CN111825442B - Sr, ni and Cr co-doped LaAlO 3 Method for preparing ceramic material and product thereof - Google Patents
Sr, ni and Cr co-doped LaAlO 3 Method for preparing ceramic material and product thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 31
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 22
- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims description 4
- 239000011651 chromium Substances 0.000 claims abstract description 31
- 230000005855 radiation Effects 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 15
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims abstract description 14
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 7
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims abstract description 7
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 239000013067 intermediate product Substances 0.000 claims description 5
- 229910021645 metal ion Inorganic materials 0.000 claims description 5
- 101100345589 Mus musculus Mical1 gene Proteins 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 8
- 238000001354 calcination Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000463 material Substances 0.000 description 11
- 238000012546 transfer Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- -1 lanthanum aluminate Chemical class 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- SXAMGRAIZSSWIH-UHFFFAOYSA-N 2-[3-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,2,4-oxadiazol-5-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NOC(=N1)CC(=O)N1CC2=C(CC1)NN=N2 SXAMGRAIZSSWIH-UHFFFAOYSA-N 0.000 description 1
- YJLUBHOZZTYQIP-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)NN=N2 YJLUBHOZZTYQIP-UHFFFAOYSA-N 0.000 description 1
- 101100341510 Mus musculus Itgal gene Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
The invention discloses Sr, ni and Cr co-doped LaAlO 3 Preparation method of ceramic material and product thereof, according to chemical formula La a Sr b Ni c Al d Cr e O 3 Wherein a = 0.7-0.9, b = 0.05-0.15, c = 0.05-0.15, d = 0.7-0.9, e = 0.1-0.3, strontium nitrate, nickel nitrate, chromium nitrate, lanthanum nitrate and aluminum nitrate are weighed, dissolved in water, then a certain amount of urea is added, ultrasonic dispersion, microwave heating, drying, roasting, grinding, press forming and calcining are carried out for a certain time to obtain the product, the product has good compactness and excellent radiation performance, the infrared emissivity at 0.76-2.5 mu m is 0.95-0.97, and the lower heat conductivity at 1200 ℃ is 1.986-2.103 W.m ‑1 ·K ‑1 The forbidden band width is 1.31-1.35 eV.
Description
Technical Field
The invention belongs to the field of ceramic preparation, and particularly relates to Sr, ni and Cr co-doped LaAlO 3 A method for preparing ceramic material and a product thereof.
Background
The high emissivity energy-saving material is a novel material widely applied to the field of high temperature energy saving, and radiation heat transfer is a main heat transfer mode in a high temperature environment, so that the heat efficiency of high energy consumption equipment represented by a thermal furnace is improved, and the radiation heat transfer capacity of thermal equipment is required to be improved. According to the Wien law and the Plank law, radiant heat under the high-temperature condition of more than 800 ℃ is mainly concentrated in the near-infrared band of 0.76-2.50 mu m, so the emissivity of the near-infrared band is particularly concerned in the field of high-temperature energy conservation.
At present, siC and SiB 6 Infrared radiation materials such as cordierite and the like have been applied to thermal equipment to improve radiation heat transfer capacity at high temperature, but the materials cause radiation rate attenuation due to poor oxidation resistance at high temperature in a long-term high-temperature service environment. Therefore, aiming at the energy-saving application of high-temperature thermal equipment, the development of a novel oxide material with high emissivity in the near infrared range of 0.76-2.50 mu m is very important.
LaAlO 3 The perovskite type semiconductor has high melting point (2180 ℃) and good high-temperature stability, and has a typical indirect transition type energy band structure. Therefore, the doping of the material to improve the performance thereof has received great attention, and common doping elements areFe. Cr and the like greatly improve the infrared radiation performance of the lanthanum aluminate ceramic material. However, the above research does not consider the influence of compactness of the lanthanum aluminate ceramic material on other properties, and the development of a ceramic material with higher radiation performance in a near infrared band and lower thermal conductivity is still a problem to be solved at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a Sr, ni and Cr codoped LaAlO aiming at the defects in the prior art 3 The ceramic material and the preparation method thereof have the advantages of good compactness, excellent radiation performance, lower thermal conductivity and forbidden band width value.
