CN108458948B - Quantitative analysis SiC-SiO2Method for mixing components - Google Patents
Quantitative analysis SiC-SiO2Method for mixing components Download PDFInfo
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Abstract
The invention provides a method for quantitatively analyzing SiC-SiO2A method of mixing components, the method comprising: step S1: mass m is taken1Of SiC-SiO2Mixing powder samples, mixing the SiC-SiO2Mixing a powder sample and NaOH to serve as a reaction system, and weighing the mixture before reactionTotal mass m of the reaction system2(ii) a Step S2: carrying out high-temperature melting reaction on the reaction system in an oxygen-free sealed environment; wherein the high-temperature melting reaction conditions are as follows: uniformly heating from 0 ℃ to 320-350 ℃ within 90min, and then carrying out heat preservation reaction for 20 min; step S3: weighing the total mass m of the reacted reaction system3Obtaining SiO by a calculation formula2In percentage by mass. The invention provides a method for quantitatively analyzing SiC-SiO2The method for mixing the components has the advantages of simple analysis process, simple and safe operation, few influencing factors, high accuracy of quantitative analysis results and good repeatability.
Description
Technical Field
The invention relates to a method for measuring chemical substances, in particular to a method for quantitatively analyzing SiC-SiO2A method of mixing the components.
Background
The novel SiC quantum dot developed in recent years is an inert ceramic material, has the advantages of low chemical activity, high temperature resistance, good mechanical property, no toxicity and the like compared with other quantum dots, and is an ideal material applied to medical treatment, biological fluorescent probes, photoelectric devices and the like. Therefore, the preparation of the silicon carbide quantum dots with uniform sizes has important significance. Generally, the silicon carbide quantum dots are prepared by taking silicon carbide nanoparticles as raw materials, and SiO is easily formed on the surfaces of the silicon carbide nanoparticles when the silicon carbide nanoparticles are stored in the air2Thin films, however, it is difficult to accurately calculate SiC-SiO2The corrosion process for preparing the silicon carbide quantum dots cannot be quantified to properly proportion the raw materials, so that the size of the prepared silicon carbide quantum dots is difficult to control and the distribution is not uniform.
Conventional methods for analyzing the composition of silicon carbide involve high temperature and highly corrosive acidic solutions, such as hydrofluoric acid, concentrated sulfuric acid, and the like. The chemicals used for analysis relate to chemical reagents with extremely strong corrosivity such as hydrofluoric acid and the like, and bring great potential safety hazard to experimenters in the operation processMeanwhile, the traditional analysis and detection method has a complicated analysis process, needs multiple steps of sample transfer, washing, filtering, centrifuging and the like, brings great errors to the experimental result, and is difficult to obtain accurate SiC-SiO2And (4) component ratio results.
Disclosure of Invention
The invention aims to solve the problem of the prior SiC-SiO2The problems of complicated analysis process, low accuracy and poor reproducibility of the analysis and determination method are solved, and the quantitative analysis of SiC-SiO is provided2A method of mixing the components.
The invention provides a method for quantitatively analyzing SiC-SiO2A method for mixing components, the analysis process of which comprises the following steps:
step S1: mass m is taken1Of SiC-SiO2Mixing powder samples, mixing the SiC-SiO2Mixing a powder sample and NaOH to obtain a reaction system, and weighing the total mass m of the reaction system before reaction2；
Step S2: carrying out high-temperature melting reaction on the reaction system in an oxygen-free sealed environment; wherein the high-temperature melting reaction conditions are as follows: uniformly heating from 0 ℃ to 320-350 ℃ within 90min, and then carrying out heat preservation reaction for 20 min;
step S3: weighing the total mass m of the reaction system after the reaction in the step S23And obtaining SiO according to the following calculation formula2The mass percentage of:
the quantitative analysis method of the invention is that NaOH reacts with silicon dioxide under the condition of high-temperature melting to generate sodium silicate and water, the water is evaporated and removed under the condition of high temperature, the mass of the generated water can be calculated according to the mass difference before and after the reaction according to the mass conservation law of the chemical reaction, the amount of the silicon dioxide component is obtained according to the chemical reaction equation, and further SiC-SiO can be calculated2The component ratio. The whole analysis process does not involve liquid strong acid, avoids potential safety hazard, is safe to operate, and does not involve liquid strong acidThe method needs sample transfer and processing steps of dissolution, washing, centrifugation, filtration and the like, has simple analysis process, few influencing factors, high accuracy of quantitative analysis result and good reproducibility and repeatability.
