CN106610374A - Analysis detection method for anions adsorbed on SiC particle surface - Google Patents
Analysis detection method for anions adsorbed on SiC particle surface Download PDFInfo
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- CN106610374A CN106610374A CN201510700074.0A CN201510700074A CN106610374A CN 106610374 A CN106610374 A CN 106610374A CN 201510700074 A CN201510700074 A CN 201510700074A CN 106610374 A CN106610374 A CN 106610374A
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Abstract
The invention relates to an analysis detection method for the anions adsorbed on the SiC particle surface. According to the present invention, SiC particles are completely separated from an electrolyte containing anions through a series of treatment processes, and the infrared characteristic peaks of the adsorbed anions are rapidly detected by using a Fourier transform infrared spectrometer so as to determine the adsorbed anions; and the analysis detection method has characteristics of simple operation process and rapid detection, and has wide application prospects in the fields of composite electroplating and the like.
Description
Technical field
The invention belongs to field of surface technology, the specially analyzing detecting method of SiC particulate surface adsorption anion.
Background technology
SiC particulate and metal can be formed composite deposite in surface of the work by electro-deposition techniques, so as to significantly improve the wear and corrosion behavior of workpiece.Surface of SiC can adsorb specific ion, so as to change plating mechanism, and occur to be co-deposited with metal, obtain the composite deposite of excellent performance SiC and metal.It has been found that surface of SiC absorption meeting cation, such as Cs+Ion (Rudnik
Ewa, Burzyńska Lidia, Jędruch Jacek, et al. Codeposition
of SiC particles with electrolytic cobalt in the
presence of Cs+Ions. 255 (2009) 7164-7171 of Applied Surface Science.), so as to accelerate the co-deposition of SiC and metal.Change in document using atomic absorption spectrography (AAS), ultraviolet-uisible spectrophotometer method to the anions in solution after absorption is analyzed, and analyzes indirectly the cation (Rudnik of SiC absorption
Ewa, Burzyńska Lidia, Gut Marcin. The effect of Cs+ ions on codeposition of SiC particles
with nickel. Materials Chemistry and Physics. 126 (2011) 573-579).Surface of SiC can also adsorpting anion, but, how to detect the also no available direct method of anion of absorption.
For this point, the art of this patent provides a kind of analyzing detecting method suitable for surface of SiC adsorpting anion, agents useful for same is with low cost, operating process is simple, and the characteristic infrared peak of the anion of absorption is detected by Fourier spectrometer, it is possible to the anion of quick detection surface of SiC absorption, this method has widened the research range of adion, has broad application prospects.
The content of the invention
The purpose of the present invention aims to provide a kind of analyzing detecting method of SiC particulate surface adsorption anion.First the SiC particulate of adion is centrifuged, is allowed to be completely separated with electrolyte, and is avoided electrolyte from remaining in SiC powder granule;Recycle the characteristic infrared spectrum peak of the anion of infrared spectrum technology quick detection SiC particulate surface adsorption.
The technical scheme for realizing the object of the invention is:
First, electrolyte of the finite concentration containing the anion for possessing some special knowledge is prepared, and adds SiC particulate, magnetic agitation is for a period of time;Secondly, take a small amount of mixed liquor and be centrifuged, retain bottom SiC particulate, add suitable organic solvent to be centrifuged off remaining in the electrolyte in SiC powder granule;Again, the SiC after drying and spectroscopic pure potassium bromide mixed pressuring plate in specific proportions, the infrared light spectral peak of SiC particulate surface adsorption anion is detected using Fourier infrared spectrograph;The standard IR spectrum spectrogram of the last and salt containing anion is compared, and is confirmed whether to have adsorbed the anion.
Comprise the following steps that:
The process of a.SiC granules
After SiC particulate soaks enough time in saline solution, stop stirring, separated using centrifuge.CHCl is added in SiC particulate powder again3Solution, ultrasonic disperse 10min, using density variation by SiC particulate and the electrolyte centrifugation that is trapped in SiC particulate powder.Finally, in order to remove a small amount of CHCl of residual3Liquid, toasts SiC particulate in drying baker, obtains the SiC samples of adsorpting anion, standby;
B. FTIR spectrum measuring technology
By the SiC samples and KBr of adsorpting anion(Spectroscopic pure)According to 1:300 ratio mixing, and grind in agate mortar, it is pressed into disk;With pure KBr pieces as background, the infrared light spectral peak of the anion of detection SiC particulate surface adsorption is quickly analyzed using Fourier spectrometer.
