CN113029855A - Analysis method for segregation distribution of quartz crystal lattice impurity elements - Google Patents

Analysis method for segregation distribution of quartz crystal lattice impurity elements Download PDF

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CN113029855A
CN113029855A CN202110269511.3A CN202110269511A CN113029855A CN 113029855 A CN113029855 A CN 113029855A CN 202110269511 A CN202110269511 A CN 202110269511A CN 113029855 A CN113029855 A CN 113029855A
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李育彪
肖蕲航
裴振宇
马强
雷绍民
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Abstract

The invention relates to a method for analyzing the segregation distribution of quartz crystal lattice impurity elements, which comprises the following steps: obtaining the mass, the volume and the initial impurity content of the quartz to be analyzed; using the strippers with different concentrations to strip the surface of the quartz, and obtaining the quality of the stripped quartz each time and the impurity content in the quartz after each stripping; establishing a mathematical model based on the average content of impurities in the denuded quartz and the depth of the corresponding part from the surface of the quartz according to the parameters; and then, calculating the content and the depth of impurity elements from the surface to the inside of a certain impurity according to a mathematical model through a plurality of groups of denudation tests. The analysis method provided by the invention can obtain the enrichment area and the loss area of the impurities, has small deviation of the calculation result from the actual condition, and can make up the technical defect that the conventional quantitative analysis methods such as EMPA (empirical mode amplification) and the like cannot accurately measure the distribution of the impurities in the quartz in situ.

Description

Analysis method for segregation distribution of quartz crystal lattice impurity elements
Technical Field
The invention relates to the technical field of quartz impurity detection, in particular to a method for analyzing the segregation distribution of quartz crystal lattice impurity elements.
Background
Current testing methods for the quantitative analysis of elemental concentrations in quartz include plasma mass spectrometry (LA-ICP-MS), Secondary Ion Mass Spectrometry (SIMS), and electron probe wave spectrometry (EPMA-WDS). As shown in FIG. 1, the EPMA, SIMS and LA-ICP-MS are compared with each other to obtain a comparison of the minimum required quantity of EPMA volume of 150 μm3The method is most suitable for quantitative analysis of low-concentration trace elements, the lower limit of the analysis concentration can reach tens of mu g/g, and the scale can be accurate to 10 mu m. However, the average content of each trace element in the high-purity quartz is generally lower than 10 mu g/g, only part of elements can reach dozens of mu g/g and is lower than the detection lower limit of EPMA. Because the content of trace elements in the high-purity quartz is low, the segregation scale is small, and the thicknesses of an enrichment area and a depletion area are only a few tenths of micrometers to a few micrometers and are far lower than the single detection lower limit of EPMA. In addition, trace elements in actual minerals are extremely unevenly distributed in quartz particles, so that great difficulty exists in quantitative analysis of segregation concentration change of the trace elements in the high-purity quartz by using EMPA, and the concentration change of the trace elements in the high-purity quartz cannot be accurately measured.
Disclosure of Invention
In view of the above, it is necessary to provide a method for analyzing the segregation distribution of impurity elements in quartz crystal lattices, which can overcome the problem that the prior art cannot accurately measure the impurity elements in the crystal lattices in natural quartz by approximately calculating the segregation concentration of trace impurity elements in crystal lattices in quartz.
The invention provides a method for analyzing the segregation distribution of quartz crystal lattice impurity elements, which comprises the following steps:
s1, acquiring the mass, the volume and the initial impurity content of the quartz to be analyzed;
s2, using the strippers with different concentrations to strip the surface of the quartz, and obtaining the quality of the stripped quartz each time and the impurity content in the quartz after each stripping;
s3, establishing a mathematical model based on the average content of impurities in the denuded quartz and the depth of the corresponding part from the surface of the quartz according to the parameters obtained in the steps S1 and S2;
and S4, calculating the content and depth of a certain impurity from the surface to the inside according to the mathematical model through a plurality of groups of denudation tests, and further obtaining the segregation distribution condition of the certain impurity in the quartz crystal lattice.
Specifically, in a plurality of tests with different denudation amounts, the quartz surface is eroded to the inside thereof, and the concentration of the used denudation agent is increased.
Specifically, the concentration of the denudating agent has a linear relation with the mass of the denudated quartz.
