CN113984705B - Method for measuring oxygen content of aluminum nitride crystal lattice - Google Patents
Method for measuring oxygen content of aluminum nitride crystal lattice Download PDFInfo
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 239000001301 oxygen Substances 0.000 title claims abstract description 87
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 87
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 68
- 239000013078 crystal Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000004566 IR spectroscopy Methods 0.000 claims abstract description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 26
- 229910052802 copper Inorganic materials 0.000 claims description 24
- 239000010949 copper Substances 0.000 claims description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 4
- 238000000862 absorption spectrum Methods 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 43
- 239000000919 ceramic Substances 0.000 abstract description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 2
- 238000003908 quality control method Methods 0.000 abstract description 2
- 229910052718 tin Inorganic materials 0.000 description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 238000007872 degassing Methods 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000001307 helium Substances 0.000 description 6
- 229910052734 helium Inorganic materials 0.000 description 6
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 6
- 230000010354 integration Effects 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- SDBXSNOPWLYUNT-UHFFFAOYSA-M [O-2].[OH-].O.O.O.[Y+3] Chemical compound [O-2].[OH-].O.O.O.[Y+3] SDBXSNOPWLYUNT-UHFFFAOYSA-M 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 239000013040 bath agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CLDVQCMGOSGNIW-UHFFFAOYSA-N nickel tin Chemical compound [Ni].[Sn] CLDVQCMGOSGNIW-UHFFFAOYSA-N 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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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
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
- G01N2021/3572—Preparation of samples, e.g. salt matrices
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Abstract
The invention discloses a method for measuring the oxygen content of aluminum nitride crystal lattices, belonging to the technical field of analysis and test. The method for measuring the oxygen content of the aluminum nitride crystal lattice comprises the following steps: adding an aluminum nitride sample containing a sintering aid, graphite powder and a tin-copper binary bath material into a high-temperature-resistant container, heating a mixture in the high-temperature-resistant container in a sectional heating mode, measuring oxygen released by the aluminum nitride sample in a sectional manner by using an infrared absorption spectrometry, and calculating the oxygen content of an aluminum nitride crystal lattice. The method utilizes an inert melting-infrared absorption method to accurately determine the oxygen content of the aluminum nitride crystal lattice, and accurately determines the oxygen content of the aluminum nitride crystal lattice by selecting a proper crucible, an additive and bath materials and setting reasonable analysis parameters. The method is simple to operate and easy to master, can effectively distinguish and measure the lattice oxygen and other oxygen contents, and provides reliable guarantee for the quality control of the production, scientific research and application of the high-performance aluminum nitride ceramic.
Description
Technical Field
The invention relates to the technical field of analysis and test, in particular to a method for measuring the oxygen content of an aluminum nitride crystal lattice.
Background
Aluminum nitride (AlN) has high thermal conductivity (theoretically up to 320 W.m)-1·K-1) The high-dielectric-constant composite material has good insulativity, low dielectric constant and dielectric loss, is widely applied to the fields of semiconductors, electric vacuum and the like, and is also a key material of electronic components for automotive electronics, aerospace, military and national defense. But the oxygen content of the impurity directly influences the heat-conducting property of the aluminum nitride ceramic product, and the differential determination of the oxygen content at different positions plays an important role in the production, scientific research and application of the aluminum nitride ceramic. Oxygen in aluminum nitride ceramic materials is mainly classified into three forms: the first is adsorbed on the surface of the powder material (surface oxygen for short), the second is oxide in the aluminum nitride crystal boundary (crystal boundary oxygen for short), and the third is solid-dissolved in the aluminum nitride crystal lattice (crystal lattice oxygen for short). The content of lattice oxygen has very important influence on the heat-conducting property of the aluminum nitride ceramic materialAccordingly, there is a need to accurately determine the oxygen content within the aluminum nitride crystal lattice. However, since the decomposition temperature of the aluminum nitride crystal lattice is high, lattice oxygen and other oxygen are released simultaneously by the flux addition method, and thus it is difficult to distinguish them.
The detection means such as energy spectrum and XPS can only detect the content of surface elements and is not high in precision, and the concentration of oxygen can be accurately detected by means of neutron radiation and the like, but equipment thereof is expensive and detection cost is high. The oxygen content in the aluminum nitride can be determined by an inert melting-infrared absorption method, but the total oxygen content in the aluminum nitride is determined by a tin-nickel fluxing agent in the literature at present, and how to determine the lattice oxygen content in the aluminum nitride is not reported.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for measuring the oxygen content of aluminum nitride crystal lattices. The oxygen content in the aluminum nitride crystal lattice is accurately determined by utilizing an inert melting-infrared absorption method, adopting a sectional heating mode, reaching the temperature required by the oxygen release of the aluminum nitride crystal lattice through a high-temperature crucible, orderly and properly adding tin and copper binary bath materials and graphite powder and reasonable analysis parameters.