The invention adopts the following technical scheme:
sr, ni and Cr co-doped LaAlO 3 The preparation method of the ceramic material comprises the following steps:
1) According to the chemical formula La a Sr b Ni c Al d Cr e O 3 The stoichiometric ratio of (1), wherein a = 0.7-0.9, b = 0.05-0.15, c = 0.05-0.15, d = 0.7-0.9, e = 0.1-0.3, strontium nitrate, nickel nitrate, chromium nitrate, lanthanum nitrate and aluminum nitrate are weighed and put into a beaker, and a proper amount of distilled water is added to fully stir and dissolve;
2) Adding a certain amount of urea into a beaker under the condition of stirring, performing ultrasonic dispersion, then performing microwave heating, and evaporating to obtain an intermediate product A;
3) Putting the product A into a drying oven for drying, then grinding the dried sample, then putting the sample into a muffle furnace for roasting, taking out the sample, cooling to room temperature, and then fully grinding to obtain loose powder;
4) Then the loose powder is put into a mould and is pressed and molded under the pressure of 100MPa to 150MPa, and then is sintered for 1 to 3 hours in the air atmosphere of 1400 to 1700 ℃ to obtain Sr, ni and Cr codoped LaAlO 3 A ceramic material.
Preferably, in the step 2), the amount of the urea added is 1 to 1.5 times the total molar amount of the metal ions.
Preferably, in the step 2), the ultrasonic dispersion time is 1-3 h, the microwave heating temperature is 70-90 ℃, and the heating time is 1-3 h.
Preferably, in the step 3), the drying temperature is 100-140 ℃, the drying time is 10-16 h, the roasting temperature is 1100-1300 ℃, and the roasting time is 1-3 h.
According to another technical scheme, the Sr, ni and Cr co-doped LaAlO prepared based on the preparation method 3 A ceramic material.
The ceramic material has good compactness and excellent radiation performance, the infrared emissivity of 0.95-0.97 at 0.76-2.5 mu m and the lower thermal conductivity of 1.986-2.103 W.m at 1200 DEG C -1 ·K -1 The forbidden band width is 1.31-1.35 eV.
Compared with the prior art, the invention has at least the following beneficial effects:
1) The Sr, ni and Cr co-doped LaAlO provided by the invention 3 Ceramic material according to the formula La a Sr b Ni c Al d Cr e O 3 Wherein a = 0.7-0.9, b = 0.05-0.15, c = 0.05-0.15, d = 0.7-0.9, e = 0.1-0.3, strontium nitrate, nickel nitrate, chromium nitrate, lanthanum nitrate and aluminum nitrate are weighed, dissolved in water, then a certain amount of urea is added, ultrasonic dispersion, microwave heating, drying, roasting, grinding, press forming and calcining are carried out for a certain time to obtain the product, the product has good compactness and excellent radiation performance, the infrared emissivity at 0.76-2.5 mu m is 0.95-0.97, and the thermal conductivity at 1200 ℃ is lower and is 1.986-2.103 W.m -1 ·K -1 The forbidden band width is 1.31-1.35 eV.
2) Doping Sr, ni and Cr into LaAlO 3 In the crystal lattice, the synergistic effect of the three elements promotes LaAlO 3 The radiation performance of the ceramic material is obviously improved, the doping of the elements enhances phonon scattering, and the mean free path of phonons is reduced, so that the heat conductivity of the material is reduced, the impurity energy level is formed in the forbidden band of the material due to the doping of the elements, and the impurity energy level corresponding to electron transitionAnd the infrared radiation device is positioned in a near infrared spectrum region, so that the forbidden band width value is reduced, and the radiation capability is enhanced.
3) La is synthesized by two steps by using an ultrasonic-microwave auxiliary self-combustion method a Sr b Ni c Al d Cr e O 3 Wherein a = 0.7-0.9, b = 0.05-0.15, c = 0.05-0.15, d = 0.7-0.9, e = 0.1-0.3, so that the ceramic material has good sintering characteristics, the porosity of the ceramic material is remarkably reduced, the compactness is improved, the radiation performance is further improved, and the heat conductivity and the forbidden bandwidth value are reduced.
In conclusion, the Sr, ni and Cr co-doped LaAlO prepared by the invention 3 The ceramic material has good compactness, excellent radiation performance, lower thermal conductivity and forbidden band width value, and is an ideal material.
The technical solution of the present invention is further described in detail by the following examples.
