CN109060773A - The easy measuring method of silicone content in a kind of Polycarbosilane - Google Patents
The easy measuring method of silicone content in a kind of Polycarbosilane Download PDFInfo
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Abstract
The present invention relates to a kind of easy measuring methods of silicone content in Polycarbosilane.Polycarbosilane sample is heat-treated by this method, it is allowed to form gelinite, it is reacted under certain condition with molten caustic soda again, reaction product is deployed into neutral solution to be measured, then test solution is introduced into inductive coupling plasma emission spectrograph, measures the intensity of spectral line of element silicon, be then compared with the intensity of spectral line of element silicon-mass fraction standard working curve, the content of element silicon in test solution is obtained, then is scaled the content of element silicon in Polycarbosilane.This method is simple and easy, and measurement accuracy is high.
Description
Technical field
The invention belongs to silicon carbide precursor detection technique fields, and in particular to the simplicity of silicone content in a kind of Polycarbosilane
Measuring method.
Background technique
Polycarbosilane (PCS) and the Polycarbosilane (PMCS) for containing heterogeneous element (aluminium, iron, zirconium, boron etc.) are silicon carbide fibres
The important precursor of dimension and ceramics.PCS is usually heavy through cracking under 400-500 DEG C, inert gas shielding by polydimethylsiloxane
Row's reaction obtains.PMCS usually is reacted to obtain by PCS with the compound containing heterogeneous element.Carbon, element silicon group in PCS and PMCS
The performance of final silicon carbide fibre or ceramics has a significant impact in pairs.Therefore, accurately carbon, element silicon contain in measurement PCS and PMCS
It measures particularly important.
Currently, the measurement of carbon element content generallys use organic element analyzer in Polycarbosilane, and the measurement of silicone content
Ununified method and standard, there are commonly the reagents that molybdenum blue spectrophotometry and the potassium fluosilicate precipitation method, this two methods need
More with solvent, step is more many and diverse, be easy to cause measurement error bigger than normal.Further, since Polycarbosilane belongs to organic matter, to it
(such as alkali fusion, 400 DEG C or more) is volatile when progress high temperature pre-treatment, and sample segment is caused to lose, and measurement result is inaccurate.
Therefore, a kind of method for exploring silicone content easily, in accurate measurement Polycarbosilane is particularly important.
Inductively coupled plasma emission spectrography (ICP) measures constituent content with easy to operate, specificity is strong, interference
The advantages that few, but its analysis for being mainly used for microelement in sample, and more (the usual quality of silicone content in Polycarbosilane sample
40% or more score) sample, whether this method feasible also to need further to explore.
Summary of the invention
For in above-mentioned Polycarbosilane the problem of silica test, the present invention provides silicon in a kind of Polycarbosilane and contains
The measuring method of amount has the advantages that simple and easy, measurement essence is high.
Technical solution provided by the invention are as follows: the easy measuring method of silicone content in a kind of Polycarbosilane,
(1) Polycarbosilane sample is heat-treated, is allowed to form gelinite；
(2) Polycarbosilane gelinite is reacted with the alkaloid compound of melting, obtains the mixture of silicate-containing；It will mixing
Object deionized water dissolving, obtains clear solution, is adjusted to solution with acidic materials and is in neutrality, and is then diluted to deionized water molten
Liquid quality is the 10 of Polycarbosilane quality5-106Times, obtain test solution；
(3) test solution is introduced into inductive coupling plasma emission spectrograph (ICP-OES), measures the spectrum of element silicon
Then line intensity is compared with element silicon standard working curve, obtain the content of element silicon in test solution, then is scaled poly-
The content of element silicon in carbon silane；
The measuring method of the element silicon standard working curve are as follows: the standard solution for weighing a certain amount of element silicon is put into not
In the volumetric flask of same volume, deionized water constant volume is added, obtains a series of solution with different silicon concentrations, wherein the concentration of silicon
For 1ppm-100ppm；The solution of the difference silicon concentration is introduced into inductive coupling plasma emission spectrograph and is measured, is obtained
To the intensity of spectral line-mass fraction standard working curve of element silicon.
