CN105088316B - A kind of preparation method of rear-earth-doped ceria film - Google Patents
A kind of preparation method of rear-earth-doped ceria film Download PDFInfo
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Abstract
The invention provides a kind of preparation method of rear-earth-doped ceria film, rare earth oxide is dissolved in nitric acid, is configured to rare earths salt；The pH value for adjusting above-mentioned rare earths salt with ammonia spirit is 6.3~7.8, plus ethylene glycol, and ammonification water, is made electrolyte under agitation；The carborundum waterproof abrasive paper soaked with absolute ethyl alcohol is polished cerium tablet and clean with washes of absolute alcohol, it is sprayed on flannelette with diamond spraying polishing agent, cerium tablet is polished on the flannelette for having diamond to spray polishing agent up to being minute surface, the cerium tablet after polishing is put into anhydrous alcohol solution and is cleaned by ultrasonic；To treat that the cerium tablet of anodic oxidation is put into electrolyte Anodic Oxidation, anodic oxidation part is rinsed with water, is air-dried；Anodic oxidation part is put into Muffle furnace and is calcined, cooling takes out obtain two sides to be to be fine and close rear-earth-doped ceria film in the middle of many nanometers of straight holes.The hole for determining many nanometers of straight holes in two sides using Fisher MPO calibrators is long respectively 15~97 μm.
Description
Technical field
The invention belongs to materialogy field, it is related to a kind of ceria film, specifically a kind of rear-earth-doped titanium dioxide
The preparation method of cerium film.
Background technology
Because doping cerium dioxide has oxygen storage capacity and oxygen ionic conductivity high, can be used for solid oxide fuel
The electrolyte of battery.The electrolyte of current SOFC is usually supported on electrode on especially anode, existing
Silk screen print method, altogether the tape casting, platen press, spin coating method, dip-coating method, sol-gel membrane formation process, spray decomposition method etc..
These film preparing technologies have obtained very big development during the preparation and application of electrolyte, but there are still it is certain not
, such as the controllability of electrolyte thin film thickness, adhesive force and there is defect when generally need to sinter and burn till more than 1000 DEG C in foot
Deng.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of preparation of rear-earth-doped ceria film
Method, the preparation method of described this rear-earth-doped ceria film solves the electrolyte thin film thickness of prior art, attached
Put forth effort uncontrollable, and easily the technical problem of defect occur during sintering.
The invention provides a kind of preparation method of rear-earth-doped ceria film, comprise the following steps：
（1）Rare earth oxide is dissolved in nitric acid, rare earths salt is configured to；
Its middle rare earth is lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium, scandium rare earth oxygen
The mixture of one or more the rare earth oxide in compound；The concentration of rare earths salt middle rare earth is 300~500g/
L；
（2）The pH value for adjusting above-mentioned rare earths salt with ammonia spirit is 6.3~7.8, plus ethylene glycol, ammonification under agitation
Water, is made electrolyte；In ethylene glycol, the concentration of ammoniacal liquor is 2.5 ~ 400g/L, the concentration of rare-earth salts is 30 ~ 50g/L；
（3）The carborundum waterproof abrasive paper soaked with absolute ethyl alcohol is to thickness for 0.1 ~ 0.3mm cerium tablet is polished and uses anhydrous
Ethanol is cleaned up, and is sprayed on flannelette with 0.5 ~ 1.5 μm of diamond spraying polishing agent, and cerium tablet is being had into diamond spraying polishing
Be put into the cerium tablet after polishing in anhydrous alcohol solution and be cleaned by ultrasonic by polishing up to being minute surface on the flannelette of agent；
（4）To treat that the cerium tablet of anodic oxidation is put into electrolyte Anodic Oxidation, negative electrode is platinum or lead, and cerium tablet is anode, sun
The process conditions of pole oxidation are 8~200mA/dm of current density2, 0~20 DEG C of oxidizing temperature, 100~600rpm of speed of agitator, oxygen
3~17h of change time, after anodic oxidation is finished, anodic oxidation part is rinsed with water, is air-dried；
（5）Anodic oxidation part is put into Muffle furnace, with 0.4`0.6 DEG C/min temperature programmings to 320~800 DEG C,
320~400 DEG C of 0.5~2 h of roasting, are cooled to room temperature, and it is the rear-earth-doped of densification in the middle of many nanometers of straight holes that taking-up obtain two sides to be
Ceria film.
