CN115541440A - Method for determining purity of common assistant tetraethoxysilane for YAG (yttrium aluminum garnet) ceramic - Google Patents
Method for determining purity of common assistant tetraethoxysilane for YAG (yttrium aluminum garnet) ceramic Download PDFInfo
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- CN115541440A CN115541440A CN202211330164.1A CN202211330164A CN115541440A CN 115541440 A CN115541440 A CN 115541440A CN 202211330164 A CN202211330164 A CN 202211330164A CN 115541440 A CN115541440 A CN 115541440A
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Abstract
The application relates to a method for determining the purity of a common assistant tetraethoxysilane for YAG ceramics, which comprises the following steps: weighing a tetraethoxysilane sample, and determining the mass m of the tetraethoxysilane sample 1 (ii) a Acidizing the tetraethoxysilane sample, and removing acid to obtain an acidized sample; thermally decomposing the acidified sample to obtain a thermally decomposed sample, and determining the mass of the thermally decomposed sample as m 2 (ii) a The purity omega of the tetraethoxysilane sample is calculated to be m 2 /m 1 *100% 208.33/60.08. The purity of tetraethoxysilane measured by the method is relatively stable, the error of the numerical value measured by a plurality of samples is not more than 0.1%, only one type of required reagent medicine is needed, the method is simple, and the operation is simple.
Description
Technical Field
The application relates to a purity determination method, in particular to a purity determination method of tetraethoxysilane which is a common assistant for YAG ceramics.
Background
YAG ceramics, as a transparent ceramic with high optical performance, has strict requirements on the purity control of raw materials, causes defects such as scattering points, grain boundary pores, impurity phases and the like in an optical piece due to excessive impurity ions, and has color difference in appearance, so that the purity determination is carried out on a plurality of raw materials. Tetraethoxysilane is a brown bottled liquid raw material, the theoretical purity reaches more than 99.9 percent, but the substance is easy to hydrolyze, the products are ethanol and silicon dioxide, the purity is determined by a gas chromatography, the purity of a new unsealing product reaches 99.7 percent, the use requirement is not met, and a method for more accurately determining the purity is required to be found.
Disclosure of Invention
In order to solve the problems existing in the prior art, the embodiment of the application provides a method for determining the purity of tetraethoxysilane, a common assistant for YAG ceramics. The specific technical scheme is as follows:
in a first aspect, a method for determining the purity of tetraethoxysilane, a common assistant for YAG ceramics, is provided, which comprises the following steps: weighing a tetraethoxysilane sample, and determining the mass m of the tetraethoxysilane sample 1 (ii) a Acidizing the tetraethoxysilane sample, and removing acid to obtain an acidized sample; thermally decomposing the acidified sample to obtain a thermally decomposed sample, and determining the mass of the thermally decomposed sample as m 2 (ii) a The purity omega of the tetraethoxysilane sample is calculated to be m 2 /m 1 *100％*208.33/60.08。
In a first possible implementation manner of the first aspect, the tetraethoxysilane sample is weighed to a mass of 2-3g.
In a second possible implementation manner of the first aspect, the tetraethoxysilane sample is treated by being acidified by soaking the tetraethoxysilane sample with concentrated hydrochloric acid.
With reference to the second possible implementation manner of the first aspect, in a third possible implementation manner of the first aspect, when the tetraethoxysilane sample is acidified, the tetraethoxysilane sample is firstly added into the crucible, and then 5 to 10ml of concentrated hydrochloric acid is added into the crucible to be soaked for 10 to 15min.
With reference to the third possible implementation manner of the first aspect, in a fourth possible implementation manner of the first aspect, during acid removal, the crucible is placed in an electric furnace with a weighing function to be heated, and excessive concentrated hydrochloric acid is removed until the overall weight of the crucible is not changed.
With reference to the fourth possible implementation manner of the first aspect, in a fifth possible implementation manner of the first aspect, the heating temperature of the electric furnace is 130 ℃.
With reference to the third possible implementation manner of the first aspect, in a sixth possible implementation manner of the first aspect, during the thermal decomposition treatment of the acidified sample, the crucible is heated, the acidified sample is burned and decomposed, and then the acidified sample is naturally cooled to room temperature.
With reference to the sixth possible implementation manner of the first aspect, in a seventh possible implementation manner of the first aspect, the crucible is placed in a muffle furnace, and is heated to 975-1025 ℃ at a heating rate of 4 ℃/min, and the burning time is 4h.
With reference to the seventh possible implementation manner of the first aspect, in an eighth possible implementation manner of the first aspect, after the firing is completed, the crucible is naturally cooled to 100 ℃, and then the crucible is taken out and placed in a dryer to be cooled to room temperature.