The Polycarbosilane is to contain CH in molecular structure3SiHCH2The compound of structural unit is in solid-state at room temperature.Institute
Stating Polycarbosilane may also comprise the Polycarbosilane containing heterogeneous element, heterogeneous element include but is not limited to aluminium, iron, titanium, zirconium, cobalt,
One or more of nickel, boron, lanthanum, yttrium, niobium.
Preferably, the mass ratio of Polycarbosilane and alkaloid compound is 0.01-0.2, further preferably 0.02-01..
In the step (1), heat treatment temperature is lower than the softening temperature of Polycarbosilane sample.
In the step (1), heat-treating atmosphere can be one of air, oxygen, ozone or mixing.
Preferably, heat treatment temperature is 100-250 DEG C in the step (1)；Heat treatment time is 05.h-20h.
In the step (2), preferably, reaction temperature is 350-550 DEG C.
In the step (2), preferably, the reaction time is 10min-60min.
In the step (2), alkaloid compound is unlimited, including sodium hydroxide, sodium peroxide, sodium carbonate, sodium bicarbonate,
One or more of potassium hydroxide, potassium peroxide etc..
Compared with prior art, measuring method of the invention has the following beneficial effects:
(1) using the silicone content in ICP method measurement Polycarbosilane, operating procedure is few, measurement accuracy is high；
(2) Polycarbosilane sample is heat-treated, forms it into gelinite, can effectively avoid subsequent reacting with molten caustic soda
When sample volatilize the problem of, to greatly reduce evaluated error；
(3) reaction condition that Polycarbosilane gelinite is reacted with the alkaloid compound of melting is optimized, poly- carbon silicon is worked as in discovery
The mass ratio of alkane and alkaloid compound is 0.01-0.2, reaction temperature is 350-550 DEG C, when the reaction time is 10min-60min,
Molten alkali reaction is abundant, that is, so that the element silicon in Polycarbosilane is fully converted into silicate, while guaranteeing reaction product subsequent molten
It is generated in solution preocess without insoluble object, improves measurement accuracy.
(4) reaction product dissolved, neutralized and is diluted, can ensure that the validity of subsequent ICP method measurement and accurate
Property.
Specific embodiment
Below with reference to embodiment, present invention is further described in detail, it should be pointed out that embodiment described below purport
It is being convenient for the understanding of the present invention, and is not playing any restriction effect to it.
Embodiment 1:
The Determination of Silicon Content is as follows in Polycarbosilane PCS1:
(1) it is measured through melting point apparatus, the softening point of PCS1 is 195 DEG C；0.2gPCS1 sample is taken, is put into crucible.Then will
The sample is put into togerther 160 DEG C of baking ovens together with crucible, takes out after placing 5h.
(2) KOH2g is added in step (1) treated sample, is then placed in tube furnace and is warming up to 400 DEG C, heat preservation
1h takes out wait be cooled to room temperature.
Deionized water dissolving is added into crucible to solution state, hydrochloric acid is then added to neutrality.Solution is transferred to
In 200ml volumetric flask, deionized water constant volume is added.Then 100 μ l are taken out from volumetric flask, are diluted to 100ml with deionized water,
Obtain test solution.
(3) above-mentioned test solution is introduced into inductive coupling plasma emission spectrograph, the spectral line for measuring element silicon is strong
Then degree compares the intensity of spectral line-mass fraction standard curve of element silicon.
The measuring method of the intensity of spectral line-mass fraction standard curve of the element silicon is as follows:
The volumetric flask that volume is 100ml, 50ml, 25ml is chosen, the silicon standard solution of 100 μ l is added thereto respectively
(500ppm), respectively with deionized water dilution and constant volume, the mass fraction for obtaining element silicon is the molten of 0.5ppm, 1ppm, 2ppm
Liquid.This serial solution is introduced into inductive coupling plasma emission spectrograph to be measured, obtains the intensity of spectral line-of element silicon
The standard curve of mass fraction.