Further, the thickness of cerium tablet is 0.2mm.
Further, it is sprayed on flannelette with 1 μm of diamond spraying polishing agent.
Further, described rare earth oxide be lanthana, samarium oxide, neodymia, luteium oxide, gadolinium oxide, europium oxide,
Any one in terbium oxide or praseodymium oxide.
It is fine and close rear-earth-doped ceria film in the middle of many nanometers of straight holes that the present invention prepared two sides to be.Using
The hole that Fisher MPO calibrators determine many nanometers of straight holes in two sides is long respectively 15~97 μm.Using Bruker AXS
The content that Microanalysis GmbH energy disperse spectroscopies determine rear-earth-doped ceria film middle rare earth is by mass percentage
5.2~27.1%.
The present invention is compared with prior art, and its technological progress is significant.The present invention uses anodizing and heat treatment
It is fine and close rear-earth-doped ceria film in the middle of many nanometers of straight holes that method be prepared for two sides to be.The present invention can be by controlling cerium paper tinsel
Anodizing time, so as to can control the thickness of rear-earth-doped ceria film film.
Specific embodiment
The present invention is expanded on further below by specific embodiment, but is not intended to limit the present invention.
Embodiment 1
35.1840g lanthanas are weighed in 100mL small beakers, 50mL concentrated nitric acids are added under agitation, heating dissolves it,
After after its cooling, move in the volumetric flask of 100mL, be diluted with water to scale, la concn is 300g/L in the solution.In the burning of 2L
The solution 100mL that above-mentioned la concn is 300g/L is added in cup, it is 7.8 to adjust solution ph with ammonia spirit, plus 785mL second two
Alcohol, adds 2.5g ammoniacal liquor under agitation, and dissolving forms lanthanum nitrate-ammonia water-ethylene glycol mixed solution, moves into 1L volumetric flasks, uses second
Glycol is diluted to scale, and electrolyte is obtained.The carborundum waterproof abrasive paper soaked with absolute ethyl alcohol is treated to 100mm × 100mm × 0.1mm
The cerium paper tinsel of anodic oxidation is polished and clean with washes of absolute alcohol, and flannelette is sprayed on 0.5 μm of diamond spraying polishing agent
On, cerium tablet is polished on the flannelette for having diamond to spray polishing agent until being minute surface.Cerium paper tinsel after polishing is put into anhydrous second
It is cleaned by ultrasonic in alcohol liquid.Above-mentioned electrolyte is transferred in the beaker of 2L, above-mentioned 100mm × 100mm × 0.1mm is treated into anodic oxygen
Change cerium paper tinsel is put into electrolyte and is anode, and negative electrode is the platinum sheet of 150mm × 150mm × 0.5mm, magnetic agitation, speed of agitator
It is 100rpm, current density is 8mA/dm2, 0 DEG C of oxidizing temperature, oxidization time 3h, take out anodic oxidation part, rushed with deionized water
Clean, air-dry, be put into crucible, be put into Muffle furnace, with 0.5 DEG C/min temperature programmings to 400 DEG C, 0.5 is calcined at 400 DEG C
h.It is cooled to room temperature, it is fine and close lanthanum doping cerium dioxide film in the middle of many nanometers of straight holes that taking-up obtain two sides to be.It is public using Fisher
The hole for taking charge of the MPO calibrators measure many nanometers of straight holes in two sides of production is long respectively 15 μm.Using Bruker AXS
It is 5.2% that the content of lanthanum is calculated by mass percentage in Microanalysis GmbH energy disperse spectroscopies measure lanthanum doping cerium dioxide film.