Wherein, the reaction chemical equation is as follows: 2NaOH + SiO2＝Na2SiO3+H2O
During the reaction, an excessive amount of NaOH is added to make SiO in the mixed components2And (4) completely reacting. Slowly raising the temperature for 90min, and then preserving the heat for 20min to ensure that the reaction is completely carried out, wherein SiO is2And if the reaction time is too short, the reaction is incomplete, and if the reaction time is too long, the molten NaOH can generate corrosivity on a reaction system, the measurement result is influenced, and the repeatability is poor. To ensure that NaOH reaches a better molten state in the reaction, the optimal temperature of the reaction is 320-350 ℃, and if the temperature is too low, the NaOH is difficult to completely melt, thereby affecting SiO2The reaction time is difficult to control, the reproducibility and repeatability are difficult to guarantee, if the temperature is too high, NaOH will bubble and lose, the final determination result is affected, and the accuracy is low.
Preferably, the SiC-SiO2The mass ratio of the mixed powder sample to the NaOH is 1: 10-3: 4. During the reaction, an excessive amount of NaOH is added to make SiO in the mixed components2However, the amount of NaOH is not so high that the NaOH is difficult to melt and thus the reaction is inhibited, and the reaction time is too long.
Preferably, in the step S1, SiC — SiO in the reaction system is added before the reaction2The mixed powder sample is fully ground until the particle size is 100-1000 meshes, and is fully stirred uniformly at the same time, so that reactants are uniformly mixed. The finer the granularity of reactants in the reaction system, the more uniform the mixing, the more sufficient the reaction contact, and the smooth the reaction is ensured.
Preferably, in the step S1, the NaOH is dried at 80 to 100 ℃ to remove moisture in the NaOH before the reaction. The analytical method mainly adopts a difference weight method to calculate the moisture content produced by the reaction, thereby obtaining SiO by chemical formula calculation2The NaOH is easy to absorb moisture in the airTherefore, before weighing, the sodium hydroxide needs to be dried, the crystal water in the sodium hydroxide is completely removed, and the sodium hydroxide is stored in a sealed manner, so that the measurement result is prevented from being influenced.
Preferably, the reaction system is subjected to oxygen-free sealing reaction in a nickel crucible to ensure that the reaction system is not oxidized in the air and is not corroded under a high-temperature melting reaction system, and meanwhile, the reaction system is not permeated by reactants and products at high temperature, so that the accuracy and the repeatability of an experiment are ensured.
Preferably, in the step S2, argon gas with a constant flow rate is introduced into the reaction system during the reaction, and the flow rate is 0.1 to 10L/min. Generally, a weighed sample to be detected and NaOH are put into a nickel crucible to be uniformly ground, then the sample to be detected and the NaOH are put into a tubular heating furnace to be subjected to high-temperature melting reaction, argon with the flow of 0.1-10L/min is introduced into the tubular heating furnace to obtain an inert environment, silicon carbide is prevented from being further oxidized, generated water vapor can be blown away to a pipe port to be condensed, the accuracy of experimental data is ensured, meanwhile, the flow rate of the argon gas cannot be too small or too large, the flow rate is too small to bring the generated water vapor, the flow rate is too large to cause strong turbulence, dust can be brought away by too strong entrainment force, data are inaccurate, meanwhile, the gas is difficult to be discharged in time due to the small exhaust pipe diameter, and safety accidents are caused by too large air pressure in the tubular heating furnace.