Comparison result are as follows: the content of element silicon is 0.48ppm in the test solution.Therefore in the PCS1 silicon mass fraction
For 0.48 × 1000 × 200 ÷, 1,000,000 0.2 × 100%=48% of ÷.
Comparative example 1:
In this comparative example, Polycarbosilane is identical with the Polycarbosilane in embodiment 1, and silicon contains in the Polycarbosilane
Quantity measuring method is as follows:
(1) 0.2gPCS1 sample is taken, is put into crucible.Then sample is put into togerther 160 DEG C of baking ovens together with crucible, placed
It is taken out after 5h.
(2) KOH2g is added in step (1) treated sample, is then placed in tube furnace and is warming up to 650 DEG C, heat preservation
1h.It is taken out wait be cooled to room temperature.
Deionized water dissolving is added into crucible, discovery has part insoluble matter, and hydrochloric acid is added to neutrality.It will be dissolved molten
Liquid is transferred in 200ml volumetric flask, and deionized water, constant volume is added.Then 100 μ l are taken out from volumetric flask, it is dilute with deionized water
It releases to 100ml, obtains test solution.
(3) above-mentioned test solution is introduced into inductive coupling plasma emission spectrograph, the spectral line for measuring element silicon is strong
Then degree compares the intensity of spectral line-mass fraction standard curve of element silicon.The intensity of spectral line-mass fraction of the element silicon
Standard curve is identical with the intensity of spectral line-mass fraction standard curve of element silicon in embodiment 1.
Comparison result are as follows: the content of element silicon is 0.38ppm in test solution.The mass fraction for being scaled silicon in PCS1 is
38%.
In the comparative example 1, since molten alkali reaction condition is not suitable for, cause gained silicone content in PCS1 obviously relatively low.
Comparative example 2:
In this comparative example, Polycarbosilane is identical with the Polycarbosilane in embodiment 1, and silicon contains in the Polycarbosilane
Quantity measuring method is as follows:
(1) the PCS1 sample in 0.2g comparative example 1 is taken, is put into crucible, KOH2g is added, is then placed in tube furnace and rises
Temperature keeps the temperature 1h to 400 DEG C, takes out wait be cooled to room temperature.
(2) deionized water dissolving is added into crucible to solution state, hydrochloric acid is then added to neutrality.Solution is transferred to
In 200ml volumetric flask, deionized water, constant volume is added.Then 100 μ l are taken out from volumetric flask, are diluted to deionized water
100ml obtains test solution.
(3) above-mentioned test solution is introduced into inductive coupling plasma emission spectrograph, the spectral line for measuring element silicon is strong
Then degree compares the intensity of spectral line-mass fraction standard curve of element silicon.The intensity of spectral line-mass fraction of the element silicon
Standard curve is identical with the intensity of spectral line-mass fraction standard curve of element silicon in embodiment 1.
Comparison result are as follows: the content of element silicon is 0.35ppm in test solution, and the mass fraction for being scaled silicon in PCS1 is
35%.
In the comparative example, due to not being heat-treated to PCS1 sample, sample segment is caused in the reaction of molten alkali
Volatilization causes gained silicone content in PCS1 obviously relatively low.
Embodiment 2:
The Determination of Silicon Content is as follows in polyaluminocarbosilane PACS1:
(1) it is measured through melting point apparatus, the softening point of PACS1 is 200 DEG C.0.2gPACS1 sample is taken, is put into crucible.Then
Sample is put into togerther 170 DEG C of baking ovens together with crucible, is taken out after placing 4h.
(2) the mixture 2.5g of sodium hydroxide and sodium peroxide is added in step (1) treated sample, is then placed in
It is warming up to 500 DEG C in tube furnace, keeps the temperature 1h.It is taken out wait be cooled to room temperature, deionized water dissolving is added into crucible to solution shape
Then nitric acid is added to neutrality in state.Solution is transferred in 200ml volumetric flask, deionized water, constant volume is added.Then from capacity
100 μ l are taken out in bottle, 100ml is diluted to deionized water, obtains test solution.