Detailed Description
The Sr, ni and Cr co-doped LaAlO provided by the invention 3 The preparation method of the ceramic material comprises the following steps:
1) According to the chemical formula La a Sr b Ni c Al d Cr e O 3 The stoichiometric ratio of (1), wherein a = 0.7-0.9, b = 0.05-0.15, c = 0.05-0.15, d = 0.7-0.9, e = 0.1-0.3, strontium nitrate, nickel nitrate, chromium nitrate, lanthanum nitrate and aluminum nitrate are weighed and put into a beaker, and a proper amount of distilled water is added to fully stir and dissolve;
2) Adding urea which is 1-1.5 times of the total mole amount of metal ions into a beaker under the condition of stirring, ultrasonically dispersing for 1-3 h, then carrying out microwave heating for 1-3 h in a microwave chemical reactor at 70-90 ℃, and evaporating to obtain an intermediate product A;
3) Putting the product A into a drying oven to be dried for 10-16 h at the temperature of 100-140 ℃, then grinding the dried sample, then putting the sample into a muffle furnace to be roasted for 1-3 at the temperature of 1100-1300 ℃, taking out the sample, cooling the sample to room temperature, and then fully grinding the sample to obtain loose powder;
4) Then putting the loose powder intoIn a mould, pressing and molding under the pressure of 100 MPa-150 MPa, and then sintering for 1-3 h in the air atmosphere at 1400-1700 ℃ to obtain Sr, ni and Cr co-doped LaAlO 3 A ceramic material.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. The components of the embodiments of the present invention generally shown may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Sr, ni and Cr co-doped LaAlO 3 The preparation method of the ceramic material comprises the following steps:
1) According to the chemical formula La a Sr b Ni c Al d Cr e O 3 Wherein a =0.8, b =0.1, c =0.1, d =0.8, e =0.2, strontium nitrate, nickel nitrate, chromium nitrate, lanthanum nitrate and aluminum nitrate are weighed and put into a beaker, and an appropriate amount of distilled water is added to fully stir and dissolve;
2) Adding urea which is 1.5 times of the total mole amount of metal ions into a beaker under the condition of stirring, ultrasonically dispersing for 2 hours, then heating for 2 hours in a microwave chemical reactor at 85 ℃ by microwave, and evaporating to obtain an intermediate product A;
3) Drying the product A in a drying oven at 120 ℃ for 14h, grinding the dried sample, roasting in a muffle furnace at 1250 ℃ for 2h, taking out the sample, cooling to room temperature, and fully grinding to obtain loose powder;
4) Then putting the loose powder into a mould, pressing and forming the loose powder at the pressure of 120MPa, and then carrying out air atmosphere at the temperature of 1600 DEG CSintering for 2h to obtain Sr, ni and Cr co-doped LaAlO 3 A ceramic material.
Example 2
Sr, ni and Cr co-doped LaAlO 3 The preparation method of the ceramic material comprises the following steps:
1) According to the chemical formula La a Sr b Ni c Al d Cr e O 3 Wherein a =0.8, b =0.15, c =0.05, d =085, and e =0.15, strontium nitrate, nickel nitrate, chromium nitrate, lanthanum nitrate, and aluminum nitrate are weighed and placed into a beaker, and an appropriate amount of distilled water is added to fully stir and dissolve;
2) Adding urea which is 1 time of the total mole amount of metal ions into a beaker under the condition of stirring, carrying out ultrasonic dispersion for 3 hours, then carrying out microwave heating for 3 hours at 75 ℃ in a microwave chemical reactor, and evaporating to obtain an intermediate product A;
3) Putting the product A into a drying oven, drying for 16h at 100 ℃, then grinding the dried sample, then putting the sample into a muffle furnace, roasting for 1h at 1300 ℃, taking out the sample, cooling to room temperature, and then fully grinding to obtain loose powder;
4) Then the loose powder is put into a die and is pressed and molded under the pressure of 100MPa, and then is sintered for 3 hours in the air atmosphere of 1500 ℃ to obtain Sr, ni and Cr codoped LaAlO 3 A ceramic material.
Comparative example
Comparative examples 1 to 7 according to the formula La a Sr b Ni c Al d Cr e O 3 Wherein the total amount of doping elements is the same, except that a, b, c, d, e are different, and the other preparation conditions and parameters are the same as in example 1.
Comparative example 8 the microwave-assisted mode was omitted and the other preparation conditions and parameters were the same as in example 1.
