CN111257267A - Method for measuring oxygen content in silicon carbide ceramic material - Google Patents
Method for measuring oxygen content in silicon carbide ceramic material Download PDFInfo
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- 239000001301 oxygen Substances 0.000 title claims abstract description 155
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 155
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 154
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 98
- 238000000034 method Methods 0.000 title claims abstract description 67
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 88
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 81
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 56
- 239000010439 graphite Substances 0.000 claims abstract description 56
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 39
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000007770 graphite material Substances 0.000 claims abstract description 30
- 238000004458 analytical method Methods 0.000 claims abstract description 28
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 28
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 28
- 239000000126 substance Substances 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000000835 fiber Substances 0.000 claims description 65
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- 229910052751 metal Inorganic materials 0.000 claims description 27
- 239000002184 metal Substances 0.000 claims description 27
- 238000012937 correction Methods 0.000 claims description 22
- 238000002844 melting Methods 0.000 claims description 22
- 230000008018 melting Effects 0.000 claims description 22
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000002775 capsule Substances 0.000 claims description 17
- 229920003257 polycarbosilane Polymers 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 239000002243 precursor Substances 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 238000007865 diluting Methods 0.000 claims description 13
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 9
- 239000004408 titanium dioxide Substances 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 5
- -1 polypropylen Polymers 0.000 claims description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
- OOAWCECZEHPMBX-UHFFFAOYSA-N oxygen(2-);uranium(4+) Chemical compound [O-2].[O-2].[U+4] OOAWCECZEHPMBX-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 claims description 3
- FCTBKIHDJGHPPO-UHFFFAOYSA-N uranium dioxide Inorganic materials O=[U]=O FCTBKIHDJGHPPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- 229910003443 lutetium oxide Inorganic materials 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- MPARYNQUYZOBJM-UHFFFAOYSA-N oxo(oxolutetiooxy)lutetium Chemical compound O=[Lu]O[Lu]=O MPARYNQUYZOBJM-UHFFFAOYSA-N 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 10
- 238000001304 sample melting Methods 0.000 abstract 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 34
- 238000012360 testing method Methods 0.000 description 26
- 238000005303 weighing Methods 0.000 description 10
- 238000011088 calibration curve Methods 0.000 description 9
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000007792 addition Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 239000011153 ceramic matrix composite Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000011157 advanced composite material Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- UGBIHFMRUDAMBY-UHFFFAOYSA-N lutetium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Lu+3].[Lu+3] UGBIHFMRUDAMBY-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method for measuring the oxygen content in a silicon carbide ceramic material. The method for determining the oxygen content in the silicon carbide ceramic material comprises the following steps: firstly, metal oxide is used as a standard substance, the metal oxide standard substance is diluted by a graphite material to form a standard substance, an oxygen element standard working curve is established, then a silicon carbide ceramic material is wrapped by a nickel material, the wrapped silicon carbide ceramic material and the graphite material are uniformly mixed, then an oxygen nitrogen analysis device is used for analyzing, so that the oxygen content of the silicon carbide ceramic material is measured, and the correlation coefficient R of the curve is2Not less than 0.99. The determination method has the advantages of high accuracy, good repeatability, more sufficient sample melting, simple and rapid operation, low cost and the like when the determination method is used for detecting the oxygen content sample in the ceramic material; meanwhile, the graphite material is added during detection, so that the occurrence of the burning-through situation of the graphite crucible can be effectively avoided.
Description
Technical Field
The invention belongs to the technical field of analysis and test, and particularly relates to a method for measuring oxygen content in a silicon carbide ceramic material.
Background
The continuous silicon carbide (SiC) fiber is a novel ceramic fiber with high specific strength, high specific modulus, high creep resistance, high temperature resistance, oxidation resistance, corrosion resistance and good compatibility with a ceramic matrix, and has wide application prospect in the high-tech fields of aerospace, aviation, weapons, ships, nuclear industry and the like. The excellent performance of the SiC fiber makes the SiC fiber become a preferred reinforcement for preparing ceramic matrix composite materials with excellent performances of high temperature resistance, oxidation resistance, good wear resistance, small thermal expansion rate, good electric and thermal conductivity, high hardness, corrosion resistance and the like. The SiC ceramic matrix composite (SiCf/SiC) toughened by the continuous SiC fibers is applied to the front edges of the heads and wings of space shuttles, combustion chambers-jet pipes of aerospace engines, hot end parts of engines for advanced tanks, large carrier rocket expansion sections, hot structural parts of liquid rocket engines and ramjets, nuclear fusion first wall materials and the like. The SiC fiber and the composite material thereof are widely applied to armed forces systems and the fields of aviation, aerospace and the like which have strategic significance. Meanwhile, due to the wide application prospect in the military field, the high-performance continuous SiC fiber is always a prohibited product of western countries to China. In order to break through technical blockade in western countries and meet the requirements of advanced composite materials and weapon equipment development in China, on the basis of the existing research in China, high-temperature resistant continuous SiC fibers with independent intellectual property rights are developed, and the method has important significance for improving the military strength and comprehensive national strength in China, so that the corresponding detection and characterization method must follow the research and industrialized development of high-performance SiC fibers.