Optionally, when the etchant is hydrofluoric acid, the linear fitting mathematical formula is as follows:
y＝0.2069x+0.00097，R20.99961; wherein y is the ablated quartz mass, x is the ablation agent concentration, R2To fit the correlation coefficients.
Optionally, when the corrosion inhibitor is sodium hydroxide, the linear fitting mathematical formula is as follows:
y＝0.2069x+0.00097，R20.99961; wherein y is the ablated quartz mass, x is the ablation agent concentration, R2To fit the correlation coefficients.
More specifically, if the amount of the denudation agent is m for each two different concentrationsaAnd mbAnd m isa<mbThe amount of denudation is mb-maThe average content of impurity elements in the mass of the dissolved quartz is Cab，
Cab＝[Cb(m0-mb)-Ca(m0-ma)]/[(m0-mb)-(m0-ma)]；
Wherein the initial mass of the quartz sample is m0. The impurity element content in the residual quartz sample after the two times of leaching by using the stripping agent is respectively CaAnd CbSince the two contents are generally not lower than the lower limit of the quantitative analysis of EMPA, they can be directly known by measurement.
Further, the analysis method also comprises the step of analyzing the content of CabDepth D of corresponding impurities in the quartz crystal latticeab，
Figure BDA0002973654480000031
Wherein r is the initial radius of the ideal quartz sphere, Δ V is the mass of the ideal quartz sphere denuded and dissolved, and Δ V ═ V0-Vr，V0Is the initial volume of ideal quartz sphere particles, VrPi is the circumference ratio, which is the volume remaining after the ideal quartz sphere is ablated.
Has the advantages that:
according to the invention, after the quality and the volume of the quartz particles are obtained, a plurality of denudation tests are carried out by the denudation agent, a mathematical model based on the average content of impurities in denudated quartz and the corresponding depth from the surface of the quartz is established, the content and the depth of the impurity elements in the quartz crystal lattice can be indirectly calculated, the segregation distribution condition of certain impurities in the quartz crystal lattice is obtained, the segregation curve of the impurities in the quartz crystal lattice is further drawn, an impurity enrichment area and a loss area are obtained, the deviation of the calculation result and the actual condition is small, and the technical defect that the existing EMPA can not be accurately measured in quantitative analysis can be overcome.
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FIG. 1 is a comparison of minimum sample amounts required for EPMA, SIMS and LA-ICP-MS analysis methods provided by the present invention.
Fig. 2 is a schematic diagram of the relationship between the amount of leached etchant and the amount of dissolved quartz according to an embodiment of the present invention.
Fig. 3 is a hypothetical schematic diagram of the amount of degradation provided by the embodiment of the present invention.
FIG. 4 is a diagram of Al segregation when a certain quartz lattice is baked at 1000 ℃ for 5 hours according to an embodiment of the present invention.
FIG. 5 is a diagram of Al segregation when a certain quartz lattice is baked at 1000 ℃ for 15h according to an embodiment of the present invention.
FIG. 6 is a diagram of the segregation of Al element in a certain quartz crystal lattice baked at 1000 ℃ for 30h according to an embodiment of the present invention.
FIG. 7 is a diagram of Al segregation during 45h of a certain quartz crystal lattice baked at 1000 ℃ according to an embodiment of the present invention.
FIG. 8 is a cross-sectional view showing the distribution of Al element concentration with time under the firing condition of 1000 ℃ in quartz crystal lattices according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a method for analyzing the segregation distribution of impurity elements in quartz crystal lattices, which comprises the following steps of:
s1, acquiring the mass, the volume and the initial impurity content of the quartz to be analyzed;
s2, using the strippers with different concentrations to strip the surface of the quartz, and obtaining the quality of the stripped quartz each time and the impurity content in the quartz after each stripping;
s3, establishing a mathematical model based on the average content of impurities in the quartz after two times of denudation and the depth from the corresponding part to the surface of the quartz according to the parameters obtained in the steps S1 and S2;
and S4, calculating the content and depth of impurity elements from the surface to the inside of the certain impurity according to the mathematical model through a plurality of groups of denudation tests, and further obtaining the segregation distribution condition of the certain impurity in the quartz crystal lattice.