Preferably, in the step S3, after the reaction system is cooled to room temperature after the reaction is finished, the total mass m of the reaction system is weighed3。
Preferably, the instrument is dried during the whole analysis process, and the reaction system is in an oxygen-free sealed environment. All the instruments are dried, so that the interference of external moisture can be fully avoided; the reaction can be carried out in an oxygen-free sealed environment, and SiC-SiO can be prevented2The SiC in the mixed components is continuously oxidized into SiO at high temperature2Affecting the assay result.
The invention has the beneficial effects that: the invention provides a method for quantitatively analyzing SiC-SiO2The components are mixed by melting sodium hydroxide at high temperature and reacting with silicaThe water is evaporated and removed, the quality of the water generated by the reaction is calculated by a difference weight method, so that the content of the silicon dioxide is calculated, the whole process does not involve liquid strong acid, the potential safety hazard is avoided, the operation is safe, meanwhile, the sample does not need to be transferred, and the processing steps of dissolving, washing, centrifuging, filtering and the like are not needed, the analysis process is simple, the influence factors are few, the accuracy of the quantitative analysis result is high, and the reproducibility and the repeatability are good.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. 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. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
Example 1
1. Materials and instruments
Materials: deionized water (provided in the laboratory); sodium hydroxide (analytical grade; chemical reagents of national drug group, Ltd.); SiO 22Powder (commercially available); oxidized silicon carbide powder (sample to be analyzed: 1# silicon carbide powder, 2# silicon carbide powder, 3# silicon carbide powder, 4# silicon carbide powder)
The instrument comprises the following steps: crucibles (nickel crucible 30 ml; super Jie apparatus); medicine spoon (middle size; super jie instrument); tube furnaces (SK-1200 ℃ open type vacuum/atmosphere tube furnace; Tianjin medium-ring electric furnace Co., Ltd.); an electronic balance (FAl 604; Shanghai balance instrumentation plant); a drying oven (GZX-9030MBE electric heating air drying oven; Shanghai Bo Bing Kogyo Co., Ltd.).
2. Sample pretreatment
2.1 crucible weighing: taking 10 crucibles, numbering 1-10, cleaning the crucibles and the medicine spoon by deionized water, drying the crucibles and the medicine spoon in a drying oven at 80 ℃ for 30min, taking out the crucibles and the medicine spoon, weighing the total mass of the crucibles and the crucible covers, wherein the crucibles with the numbering 1-5 respectively have the following mass: 38.1850g, 40.4085g, 39.1098g, 42.1252g, 40.8590g, 40.8022g, 37.6272g, 39.1960g, 40.0172g and 40.5784 g.
2.2 sodium hydroxide pretreatment: drying sodium hydroxide at 80-100 ℃, and then placing the dried sodium hydroxide in a sealed reagent bottle for storage for later use. When sodium hydroxide is used, the weighed sodium hydroxide is immediately placed in a crucible with a cover and sealed.
2.3 grouping and weighing of samples
And in the weighing process, the electronic balances of the same model are used for weighing, and the weighed sample is immediately placed into a crucible for sealing.
Control group:
number 1: weighing 1.0010gSiO2Powder, 2.0021g sodium hydroxide, was added to crucible No. 1 with a spatula and the total mass m recorded241.1881g, fully grinding the mixture until the particle size is 100-500 meshes, uniformly stirring the mixture, and sealing the mixture by using a cover;
number 6: weighing 1.0128g of SiO2Powder, 3.0045g sodium hydroxide, was added to crucible No. 6 with a spatula and the total mass m recorded244.8105g, fully grinding to the particle size of 100-500 meshes, uniformly stirring and sealing by a cover.