Embodiment 2
57.9800g samarium oxides are weighed in 200mL small beakers, 80mL concentrated nitric acids are added under agitation, heating dissolves it,
After after its cooling, move in the volumetric flask of 100mL, be diluted with water to scale, samarium concentration is 500g/L in the solution.In the burning of 2L
The solution 100mL that above-mentioned samarium concentration is 500g/L is added in cup, it is 6.9 to adjust solution ph with ammonia spirit, plus 375mL second two
Alcohol, adds 400g ammoniacal liquor under agitation, and dissolving forms samaric nitrate-ammonia water-ethylene glycol mixed solution, moves into 1L volumetric flasks, uses second
Glycol is diluted to scale, and electrolyte is obtained.The carborundum waterproof abrasive paper soaked with absolute ethyl alcohol is treated to 100mm × 100mm × 0.3mm
The cerium paper tinsel of anodic oxidation is polished and clean with washes of absolute alcohol, and flannelette is sprayed on 1.5 μm of diamonds spraying polishing agent
On, cerium tablet is polished on the flannelette for having diamond to spray polishing agent until being minute surface.Cerium paper tinsel after polishing is put into anhydrous second
It is cleaned by ultrasonic in alcohol liquid.Above-mentioned electrolyte is transferred in the beaker of 2L, above-mentioned 100mm × 100mm × 0.3mm is treated into anodic oxygen
Change cerium paper tinsel to be put into electrolyte and for anode, negative electrode is the stereotype of 150mm × 150mm × 2mm, magnetic agitation, speed of agitator is
600rpm, current density is 200mA/dm2, 20 DEG C of oxidizing temperature, oxidization time 17h, take out anodic oxidation part, use deionized water
Rinse net, air-dry, be put into crucible, be put into Muffle furnace, with 0.5 DEG C/min temperature programmings to 320 DEG C, in 320 DEG C of roastings
2h.It is cooled to room temperature, it is fine and close samarium doping ceria film in the middle of many nanometers of straight holes that taking-up obtain two sides to be.It is public using Fisher
The hole for taking charge of the MPO calibrators measure many nanometers of straight holes in two sides of production is long respectively 97 μm.Using Bruker AXS
The content of samarium is by mass percentage in Microanalysis GmbH energy disperse spectroscopies measure samarium doping ceria film
27.1%。
Embodiment 3
46.6560g neodymia is weighed in 200mL small beakers, 80mL concentrated nitric acids is added under agitation, heating dissolves it,
After after its cooling, move in the volumetric flask of 100mL, be diluted with water to scale, neodymium concentration is 400g/L in the solution.Weigh
50.8000g yittrium oxide adds 80mL concentrated nitric acids under agitation in 100mL small beakers, and heating dissolves it, after it is cooled down,
Move in the volumetric flask of 100mL, be diluted with water to scale, yttrium concentration is 400g/L in the solution.Added in the beaker of 2L
It is the solution 50mL of 400g/L to state solution 50mL and above-mentioned yttrium concentration that neodymium concentration is 400g/L, and pH value of solution is adjusted with ammonia spirit
It is 6.9 to be worth, plus 575mL ethylene glycol, and 200g ammoniacal liquor is added under agitation, and dissolving forms neodymium nitrate-yttrium nitrate-ammonia water-ethylene glycol and mixes
Solution is closed, is moved into 1L volumetric flasks, spent glycol is diluted to scale, electrolyte is obtained.The carborundum water soaked with absolute ethyl alcohol
Sand paper treats that the cerium paper tinsel of anodic oxidation is polished and clean with washes of absolute alcohol to 100mm × 100mm × 0.2mm, with 1 μm
Diamond spraying polishing agent is sprayed on flannelette, cerium tablet is polished on the flannelette for having diamond to spray polishing agent until being minute surface.
Cerium paper tinsel after polishing is put into anhydrous alcohol solution and is cleaned by ultrasonic.Above-mentioned electrolyte is transferred in the beaker of 2L, by above-mentioned 100mm
× 100mm × 0.2mm's treats that anodic oxidation cerium paper tinsel is put into electrolyte and for anode, and negative electrode is 150mm × 150mm × 0.5mm
Platinum sheet, magnetic agitation, speed of agitator is 300rpm, and current density is 100mA/dm2, 10 DEG C of oxidizing temperature, oxidization time
10h, takes out anodic oxidation part, net with deionized water rinsing, air-dries, and is put into crucible, is put into Muffle furnace, with 0.5 DEG C/min
Temperature programming is calcined 1h to 360 DEG C at 360 DEG C.It is cooled to room temperature, it is fine and close neodymium in the middle of many nanometers of straight holes that taking-up obtain two sides to be
With doped yttrium ceria film.The MPO calibrators produced using Fisher companies determine the hole difference long of many nanometers of straight holes in two sides
It is 68 μm.Using Bruker AXS Microanalysis GmbH energy disperse spectroscopies determine in neodymium and doped yttrium ceria film neodymium and
The content of yttrium calculates respectively 8.6% and 6.2% by mass percentage.
