CN111795983A - Preparation method of standard sample for aluminum oxide alpha-phase determination - Google Patents
Preparation method of standard sample for aluminum oxide alpha-phase determination Download PDFInfo
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- CN111795983A CN111795983A CN202010609188.5A CN202010609188A CN111795983A CN 111795983 A CN111795983 A CN 111795983A CN 202010609188 A CN202010609188 A CN 202010609188A CN 111795983 A CN111795983 A CN 111795983A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
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- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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Abstract
The invention discloses a preparation method of a standard sample for measuring alumina alpha-phase, which comprises the steps of selecting a boehmite precursor, preserving heat for 1-48h in a high-temperature kiln at 1250-1500 ℃, naturally cooling, and grinding to obtain a white powdery standard sample, wherein the boehmite purity is more than or equal to 99.95%, Fe is less than or equal to 150ppm, Na is less than or equal to 400ppm, Si is less than or equal to 100ppm, the granularity D50 is less than or equal to 3um, and the length-diameter ratio is 1-100. The standard sample prepared by the preparation method can accurately determine the alpha-phase content in the alumina, determine the I/Ic value and calibrate the position and the line shape of the diffraction line.
Description
Technical Field
The invention relates to alumina production, in particular to a preparation method of a standard sample for phase analysis of an alumina product.
Background
Alumina is one of the most common chemical feedstocks. At present, more than ten kinds of phases such as alpha phase, rho phase and gamma phase are common. Use of alumina sources in ceramics and catalyst industriesThe content of the alpha-phase of alumina is one of the important indicators of concern when feeding. alpha-Al2O3The crystal structure is compact, the hardness is high, the abrasion resistance, the acid and alkali resistance and the high-temperature stability are strong, and the crystal structure can be used as one of raw materials to ensure that the ceramic material and the catalyst carrier have excellent performances. alpha-Al occurring in nature2O3There are natural corundum, ruby, sapphire, etc. Industrial alpha-Al2O3The aluminum source is obtained by roasting aluminum sources such as aluminum hydroxide, transition state aluminum oxide, boehmite or common industrial-grade aluminum oxide at high temperature, and besides impurity elements, other phase states can cause adverse effects such as volume shrinkage, strength reduction and internal stress defect of downstream products.
The alpha phase content in the alumina is effectively and accurately analyzed and detected, and the method is of great importance to the quality control of alumina raw materials and the improvement of the quality of ceramic materials and catalyst carriers. At present, the alpha phase content of alumina is detected at home and abroad by adopting an X-ray diffraction method, a reference sample is regarded as 100 percent of alpha phase, and the alpha phase-alumina content in a test sample is obtained by detecting the integral intensity of characteristic peaks of the reference sample and the test sample and calculating through comparison. A reference sample in GB/T6609.32 'chemical analysis method of alumina and determination method of physical properties of alpha-alumina content x-ray diffraction method' in the current domestic standard is prepared by taking about 100g of metallurgical-grade alumina, putting into a 600ml beaker, adding 250ml of hydrochloric acid, stirring for 3h at normal temperature, filtering, washing, drying for 2h at 105 ℃, calcining for 24h at 1300 ℃, and cooling to obtain the reference sample. A method for preparing a reference sample in a color industry standard YS/T976-2014 & lt X-ray diffraction method for measuring calcined alpha-alumina content & gt is as follows: putting high-purity alumina (the content of Al2O3 is not less than 99.99%) micro powder into a corundum crucible, and burning for 4 hours at 1450 ℃ to obtain a reference sample. The two preparation methods have shown a certain technical lagging for the development and detection of the current domestic alpha-alumina production technology, and can not meet the requirements of analysis and detection gradually, and the two preparation methods are mainly expressed as follows: (1) the alpha phase content of the prepared reference sample is not enough to reach 100 percent; (2) the net integral intensity of the characteristic peak of the reference sample is not strong enough, the crystal lattice has many vacancies, and the crystallization is imperfect; (3) the reproducibility of a reference sample is poor, and the using effect is poor; (4) the selection of the precursor is not optimal, and the range of performance indexes is too wide.