Experimental group 1:
number 2: weighing m11.0103g of 1# silicon carbide powder and 2.0388g of sodium hydroxide, adding the mixture into a No. 2 crucible by using a medicine spoon, recording the total mass as 43.4576g, fully grinding the mixture until the particle size is 100-500 meshes, and sealing the mixture by using a cover after the mixture is uniformly stirred;
number 3: 1.0096g of 1# silicon carbide powder and 3.0432g of sodium hydroxide are weighed, added into a No. 3 crucible by using a medicine spoon, and the total mass m is recorded243.1626g, fully grinding the mixture until the particle size is 100-500 meshes, and sealing the mixture with a cover after uniformly stirring.
Experimental group 2:
number 4: weighing m11.0022g of No. 2 silicon carbide powder and 2.0456g of sodium hydroxide are added into a No. 4 crucible by a medicine spoon, the total mass is recorded as 45.1730g, the mixture is fully ground to the particle size of 100-500 meshes, and the mixture is sealed by a cover after being stirred uniformly;
number 5: 1.0120g of No. 2 silicon carbide powder and 3.0151g of sodium hydroxide are weighed and added into a No. 5 crucible by using a medicine spoon, and the total mass m is recorded2Is 44.8861gFully grinding the mixture to the granularity of 100-500 meshes, uniformly stirring the mixture and sealing the mixture by using a cover.
Experimental group 3:
number 7: weighing m11.0162g of No. 3 silicon carbide powder and 2.0128g of sodium hydroxide are added into a No. 7 crucible by a medicine spoon, the total mass is recorded as 40.6562g, the mixture is fully ground to the particle size of 100-500 meshes, and the mixture is sealed by a cover after being stirred uniformly;
number 8: weighing m11.0072g of 3# silicon carbide powder and 2.9909g of sodium hydroxide are added into a No. 7 crucible by a medicine spoon, the total mass is recorded as 43.1941g, the mixture is fully ground to the particle size of 100-500 meshes, and the mixture is sealed by a cover after being stirred uniformly.
Experimental group 4:
number 9: weighing m11.0093g of No. 4 silicon carbide powder and 3.0661g of sodium hydroxide, adding the mixture into a No. 7 crucible by using a medicine spoon, recording the total mass as 44.0926g, fully grinding the mixture to the particle size of 100-500 meshes, and sealing the mixture by using a cover after uniformly stirring the mixture;
number 10: weighing m11.0044g of No. 4 silicon carbide powder and 2.0058g of sodium hydroxide are added into a No. 7 crucible by a medicine spoon, the total mass is recorded as 43.5886g, the mixture is fully ground to the particle size of 100-500 meshes, and the mixture is sealed by a cover after being stirred uniformly.
3. Procedure of experiment
The crucible of serial number 1 ~ 5 after will adding the sample is put into the tube furnace respectively, encapsulates the tube furnace, and the evacuation is gone into argon gas again, opens each way valve and makes argon gas keep steady flow, and the velocity of flow is 0.1L/min, sets up the procedure at last and heaies up: uniformly heating from 0 ℃ to 350 ℃ within 90min, then preserving heat at 350 ℃ for 20min, finally naturally cooling in argon atmosphere, taking out the crucible when the temperature is cooled to room temperature, and weighing the total mass m of the numbered 1-10 crucibles340.8856g, 43.3188g, 43.0219g, 45.0119g, 44.7253g, 44.5055g, 40.4740g, 43.0152g, 43.9829g and 43.4782g respectively.
4. Experimental calculations and results
4.1 calculation formula: SiO in oxidized silicon carbide powder sample to be measured2The mass percentage of:
wherein m is1M is the mass of the oxidized silicon carbide powder of the sample to be measured2Is the total mass of the crucible and the sample, m3The total mass of the crucible and the sample after the reaction.