According to the difference of SiC fiber temperature resistance, oxidation resistance, fiber structure composition and the like, SiC fiber can be generally divided into first generation, second generation and third generation SiC fiber, the most fundamental difference of the three generation products lies in the temperature resistance difference, the first generation only resists 1300 ℃, the second generation can resist 1500 ℃, the third generation can resist more than 1800 ℃, the amount of oxygen content of the fiber plays a key role in the temperature resistance, and the lower the oxygen content is, the better the temperature resistance and the oxidation resistance are. In addition, in the preparation process of the SiC fiber, after melt spinning, the silicon carbide precursor needs to be subjected to oxidation crosslinking, namely, the fiber reacts with oxygen in the air to become crosslinked fiber, and then the fiber can be subjected to inorganic fiber conversion and high-temperature sintering treatment process to prepare the SiC fiber. Therefore, no matter the SiC fiber performance evaluation and the process control of the oxygen content in the fiber preparation process, the fiber oxygen content test has very important significance for the silicon carbide fiber. At present, there is no unified method for detecting oxygen content of silicon carbide precursor and corresponding fiber, and the literature is only limited to reference to GB/T11261-2006 (pulse heating inert gas melting-infrared absorption method for determining oxygen content of steel) or directly mentioning that a high temperature oxygen nitrogen analyzer is used for oxygen content test, etc., both of which are that a metal or inorganic sample is melted at high temperature under an inert atmosphere by using the oxygen nitrogen analyzer, and the test is performed by using the infrared absorption method. The method has higher detection sensitivity and accuracy under the condition of lower oxygen content (mg/kg grade) of metal and inorganic samples, and has certain difficulty in testing under the condition of higher oxygen content of the silicon carbide precursor and the fiber in the process of the silicon carbide precursor, wherein the oxygen content of the fiber is generally in a range of about 5-30 percent. The usual approach taken for high oxygen samples is to reduce the sample weight and establish a standard curve using low oxygen metal standards, which is effective for samples below 5%, but is greatly limited in accuracy and sensitivity for silicon carbide precursors and samples with fiber oxygen content above 5%. The most fundamental reason for this is that there is no suitable high oxygen content standard to establish a suitable standard working curve calibration instrument. It is seen that it is not ideal to use the current high temperature oxygen nitrogen analyzer and use the metal industry standard for testing the high oxygen content samples of the silicon carbide precursor and its fibers.
Disclosure of Invention
The invention mainly aims to provide a method for measuring the oxygen content in a silicon carbide ceramic material so as to overcome the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a method for measuring the oxygen content in a silicon carbide ceramic material, which comprises the following steps:
adopting metal oxide as a standard substance, diluting the metal oxide standard substance by using a graphite material to form a standard substance, and establishing an oxygen element standard working curve; coefficient of correlation R of said curve2≥0.99；
And coating the silicon carbide ceramic material with a nickel material, uniformly mixing the coated silicon carbide ceramic material with a graphite material, and analyzing by using an oxygen-nitrogen analysis device, thereby determining the oxygen content of the silicon carbide ceramic material.
When a sample with higher oxygen content in the silicon carbide ceramic material is measured, one-point or multi-point calibration working curve is established by taking metal oxides and metal oxides with different diluted concentrations as standard substances to measure the oxygen content of the silicon carbide precursor and the fiber thereof; according to an inert gas melting sample of an electrode pulse furnace of an oxygen and nitrogen analysis device (an oxygen and nitrogen analyzer), the content of oxygen in the sample is determined by an infrared absorption method, and high-purity graphite is added into a graphite crucible, so that the data stability of the high-oxygen-content sample is improved, and the situation that the graphite crucible is burnt through is prevented.
Compared with the prior art, the invention has the beneficial effects that:
(1) the standard metal oxide adopted in the experimental process has stable performance, is convenient to store and easy to obtain, has higher oxygen content, is usually more than 10 percent, can realize the establishment of a working curve with high oxygen content, and is beneficial to improving the accuracy and the sensitivity of the detection of a sample with high oxygen content; in the detection process, standard samples with different oxygen concentrations are prepared by diluting a graphite material, a multi-point calibration working curve can be established, the graphite material is low in price and easy to obtain, the detection accuracy of a sample with high oxygen content is improved, and the graphite material is beneficial to more sufficient melting of the detected sample;
(2) in the experimental process, the silicon carbide ceramic material sample wrapped by the nickel capsule is placed in the graphite material, so that the contact area between the sample and the graphite is larger, the melting is more sufficient, the reaction between the sample and the graphite is accelerated, the oxygen content test result is more accurate, and the repeatability of the oxygen content data of the sample is better; because the silicon carbide ceramic material has higher oxygen content and higher melting point, the furnace body setting power or temperature is higher than that of other metal samples in the experimental process so as to ensure that the silicon carbide ceramic material sample can be completely melted, which can cause the burn-through situation in the melting process of the graphite crucible; compared with the method of using a sleeve crucible in the literature, the method has the advantages that the cost of graphite materials is lower, the same purpose of using the sleeve crucible is achieved, the sample is heated more uniformly and melted more fully, and the method provided by the invention reduces the cost of sample analysis;
(3) the method provided by the invention is simple to operate, the required reagents are extremely easy to obtain, and the standard substances with different oxygen content concentrations are diluted and uniformly mixed only by weighing according to a proportion without redundant operation steps.