Description of the drawings
Fig. 1 is SiC particulate absorption Na2SO4Infrared spectrum in electrolyte after sulfate anion;
Fig. 2 is SiC particulate absorption Na3Infrared spectrum in Cit electrolyte after citrate anion.
Specific embodiment
Embodiment 1
Weigh Na2SO41.42 g of granule, is put in 250m L beakers, adds water to 100ml, be configured to the saline solution of 0.1M, is put into the dissolving of stirrer magnetic agitation, obtains containing SO4 2-The electrolyte of anion.Micrometer silicon carbide silicon grain 3g is weighed, about 5 microns of granular size is poured in above-mentioned electrolyte, sealed using preservative film, and magnetic agitation 70h draws a certain amount of mixed liquor, and centrifugation goes out SiC particulate;10mlCHCl is added in the SiC particulate separated again3, ultrasonic disperse 10min, recentrifuge are separated;Finally SiC particulate is put in 80 DEG C of air dry oven and is dried 30min, make CHCl3Volatilize completely, obtain adsorbing the SiC particulate sample of sulfate ion.
The SiC particulate of above-mentioned acquisition and spectroscopic pure KBr according to 1:300 ratios are ground, and suppress flakiness, using spectroscopic pure KBr as background peaks, detect anion SO of SiC particulate surface adsorption by Fourier infrared spectrograph4 2-Spectrum peak, as shown in Figure 1.From the figure, it can be seen that being 1112 and 620cm in wave number-1The peak at place is SO4 2-The characteristic absorption peak of anion, indicates SiC particulate surface and can adsorb SO4 2-Anion.
Embodiment 2
In order to investigate the impact of cation, it is (NH to change electrolyte on the basis of embodiment 14)2SO4And NiSO4, also observed SO4 2-The characteristic absorption peak of anion, shows in SiC particulate surface adsorption SO4 2-Anion is not affected by cation.
Embodiment 3
It is Na to change electrolyte on the basis of embodiment 13Cit, observes SiC particulate to Na by Fourier infrared spectrograph3The absorption situation of Cit(See Fig. 2), as can be seen from the figure SiC particulate is to Cit3-Ion there occurs absorption, wave number 1586 and 1391cm-1The peak at place is due to COO-Symmetrical stretching vibration and asymmetrical stretching vibration formed.
Claims (2)
1. a kind of analyzing detecting method of SiC particulate surface adsorption anion, it is characterised in that:First, by Organic substance liquid the SiC particulate of adsorpting anion and electrolyte centrifugation;Infrared spectrometer is recycled quickly to measure the infrared spectrum of ADSORPTION STATE SiC particulate;Finally, compare with the standard IR spectrum of the salt containing anion, determine whether SiC particulate has adsorbed anion.
2. Organic substance liquid according to claim 1, it is characterised in that:From Organic substance be carbon trichloride(CHCl3).
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2002083980A1 (en) * | 2001-04-12 | 2002-10-24 | National University Of Ireland, Cork | Electroless plating |
CN101161800A (en) * | 2007-09-18 | 2008-04-16 | 朱辰 | Aqueous suspension grinding fluid |
CN101306591A (en) * | 2008-06-30 | 2008-11-19 | 河北理工大学 | Copper surface functional material and preparation method |
-
2015
- 2015-10-26 CN CN201510700074.0A patent/CN106610374A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2002083980A1 (en) * | 2001-04-12 | 2002-10-24 | National University Of Ireland, Cork | Electroless plating |
CN101161800A (en) * | 2007-09-18 | 2008-04-16 | 朱辰 | Aqueous suspension grinding fluid |
CN101306591A (en) * | 2008-06-30 | 2008-11-19 | 河北理工大学 | Copper surface functional material and preparation method |
Non-Patent Citations (3)
Title |
---|
WEI WANG等: "Molten salt synthesis of mullite whiskers on the surface of SiC ceramics", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
王平: "电沉积Ni-SiC纳米复合镀层的制备与研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
薛若茵等: "电沉积制备羟基磷灰石-碳化硅复合涂层", 《电镀与精饰》 * |
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Application publication date: 20170503 |