4.2 calculation results:
SiO consumed by reaction in crucible No. 12The quality is as follows:
SiO for reacting No. 1 silicon carbide powder in No. 2 crucible2The mass percentage is as follows:
SiO for reacting No. 1 silicon carbide powder in No. 3 crucible2The mass percentage is as follows:
SiO for reacting 2# silicon carbide powder in No. 4 crucible2The mass percentage is as follows:
SiO for reacting 2# silicon carbide powder in No. 5 crucible2The mass percentage is as follows:
SiO consumed by reaction in crucible No. 62The quality is as follows:
SiO for reacting No. 3 silicon carbide powder in No. 7 crucible2The mass percentage is as follows:
SiO for reacting No. 3 silicon carbide powder in No. 8 crucible2The mass percentage is as follows:
SiO for reacting No. 4 silicon carbide powder in No. 9 crucible2The mass percentage is as follows:
SiO for reacting No. 4 silicon carbide powder in No. 10 crucible2The mass percentage is as follows:
from the calculation results, it was found that the contents of silica measured in the crucibles of numbers 1 and 6 of the control group were 1.0083g and 1.0167g, respectively, which were almost equal to the actual amounts of 1.0010g and 1.0128g, and that the reactants in the crucibles of numbers 1 and 6 were completely dissolved, i.e., the silica was completely reacted, by adding an excessive amount of deionized water to the crucibles of numbers 1 and 6, respectively, and it was confirmed that the analysis method of the present invention was possible. The raw materials of the samples in each group of crucibles in the experimental groups 1-4 are the same, and the mass percentages of the silicon dioxide obtained by the final measurement and calculation are basically the same (the phase difference is only within 1 percent), which shows that the SiC-SiO obtained by the analysis method of the invention2The measurement accuracy of the chemical component ratio is high, and the repeatability and the reproducibility are good.
Example 2
1. Materials and instruments: same as example 1
2. Sample pretreatment: taking the crucibles with the numbers of 1-5.
2.1 crucible weighing: the same as in example 1.
2.2 sodium hydroxide pretreatment: the same as in example 1.
2.3 grouping and weighing of samples
And in the weighing process, the electronic balances of the same model are used for weighing, and the weighed sample is immediately placed into a crucible for sealing.
Control group:
number 1: weighing 1.0015gSiO2Powder, 2.0032g sodium hydroxide, was added to crucible No. 11 with a spatula and the total mass m recorded241.1897g, fully grinding the mixture until the particle size is 500-1000 meshes, uniformly stirring the mixture, and sealing the mixture by using a cover;
experimental group 1:
number 2: weighing m11.0114g of 1# silicon carbide powder and 2.0378g of sodium hydroxide, adding the mixture into a No. 2 crucible by using a medicine spoon, recording the total mass as 43.4577g, fully grinding the mixture until the particle size is 500-1000 meshes, and sealing the mixture by using a cover after the mixture is uniformly stirred;
number 3: 1.0085g of 1# silicon carbide powder and 3.0446g of sodium hydroxide are weighed, added into a No. 3 crucible by using a medicine spoon, and the total mass m is recorded243.1630g, fully grinding the mixture until the particle size is 500-1000 meshes, and sealing the mixture with a cover after uniformly stirring.
Experimental group 2:
number 4: weighing m11.0045g of No. 2 silicon carbide powder and 2.0432g of sodium hydroxide are added into a No. 4 crucible by a medicine spoon, the total mass is recorded as 45.1729g, the mixture is fully ground to the particle size of 500-1000 meshes, and the mixture is sealed by a cover after being stirred uniformly;
number 5: 1.0131g of No. 2 silicon carbide powder and 3.0168g of sodium hydroxide are weighed and added into a No. 5 crucible by using a medicine spoon, and the total mass m is recorded244.8889g, fully grinding to the particle size of 500-1000 meshes, uniformly stirring and sealing by a cover.
3. Procedure of experiment
The crucible of serial number 1 ~ 5 after will adding the sample is put into the tube furnace respectively, encapsulates the tube furnace, and the evacuation is gone into argon gas again, opens each way valve and makes argon gas keep steady flow, and the velocity of flow is 10L/min, sets up the procedure at last and heaies up: uniformly heating from 0 ℃ to 320 ℃ within 90min, then preserving heat at 320 ℃ for 20min, finally naturally cooling in argon atmosphere, taking out the crucible when the temperature is cooled to room temperature, and weighing the total mass of the numbered 1-5 cruciblesQuantity m340.8890g, 43.3212g, 43.0259g, 45.0159g and 44.7291g respectively.