According to the analysis method provided by the embodiment of the invention, after the mass and the volume of the quartz particles are obtained, a plurality of denudation tests are carried out by the denudation agent, a mathematical model of the average content of impurities in the quartz between every two denudations and the depth of the corresponding part from the surface of the quartz is established, the content and the depth of the impurity elements in the quartz crystal lattice can be indirectly calculated, the segregation distribution condition of certain impurities in the quartz crystal lattice is obtained, the segregation curve of the impurities in the quartz crystal lattice is further drawn, the enrichment region and the loss region of the impurities are obtained, the deviation of the calculation result from the actual condition is small, and the technical defect that the existing quantitative analysis methods such as EMPA (empirical mode amplification) cannot accurately measure the distribution of the impurities.
The mass of the quartz particles can be obtained by adopting an analytical balance for weighing, the analytical balance can adopt an transcendental series analytical balance of Mettler, the reading precision range is 0.001mg, and the measuring range can reach 320.00 g.
In the actual test of a plurality of groups of different denudation amounts, the denudation agent used is continuously eroded from the surface to the inside of the quartz, and the concentration of the denudation agent used is continuously increased. Because weighing in each time is troublesome in the indirect calculation method, and because the denuded quantity is small, the influence of errors generated in the steps of washing, drying and the like after denuded on the denuded quantity is large, the mass of a denuded quartz sample is difficult to accurately weigh, and in order to reduce the error and inconvenience brought by weighing the mass of the denuded quartz in each time, quartz particles are processed by a plurality of groups of denuded agents with different concentrations so as to establish the relationship between the consumption of the denuded agents and the consumption of the denuded quartz.
The relationship between the amount of different denudation agents and the amount of denudated quartz is shown in figure 2, the quartz is denudated by adopting two denudation agents of hydrofluoric acid and sodium hydroxide, and the amount of the denudation agents and the mass of the denudated quartz are in a linear relationship.
When the denudation agent is hydrofluoric acid, a linear fitting mathematical formula is as follows:
y＝0.2069x+0.00097，R20.99961; wherein y is the ablated quartz mass, x is the ablation agent concentration, R2To fit the correlation coefficients.
When the denudation agent is sodium hydroxide, the linear fitting mathematical formula is as follows:
y＝0.53422x+0.00194，R20.98493; wherein y is the mass of the denuded quartz, x is the concentration of the denuded agent, R2To fit the correlation coefficients.
When hydrofluoric acid is used as the stripping agent, the linear correlation coefficient R of the stripping agent is2And more accurately, the hydrofluoric acid is preferably adopted for denudation, and the denudation agent concentration and the dosage can be determined only, so that the denudation agent quantity can be calculated through a linear equation of the denudation agent concentration and the dosage, and a mathematical model of the average content of impurities in the quartz between every two denudations and the depth of a part corresponding to the impurity from the surface of the quartz is established in the following time. The invention uses the leaching agents of hydrofluoric acid and sodium hydroxide which can effectively destroy the structure of silicon dioxide. After the fitting curve of hydrofluoric acid is determined, the later stageWhen analyzing the impurity segregation situation, the concentration of hydrofluoric acid solution is 2mol/L, and the liquid-solid ratio of the hydrofluoric acid solution to quartz solid is 6mL:1 g.
More specifically, when the leaching agent with different concentrations is used for denudating the quartz, if the denudation amount of the denudation agent with each two different concentrations is m respectivelyaAnd mbAnd m isa<mbThe impurity element content in the residual quartz sample after the two times of leaching by using the stripping agent is respectively CaAnd CbInitial mass of the quartz sample is m0The amount of denudation is assumed to be schematically shown in fig. 3. The amount of denudation is maIncrease to mbThe dissolved part of the quartz, which is shaded in FIG. 3, has a mass mabWherein the average content C of impurity elements in the mass of the dissolved part of the quartzabCan be represented by the following equation 1:
Cab＝[Cb(V0-Vb)-Ca(V0-Va)]/[(V0-Vb)-(V0-Va)]
＝[Cbρ(m0-mb)-Caρ(m0-ma)]/[ρ(m0-mb)-ρ(m0-ma)]
＝[Cb(m0-mb)-Ca(m0-ma)]/[(m0-mb)-(m0-ma)]
wherein, VaFor the amount of denudation is maVolume of dissolved quartz, VbFor the amount of denudation is mbThe volume of dissolved quartz, ρ is the density of the quartz.