In order to realize the purpose, the invention provides the following technical scheme:
one of the technical schemes of the invention is as follows: the method for measuring the oxygen content of the aluminum nitride crystal lattice comprises the following steps:
adding an aluminum nitride sample containing a sintering aid, graphite powder and a tin-copper binary bath material into a high-temperature resistant container, heating the mixture in the high-temperature resistant container in a sectional heating mode, measuring oxygen released by the aluminum nitride sample in a sectional manner by using an infrared absorption spectroscopy, and calculating the oxygen content of aluminum nitride crystal lattices.
The invention inhibits the volatilization of the metallic aluminum by adding the tin and copper binary bath material. Tin, copper and nickel are common auxiliary materials, nickel has a good fluxing effect, but the addition of nickel can decompose aluminum nitride crystal lattices at a medium temperature section, so that the release of crystal lattice oxygen and crystal boundary oxygen generates intersection and cannot be distinguished. The fluxing effect of tin and copper is relatively weak, so that aluminum nitride crystal lattices cannot be decomposed at a medium temperature; in addition, after tin and copper are melted, the binary metal liquid has a good bath material effect and can completely wrap metal aluminum generated in the medium-temperature section and the high-temperature section, so that volatilization of the metal aluminum is effectively inhibited, and overflow of aluminum nitride is prevented.
The added graphite powder can promote the carbon-oxygen reaction at the crystal boundary. Because yttrium aluminate exists at the crystal boundary of aluminum nitride, the yttrium aluminate generates carbon-oxygen reaction at a medium temperature section, if graphite powder is not added, carbon elements required by the reaction are provided by a graphite crucible, the graphite powder is added, the carbon elements can be provided by the graphite powder, and the graphite powder is fully mixed with a sample, so that the carbon-oxygen reaction can be effectively promoted, and the release time of crystal boundary oxygen is shortened.
Preferably, the mass ratio of the aluminum nitride sample containing the sintering aid to the graphite powder is 1 (0.8-1.2); the mass ratio of the aluminum nitride sample containing the sintering aid to the tin-copper binary bath material is 1 (30-50), and the mass ratio of tin to copper is 1 (0.9-1.1).
Preferably, the mass percent of the sintering aid in the aluminum nitride sample containing the sintering aid is 3-5%; the sintering aid comprises yttrium pentoxide.
Preferably, the particle size of the aluminum nitride sample containing the sintering aid is less than or equal to 75 mu m.
Preferably, the particle size of the graphite powder is 20-50 μm; the tin in the tin-copper binary bath material is a tin sheet with the thickness of 0.5mm, and the copper is copper scraps with the diameter of 0.2mm and the length of 1 mm.
More preferably, the aluminum nitride sample containing the sintering aid, the graphite powder and the tin-copper binary bath material are sequentially added into the aluminum nitride sample containing the sintering aid, the graphite powder, the tin and the copper.
The invention prevents aluminum nitride crystal lattice from fluxing decomposition in the middle temperature section by adding auxiliary materials and limiting the adding sequence of the auxiliary materials.
Preferably, the high temperature resistant container is a high temperature graphite crucible.
Preferably, the specific parameters of the segmented temperature increasing mode are as follows: the first stage is as follows: staying for 40-60 s under the power of 1.4-1.6 kW; and a second stage: staying for 100-120 s under the power of 2.4-2.6 kW; and a third stage: the power is 4.5-5.0 kW and the time is 60-70 s.
According to the invention, a three-section stepping heating mode is set according to different release temperatures of surface oxygen, crystal boundary oxygen and lattice oxygen, so that three kinds of oxygen are released at different temperature stages respectively without generating release intersection. Because surface oxygen is adsorbed on the surface of the sample, the surface oxygen is easy to separate from the particle powder after being heated and can be released in a low-temperature section; the crystal boundary oxygen is mainly yttrium aluminate and can be released in a medium-temperature section; the release of the lattice oxygen requires the aluminum nitride lattice to be decomposed, and the temperature required by the lattice decomposition is higher, so that the lattice oxygen is released at a high temperature stage, and the temperature required by the aluminum nitride lattice decomposition is reached through a high-temperature crucible.
Preferably, the oxygen released by the aluminum nitride sample segments is sequentially carried into an infrared absorption spectrum detector by inert carrier gas for detection.
The second technical scheme of the invention is as follows: the method for determining the oxygen content of the aluminum nitride crystal lattice by using the oxygen-nitrogen-hydrogen analyzer comprises the following steps:
(1) starting a preheating oxygen-nitrogen-hydrogen analyzer, introducing high-purity helium and nitrogen, adjusting to a specified partial pressure, and checking whether the flow and the temperature of the helium are normal;
(2) establishing an analysis method;
(3) performing blank analysis and standard sample analysis by adopting the analysis method in the step (2), and calibrating an analysis instrument;
(4) and (3) analyzing the prepared sample by adopting the analysis method in the step (2), and processing data of the analysis result to obtain the oxygen content in the aluminum nitride crystal lattice.