With reference to the sixth possible implementation manner of the first aspect, in a ninth possible implementation manner of the first aspect, when the mass of the pyrolysis sample is measured, the net weight of the crucible is measured in advance to be m 3 And measuring the mass of the thermal decomposition sample and the crucible as m 4 Calculating the mass m of the thermally decomposed sample 2 Is m 4 -m 3 。
Compared with the prior art, the application has the advantages that:
according to the method for determining the purity of the tetraethoxysilane, which is a common YAG ceramic auxiliary, the determined tetraethoxysilane has relatively stable purity, the numerical error of multiple sample determination is not more than 0.1%, only one type of required reagent medicine is needed, the method is simple, and the operation is simple.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a flow chart illustrating the steps of a method for determining the purity of tetraethoxysilane, which is a common assistant for YAG ceramics, according to an embodiment of the present invention.
Detailed Description
To make the objects, technical solutions and advantages of the present application more clear, embodiments of the present application will be described in further detail below with reference to the accompanying drawings.
Please refer to fig. 1, which is a flowchart illustrating a method for determining purity of tetraethoxysilane, a common assistant for YAG ceramics, according to an embodiment of the present application. As shown in the figure, the purity determination method S of the common assistant tetraethoxysilane for YAG ceramics comprises the following steps S1 to S4. First, a sample is weighed in step S1. Weighing a tetraethoxysilane sample, and determining the mass m of the tetraethoxysilane sample 1 . Preferably, the sample of tetraethoxysilane is weighed to a mass of 2-3g.
The sample is then acidified in step S2. And soaking the tetraethoxysilane sample in concentrated hydrochloric acid to realize acidification treatment on the tetraethoxysilane sample, and removing acid to obtain an acidified sample. Specifically, a tetraethoxysilane sample is added into a crucible, 5-10ml of concentrated hydrochloric acid is added into the crucible to be soaked for 10-15min, then the crucible is placed into an electric furnace with a weighing function to be heated, the heating temperature of the electric furnace is 130 ℃, and excessive concentrated hydrochloric acid is removed through heating and evaporation until the whole weight of the crucible is not changed.
The acidified sample is then thermally decomposed in step S3. Thermally decomposing the acidified sample to obtain a thermally decomposed sample, and determining the mass of the thermally decomposed sample as m 2 . Specifically, the crucible after the acid removal is transferred into a muffle furnace, the crucible is heated to (1000 +/-25) DEG C at the heating rate of 4 ℃/min, a sample is burned and decomposed, the burning time is 4h, the crucible is naturally cooled to 100 ℃, then the crucible is taken out and placed in a dryer, the crucible is cooled to the room temperature, and the integral mass m of the crucible is measured at the moment 4 While previously determining the net weight of the crucible as m before step S2 3 Calculating the mass m of the thermally decomposed sample 2 Is m 4 -m 3 。
Finally, the purity of the tetraethoxysilane sample is calculated in step S4. TetraethoxysilaneThe relative molecular mass of the alkane was 208.33, and the relative molecular mass of silica was 60.08, so that the product of tetraethoxysilane containing silica regardless of the degree of hydrolysis and the product of thermal decomposition itself was also silica, so that the purity of tetraethoxysilane was estimated from the ratio of the relative molecular masses, and the purity ω of a sample of tetraethoxysilane was m 2 /m 1 *100％*208.33/60.08。
The purity of tetraethoxysilane measured by the method for measuring the purity of the common assistant tetraethoxysilane for YAG ceramics in the embodiment is relatively stable, the numerical error of multiple sample measurement is not more than 0.1%, only one kind of hydrochloric acid is needed for the type of required reagent medicine, the method is simple, and the operation is simple.
The beneficial effects of the purity determination method of tetraethoxysilane, which is a common assistant for YAG ceramics of the present application, will be described in specific example 1 and example 2.
