensor, that can fast, effectively avoid occurring in laser sintered process now blows powder, the challenges such as residual stress, can save compensation process.
The preparation method that the present invention proposes achieves more accurate size Control and resistance controls, comprise each layer thickness, electrode size etc., technique does not more simply need follow-uply to repair resistance, there is better uniformity, can reach and not do compensation and spendable precision, eliminate conventional 3D and printed the rear required operation such as cleaning, polishing, efficiently solve and blow the problems such as powder, residual stress is high, intensity is low.
Accompanying drawing explanation
Fig. 1 is NO
xthe cross-section front view of sensor;
Fig. 2 is NO of the present invention
xsensor 3D prints manufacturing process flow diagram;
Wherein, 101-zirconia base, 102-conductive pin, 103-heater, 104-air duct, 105-reference electrode, 106-test electrode, 107-first chamber, 108-first pump oxygen electrode, 109-first barrier layer, 110-second pump oxygen electrode, 111-second barrier layer, 112-second chamber, 113-external electrode, 114-the 3rd chamber.
detailed description of the invention:
Fig. 1 is NO
xthe cross-section front view schematic diagram of sensor.As shown in the figure, a kind of NO
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, comprise the steps:
(1) on workbench, raw material powder is laid and preheating;
(2) adopt nanosecond laser to carry out sintering fusing to the raw material on workbench, adopt the precision of each printable layer structure of real-time monitoring system detecting sensor simultaneously;
(3) step (1) and (2) are repeatedly repeated successively, until complete NO
xthe preparation of sensor.
Also comprise in above-mentioned steps (2) and adopt integrated optical fiber laser to provide picosecond laser or femtosecond laser to carry out fine finishining to sensor.
Described NO
xsensor comprises zirconia base, and the upper surface of described zirconia base is provided with external electrode, and zirconia base inside is provided with chamber layer, air duct and heater from top to bottom successively; Described chamber layer comprises the first chamber, the second chamber and the 3rd chamber, is provided with the first barrier layer between the first chamber and the second chamber, is provided with the second barrier layer between the second chamber and the 3rd chamber, and the 3rd chamber is semiclosed; The top of described first chamber is provided with the first pump oxygen electrode, and bottom is provided with test electrode, and the top of the second chamber is provided with the second pump oxygen electrode; The top of described air duct is provided with reference electrode.
Described zirconia base material is the stable zirconia of YSZ(yttrium).
The material of described first pump oxygen electrode and the second pump oxygen electrode is platinum, ruthenium-oxide or molybdenum oxide.
The material of described test electrode is platinum, ruthenium-oxide or molybdenum oxide.
The material of described heater is platinum.
Described real-time monitoring system comprises one or more in infrared video camera, ESEM, X-ray diffractometer.
Described NO
xthe order that prints of 3D be from top to bottom or from top to bottom.
Zirconia base 101, conductive pin 102, heater 103, air duct 104, reference electrode 105, test electrode 106, barrier layer 109 and 111, first chamber 107, second chamber 112, first pump oxygen electrode 108, second pump oxygen electrode 110, external electrode 113 from top to bottom successively.All electrodes are all drawn out to NO by corresponding conductive pin
xthe lower surface of sensor, reference electrode 105 is positioned at the upper surface of air duct, combine with zirconia base 101, first pump oxygen electrode 108 and test electrode 106 are all positioned at the first chamber 107, second pump oxygen electrode 110 is positioned at the second chamber 112, first chamber 107 and the second chamber 112 are kept apart by the first barrier layer 109, and the second chamber 112 and gas to be measured are kept apart by the second barrier layer 111.
Fig. 2 is NO
xsensor prints manufacture method flow chart.The technological process of the present embodiment is: after loading raw material on the table, first use nanosecond laser to carry out scanning by integrated fiber lasers to the raw material loaded and sinter fusing, real-time monitoring system following closely carries out detection and analyzes and feed back to control system, as need fine finishining be carried out, succession optical fiber laser is then used to provide picosecond laser or femtosecond laser carry out processing to specific region and detect simultaneously, required accurately machined requirement is depended in the selection of laser, repeats said process until the size of part and precision stop after reaching requirement.
Claims (10)
1. a NO
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, it is characterized in that: comprise the steps:
(1) on workbench, raw material powder is laid and preheating;
(2) adopt nanosecond laser to carry out sintering fusing to the raw material on workbench, adopt the precision of each printable layer structure of real-time monitoring system detecting sensor simultaneously;
(3) step (1) and (2) are repeatedly repeated successively, until complete NO
xthe preparation of sensor.
2. a kind of NO according to claim 1
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, it is characterized in that: also comprise in step (2) and adopt integrated optical fiber laser to provide picosecond laser or femtosecond laser to carry out fine finishining to sensor.
3. a kind of NO according to claim 2
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, it is characterized in that: the most I machining feature size of described optical fiber laser is less than 1um, and precision is 0.1nm.
4. a kind of NO according to claim 1 or 2
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, it is characterized in that: described NO
xsensor comprises zirconia base, and the upper surface of described zirconia base is provided with external electrode, and zirconia base inside is provided with chamber layer, air duct and heater from top to bottom successively; Described chamber layer comprises the first chamber, the second chamber and the 3rd chamber, is provided with the first barrier layer between the first chamber and the second chamber, is provided with the second barrier layer between the second chamber and the 3rd chamber, and the 3rd chamber is semiclosed; The top of described first chamber is provided with the first pump oxygen electrode, and bottom is provided with test electrode, and the top of the second chamber is provided with the second pump oxygen electrode; The top of described air duct is provided with reference electrode.
5. a kind of NO according to claim 4
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, it is characterized in that: described zirconia base material is YSZ.
6. a kind of NO according to claim 4 or 5
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, it is characterized in that: the material of described first pump oxygen electrode and the second pump oxygen electrode is platinum, ruthenium-oxide or molybdenum oxide.
7. a kind of NO according to claim 4 or 5
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, it is characterized in that: the material of described test electrode is platinum, ruthenium-oxide or molybdenum oxide.
8. a kind of NO according to claim 3
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, it is characterized in that: the material of described heater is platinum.
9. a kind of NO according to claim 3
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, it is characterized in that: described real-time monitoring system comprises one or more in infrared video camera, ESEM, X-ray diffractometer.
10. a kind of NO according to claim 3 or 8 or 9
xsensor based on nanosecond-the 3D printing preparation method of psec-femtosecond laser complex technique, it is characterized in that: described NO
xthe order that prints of 3D be from top to bottom or from top to bottom.
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|---|---|---|---|
| CN201510356921.6A CN105014769A (en) | 2015-06-25 | 2015-06-25 | 3D printing preparation method based on nanosecond-picosecond-femtosecond laser compound technology for NOx sensor |
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ID=54405243
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107389770A (en) * | 2017-06-29 | 2017-11-24 | 东北大学 | The preparation method of lambda sensor dielectric substrate and fine and close diffusion layer double-decker |
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| CN107389770B (en) * | 2017-06-29 | 2019-07-02 | 东北大学 | The production method of lambda sensor electrolyte layer and fine and close diffusion layer double-layer structure |
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