Embodiment 4
19.8972g luteium oxides are weighed in 100mL small beakers, 35mL concentrated nitric acids are added under agitation, heating dissolves it,
After after its cooling, move in the volumetric flask of 50mL, be diluted with water to scale, lutetium concentration is 350g/L in the solution.Take
20.0115g erbium oxides add 35mL concentrated nitric acids under agitation in 100mL small beakers, and heating dissolves it, after it is cooled down,
Move in the volumetric flask of 50mL, be diluted with water to scale, erbium concentration is 350g/L in the solution.Added in the beaker of 2L above-mentioned
Lutetium concentration is the solution 50mL of 350g/L for the solution 50mL and above-mentioned erbium concentration of 350g/L, and solution ph is adjusted with ammonia spirit
It is 6.3, plus 775mL ethylene glycol, 100g ammoniacal liquor is added under agitation, dissolving forms lutecium nitrate-erbium nitrate-ammonia water-ethylene glycol mixing
Solution, moves into 1L volumetric flasks, and spent glycol is diluted to scale, and electrolyte is obtained.The carborundum water sand soaked with absolute ethyl alcohol
Paper treats that the cerium paper tinsel of anodic oxidation is polished and clean with washes of absolute alcohol to 100mm × 100mm × 0.2mm, with 1 μm of gold
Hard rock spraying polishing agent is sprayed on flannelette, cerium tablet is polished on the flannelette for having diamond to spray polishing agent until being minute surface.Will
Cerium paper tinsel after polishing is cleaned by ultrasonic in being put into anhydrous alcohol solution.Above-mentioned electrolyte is transferred in the beaker of 2L, by above-mentioned 100mm ×
100mm × 0.2mm's treats that anodic oxidation cerium paper tinsel is put into electrolyte and for anode, and negative electrode is the lead of 150mm × 150mm × 2mm
Plate, magnetic agitation, speed of agitator is 200rpm, and current density is 50mA/dm2, 5 DEG C of oxidizing temperature, oxidization time 6h, taking-up sun
Pole aoxidizes part, net with deionized water rinsing, air-dries, and is put into crucible, is put into Muffle furnace, with 0.5 DEG C/min temperature programmings extremely
380 DEG C, 0.75h is calcined at 380 DEG C.It is cooled to room temperature, it is for fine and close lutetium and erbium are mixed in the middle of many nanometers of straight holes that taking-up obtains two sides
Miscellaneous ceria film.The hole that the MPO calibrators produced using Fisher companies determine many nanometers of straight holes in two sides is long respectively 45 μm.
The content of lutetium and erbium in lutetium and Er ions ceria film is determined using Bruker AXS Microanalysis GmbH energy disperse spectroscopies
Calculate by mass percentage and be respectively 7.8% and 5.1%.