Detailed Description
In view of the defects of the prior art, the inventor of the present invention has made extensive research and practice to propose the technical solution of the present invention. The experimental principle is that a sample is put into a nickel basket, the nickel basket is added into a degassed graphite crucible, and the sample is heated and melted under the protection of helium. Oxygen is reduced by graphite at high temperature to produce CO, which is oxidized to CO by a glowing CuO reagent2Detecting in infrared absorption cell, and detecting nitrogen in sample with N2Releasing the helium into a thermal conductivity cell for detection; the method mainly comprises the steps of establishing a standard working curve by an oxygen-nitrogen analyzer by using a standard sample, then melting a sample by using inert gas of an electrode pulse furnace according to the oxygen-nitrogen analyzer, and measuring by using an infrared absorption methodThe oxygen content in the high-oxygen-content sample is determined, a certain amount of graphite material is added into the graphite crucible, and then sample analysis is carried out, so that the data stability of the oxygen-content sample is improved, and the graphite crucible is prevented from being burnt through.
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. 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.
One aspect of an embodiment of the present invention provides a method for determining an oxygen content in a silicon carbide ceramic material, including:
adopting metal oxide as a standard substance, diluting the metal oxide standard substance by using a graphite material to form a standard substance, and establishing an oxygen element standard working curve; coefficient of correlation R of said curve2≥0.99；
And coating the silicon carbide ceramic material with a nickel material, uniformly mixing the coated silicon carbide ceramic material with a graphite material, and analyzing by using an oxygen-nitrogen analysis device, thereby determining the oxygen content of the silicon carbide ceramic material.
In some more specific embodiments, the method for determining the oxygen content in a silicon carbide ceramic material comprises: the method comprises the steps of adopting metal oxide as a standard substance, mixing graphite material and the metal oxide to prepare required standard substances with different oxygen element concentrations, and then carrying out one-point correction analysis and/or multi-point correction analysis on the standard substances by using an oxygen and nitrogen analysis device to establish an oxygen element standard working curve.
Further, the correction analysis is preferably a multipoint correction analysis.
Further, the multi-point correction analysis includes, but is not limited to, a three-point correction analysis.
Further, the ratio of the graphite material to the metal oxide is selected according to the oxygen content of the specific sample and the selected oxidation standard.
Further, the graphite material includes any one or a combination of two or more of powdered graphite, granular graphite, and flake graphite, and is not limited thereto.
Further, the graphite material is a high-grade pure graphite material, and the purity of the graphite is more than 99%.
In some more specific embodiments, the silicon carbide ceramic material includes a silicon carbide precursor or a silicon carbide fiber, and is not limited thereto.
Further, the silicon carbide ceramic material comprises fibers of each process section in the process of preparing the silicon carbide precursor and/or the silicon carbide fiber.
Further, the silicon carbide ceramic material includes any one of a silicon carbide precursor, a silicon carbide oxide fiber, a silicon carbide infusible fiber, a silicon carbide fiber, and a ceramic fiber, and is not limited thereto.
Further, the silicon carbide ceramic material includes any one of Polycarbosilane (PCS), Polyaluminocarbosilane (PACS), polyborocarbosilane, polyborosilazane, polyyttryicarbosilane, polyzirconocene, polytitanocarbosilane, polycarbosilazane, polypropylen, boron nitride, silicon nitride, polyborosilazane, polycarbosilane air infusible fiber, polycarbosilane thermal crosslinking fiber, polyaluminocarbosilane fiber, and polyaluminocarbosilane fiber, without being limited thereto.
Further, the metal oxide includes any one of yttrium oxide (oxygen content 21.26 wt%), zirconium oxide (oxygen content 25.97 wt%), niobium oxide (oxygen content 30.10 wt%), strontium oxide (oxygen content 15.44 wt%), cerium oxide (oxygen content 18.59 wt%), titanium dioxide (oxygen content 40.0 wt%), uranium dioxide (oxygen content 11.85 wt%), calcium oxide (oxygen content 28.53 wt%), magnesium oxide (oxygen content 39.70 wt%), aluminum oxide (oxygen content 47.08 wt%), lanthanum oxide (oxygen content 14.73 wt%), lutetium oxide (oxygen content 12.06 wt%), and thorium dioxide (oxygen content 12.12 wt%), and is not limited thereto.
Further, the oxygen content of the metal oxide is greater than 10 wt%. Further, the melting points of the metal oxides are respectively: yttrium oxide (melting point 2410 ℃), zirconium oxide (melting point about 2700 ℃), niobium oxide (melting point about 1780 ℃), strontium oxide (melting point 2430 ℃), cerium oxide (melting point 2397 ℃), titanium dioxide (melting point 1850 ℃), uranium dioxide (melting point 2878 ℃), calcium oxide (melting point 2850 ℃), magnesium oxide (melting point 2852 ℃), aluminum oxide (melting point 2054 ℃), lanthanum trioxide (melting point 2217 ℃), lutetium trioxide (melting point 2510 ℃), thorium dioxide (melting point 3220 ± 50 ℃).
Further, the melting point of the metal oxide is greater than 1500 ℃.
In some more specific embodiments, the silicon carbide ceramic material is used in an amount of 0.001 to 1g, preferably 3 to 20 mg.
Further, the amount of the graphite material is 0.001 to 2g, preferably 0.05 to 0.2 g.
Furthermore, the content of oxygen element in the silicon carbide ceramic material is 1-40 wt%.
The method for measuring the content of the oxygen element is also suitable for detecting the substances with the content of the oxygen element higher than 40 wt%, and the accuracy of detected data is high.