Disclosure of Invention
The invention aims to provide a preparation method of an alumina sample with 100 percent of alpha-phase content, perfect crystallization, good dispersibility and good stability. The sample prepared by the method can be used as a standard sample for measuring the content of the alpha phase of alumina by an X-ray diffraction method, determining the I/Ic value (namely the intensity ratio of each diffraction peak I to the highest diffraction peak Ic), and calibrating the position and the line shape of the diffraction line.
The invention is realized by the following technical scheme.
The invention comprises a preparation method of a standard sample for measuring alumina alpha-phase, which comprises the steps of selecting a boehmite precursor, preserving heat for 1-48h in a high-temperature kiln at 1250-1500 ℃, and grinding to obtain a white powdery standard sample after natural cooling. The roasting temperature rise speed is 3-20 ℃/min, preferably 5-12 ℃/min. The final temperature is 1250-1500 ℃, preferably 1350-1450 ℃, and the heat preservation time is 1-48h, preferably 4-8 h. When a sample is ground, in order to avoid damaging a grain-crystal interface, reduce the phase transformation rate and prevent the introduction of impurity elements, a polyurethane mill or an air flow mill with proper grinding force is selected, and a ball-milling medium is zirconia balls or zirconium silicate balls, preferably zirconia balls.
The purity of boehmite is more than or equal to 99.95 percent, wherein Fe is less than or equal to 100ppm, Na is less than or equal to 300ppm, and Si is less than or equal to 50 ppm. The boehmite granularity D50 is less than or equal to 3um, the length-diameter ratio is 1-100, and the morphology is spherical, spheroidal, dumbbell-shaped, vermicular, rod-shaped, needle-shaped, banded or flaky.
According to the preparation method, in order to meet the requirement that the standard sample can be uniformly heated and influence of heat transfer on phase inversion is not influenced, boehmite is loaded in a corundum sagger with a certain volume for roasting, and the volume of the sagger is less than or equal to 5L, preferably 0.5L-2L.
The standard sample for measuring the alpha-phase of the alumina prepared by the invention has the alpha-phase content of 100 percent and the purity (mass percent) of not less than 99.95 percent. Impurity elements in the raw material have an effect on the alpha-phase content of the alumina sample, for example, the alpha phase of the alumina is significantly reduced by the Na element. The invention controls the impurity elements of iron less than or equal to 200ppm, sodium less than or equal to 500ppm, silicon less than or equal to 150ppm, preferably Fe less than or equal to 100ppm, Na less than or equal to 300ppm and Si less than or equal to 50ppm in the raw materials, thereby preparing an alumina sample with the alpha-phase content of 100 percent.
The precursor used in the invention is boehmite, and can be transformed into alpha phase under lower activation energy, and the prepared alpha-alumina has fewer crystal lattice vacancies and more perfect crystallization, and better meets the detection requirement. Alpha-alumina is an aluminum oxide hexaligand close-packed structure, the precursor of the existing preparation method is metallurgical-grade alumina or high-purity alumina, which is a mixed lattice structure of the aluminum oxide hexaligand (about 60%) and the aluminum oxide tetraligand, and not only higher conversion energy is needed in the phase inversion process, but also the lattice difference of the two lattice structures can cause that the prepared alpha-alumina has more crystal lattice vacancies and imperfect crystallization. The precursor used in the invention is boehmite which is a hexagonal close-packed layered structure, the layers are connected by hydrogen bonds, and after the hydrogen bonds between the boehmite layers are opened at high temperature, the boehmite layers can be converted into alpha phase under lower activation energy, so that the prepared alpha-alumina has fewer crystal lattice vacancies and more perfect crystallization.