(3) above-mentioned test solution is introduced into inductive coupling plasma emission spectrograph, the spectral line for measuring element silicon is strong
Then degree compares the intensity of spectral line-mass fraction standard curve of element silicon.The intensity of spectral line-mass fraction of the element silicon
Standard curve is identical with the intensity of spectral line-mass fraction standard curve of element silicon in embodiment 1.
Comparison result are as follows: the content of element silicon is 0.45ppm in test solution, is scaled the mass fraction of silicon in PACS1
It is 45%.
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
For specific embodiments of the present invention, it is not intended to restrict the invention, all any modifications made in spirit of the invention,
Supplement or similar fashion substitution etc., should all be included in the protection scope of the present invention.
Claims (9)
1. the easy measuring method of silicone content in a kind of Polycarbosilane, it is characterized in that: including the following steps:
(1) Polycarbosilane sample is heat-treated, is allowed to form gelinite；
(2) Polycarbosilane gelinite is reacted with the alkaloid compound of melting, obtains the mixture of silicate-containing；Mixture is used
Deionized water dissolving obtains clear solution, is adjusted to solution with acidic materials and is in neutrality, and is then diluted to solution matter with deionized water
Amount is the 10 of Polycarbosilane quality5-106Times, obtain test solution；
(3) test solution is introduced into inductive coupling plasma emission spectrograph, measures the intensity of spectral line of element silicon, then with
Element silicon standard working curve is compared, and obtains the content of element silicon in test solution, then is scaled silicon member in Polycarbosilane
The content of element；
The measuring method of the element silicon standard working curve are as follows: weigh a certain amount of element silicon standard solution be put into it is not androgynous
In long-pending volumetric flask, deionized water constant volume is added, obtains a series of solution with different silicon concentrations, wherein the concentration of silicon is
1ppm-100ppm；The solution of the difference silicon concentration is introduced into inductive coupling plasma emission spectrograph and is measured, is obtained
The intensity of spectral line of element silicon-mass fraction standard working curve.
2. the easy measuring method of silicone content in Polycarbosilane as described in claim 1, it is characterized in that: the Polycarbosilane is
Contain CH in molecular structure3SiHCH2The compound of structural unit is in solid-state at room temperature.
3. the easy measuring method of silicone content in Polycarbosilane as claimed in claim 2, it is characterized in that: the Polycarbosilane packet
Containing heterogeneous element；The heterogeneous element includes one or more of aluminium, iron, titanium, zirconium, cobalt, nickel, boron, lanthanum, yttrium, niobium.
4. the easy measuring method of silicone content in Polycarbosilane as described in claim 1, it is characterized in that: the step (1)
In, heat treatment temperature is lower than the softening temperature of Polycarbosilane sample；
Preferably, the heat treatment temperature is 100-250 DEG C, heat treatment time 0.5h-20h.
5. the easy measuring method of silicone content in Polycarbosilane as described in claim 1, it is characterized in that: the step (1)
In, when heat treatment it is gases used including air, oxygen, ozone it is one or more.
6. the easy measuring method of silicone content in Polycarbosilane as described in claim 1, it is characterized in that: the step (2)
In, reaction temperature is 350-550 DEG C, reaction time 10min-60min.
7. the easy measuring method of silicone content in Polycarbosilane as described in claim 1, it is characterized in that: the step (2)
In, alkaloid compound includes one of sodium hydroxide, sodium peroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium peroxide
Or it is several.
8. the easy measuring method of silicone content, feature in the Polycarbosilane as described in any claim in claim 1 to 7
Be: the mass ratio of the Polycarbosilane and alkaloid compound is 0.01-0.2.
9. the easy measuring method of silicone content, feature in the Polycarbosilane as described in any claim in claim 1 to 7
Be: the acidic materials are one of hydrochloric acid, nitric acid, sulfuric acid or several.
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