In some more specific embodiments, the method for determining the oxygen content in a silicon carbide ceramic material further comprises:
grinding a silicon carbide ceramic material into powder, adding the powder into a nickel capsule, and compressing to obtain the nickel capsule wrapped with a sample to be detected;
and placing the nickel capsule wrapped with the sample to be detected in a graphite crucible of a sample inlet of an oxygen-nitrogen analyzer, adding a graphite material into the graphite crucible of the oxygen-nitrogen analyzer, analyzing by using the oxygen-nitrogen analyzer, and comparing the established oxygen element standard working curve, thereby determining the oxygen content in the sample to be detected.
Further, the nickel material includes any one of a nickel pouch, a nickel foil cup, or a nickel basket, but is not limited thereto.
Further, the nickel capsule includes any one of a cylindrical nickel capsule, a conical nickel capsule, or a split nickel capsule with a cover, and is not limited thereto.
Further, the graphite crucible includes a standard crucible of high purity graphite composition and/or a jacketed crucible of high purity graphite composition.
In some more specific embodiments, the method further comprises: and (3) placing the graphite crucible in front of a clamping groove at the lower electrode of the oxygen-nitrogen analyzer, and adding a graphite material into the graphite crucible.
Further, the oxygen-nitrogen analyzer takes a pulse heating inert gas melting-infrared absorption method as a measurement principle.
In some more specific embodiments, the method of determining the oxygen content in a silicon carbide ceramic material comprises:
(1) adopting metal oxide as a standard substance, and then mixing the graphite material and the metal oxide to prepare three standard substances with different oxygen element concentrations;
(2) according to the operating rules of the oxygen-nitrogen analyzer, three-point correction is carried out on the three concentrations of oxygen element metal oxides in the step (1) to prepare an oxygen element standard working curve;
(3) grinding a ceramic material into powder, adding the powder into a nickel capsule, and compressing to obtain the nickel capsule wrapped with a sample to be detected;
(4) and placing the nickel sac wrapped with the sample to be detected in a sample inlet of an oxygen-nitrogen analyzer, adding a graphite material into the graphite crucible, placing the graphite crucible in a clamping groove of a graphite crucible of a lower electrode of the oxygen-nitrogen analyzer, and then determining the oxygen content in the sample to be detected by adopting an infrared absorption method.
Compared with the method of using a sleeve crucible in the literature, the detection method of the invention has the advantages that the cost of graphite is lower, the price of graphite with the purity of 99.85 percent and 500g in one bottle is 18 yuan (refer to the price of reagents in national medicine group), 5000 times of sample analysis can be performed according to the dosage of 0.1g of one sample, and the use of the sleeve crucible has the same purpose, even if the sample is heated more uniformly, the melting is more sufficient; when the crucible is used, the outer crucible can be repeatedly used, but the outer crucible needs to be frequently replaced, for example, the purchase price in the laboratory (Changzhou Weikang graphite products Co., Ltd.) is about 4.5 yuan per crucible, the use times of the outer crucible can be greatly reduced due to the large oxygen content, the outer crucible can be repeatedly used for 3 times, the single cost is 1.5 yuan, the inner crucible needs to be used once, the single cost is 2.5 yuan per crucible, and the single sample analysis cost of the inner crucible and the outer crucible is 4 yuan. The detection method adopts a common standard graphite crucible with the cost of 3 yuan/piece, and the cost of weak graphite powder can be ignored. It can be seen that the detection method of the present invention reduces the cost of sample analysis.
The technical solution of the present invention is further described in detail with reference to several preferred embodiments, which are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of the present invention is not limited to the following embodiments.
The experimental materials used in the examples used below were all available from conventional biochemical reagents companies, unless otherwise specified.
Example 1
Establishing a standard working curve: the metal yttrium oxide is used as a standard product, the oxygen content of the metal yttrium oxide is 21.26%, and the metal yttrium oxide can be used after being calcined in a muffle furnace air atmosphere at 1000 ℃ for at least 2 hours before being used. Respectively diluting yttrium oxide standard samples with different oxygen concentrations by using graphite powder, wherein the ratio of yttrium oxide: the mass ratio of the graphite powder is 1:0, 1:1 and 1:20 respectively, namely the actual oxygen content of the prepared yttrium oxide is 21.26%, 10.63% and 1.06% respectively. Testing the prepared standard sample according to the operation procedure of the instrument to form a three-point correction working curve, wherein the calibration curve is that y is 5.05x-9.216, and R is2＝0.999。
Grinding polycarbosilane (silicon carbide precursor) blocks into powder, accurately weighing about 200mg of ground sample, adding the sample into a nickel bag, compressing and wrapping the sample by using a pliers, putting the sample into a feed inlet of an oxygen-nitrogen analyzer, adding about 0.05g of graphite powder into an empty graphite crucible, putting the graphite powder into a clamping groove of a graphite crucible of a lower electrode, and carrying out parallel analysis on the sample 10 times by the oxygen-nitrogen analyzer strictly according to the operation rules of the analyzer. High temperature oxynitrides analyzer (Likeco ON836) experimental conditions: furnace degassing cycle 3; 5900W of power; time 15 s; cooling time is 6 s; power mode: keeping the temperature constant; analytical power 5500 w. The results are shown in Table 1.