The method is simplified as follows:
Cab＝[Cb(m0-mb)-Ca(m0-ma)]/[(m0-mb)-(m0-ma)]
equation 1 is calculated.
Therefore, the change condition of the impurity element content from the surface to the inside of the segregation zone can be calculated through a plurality of groups of tests with different denudation amounts.
In order to make the calculation feasible, the actual quartz particles need to be processed uniformly and approximately. Assuming that each quartz grain is the same size and is a standard ideal sphere, the dissolution of each quartz face is the same during the denudation. Taking the average particle diameter of the actual quartz particles as the diameter of an ideal quartz sphere, the radius r of the ideal quartz sphere can be used for calculating the volume V of a single ideal quartz particle under the assumed conditions0。
From the volume relationship of the ideal sphere before and after ablation, equation 2 can be derived:
Figure BDA0002973654480000071
further, the denudation depth D can be calculatedab。
And the analysis content is CabDepth D of partial concentration of corresponding impurities in quartz crystal latticeabAs shown in the formula 3, as shown in the formula,
Figure BDA0002973654480000072
wherein r is the initial radius of the ideal quartz sphere, Δ V is the mass of the ideal quartz sphere denuded and dissolved, and Δ V ═ V0-Vr，V0Is the initial volume of ideal quartz sphere particles, VrPi is the circumference ratio, which is the volume remaining after the ideal quartz sphere is ablated.
Establishing a mathematical model of the average content of impurities in the quartz between every two times of denudation and the depth from the corresponding part to the surface of the quartz according to the step of S3; obtaining an initial mass m of a quartz sample0And calculating the content and the depth of the impurity elements in the quartz crystal lattice according to the denudation amount of a plurality of groups of denudation tests and the volume of the denudated quartz, obtaining the segregation distribution condition of certain impurities in the quartz crystal lattice, and further drawing a segregation curve of the impurities in the quartz crystal lattice to obtain an enrichment area and a loss area of the impurities.
Therefore, when the quartz is roasted, the roasting condition can be controlled, and the impurity elements are controlled to move to the enrichment region, so that the impurities are further concentrated, the impurities in the quartz can be conveniently and intensively removed, and the quartz material with higher purity can be obtained. Specifically, as shown in fig. 4-7, in the roasting process of 5-45 hours, the Al element in the enrichment area is continuously increased, and the Al element in the loss area is continuously decreased, which indicates that the Al element continuously moves to the enrichment area, and the roasting condition is appropriate. In fig. 4-7, the limits of the distance from the quartz surface of the enrichment region and the depletion region are determined based on the distance from the quartz surface of the point where the baseline of the limits of the distance from the quartz surface of each of the enrichment region and the depletion region intersects the actual concentration change curve.
The segregation condition of impurity Al elements in quartz is estimated by adopting the formula, then roasting is carried out under different roasting time conditions (roasting for 5h, 15h, 30h and 45h), then alkali liquor is used for leaching treatment, the relation between the amount of quartz dissolved in the treatment process and the content of Al elements in the residual quartz is shown in figures 4-8, EPMA detection is not needed in the roasting process, the segregation condition of the Al elements in quartz crystal lattices and the migration condition after roasting can be directly predicted, and therefore the Al elements can be effectively removed.
The minimum distance between every two adjacent scattered points shown in FIGS. 4-7 and the surface distance can reach 1 μm, that is, the quartz dissolution amount generated by the denudation of every two adjacent sides is lower than the minimum amount (150 μm) required by EPMA detection3) Namely, the invention providesabIs calculated according to the formula of (C)abThe technical defect that the content of impurities cannot be detected by EPMA can be overcome, and the distribution of the impurity elements in the quartz crystal lattice is important.
