CN114291844A - Preparation method of bismuth oxide coated YSZ powder - Google Patents
Preparation method of bismuth oxide coated YSZ powder Download PDFInfo
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- CN114291844A CN114291844A CN202111647005.XA CN202111647005A CN114291844A CN 114291844 A CN114291844 A CN 114291844A CN 202111647005 A CN202111647005 A CN 202111647005A CN 114291844 A CN114291844 A CN 114291844A
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- ysz powder
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- 239000000843 powder Substances 0.000 title claims abstract description 48
- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 29
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 16
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000012456 homogeneous solution Substances 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- TZSXPYWRDWEXHG-UHFFFAOYSA-K bismuth;trihydroxide Chemical compound [OH-].[OH-].[OH-].[Bi+3] TZSXPYWRDWEXHG-UHFFFAOYSA-K 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims description 9
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 238000009827 uniform distribution Methods 0.000 abstract description 3
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 35
- 239000000243 solution Substances 0.000 description 21
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000011978 dissolution method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- -1 oxygen ion Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a preparation method of bismuth oxide coated YSZ powder, which comprises the following steps: step one, adding bismuth nitrate or hydrate thereof into concentrated nitric acid solution to form Bi3+The concentration is 0.001mol/L-2 mol/L; adding urea, YSZ powder and PVP into an ethylene glycol solution, and magnetically stirring to form a homogeneous solution; step three, mixing the solution prepared in the step one with the solution prepared in the step two to form a homogeneous solution; step four, transferring the solution obtained in the step three into a hydrothermal reaction kettle, reacting to obtain a mixture, and cooling to room temperature; step five, centrifugally washing the mixture prepared in the step four to obtain a precipitate, and drying to obtain Bi2O3Coating YSZ powder with the precursor; step six, the Bi in the step five is added2O3Precursor-coated YSZ powderCalcining for 1-10 h at 200-800 ℃ to obtain bismuth oxide coated YSZ powder. The method disclosed by the invention can be used for preparing nano Bi with uniform distribution and large specific surface area2O3Coating YSZ powder, and has simple and efficient process and easy control of operation.
Description
Technical Field
The present disclosure relates to ceramic powdersIn particular to the field of bismuth oxide (Bi)2O3) A method for preparing coated Yttria Stabilized Zirconia (YSZ) powder.
Background
YSZ has good oxygen ion conductivity and excellent mechanical properties, is widely applied to solid fuel cells, oxygen sensors, wear-resistant devices and the like, but the high sintering temperature limits the popularization of the application of the YSZ. Bismuth oxide (Bi)2O3) The addition of (2) can greatly reduce the sintering temperature, but at this stage, Bi2O3Is added in a mechanical mixing manner so that Bi is added2O3The mixing is not uniform, and serious agglomeration phenomenon exists.
Disclosure of Invention
In view of the problems in the prior art, the present disclosure is directed to a method for preparing bismuth oxide coated YSZ powder, which enables nano Bi to be obtained2O3The distribution is uniform.
In order to achieve the above object, the present disclosure provides a method for preparing bismuth oxide coated YSZ powder, comprising the following steps: step one, adding bismuth nitrate or hydrate thereof into concentrated nitric acid solution, dissolving and stirring to form homogeneous Bi3+Solution of Bi3+The concentration is 0.001mol/L-2 mol/L; adding urea, YSZ powder and PVP into an ethylene glycol solution, and magnetically stirring to form a homogeneous solution; step three, mixing the solution prepared in the step one with the solution prepared in the step two, and stirring to form a homogeneous solution; step four, transferring the solution obtained in the step three into a hydrothermal reaction kettle, reacting for 0.5-20 h at the temperature of 100-250 ℃ to obtain a mixture, and cooling to room temperature; step five, centrifugally washing the mixture prepared in the step four to obtain a precipitate, and drying to obtain Bi2O3Coating YSZ powder with the precursor; step six, the Bi in the step five is added2O3Calcining the precursor-coated YSZ powder for 1-10 h at 200-800 ℃ to obtain bismuth oxide-coated YSZ powder.