TABLE 1 Polycarbosilane oxygen content test results
| Number of samples | Oxygen content% |
| 1 | 4.06 |
| 2 | 4.14 |
| 3 | 4.09 |
| 4 | 4.16 |
| 5 | 4.20 |
| 6 | 4.12 |
| 7 | 4.08 |
| 8 | 4.10 |
| 9 | 4.11 |
| 10 | 4.09 |
| Mean value of | 4.11 |
| RSD | 0.0395 |
| CV value | 0.96 |
Example 2
Establishing a standard working curve: the metal yttrium oxide is used as a standard product, the oxygen content of the metal yttrium oxide is 21.26%, and the metal yttrium oxide can be used after being calcined in a muffle furnace air atmosphere at 1000 ℃ for at least 2 hours before being used. Respectively diluting yttrium oxide standard samples with different oxygen concentrations by using graphite powder, wherein the ratio of yttrium oxide: the mass ratio of the graphite powder is 1:0, 1:1 and 1:20 respectively, namely the actual oxygen content of the prepared yttrium oxide is 21.26%, 10.63% and 1.06% respectively. Testing the prepared standard sample according to the operation procedure of the instrument to form a three-point correction working curve, wherein the calibration curve is that y is 5.05x-9.216, and R is2＝0.999。
Grinding polycarbosilane air infusible fiber into powder, accurately weighing 10mg of left and right ground samples, adding the samples into a nickel bag, compressing and wrapping the samples by using pliers, putting the samples into a feed inlet of an oxygen-nitrogen analyzer, adding 0.1g of left and right graphite powder into an empty graphite crucible, putting the samples into a clamping groove of a lower electrode graphite crucible, and carrying out parallel analysis on the samples 10 times by the oxygen-nitrogen analyzer strictly according to the operation rules of the analyzer. The conditions of the oxygen and nitrogen analyzer were the same as in example 1, and the results are shown in Table 2.
TABLE 2 Polycarbosilane air infusible fiber oxygen content test results
| Number of samples | Oxygen content% |
| 1 | 10.30 |
| 2 | 10.29 |
| 3 | 10.34 |
| 4 | 10.28 |
| 5 | 10.31 |
| 6 | 10.30 |
| 7 | 10.41 |
| 8 | 10.40 |
| 9 | 10.32 |
| 10 | 10.33 |
| Mean value of | 10.33 |
| RSD | 0.044 |
| CV value | 0.43 |
Example 3
Establishing a standard working curve: the method adopts metal zirconia as a standard substance, the oxygen content of the metal zirconia is 25.97 percent, and the metal zirconia can be used after being calcined in a muffle furnace air atmosphere at 1000 ℃ for at least 2 hours before being used. Respectively diluting zirconia standard samples with different oxygen concentrations by graphite powder, wherein the weight ratio of zirconia: the mass ratio of the graphite powder is 1:0, 1:1 and 1:20 respectively, namely the actual oxygen content of the prepared zirconia is 25.97%, 12.98% and 1.30% respectively. Testing the prepared standard sample according to the operation procedure of the instrument to form a three-point correction working curve, wherein the calibration curve is that y is 4.111x-11.25, R2＝0.999。
Grinding polycarbosilane crosslinked fibers into powder, accurately weighing about 50mg of ground sample, adding the sample into a nickel bag, compressing and wrapping the sample by using a pliers, putting the sample into a feed inlet of an oxygen-nitrogen analyzer, adding about 0.2g of graphite powder into an empty graphite crucible, putting the graphite powder into a clamping groove of a lower electrode graphite crucible, and carrying out parallel analysis on the sample 10 times by the oxygen-nitrogen analyzer strictly according to the operation rules of the analyzer. The conditions of the oxygen and nitrogen analyzer were the same as in example 1, and the results are shown in Table 3.
TABLE 3 polycarbosilane crosslinked fiber oxygen content test results
| Number of samples | Oxygen content% |
| 1 | 13.65 |
| 2 | 13.58 |
| 3 | 13.60 |
| 4 | 13.59 |
| 5 | 13.70 |
| 6 | 13.49 |
| 7 | 13.66 |
| 8 | 13.68 |
| 9 | 13.56 |
| 10 | 13.70 |
| Mean value of | 13.62 |
| RSD | 0.0685 |
| CV value | 0.50 |
Example 4
Establishing a standard working curve: the method adopts metal zirconia as a standard substance, the oxygen content of the metal zirconia is 25.97 percent, and the metal zirconia can be used after being calcined in a muffle furnace air atmosphere at 1000 ℃ for at least 2 hours before being used. Respectively diluting zirconia standard samples with different oxygen concentrations by graphite powder, wherein the weight ratio of zirconia: the mass ratio of the graphite powder is 1:0, 1:1 and 1:20 respectively, namely the actual oxygen content of the prepared zirconia25.97%, 12.98% and 1.30% respectively. Testing the prepared standard sample according to the operation procedure of the instrument to form a three-point correction working curve, wherein the calibration curve is that y is 4.111x-11.25, R2＝0.999。
Grinding silicon carbide fiber into powder, accurately weighing about 10mg of ground sample, adding into a nickel bag, compressing and wrapping the sample with a clamp, putting the sample into a feed inlet of an oxygen-nitrogen analyzer, adding about 0.1g of graphite powder into an empty graphite crucible, putting into a clamping groove of a graphite crucible of a lower electrode, strictly executing the oxygen-nitrogen analyzer according to the operation rules of the analyzer, and parallelly analyzing the sample for 10 times. The conditions of the oxygen and nitrogen analyzer were the same as in example 1, and the results are shown in Table 4.