The spectral absorption rate of the sample at 760-2 500nm and the spectral absorption curve at 200-800 nm are tested by using a Lambda 750S type ultraviolet-visible-near infrared spectrophotometer and a barium sulfate integrating sphere attached to the spectrophotometer. The thermal diffusivity and specific heat were measured using an LFA 1 000 type laser thermal conductivity instrument. Specific parameters are shown in table 1:
TABLE 1 a, b, c, d, e specific values
a | b | c | d | e | |
Example 1 | 0.8 | 0.1 | 0.1 | 0.8 | 0.2 |
Comparative example 1 | 0.8 | 0.2 | 0 | 0.8 | 0.2 |
Comparative example 2 | 0.8 | 0 | 0.2 | 0.8 | 0.2 |
Comparative example 3 | 0.8 | 0.1 | 0.1 | 1 | 0 |
Comparative example 4 | 0.8 | 0.2 | 0 | 1 | 0 |
Comparative example 5 | 0.8 | 0 | 0.2 | 1 | 0 |
Comparative example 6 | 1 | 0 | 0 | 0.8 | 0.2 |
Comparative example 7 | 1 | 0 | 0 | 1 | 0 |
Comparative example 8 | 0.8 | 0.1 | 0.1 | 0.8 | 0.2 |
TABLE 2 LaAlO 3 Main properties of ceramic material
In conclusion, the Sr, ni and Cr co-doped LaAlO prepared by the invention 3 The ceramic material is an ideal material because of its compactness, excellent radiation property, low thermal conductivity and forbidden bandwidth value, and the synergistic effect between Sr, ni and Cr promotes LaAlO by comparing example 1 with comparative examples 1-7 3 The radiation performance of the ceramic material is obviously improved, the heat conductivity of the material is reduced, the forbidden bandwidth value is reduced, and the radiation capability is enhanced; it can be found by comparing example 1 with comparative example 8 that the densification is improved by the microwave-assisted self-combustion method, thereby promoting the improvement of the radiation performance and reducing the thermal conductivity and the forbidden bandwidth value.
The above contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention should not be limited thereby, and any modification made on the basis of the technical idea proposed by the present invention falls within the protection scope of the claims of the present invention.
Claims (4)
1. Sr, ni and Cr co-doped LaAlO 3 The preparation method of the ceramic material is characterized by comprising the following steps: 1) According to the chemical formula La a Sr b NicAl d Cr e O 3 Wherein a = 0.7-0.9, b = 0.05-0.15, c = 0.05-0.15, d =0.7 ∞0.9,e = 0.1-0.3, weighing strontium nitrate, nickel nitrate, chromium nitrate, lanthanum nitrate and aluminum nitrate, putting into a beaker, adding a proper amount of distilled water, and fully stirring and dissolving; 2) Adding a certain amount of urea into a beaker under the stirring condition, performing ultrasonic dispersion, then performing microwave heating, and evaporating to obtain an intermediate product A; 3) Putting the product A into a drying oven for drying, then grinding the dried sample, then putting the ground sample into a muffle furnace for roasting, taking out the sample, cooling the sample to room temperature, and then fully grinding the sample to obtain loose powder; 4) Then the loose powder is put into a mould and is pressed and molded under the pressure of 100MPa to 150MPa, and then is sintered for 1 to 3 hours in the air atmosphere of 1400 to 1700 ℃ to obtain Sr, ni and Cr codoped LaAlO 3 A ceramic material;
in the step 2), the addition amount of the urea is 1-1.5 times of the total mole amount of the metal ions;
in the step 3), the drying temperature is 100-140 ℃, the drying time is 10-16 h, the roasting temperature is 1100-1300 ℃, and the roasting time is 1-3 h.
2. The method of claim 1, wherein: in the step 2), the ultrasonic dispersion time is 1-3 h, the microwave heating temperature is 70-90 ℃, and the heating time is 1-3 h.
3. Sr, ni and Cr codoped LaAlO prepared by the preparation method according to any one of claims 1-2 3 A ceramic material.
4. The ceramic material of claim 3, wherein the ceramic material has good compactness and excellent radiation performance, has an infrared emissivity of 0.95-0.97 at 0.76-2.5 μm, and has a low thermal conductivity of 1.986-2.103W-m at 1200 ℃ -1 ·K -1 The forbidden band width is 1.31-1.35 eV.
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