The standard sample for determining the alpha-phase of the aluminum oxide prepared by the invention has strong stability and good reproducibility, and can better meet the requirements of detection technology. The existing preparation method has no requirement on sample granularity, and the sample granularity has great influence on products and detection: firstly, the particle size is large, the sample is not easy to completely convert the phase in the preparation process, a small amount of inclusion phase exists, and the phase conversion rate is reduced; secondly, the existing alumina product has more irregular shapes and large particle size range, when X-rays are incident from large particles or along the length direction of the particles during detection, the number of the actually detected particles is small, the particle layer which can be penetrated by a ray incident sample is different along with the different scanning positions of the rays, so that an obvious orientation effect is caused, the accidental errors of the system are obviously increased, and the detection reproducibility is poor. The particle size D50 of the boehmite particles is less than or equal to 3um, preferably D50 is less than or equal to 1.0um, most preferably D50 is less than or equal to 0.6um, the length-diameter ratio is 1-100, preferably 1-20, the complete phase inversion of a sample can be ensured, and the orientation effect of rays existing in a standard sample in use can be reduced.
The requirement on the morphology of the sample particles is to reduce the orientation effect of rays during detection as much as possible, the detection stability and the reproducibility are good, the standard requirement of a standard sample is met, and the length-diameter ratio of the sample particles is less than or equal to 10, preferably 1-4. The topography can be spherical, spheroidal, dumbbell, vermiform, rod, needle, ribbon, sheet, and the like, with spherical, spheroidal, and dumbbell being preferred.
In the invention, no mineralizer or additive is used in the preparation process of the standard sample, and no impurity element is introduced while the complete phase inversion dispersity of the sample is ensured to be good through process adjustment.
The standard sample for measuring the alpha-phase of the alumina prepared by the invention adopts an X-ray diffraction method to carry out value determination on a standard sample candidate.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of a standard sample for measuring an alumina alpha-phase, which comprises the following steps:
precursor boehmite with the purity being equal to or greater than 99.95% and the particle size D50 being equal to or less than 3um is placed in a corundum sagger with the volume being equal to or less than 5L, is kept warm for 1-48h in a high-temperature kiln at 1250-1500 ℃, is naturally cooled, is ground by using an air flow mill or a ball milling tank with a polyurethane lining, and is subjected to ball milling by using zirconia balls or zirconium silicate balls as a ball milling medium, and then is screened by a 60-mesh sieve, so that a white powdery standard sample is obtained.
In order to meet the product quality requirement, the purity of boehmite is equal to or greater than 99.95%, Fe is equal to or less than 150ppm, Na is equal to or less than 400ppm, and Si is equal to or less than 100ppm, preferably Fe is equal to or less than 100ppm, Na is equal to or less than 300ppm, and Si is equal to or less than 50 ppm. Particle size D50 ≦ 3um, preferably D50 ≦ 1um, most preferably D50 ≦ 0.6um, and aspect ratio 1-100, preferably 1-20. The topography can be spherical, spheroidal, dumbbell, vermiform, rod, needle, ribbon, sheet, and the like, with spherical, spheroidal, and dumbbell being preferred.
The temperature rising speed in the sintering process is 3-20 ℃/min, preferably 5-12 ℃/min, the final temperature is 1250-1500 ℃, preferably 1350-.
The standard sample prepared by the method is used for measuring the alpha-phase content in alumina, determining the I/Ic value, and calibrating the position and the line shape of a diffraction line, and is mainly used in an X-ray diffractometer. The standard sample is evaluated by X-ray diffraction.
Example 1
100g of strip boehmite (D502.5um, 99.95 percent, Fe 102ppm, Na 308ppm, Si 57ppm and the length-diameter ratio of 35-80) is placed in a 700mL corundum crucible, is roasted at 1350 ℃ in a high-temperature furnace, the heating rate is 8 ℃/min, the heat preservation time is 8h, is naturally cooled, is ground for 1h by adopting a polyurethane mill, and is sieved by a 60-mesh sieve to obtain a sample with the purity of 99.93 percent and the granularity of D503.5um, the sample has the phase inversion rate of 100 percent through detection, and the requirement of the content of alpha-phase in alumina through X-ray diffraction method determination is met.