In some embodiments, in step one, the concentration of the concentrated nitric acid solution is 68% wt.
In some embodiments, in step one, the dissolution method is ultrasonic dissolution, and the ultrasonic dissolution time is 10-20 min; the stirring time is 20-30 min.
In some embodiments, in step two, the magnetic stirring temperature is room temperature.
In some embodiments, in step two, the molar ratio of the bismuth nitrate or the hydrate thereof to the urea is 1: 2-3.
In some embodiments, in step two, the molar content of the bismuth source is 10% to 50% based on the molar content of the YSZ powder. In some embodiments, in step two, the amount of PVP is 4% to 6% based on the total mass of the bismuth nitrate or hydrate thereof and YSZ powder.
In some embodiments, in step two, the amount of ethylene glycol is 40ml to 60 ml.
In some embodiments, in step five, the number of centrifugal washes is 2-3.
The beneficial effects of this disclosure are as follows:
the method disclosed by the invention can be used for preparing the nano Bi with uniform distribution and large specific surface area by controlling the hydrothermal reaction temperature and the raw material ratio without additional complex procedures2O3Coating YSZ powder. The method disclosed by the invention is simple and efficient in process and easy to control in operation.
Drawings
Fig. 1 is a morphology diagram of the bismuth oxide coated YSZ powder of examples 1-3.
Fig. 2 is an XRD pattern of the bismuth oxide coated YSZ powder of examples 1-3.
Fig. 3 is an XRD chart of the bismuth oxide-coated YSZ powder of examples 1 and 4 to 5.
Fig. 4 is a distribution diagram of Bi elements in the bismuth oxide-coated YSZ powder of example 1.
Detailed Description
The method for preparing bismuth oxide coated YSZ powder according to the present disclosure is described in detail below.
The preparation method of the bismuth oxide coated YSZ powder comprises the following steps:
step one, bismuth nitrate or hydration thereofAdding the mixture into concentrated nitric acid solution, dissolving and stirring to form homogeneous Bi3+Solution of Bi3+The concentration is 0.001mol/L-2 mol/L; adding urea, YSZ powder and PVP into an ethylene glycol solution, and magnetically stirring to form a homogeneous solution; step three, mixing the solution prepared in the step one with the solution prepared in the step two, and stirring to form a homogeneous solution; step four, transferring the solution obtained in the step three into a hydrothermal reaction kettle, reacting for 0.5-20 h at the temperature of 100-250 ℃ to obtain a mixture, and cooling to room temperature; step five, centrifugally washing the mixture prepared in the step four to obtain a precipitate, and drying to obtain Bi2O3Coating YSZ powder with the precursor; step six, the Bi in the step five is added2O3Calcining the precursor-coated YSZ powder for 1-10 h at 200-800 ℃ to obtain bismuth oxide-coated YSZ powder.
The bismuth oxide coated YSZ powder is prepared by a hydrothermal method, reactants are added into a hydrothermal reaction kettle for heating reaction, wherein if the temperature is lower than 100 ℃ in the reaction process, the reaction can not be carried out, and bismuth oxide can not be generated.
In some embodiments, in step one, the concentration of the concentrated nitric acid solution is 68% wt.
In some embodiments, in step one, the dissolution method is ultrasonic dissolution, and the ultrasonic dissolution time is 10-20 min; the stirring time is 20-30 min. The particles of bismuth nitrate or hydrate thereof are dissolved in nitric acid by stirring, the dissolution is more uniform by ultrasonic waves, and the dissolution is insufficient by a short time.
In some embodiments, in step two, the magnetic stirring temperature is room temperature.