Example 1
1. Acidifying: selecting a clean and dry alumina crucible, placing the alumina crucible on an analytical balance with constant mass m 3 =95.804g, weigh m 1 =2.558g of sample, soak sample with 10ml of concentrated hydrochloric acid for 15min;
2. acid removal: placing the alumina crucible with the sample on an electric furnace with a weighing function, heating to 130 ℃, and heating to remove excessive hydrochloric acid until the weight is not changed;
3. thermal decomposition: transferring the alumina crucible with complete acid removal into a muffle furnace, heating to (1000 +/-25) DEG C at a heating rate of 4 ℃/min, firing for 4h, naturally cooling to 100 ℃, taking out the alumina crucible, placing the alumina crucible into a dryer, cooling to room temperature, weighing m 4 ＝96.541g。
4. The tetraethoxysilane purity is calculated as mass fraction ω, the value is expressed in%, calculated according to the following formula: ω = (m) 4 -m 3 )/m 1 *100％*208.33/60.08＝99.91％。
Example 2
1. Acidifying: selecting a clean and dry alumina crucible, placing the alumina crucible on an analytical balance at a constant weight, and measuring the mass m 3 =118.072g, weigh m 1 Sample of =2.868g, the sample is soaked with 10ml of concentrated hydrochloric acid for 15min;
2. acid removal: placing the alumina crucible with the sample on an electric furnace with a weighing function, heating to 130 ℃, and heating to remove excessive hydrochloric acid until the weight is not changed;
3. thermal decomposition: transferring the alumina crucible with complete acid removal into a muffle furnace, heating to 1000 +/-25 ℃ at the heating rate of 4 ℃/min, burning for 4h, naturally cooling to 100 ℃, taking out the alumina crucible, placing the alumina crucible into a dryer, cooling to room temperature, weighing m 4 ＝118.899g。
4. The tetraethoxysilane purity is calculated as mass fraction ω, the value is expressed in%, and the calculation is made according to the following formula: ω = (m) 4 -m 3 )/m 1 *100％*208.33/60.08＝99.98％
In summary, the application provides a method for determining the purity of tetraethoxysilane which is a common assistant for YAG ceramics. The purity of tetraethoxysilane measured by the method is relatively stable, the error of the numerical value measured by a plurality of samples is not more than 0.1%, only one type of required reagent medicine is needed, the method is simple, and the operation is simple.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising a component of' 8230; \8230;" does not exclude the presence of another like element in a process, method, article, or apparatus that comprises the element.
While the present embodiments have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise embodiments described above, which are meant to be illustrative and not restrictive, and that various changes may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A method for measuring the purity of a common assistant tetraethoxysilane for YAG ceramics is characterized by comprising the following steps:
weighing a tetraethoxysilane sample, and determining the mass of the tetraethoxysilane sample as m 1 ；
Acidifying the tetraethoxysilane sample, and removing acid to obtain an acidified sample;
thermally decomposing the acidified sample to obtain a thermally decomposed sample, and determining the mass of the thermally decomposed sample as m 2 ；
The purity omega of the tetraethoxysilane sample is calculated to be m 2 /m 1 *100％*208.33/60.08。
2. The method for determining the purity of the YAG ceramic common additive tetraethoxysilane of the claim 1, wherein the tetraethoxysilane sample is weighed to have a mass of 2-3g.
3. The method for determining the purity of tetraethoxysilane of a YAG ceramic common additive according to claim 1, wherein the tetraethoxysilane sample is acidified by immersing the tetraethoxysilane sample in concentrated hydrochloric acid.
4. The method for determining the purity of the tetraethoxysilane of the YAG ceramic common additive according to claim 3, wherein the tetraethoxysilane sample is firstly added into a crucible when being acidified, and then 5-10ml of concentrated hydrochloric acid is added into the crucible to be soaked for 10-15min.
5. The method for determining the purity of tetraethoxysilane, a common assistant for YAG ceramics, as defined in claim 4, wherein in the step of removing acid, the crucible is heated in an electric furnace with a weighing function to remove the excessive concentrated hydrochloric acid until the weight of the crucible is not changed.
6. The method for measuring the purity of tetraethoxysilane which is a common assistant for YAG ceramics, as claimed in claim 5, wherein the heating temperature of said electric furnace is 130 ℃.
7. The method for determining the purity of tetraethoxysilane, a common assistant for YAG ceramics, as defined in claim 4, wherein said thermal decomposition treatment of said acidified sample comprises heating said crucible, burning to decompose said acidified sample, and naturally cooling to room temperature.
8. The method for determining the purity of the YAG ceramic common additive tetraethoxysilane of the claim 7, wherein the crucible is placed in a muffle furnace, and is heated to 975-1025 ℃ with a heating rate of 4 ℃/min, and the burning time is 4h.
9. The method for determining the purity of the frequently used assistant tetraethoxysilane for YAG ceramics of claim 8, wherein after the completion of firing, the crucible is naturally cooled to 100 ℃, and then the crucible is taken out and placed in a dryer, and cooled to room temperature.
10. The method for determining the purity of tetraethoxysilane, a common assistant for YAG ceramics, as defined in claim 7, wherein the mass of said thermally decomposed sample is determined by preliminarily determining the dry weight of said crucible as m 3 And then determining the mass of the whole of the thermal decomposition sample and the crucible as m 4 Calculating the mass m of the thermally decomposed sample 2 Is m 4 -m 3 。
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| CN202211330164.1A CN115541440A (en) | 2022-10-27 | 2022-10-27 | Method for determining purity of common assistant tetraethoxysilane for YAG (yttrium aluminum garnet) ceramic |
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| CN202211330164.1A CN115541440A (en) | 2022-10-27 | 2022-10-27 | Method for determining purity of common assistant tetraethoxysilane for YAG (yttrium aluminum garnet) ceramic |
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