Example 2
5kg of flaky boehmite (D501.0um, 99.96%, Fe 97ppm, Na 326ppm, Si 82ppm and the length-diameter ratio of 15-48) is placed in 25 corundum crucibles of 1.2L, the corundum crucibles are roasted in a tunnel kiln at 1400 ℃, the heating rate is 10 ℃/min, the heat preservation time is 6h, the corundum crucibles are naturally cooled and ground for 45min by a polyurethane mill, and the corundum crucibles are sieved by a 60-mesh sieve to obtain a sample with the purity of 99.91% and the granularity of D501.2um, and the sample has the phase inversion rate of 100% after detection, so that the use requirement of determining the alpha-phase content in alumina by an X-ray diffraction method is met.
Example 3
70kg of plate-shaped boehmite (D500.6um, 99.97%, Fe 84ppm, Na 305ppm, Si 52ppm, and the length-diameter ratio of 1.5-3.5) is placed in 140 corundum crucibles of 2L, and is roasted in a 1-ton electric heating furnace, the heating rate is 12 ℃/min, the final temperature is 1450 ℃, the heat preservation time is 4h, after natural cooling, a sample is ground by an air flow mill and passes through a 60-mesh sieve, so that the sample with the purity of 99.94% and the granularity of D500.8um is obtained, the phase inversion rate is 100% after detection, the use requirement of measuring the alpha-phase content in alumina by an X-ray diffraction method is met, the sample is subjected to uniformity and stability investigation and determination by the X-ray diffraction method, and the sample meets the requirement of GB/T15000 specification on a standard sample.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (9)
1. A preparation method of a standard sample for measuring an alumina alpha-phase is characterized in that a boehmite precursor is selected to be insulated for 1-48h in a high-temperature kiln at 1250-1500 ℃, and after natural cooling, a white powdery standard sample is obtained by grinding, wherein the boehmite purity is more than or equal to 99.95%, Fe is less than or equal to 150ppm, Na is less than or equal to 400ppm, Si is less than or equal to 100ppm, the granularity D50 is less than or equal to 3um, and the length-diameter ratio is 1-100.
2. The method for preparing a standard sample for the measurement of an alumina α -phase according to claim 1, wherein the standard sample is prepared from boehmite having a purity of 99.95% or more, Fe of 100ppm or less, Na of 300ppm or less, and Si of 50ppm or less.
3. The method for preparing a standard sample for the alpha-phase measurement of alumina according to claim 1, wherein the boehmite particle size D50 is not more than 3um, the aspect ratio is 1-100, and the morphology is spherical, spheroidal, dumbbell, worm-like, rod-like, needle-like, ribbon-like, or plate-like.
4. The method for preparing a standard sample for alumina alpha-phase measurement according to claim 1, wherein the temperature rising rate during boehmite sintering is 3-20 ℃/min.
5. The method for preparing a standard sample for the alpha-phase measurement of alumina according to claim 1, wherein the boehmite retention temperature is 1350-.
6. The method for preparing a standard sample for alumina α -phase measurement according to claim 1, wherein boehmite is calcined in a corundum sagger having a volume of ≦ 5L.
7. The method for preparing a standard sample for the alpha-phase determination of alumina according to claim 1, wherein the milling apparatus is a ball mill pot or a jet mill.
8. The method for preparing a standard sample for the alpha-phase determination of alumina according to claim 1, wherein the prepared standard sample is alumina having an alpha-phase content of 100%, a purity, i.e., a mass percentage, of not less than 99.9%, and the impurity elements of Fe of not more than 200ppm, Na of not more than 500ppm, and Si of not more than 150 ppm; the standard sample particle size D50 is less than or equal to 5um, and the particle length-diameter ratio is less than or equal to 10.
9. The method for preparing a standard sample for the measurement of an alumina α -phase according to claim 8, wherein the standard sample has a particle aspect ratio of 1 or more and a particle aspect ratio of 4 or less.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115639040A (en) * | 2022-11-01 | 2023-01-24 | 西南石油大学 | Method for manufacturing carbonate rock in-situ micro-area ultra-micro powder pressed cake standard sample |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115639040A (en) * | 2022-11-01 | 2023-01-24 | 西南石油大学 | Method for manufacturing carbonate rock in-situ micro-area ultra-micro powder pressed cake standard sample |
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Application publication date: 20201020 |