In some embodiments, in step two, the molar ratio of the bismuth nitrate or the hydrate thereof to the urea is 1: 2-3. The urea is used as a precipitator, the urea is hydrolyzed to generate ammonia gas by matching with the high temperature and high pressure of the hydrothermal kettle, the ammonia gas is dissolved in water to make the solution alkaline, the bismuth oxide can be generated, and if the amount of the urea is too small, the reaction cannot be carried out.
In some embodiments, in step two, the molar content of the bismuth source is 10% to 50% based on the molar content of the YSZ powder.
In some embodiments, in step two, the amount of PVP is 4% to 6% based on the total mass of the bismuth nitrate or hydrate thereof and YSZ powder.
In some embodiments, in step two, the amount of ethylene glycol is 40ml to 60 ml.
In the fourth step, in the hydrothermal reaction process, the high-temperature and high-pressure conditions in the hydrothermal reaction kettle provide the energy required by the reaction of the urea and the bismuth nitrate, so that the Δ G ═ Δ H-T Δ S is less than 0, and the reaction is carried out.
In some embodiments, in step five, the number of centrifugal washes is 2-3.
In the sixth step, nano Bi can be generated within the calcining temperature range of 200-800 DEG C2O3And (3) powder.
[ test procedures and test results ]
Example 1
Step one, 2.156g of bismuth nitrate pentahydrate is added into 5ml of concentrated nitric acid solution with the concentration of 68 percent by weight, dissolved for 20min by ultrasonic, stirred for 10min to form homogeneous Bi3+Solution of Bi3+The concentration is 0.89 mol/L;
adding 0.9g of urea, 4.91g of YSZ powder and 0.9g of PVP into 55ml of ethylene glycol solution, and magnetically stirring to form a homogeneous solution;
step three, mixing the solution prepared in the step one with the solution prepared in the step two, and stirring for 10min to form a homogeneous solution;
step four, transferring the solution obtained in the step three into a 100ml hydrothermal reaction kettle, reacting for 2 hours at 150 ℃ to obtain a mixture, and cooling to room temperature;
step five, respectively filling the mixture prepared in the step four into 2 centrifugal tubes with the volume of 50ml, and carrying out centrifugal washing for 2-3 times to obtain the productThe precipitate is dried to obtain Bi2O3Coating YSZ powder with the precursor;
step six, the Bi in the step five is added2O3Calcining the precursor-coated YSZ powder for 3h at 500 ℃ to obtain bismuth oxide-coated YSZ powder.
The test results are shown in FIG. 1(a) and FIGS. 2 to 4.
Example 2
The addition amount of the hydrated bismuth nitrate in the first step is 3.423g, so that Bi is added3+The concentration was 1.41mol/L as in example 1. The test chart is shown in fig. 1(b) and fig. 2.
Example 3
The addition amount of the hydrated bismuth nitrate in the first step is 0.23g, so that Bi is added3+The concentration was 0.6mol/L as in example 1. The test chart is shown in fig. 1(c) and fig. 2.
Example 4
The calcination temperature in the sixth step was 300 ℃ as in example 1. The XRD test is shown in FIG. 3.
Example 5
The calcination temperature in the sixth step was 800 ℃ as in example 1. The XRD test is shown in FIG. 3.
Comparative example 1
The hydrothermal temperature in the fourth step was 60 ℃ as in example 1.
YSZ powder coated with bismuth oxide could not be obtained.
In the SEM test chart of FIG. 1, it can be seen that the nano Bi prepared by the present disclosure2O3The coated YSZ powder does not generate agglomeration.
It can be seen from the XRD test chart of fig. 3 that the calcination at 300 ℃ in example 4 results in incomplete reaction, but can also produce bismuth oxide, the reaction at 500 ℃ in example 1 is complete, the crystallinity is good, and the calcination at 800 ℃ in example 5 results in a decrease in the diffraction peak of bismuth oxide, which results in a solid solution of part of bismuth oxide in the YSZ lattice.
In the XRD test chart of FIG. 2, it can be seen that as the addition amount of bismuth nitrate pentahydrate increases, β -Bi2O3The intensity of the diffraction peak of (2) is obviously improved.