The results are shown in FIG. 8: in general, Al element can be effectively removed, so that the content of the Al element is reduced to be less than 20 mu g/g. When the mixture was baked for 5 hours, the Al content decreased rapidly when the amount of dissolved quartz increased from 0% to 1.36%, then decreased at a rate that reached the minimum at 5.79%, and then increased slowly. When the material is roasted for 15 hours, the Al element concentration is rapidly reduced within the range of 0% to 1.68%, is continuously reduced within the range of 1.68% to 4.25%, and is slowly increased within the range of 4.25% to 5.74%. When the mixture was baked for 30 hours, the Al element concentration decreased rapidly in the range of 0% to 0.68%, decreased at a rate of 0.68% to 2.47%, decreased at 2.47%, and then increased slowly. When the mixture is baked for 45 hours, the Al element concentration is rapidly reduced within the range of 0% to 2.26%, and after reaching the lowest point of 2.26%, the Al element concentration starts to slowly rise. In general, the Al element concentration in each roasting time period is generally in three stages of firstly rapidly decreasing, then gradually decreasing and then slowly increasing, but as the roasting time period increases, the Al element content at the lowest point decreases, the Al element concentration in the residual quartz of each denudation amount decreases, and the quartz dissolution amount required for reaching the lowest point also decreases. It is understood that the longer the firing time is and the longer the diffusion time of Al element in the quartz is at 1000 ℃ in the range of 5-45h, the more Al element is concentrated from the inside to the surface of the quartz, and the higher the concentration of Al element in the concentration region, i.e., the enrichment region, the narrower the range and the closer to the surface.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims (7)

1. A method for analyzing the segregation distribution of impurity elements in quartz crystal lattices is characterized by comprising the following steps of:
s1, acquiring the mass, the volume and the initial impurity content of the quartz to be analyzed;
s2, using the strippers with different concentrations to strip the surface of the quartz, and obtaining the quality of the stripped quartz each time and the impurity content in the quartz after each stripping;
s3, establishing a mathematical model based on the average content of impurities in the denuded quartz and the depth of the corresponding part from the surface of the quartz according to the parameters obtained in the steps S1 and S2;
and S4, calculating the content and depth of a certain impurity from the surface to the inside according to the mathematical model through a plurality of groups of denudation tests, and further obtaining the segregation distribution condition of the certain impurity in the quartz crystal lattice.
2. The analytical method according to claim 1, wherein in a plurality of tests with different amounts of denudation, the denudation agent used is increased in concentration as the quartz is eroded from the surface to the inside thereof.
3. The analytical method of claim 2, wherein the concentration of the denudating agent is linearly related to the mass of the denuded quartz.
4. The analytical method of claim 3, wherein when the stripping agent is hydrofluoric acid, a linear fit mathematical formula is:
y＝0.2069x+0.00097，R20.99961; wherein y is the ablated quartz mass, x is the ablation agent concentration, R2To fit the correlation coefficients.
5. The analytical method of claim 3, wherein when the stripping agent is sodium hydroxide, a linear fit mathematical formula is:
y＝0.53422x+0.00194，R20.98493; wherein y is the mass of the denuded quartz, x is the concentration of the denuded agent, R2To fit the correlation coefficients.
6. The analytical method according to any one of claims 1 to 5,
if the amount of the two strippers with different concentrations is maAnd mbAnd m isa<mbThe amount of denudation is mb-maThe average content of impurity elements in the mass of the dissolved quartz is Cab，
Cab＝[Cb(m0-mb)-Ca(m0-ma)]/[(m0-mb)-(m0-ma)]；
Wherein the impurity element content in the residual quartz sample after being leached twice by using the stripping agent is respectively CaAnd CbInitial mass of the quartz sample is m0。
7. The assay of claim 6, further comprising assaying for a content of CabDepth D of partial concentration of corresponding impurities in quartz crystal latticeab：
Figure FDA0002973654470000021
Where r is the initial radius of the ideal quartz sphere, Δ V is the mass of the ideal quartz sphere denuded and dissolved, Δ V ═ V0-Vr，V0Is the initial volume of ideal quartz sphere particles, VrPi is the circumference ratio, which is the volume remaining after the ideal quartz sphere is ablated.
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JPH03170393A (en) * 1989-11-28 1991-07-23 Mitsubishi Materials Corp Quartz crucible for pulling up silicon single crystal and method for detecting its impurity
CN102288561A (en) * 2011-07-11 2011-12-21 中国人民解放军国防科学技术大学 Method for detecting trace impurity in damaged layer of polished sub-surface of optical glass
CN103115927A (en) * 2013-02-04 2013-05-22 中国人民解放军国防科学技术大学 Nondestructive testing method for optical glass polishing sub-surface damages
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