TABLE 4 silicon carbide fiber oxygen content test results
| Number of samples | Oxygen content% |
| 1 | 18.67 |
| 2 | 18.65 |
| 3 | 18.60 |
| 4 | 18.72 |
| 5 | 18.74 |
| 6 | 18.69 |
| 7 | 18.79 |
| 8 | 18.60 |
| 9 | 18.66 |
| 10 | 18.73 |
| Mean value of | 18.68 |
| RSD | 0.0613 |
| CV value | 0.33 |
Example 5
Establishing a standard working curve: the metal niobium pentoxide is used as a standard substance, the oxygen content of the metal niobium pentoxide is 30.10%, and the metal niobium pentoxide can be used after being calcined in a muffle furnace air atmosphere at 1000 ℃ for at least 2 hours before use. Respectively diluting niobium pentoxide standard samples with different oxygen concentrations by using graphite powder, wherein the niobium pentoxide standard samples comprise: the mass ratio of the graphite powder is 1:0, 1:1 and 1:29 respectively, namely the actual oxygen content of the niobium pentoxide is 30.10%, 15.05% and 1.00% respectively. Testing the prepared standard product according to the instrument operating specification to form a three-point correction working curve, wherein the calibration curve is that y is 3.460x-12.30, R2＝0.999。
Grinding poly aluminium carbon silane fiber into powder, accurately weighing about 5mg and grinding the back sample, adding to the nickel bag, compressing and wrapping the sample with pliers, putting the sample into the feed inlet of an oxygen nitrogen analyzer, adding about 0.05g of graphite powder into an empty graphite crucible, putting into the neck of a lower electrode graphite crucible, and carrying out parallel analysis 10 times by the oxygen nitrogen analyzer according to the operation rules of the analyzer. The conditions of the oxygen and nitrogen analyzer were the same as in example 1, and the results are shown in Table 5.
TABLE 5 PolyAluminocarbosilane silicon fiber oxygen content test results
| Number of samples | Oxygen content% |
| 1 | 25.67 |
| 2 | 25.70 |
| 3 | 25.72 |
| 4 | 25.73 |
| 5 | 25.69 |
| 6 | 25.65 |
| 7 | 25.60 |
| 8 | 25.75 |
| 9 | 25.74 |
| 10 | 25.66 |
| Mean value of | 25.69 |
| RSD | 0.0468 |
| CV value | 0.18 |
Example 6
Establishing a standard working curve: the method adopts metal titanium dioxide as a standard substance, the oxygen content of the metal titanium dioxide is 40.05 percent, and the metal titanium dioxide can be used after being calcined in a muffle furnace air atmosphere at 1000 ℃ for at least 2 hours before being used. Respectively diluting titanium dioxide standard samples with different oxygen concentrations by using graphite powder, wherein the weight ratio of titanium dioxide: the mass ratio of the graphite powder is respectively 1:0, 1:1, 1:3 and 1:7, namely the actual oxygen content of the prepared titanium dioxide is respectively 47.08%, 23.54%, 11.77% and 5.89%. Testing the prepared standard product according to the instrument operating specification to form a three-point correction working curve, wherein the calibration curve is that y is 1.224x-0.548, and R is2＝0.998。
Grinding silicon carbide ceramic block into powder, accurately weighing 3mg left and right grinding back sample, adding into the nickel bag, compressing and wrapping the sample with a clamp, putting the sample into a feed inlet of an oxygen-nitrogen analyzer, adding 0.1g left and right graphite powder into an empty graphite crucible, putting into a clamping groove of a lower electrode graphite crucible, strictly executing the oxygen-nitrogen analyzer according to the operation rules of the analyzer, and parallelly analyzing the sample for 10 times. The conditions of the oxygen and nitrogen analyzer were the same as in example 1, and the results are shown in Table 6.
TABLE 6 test results of oxygen content of silicon carbide ceramic blocks
| Number of samples | Oxygen content% |
| 1 | 40.36 |
| 2 | 40.25 |
| 3 | 39.99 |
| 4 | 40.63 |
| 5 | 40.36 |
| 6 | 40.45 |
| 7 | 40.60 |
| 8 | 40.54 |
| 9 | 40.69 |
| 10 | 40.78 |
| Mean value of | 40.47 |
| RSD | 0.23 |
| CV value | 0.58 |
Example 7
Establishing a standard working curve: the metal yttrium oxide is used as a standard product, the oxygen content of the metal yttrium oxide is 21.26%, and the metal yttrium oxide can be used after being calcined in a muffle furnace air atmosphere at 1000 ℃ for at least 2 hours before being used. Respectively diluting yttrium oxide standard samples with different oxygen concentrations by using graphite powder, wherein the ratio of yttrium oxide: the mass ratio of the graphite powder is 1:0, 1:1 and 1:20 respectively, namely the actual oxygen content of the prepared yttrium oxide is 21.26%, 10.63% and 1.06% respectively. Testing the prepared standard sample according to the operation procedure of the instrument to form a three-point correction working curve, wherein the calibration curve is that y is 5.05x-9.216, and R is2＝0.999。
Grinding zirconium-containing silicon carbide fiber into powder, accurately weighing 200mg of left and right ground samples, adding the samples into a nickel bag, compressing and wrapping the samples by using a clamp, putting the samples into a feed inlet of an oxygen-nitrogen analyzer, adding 0.05g of left and right graphite powder into an empty graphite crucible, putting the samples into a clamping groove of a lower electrode graphite crucible, and carrying out parallel analysis on the samples 10 times by the oxygen-nitrogen analyzer strictly according to the operation rules of the analyzer. The conditions of the oxygen and nitrogen analyzer were the same as in example 1, and the results are shown in Table 7.