Can be seen in the EDS test of FIG. 4The Bi element is distributed uniformly, namely, the nano Bi with uniform distribution and large specific surface area can be prepared by the technical scheme of the disclosure2O3Coating YSZ powder.
The above-disclosed features are not intended to limit the scope of practice of the present disclosure, and therefore, all equivalent variations that are described in the claims of the present disclosure are intended to be included within the scope of the claims of the present disclosure.
Claims (9)
1. A preparation method of bismuth oxide coated YSZ powder comprises the following steps:
step one, adding bismuth nitrate or hydrate thereof into concentrated nitric acid solution, dissolving and stirring to form homogeneous Bi3+Solution of Bi3+The concentration is 0.001mol/L-2 mol/L;
adding urea, YSZ powder and PVP into an ethylene glycol solution, and magnetically stirring to form a homogeneous solution;
step three, mixing the solution prepared in the step one with the solution prepared in the step two, and stirring to form a homogeneous solution;
step four, transferring the solution obtained in the step three into a hydrothermal reaction kettle, reacting for 0.5-20 h at the temperature of 100-250 ℃ to obtain a mixture, and cooling to room temperature;
step five, centrifugally washing the mixture prepared in the step four to obtain a precipitate, and drying to obtain Bi2O3Coating YSZ powder with the precursor;
step six, the Bi in the step five is added2O3Calcining the precursor-coated YSZ powder for 1-10 h at 200-800 ℃ to obtain bismuth oxide-coated YSZ powder.
2. The method of claim 1, wherein in step one, the concentration of the concentrated nitric acid solution is 68 wt%.
3. The method for preparing bismuth oxide coated YSZ powder according to claim 1, wherein in the first step, the dissolving method is ultrasonic dissolving, and the ultrasonic dissolving time is 10-20 min; the stirring time is 20-30 min.
4. The method of claim 1, wherein in step two, the magnetic stirring temperature is room temperature.
5. The method of preparing bismuth oxide coated YSZ powder according to claim 1, wherein in step two, the molar weight ratio of the bismuth nitrate or the hydrate thereof to the urea is 1: 2-3.
6. The method of claim 1, wherein in step two, the molar content of the bismuth source is 10-50% based on the molar content of the YSZ powder.
7. The method of preparing bismuth oxide coated YSZ powder according to claim 1, wherein in step two, the amount of PVP is 4% to 6% based on the total mass of bismuth nitrate or its hydrate and YSZ powder.
8. The method of claim 1, wherein in step two, the amount of ethylene glycol is 40ml to 60 ml.
9. The method of claim 1, wherein in step five, the number of times of centrifugal washing is 2-3.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116835973A (en) * | 2023-06-16 | 2023-10-03 | 华中科技大学 | Bismuth oxide coated zinc oxide powder and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103466702A (en) * | 2013-09-27 | 2013-12-25 | 武汉工程大学 | Method for preparing porous bismuth oxide nano-material without template |
| CN104801294A (en) * | 2015-05-14 | 2015-07-29 | 北京石油化工学院 | Preparation method of bismuth trioxide nanosphere |
| CN106602115A (en) * | 2016-12-07 | 2017-04-26 | 山东大学 | Preparation method of low-temperature type solid electrolyte material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466702A (en) * | 2013-09-27 | 2013-12-25 | 武汉工程大学 | Method for preparing porous bismuth oxide nano-material without template |
| CN104801294A (en) * | 2015-05-14 | 2015-07-29 | 北京石油化工学院 | Preparation method of bismuth trioxide nanosphere |
| CN106602115A (en) * | 2016-12-07 | 2017-04-26 | 山东大学 | Preparation method of low-temperature type solid electrolyte material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116835973A (en) * | 2023-06-16 | 2023-10-03 | 华中科技大学 | Bismuth oxide coated zinc oxide powder and preparation method and application thereof |
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