Embodiment 5
51.8625g gadolinium oxides are weighed in 200mL small beakers, 90mL concentrated nitric acids are added under agitation, heating dissolves it,
After after its cooling, move in the volumetric flask of 100mL, be diluted with water to scale, gadolinium concentration is 450g/L in the solution.In the burning of 2L
The solution 100mL that above-mentioned gadolinium concentration is 450g/L is added in cup, it is 6.8 to adjust solution ph with ammonia spirit, plus 575mL second two
Alcohol, adds 300g ammoniacal liquor under agitation, and dissolving forms gadolinium nitrate-ammonia water-ethylene glycol mixed solution, moves into 1L volumetric flasks, uses second
Glycol is diluted to scale, and electrolyte is obtained.The carborundum waterproof abrasive paper soaked with absolute ethyl alcohol is treated to 100mm × 100mm × 0.2mm
The cerium paper tinsel of anodic oxidation is polished and clean with washes of absolute alcohol, is sprayed on flannelette with 1 μm of diamond spraying polishing agent,
Cerium tablet is polished on the flannelette for having diamond to spray polishing agent until being minute surface.Cerium paper tinsel after polishing is put into anhydrous alcohol solution
Middle ultrasonic cleaning.Above-mentioned electrolyte is transferred in the beaker of 2L, above-mentioned 100mm × 100mm × 0.2mm is treated into anodic oxidation cerium
Paper tinsel is put into electrolyte and for anode, and negative electrode is the platinum sheet of 150mm × 150mm × 0.5mm, magnetic agitation, and speed of agitator is
500rpm, current density is 150mA/dm2, 15 DEG C of oxidizing temperature, oxidization time 15h, take out anodic oxidation part, use deionized water
Rinse net, air-dry, be put into 5 in crucible, be put into Muffle furnace, with 0.5 DEG C/min temperature programmings to 340 DEG C, in 340 DEG C of roastings
1.75h.It is cooled to room temperature, it is fine and close Gd2 O3 ceria film in the middle of many nanometers of straight holes that taking-up obtain two sides to be.Using
The hole that the MPO calibrators of Fisher companies production determine many nanometers of straight holes in two sides is long respectively 89.3 μm.Using Bruker AXS
It is 21.6% that the content of gadolinium is calculated by mass percentage in Microanalysis GmbH energy disperse spectroscopies measure Gd2 O3 ceria film
。
Embodiment 6
37.0536g europium oxides are weighed in 100mL small beakers, 60mL concentrated nitric acids are added under agitation, heating dissolves it,
After after its cooling, move in the volumetric flask of 100mL, be diluted with water to scale, europium concentration is 320g/L in the solution.In the burning of 2L
The solution 100mL that above-mentioned europium concentration is 320g/L is added in cup, it is 6.8 to adjust solution ph with ammonia spirit, plus 715mL second two
Alcohol, adds 150g ammoniacal liquor under agitation, and dissolving forms europium nitrate-ammonia water-ethylene glycol mixed solution, moves into 1L volumetric flasks, uses second
Glycol is diluted to scale, and electrolyte is obtained.The carborundum waterproof abrasive paper soaked with absolute ethyl alcohol is treated to 100mm × 100mm × 0.2mm
The cerium paper tinsel of anodic oxidation is polished and clean with washes of absolute alcohol, is sprayed on flannelette with 1 μm of diamond spraying polishing agent,
Cerium tablet is polished on the flannelette for having diamond to spray polishing agent until being minute surface.Cerium paper tinsel after polishing is put into anhydrous alcohol solution
Middle ultrasonic cleaning.Above-mentioned electrolyte is transferred in the beaker of 2L, above-mentioned 100mm × 100mm × 0.2mm is treated into anodic oxidation cerium
Paper tinsel is put into electrolyte and for anode, and negative electrode is the platinum sheet of 150mm × 150mm × 0.5mm, magnetic agitation, and speed of agitator is
250rpm, current density is 75mA/dm2, 7 DEG C of oxidizing temperature, oxidization time 9h, take out anodic oxidation part, rushed with deionized water
Clean, air-dry, be put into 5 in crucible, be put into Muffle furnace, with 0.5 DEG C/min temperature programmings to 350 DEG C, in 350 DEG C of roastings
1.5h.It is cooled to room temperature, it is fine and close europium doping cerium dioxide film in the middle of many nanometers of straight holes that taking-up obtain two sides to be.Using Fisher
The hole that the MPO calibrators of company's production determine many nanometers of straight holes in two sides is long respectively 60.3 μm.Using Bruker AXS
The content of europium is by mass percentage in Microanalysis GmbH energy disperse spectroscopies measure europium doping cerium dioxide film
13.7%。
Embodiment 7