TABLE 7 zirconium-containing silicon carbide fiber oxygen content test results
| Number of samples | Oxygen content% |
| 1 | 1.03 |
| 2 | 1.03 |
| 3 | 1.04 |
| 4 | 1.05 |
| 5 | 1.04 |
| 6 | 1.05 |
| 7 | 1.04 |
| 8 | 1.04 |
| 9 | 1.04 |
| 10 | 1.03 |
| Mean value of | 1.04 |
| RSD | 0.007 |
| CV value | 0.71 |
The experimental data of the above embodiments show that the established multipoint correction working curve has higher linearity, and is used for detecting the silicon carbide precursor and the oxygen element content of the fiber thereof with better accuracy and reproducibility by adopting the metal oxide and diluting the metal oxide with the graphite powder to prepare the standard sample, and when the sample with high oxygen content is tested, the situation that the graphite crucible is burnt through does not occur after the graphite powder is added, and the parallelism effect of the sample is more obvious.
Comparative example 1
Establishing a standard working curve: and (3) carrying out one-point correction by adopting a commercially available steel standard product with the maximum oxygen content, wherein the oxygen content is 1.12%, testing the standard sample according to the operating procedure of an instrument to form a one-point correction curve, and the calibration curve is that y is 1.12 x. Grinding polycarbosilane air infusible fiber into powder, accurately weighing 10mg of left and right ground samples, adding the samples into a nickel bag, compressing and wrapping the samples by using pliers, putting the samples into a feed inlet of an oxygen-nitrogen analyzer, adding 0.1g of left and right graphite powder into an empty graphite crucible, putting the samples into a clamping groove of a lower electrode graphite crucible, and carrying out parallel analysis on the samples 10 times by the oxygen-nitrogen analyzer strictly according to the operation rules of the analyzer. The conditions of the oxygen and nitrogen analyzer were the same as in example 1, and the results are shown in Table 8.
TABLE 8 Polycarbosilane air infusible fiber oxygen content test results
| Number of samples | Oxygen content% |
| 1 | 8.95 |
| 2 | 8.68 |
| 3 | 9.74 |
| 4 | 9.56 |
| 5 | 8.75 |
| 6 | 7.69 |
| 7 | 8.12 |
| 8 | 7.98 |
| 9 | 7.62 |
| 10 | 7.89 |
| Mean value of | 8.50 |
| RSD | 0.76 |
| CV value | 8.92 |
Compared with the comparative example 1, the working curve formed by the low-oxygen content standard is found in example 2, the test data is lower than the actual data, the accuracy is poorer, the CV value is higher, and the data is unstable. And the multipoint correction working curve formed by adopting the metal oxide with high oxygen content has higher data accuracy and lower CV value.
Comparative example 2
Establishing a standard working curve: by means of metalsThe zirconia is used as a standard substance, the oxygen content of the zirconia is 25.97 percent, and the zirconia can be used after being calcined in a muffle furnace air atmosphere at 1000 ℃ for at least 2 hours before use. Respectively diluting zirconia standard samples with different oxygen concentrations by graphite powder, wherein the weight ratio of zirconia: the mass ratio of the graphite powder is 1:0, 1:1 and 1:20 respectively, namely the actual oxygen content of the prepared zirconia is 25.97%, 12.98% and 1.30% respectively. Testing the prepared standard sample according to the operation procedure of the instrument to form a three-point correction working curve, wherein the calibration curve is that y is 4.111x-11.25, R2＝0.999。
Grinding silicon carbide fiber into powder, accurately weighing 10mg of left and right ground sample, adding into a nickel bag, compressing and wrapping the sample with a clamp, putting the sample into a feed inlet of an oxygen-nitrogen analyzer, putting a graphite crucible into a clamping groove of a graphite crucible of a lower electrode, executing the oxygen-nitrogen analyzer according to the operation rules of the analyzer strictly, and analyzing the sample for 10 times in parallel. The conditions of the oxygen and nitrogen analyzer were the same as in example 1, and the results are shown in Table 9.
TABLE 9 silicon carbide fiber oxygen content test results
| Number of samples | Oxygen content% |
| 1 | 19.90 |
| 2 | 17.36 |
| 3 | 17.69 |
| 4 | 19.05 |
| 5 | 17.43 |
| 6 | 18.12 |
| 7 | 19.86 |
| 8 | 17.41 |
| 9 | 16.86 |
| 10 | 16.45 |
| Mean value of | 18.01 |
| RSD | 1.20 |
| CV value | 6.69 |
Compared with the comparative example 2, the example 4 can find that the addition of the graphite powder contributes to the stability and reliability of data, and the CV value is lower, while the CV value of the data without the addition of the graphite powder is higher, and the effect of the graphite powder is very obvious.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
The aspects, embodiments, features and examples of the present invention should be considered as illustrative in all respects and not intended to be limiting of the invention, the scope of which is defined only by the claims. Other embodiments, modifications, and uses will be apparent to those skilled in the art without departing from the spirit and scope of the claimed invention.