4. Experimental calculations and results
4.1 calculation formula: SiO in oxidized silicon carbide powder sample to be measured2The mass percentage of:
where m1 is the mass of the commercial silicon carbide powder in step S1, m2 is the total mass of the crucible and the sample in step S1, m3 is the total mass of the crucible and the sample after the reaction in step S3, and 60 and 18 are the relative molecular masses of silica and water, respectively:
4.2 calculation results:
SiO consumed by reaction in crucible No. 12The quality is as follows:
SiO for reacting No. 1 silicon carbide powder in No. 2 crucible2The mass percentage is as follows:
SiO for reacting No. 1 silicon carbide powder in No. 3 crucible2The mass percentage is as follows:
SiO for reacting 2# silicon carbide powder in No. 4 crucible2The mass percentage is as follows:
SiO for reacting 2# silicon carbide powder in No. 5 crucible2The mass percentage is as follows:
from the calculation results, it can be seen that the measured silica content in the crucible No. 1 of the control group was 1.0023g, which was almost equal to the actual amount of 1.0015g, and excessive deionized water was added to the crucible No. 1, and the reactants in the crucible were completely dissolved, i.e., the silica was completely reacted, thus proving that the analysis method of the present invention is feasible. The samples in each group of crucibles in the experimental groups 1 and 2 are the same in raw material, and the mass percentages of the silicon dioxide obtained by final measurement and calculation are basically the same (the difference is only within 1 percent), which shows that the SiC-SiO obtained by the analysis method of the invention2The measurement accuracy of the chemical component ratio is high, and the repeatability is good. Meanwhile, the results obtained from the crucibles with the same number in the example 1 and the example 2 are basically the same, which shows that the temperature is between 320 ℃ and 350 ℃, the substances in the reaction system are basically not decomposed, and the accuracy of the measured result is high.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. Quantitative analysis SiC-SiO2A method of mixing components, comprising the steps of:
step S1: mass m is taken1Of SiC-SiO2Mixing powder samples, mixing the SiC-SiO2Mixing a powder sample and NaOH to obtain a reaction system, and weighing the total mass m of the reaction system before reaction2；
Step S2: carrying out high-temperature melting reaction on the reaction system in an oxygen-free sealed environment; wherein the high-temperature melting reaction conditions are as follows: uniformly heating from 0 ℃ to 350 ℃ within 90min, and then carrying out heat preservation reaction for 20 min; introducing argon gas with a constant flow rate of 0.1-10L/min into the reaction system in the reaction process;
step S3: weighing the total mass m of the reaction system after the reaction in the step S23And obtaining SiO according to the following calculation formula2The mass percentage of:
in the step S1, the SiC-SiO2The mass ratio of the mixed powder sample to the NaOH is 1: 10-3: 4; and drying the NaOH at 80-100 ℃ before reaction to remove water in the NaOH.
2. The quantitative analysis SiC-SiO of claim 12A method of mixing components, characterized by: in the step S1, before the reaction, SiC-SiO in the reaction system is added2And fully grinding the mixed powder sample until the particle size is 100-1000 meshes.
3. The quantitative analysis SiC-SiO of claim 12A method of mixing components, characterized by: and putting the reaction system into a nickel crucible and placing the nickel crucible in an oxygen-free sealed environment for reaction.
4. The quantitative analysis SiC-SiO of claim 12A method of mixing components, characterized by: in the step S3, after the reaction is finished, the total mass m of the reaction system is weighed after the reaction system is cooled to room temperature3。
5. The quantitative analysis SiC-SiO of claim 12A method of mixing components, characterized by: in the whole analysis process, all instruments are subjected to drying treatment, and the reaction system is in an oxygen-free sealed environment.
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