35.6810g terbium oxides are weighed in 100mL small beakers, 60mL concentrated nitric acids are added under agitation, heating dissolves it,
After after its cooling, move in the volumetric flask of 100mL, be diluted with water to scale, terbium concentration is 310g/L in the solution.In the burning of 2L
The solution 100mL that above-mentioned terbium concentration is 310g/L is added in cup, it is 6.8 to adjust solution ph with ammonia spirit, plus 735mL second two
Alcohol, adds 130g ammoniacal liquor under agitation, and dissolving forms terbium nitrate-ammonia water-ethylene glycol mixed solution, moves into 1L volumetric flasks, uses second
Glycol is diluted to scale, and electrolyte is obtained.The carborundum waterproof abrasive paper soaked with absolute ethyl alcohol is treated to 100mm × 100mm × 0.2mm
The cerium paper tinsel of anodic oxidation is polished and clean with washes of absolute alcohol, is sprayed on flannelette with 1 μm of diamond spraying polishing agent,
Cerium tablet is polished on the flannelette for having diamond to spray polishing agent until being minute surface.Cerium paper tinsel after polishing is put into anhydrous alcohol solution
Middle ultrasonic cleaning.Above-mentioned electrolyte is transferred in the beaker of 2L, above-mentioned 100mm × 100mm × 0.2mm is treated into anodic oxidation cerium
Paper tinsel is put into electrolyte and for anode, and negative electrode is the platinum sheet of 150mm × 150mm × 0.5mm, magnetic agitation, and speed of agitator is
150rpm, current density is 30mA/dm2, 3 DEG C of oxidizing temperature, oxidization time 5h, take out anodic oxidation part, rushed with deionized water
Clean, air-dry, be put into 5 in crucible, be put into Muffle furnace, with 0.5 DEG C/min temperature programmings to 370 DEG C, in 370 DEG C of roastings
0.9h.It is cooled to room temperature, it is fine and close terbium doped ceria film in the middle of many nanometers of straight holes that taking-up obtain two sides to be.Using Fisher
The hole that the MPO calibrators of company's production determine many nanometers of straight holes in two sides is long respectively 37.8 μm.Using Bruker AXS
It is 9.8% that the content of terbium is calculated by mass percentage in the terbium doped ceria film of Microanalysis GmbH energy disperse spectroscopies measure.
Embodiment 8
35.6972g praseodymium oxides are weighed in 200mL small beakers, 60mL concentrated nitric acids are added under agitation, heating dissolves it,
After after its cooling, move in the volumetric flask of 100mL, be diluted with water to scale, praseodymium concentration is 305g/L in the solution.In the burning of 2L
The solution 100mL that above-mentioned praseodymium concentration is 310g/L is added in cup, it is 7.3 to adjust solution ph with ammonia spirit, plus 705mL second two
Alcohol, adds 140g ammoniacal liquor under agitation, and dissolving forms praseodymium nitrate-ammonia water-ethylene glycol mixed solution, moves into 1L volumetric flasks, uses second
Glycol is diluted to scale, and electrolyte is obtained.The carborundum waterproof abrasive paper soaked with absolute ethyl alcohol is treated to 100mm × 100mm × 0.2mm
The cerium paper tinsel of anodic oxidation is polished and clean with washes of absolute alcohol, is sprayed on flannelette with 1 μm of diamond spraying polishing agent,
Cerium tablet is polished on the flannelette for having diamond to spray polishing agent until being minute surface.Cerium paper tinsel after polishing is put into anhydrous alcohol solution
Middle ultrasonic cleaning.Above-mentioned electrolyte is transferred in the beaker of 2L, above-mentioned 100mm × 100mm × 0.2mm is treated into anodic oxidation cerium
Paper tinsel is put into electrolyte and for anode, and negative electrode is the platinum sheet of 150mm × 150mm × 0.5mm, magnetic agitation, and speed of agitator is
350rpm, current density is 20mA/dm2, 9 DEG C of oxidizing temperature, oxidization time 13h, take out anodic oxidation part, rushed with deionized water
Clean, air-dry, be put into 5 in crucible, be put into Muffle furnace, with 0.5 DEG C/min temperature programmings to 390 DEG C, in 390 DEG C of roastings
0.7h.It is cooled to room temperature, it is fine and close praseodymium doped ceria film in the middle of many nanometers of straight holes that taking-up obtain two sides to be.Using Fisher
The hole that the MPO calibrators of company's production determine many nanometers of straight holes in two sides is long respectively 79.3 μm.Using Bruker AXS
It is 7.2% that the content of praseodymium is calculated by mass percentage in Microanalysis GmbH energy disperse spectroscopies measure praseodymium doped ceria film.