The use of headings and chapters in this disclosure is not meant to limit the disclosure; each section may apply to any aspect, embodiment, or feature of the disclosure.
Throughout this specification, where a composition is described as having, containing, or comprising specific components or where a process is described as having, containing, or comprising specific process steps, it is contemplated that the composition of the present teachings also consist essentially of, or consist of, the recited components, and the process of the present teachings also consist essentially of, or consist of, the recited process steps.
It should be understood that the order of steps or the order in which particular actions are performed is not critical, so long as the teachings of the invention remain operable. Further, two or more steps or actions may be performed simultaneously.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims. Moreover, unless specifically stated any use of the terms first, second, etc. do not denote any order or importance, but rather the terms first, second, etc. are used to distinguish one element from another.
Claims (10)
1. A method for determining the oxygen content in a silicon carbide ceramic material is characterized by comprising the following steps:
metal oxide is adopted as a standard substance, and graphite material is used for diluting the metal oxideForming a standard substance by the standard substance, and establishing an oxygen element standard working curve; coefficient of correlation R of said curve2≥0.99；
And coating the silicon carbide ceramic material with a nickel material, uniformly mixing the coated silicon carbide ceramic material with a graphite material, and analyzing by using an oxygen-nitrogen analysis device, thereby determining the oxygen content of the silicon carbide ceramic material.
2. The method of determining the oxygen content in a silicon carbide ceramic material as claimed in claim 1, comprising: the method comprises the steps of adopting metal oxide as a standard substance, mixing graphite material and the metal oxide to prepare standard substances with different oxygen element concentrations, and then carrying out one-point correction analysis and/or multi-point correction analysis on the standard substances by using an oxygen and nitrogen analysis device to establish an oxygen element standard working curve, preferably the multi-point correction analysis.
3. The method of determining the oxygen content in a silicon carbide ceramic material as claimed in claim 1, wherein: the silicon carbide ceramic material comprises a silicon carbide precursor and/or silicon carbide fibers; preferably, the silicon carbide ceramic material comprises fibers of each process section in the process of preparing the silicon carbide precursor and/or the silicon carbide fiber; preferably any one of silicon carbide precursor, silicon carbide oxide fiber, silicon carbide infusible fiber, silicon carbide fiber and ceramic fiber; particularly preferred is any of polycarbosilane, polyaluminocarbosilane, polyborocarbosilane, polyborosilazane, polyyttrytinylsilane, polyzirconocarbonsilane, polytitanocarbosilane, polycarbosilazane, polypropylen, boron nitride, silicon nitride, polyborosilazane, polycarbosilane air infusible fiber, polycarbosilane thermal crosslinked fiber, and polyaluminocarbosilane fiber.
4. The method of determining the oxygen content in a silicon carbide ceramic material as claimed in claim 1, wherein: the metal oxide comprises any one of yttrium oxide, zirconium oxide, niobium oxide, strontium oxide, cerium oxide, titanium dioxide, uranium dioxide, calcium oxide, magnesium oxide, aluminum oxide, lanthanum oxide, lutetium oxide and thorium dioxide; preferably, the melting point of the metal oxide is greater than 1500 ℃; preferably, the oxygen content of the metal oxide is greater than 10 wt%.
5. The method of determining the oxygen content in a silicon carbide ceramic material as claimed in claim 1, wherein: the nickel material comprises a nickel bag, a nickel foil sheet, a nickel foil cup or a nickel basket; preferably, the nickel capsule comprises a cylindrical nickel capsule, a conical nickel capsule or a split nickel capsule with a cover.
6. The method of determining the oxygen content in a silicon carbide ceramic material as claimed in claim 1, wherein: the graphite material comprises any one or the combination of more than two of powdered graphite, granular graphite and flake graphite; preferably, the graphite material has a purity of greater than 99%.
7. The method of determining the oxygen content in a silicon carbide ceramic material as claimed in claim 1, wherein: the dosage of the silicon carbide ceramic material is 0.001-1g, preferably 3-20 mg;
and/or the amount of the graphite material is 0.001-2g, preferably 0.05-0.2 g;
and/or the content of oxygen element in the silicon carbide ceramic material is 1-40 wt%.
8. The method for determining the oxygen content in a silicon carbide ceramic material according to claim 1, comprising in particular:
grinding a silicon carbide ceramic material into powder, adding the powder into a nickel capsule, and compressing to obtain the nickel capsule wrapped with a sample to be detected;
and placing the nickel capsule wrapped with the sample to be detected in a graphite crucible of a sample inlet of an oxygen-nitrogen analyzer, adding a graphite material into the graphite crucible of the oxygen-nitrogen analyzer, analyzing by using the oxygen-nitrogen analyzer, and comparing the established oxygen element standard working curve, thereby determining the oxygen content in the sample to be detected.
9. The method of determining oxygen content in a silicon carbide ceramic material as claimed in claim 8 wherein said graphite crucible comprises a standard crucible of high purity graphite composition and/or a jacketed crucible of high purity graphite composition.
10. The method for determining the oxygen content in the silicon carbide ceramic material according to claim 1, wherein the oxygen and nitrogen analyzer measures the oxygen content based on a pulse heating inert gas melting-infrared absorption method as a measurement principle.
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