The above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, on the premise of the technology of the present invention principle is not departed from, some improvement and modification can also be made, these improve and become
Type also should be regarded as protection scope of the present invention.
Claims (4)
1. a kind of preparation method of rear-earth-doped ceria film, it is characterised in that comprise the following steps：
（1）Rare earth oxide is dissolved in nitric acid, rare earths salt is configured to；
Its middle rare earth is lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium, scandium rare earth oxide
In one or more rare earth oxide mixture；The concentration of rare earths salt middle rare earth is 300~500g/L；
（2）The pH value for adjusting above-mentioned rare earths salt with ammonia spirit is 6.3~7.8, plus ethylene glycol, under agitation ammonification water,
It is made electrolyte；In ethylene glycol, the concentration of ammoniacal liquor is 2.5 ~ 400g/L, the concentration of rare-earth salts is 30 ~ 50g/L；
（3）The carborundum waterproof abrasive paper soaked with absolute ethyl alcohol is to thickness for 0.1 ~ 0.3mm cerium tablet is polished and is used absolute ethyl alcohol
Clean up, be sprayed on flannelette with 0.5 ~ 1.5 μm of diamond spraying polishing agent, cerium tablet is being had into diamond spraying polishing agent
Be put into the cerium tablet after polishing in anhydrous alcohol solution and be cleaned by ultrasonic by polishing up to being minute surface on flannelette；
（4）To treat that the cerium tablet of anodic oxidation is put into electrolyte Anodic Oxidation, negative electrode is platinum or lead, and cerium tablet is anode, anodic oxygen
The process conditions of change are 8~200mA/dm of current density2, 0~20 DEG C of oxidizing temperature, 100~600rpm of speed of agitator, during oxidation
Between 3~17h, after anodic oxidation is finished, anodic oxidation part with water rinse, air-dry；
（5）Anodic oxidation part is put into Muffle furnace, with 0.4 ~ 0.6 DEG C/min temperature programmings to 320~800 DEG C, 320~
400 DEG C of 0.5~2 h of roasting, are cooled to room temperature, and it is fine and close rear-earth-doped titanium dioxide in the middle of many nanometers of straight holes that taking-up obtain two sides to be
Cerium film.
2. the preparation method of a kind of rear-earth-doped ceria film according to claim 1, it is characterised in that：The thickness of cerium tablet
It is 0.2mm to spend.
3. the preparation method of a kind of rear-earth-doped ceria film according to claim 1, it is characterised in that：With 1 μm
Diamond spraying polishing agent is sprayed on flannelette.
4. the preparation method of a kind of rear-earth-doped ceria film according to claim 1, it is characterised in that：Described is dilute
Native oxide is any in lanthana, samarium oxide, neodymia, luteium oxide, gadolinium oxide, europium oxide, terbium oxide or praseodymium oxide
It is a kind of.
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| CN107130284A (en) * | 2017-07-07 | 2017-09-05 | 上海应用技术大学 | A kind of preparation method of rare earth, calcium and nickel co-doped ceria/ceria film |
| CN107287643B (en) * | 2017-07-07 | 2019-01-18 | 上海应用技术大学 | A kind of rare earth, nickel and copper codope ceria/ceria film and preparation method thereof |
| CN107130283B (en) * | 2017-07-07 | 2019-12-03 | 上海应用技术大学 | A kind of rare earth, calcium, nickel and copper codope ceria/ceria film preparation method |
| CN107130282B (en) * | 2017-07-07 | 2019-12-03 | 上海应用技术大学 | A kind of rare earth and nickel co-doped ceria/ceria film preparation method |
| CN112158883A (en) * | 2020-10-16 | 2021-01-01 | 成都先进金属材料产业技术研究院有限公司 | Process for preparing vanadium dioxide nano powder |
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