Preferably, the specific steps of step (1) are as follows:
(1-1) starting up: starting an oxygen nitrogen hydrogen analyzer and corresponding software on a computer;
(1-2) aeration: introducing high-purity helium (carrier gas) and high-purity nitrogen (power gas), adjusting the working pressure of the high-purity helium to be 20psi through a pressure reducing valve, adjusting the working pressure of the high-purity nitrogen to be 40psi, and adjusting the ventilation time to be 3-4 hours;
(1-3) checking flow rate and temperature: check if the helium flow is 450mL/min, check if the inlet catalyst temperature and inlet scavenger temperature reach 650 ℃.
Preferably, the specific steps of step (2) are as follows:
(2-1) crucible and analysis mode: selecting a high-temperature crucible 782 and 720 from the crucible parameters of the system-furnace, and adopting a manual analysis and power control mode;
(2-2) analyzing the power by adopting a step-by-step temperature rising mode: the first stage is as follows: the power is 1.4-1.6 kW, and the mixture stays for 40-60 s; and a second stage: staying for 100-120 s under the power of 2.4-2.6 kW; and a third stage: the power is 4.5-5.0 kW, and the mixture stays for 60-70 s;
(2-3) setting analysis parameters: setting degassing power to be 5.5kW, degassing for 2 times, purging time to be 20s, degassing time to be 15s, cooling time to be 5s, analysis delay to be 60s, shortest analysis time of oxygen, nitrogen and hydrogen to be 220-240 s, oxygen integration delay to be 5s and comparator level to be 1%; nitrogen integration delay 15s, comparator level 1%; the hydrogen integration is delayed by 10s and the comparator level is 20%.
Preferably, the specific steps of step (3) are as follows:
(3-1) selecting the analysis method established in the step (2), carrying out blank analysis on the high-temperature crucible, the graphite powder, the tin and the copper scraps for 3-5 times, and then carrying out blank deduction operation, wherein the consumption of the graphite powder is 0.02-0.03 g, the consumption of the tin sheet is 0.5g and the consumption of the copper scraps is 0.45-0.55 g each time;
(3-2) A single calibration of oxygen content was performed using LECO standard 502-874 (O content 0.0366% in 1g standard).
Preferably, the specific steps of step (4) are as follows:
(4-1) preparation of sample: crushing and grinding an aluminum nitride ceramic block containing 3% of a sintering aid, sieving to obtain powder with the particle size of less than or equal to 75 mu m, respectively weighing a sieved sample, graphite powder, copper scraps and tin flakes, and accurately weighing the sieved sample, the graphite powder, the copper scraps and the tin flakes to 0.0001g, wherein the mass ratio of the sieved sample to the graphite powder is 1 (0.8-1.2), the mass ratio of the sieved sample to the total mass of the tin flakes and the copper scraps is 1 (30-50), and the mass ratio of the tin flakes to the copper scraps is 1 (0.9-1.1).
(4-2) sample analysis: and (3) the sample number prepared in the step (4-1) is input, the sample number and the quality are input, the analysis method established in the step (2) is selected for analysis operation, the sample, the bath material and the graphite powder are placed in a crucible after the crucible is degassed, and the placing sequence is as follows: sample-graphite powder-tin flakes-copper flakes. After adding the graphite powder, shaking the crucible to completely cover the sample by the graphite powder; and horizontally placing the tin sheet, so that the graphite powder is below the tin sheet as much as possible, and the copper scraps are above the tin sheet. After the crucible is filled, the crucible is placed on a lower electrode, the lower electrode is closed, and analysis is started until the analysis is completed, so that an analysis result is obtained.
(4-3) data processing: checking the oxygen content of each section in a peak-splitting mode, deducting blanks from surface oxygen and crystal boundary oxygen, and calculating the crystal lattice oxygen content according to the intensity proportion of the crystal lattice oxygen.
The beneficial technical effects of the invention are as follows:
the aluminum nitride ceramic material becomes a widely used electronic device packaging material due to high thermal conductivity, the oxygen content of the aluminum nitride crystal lattice has very important influence on the thermal conductivity of the aluminum nitride crystal lattice, and the oxygen content of the aluminum nitride crystal lattice is accurately measured by using an inert melting-infrared absorption method. The oxygen content in the aluminum nitride crystal lattice is accurately determined by selecting a proper crucible, an additive and bath materials and setting reasonable analysis parameters. The method is simple to operate and easy to master, can effectively distinguish and measure the lattice oxygen and other oxygen contents, and provides reliable guarantee for the quality control of the production, scientific research and application of the high-performance aluminum nitride ceramic.
Drawings
FIG. 1 is an analysis chart of the oxygen content of sample 1 measured by an oxygen-nitrogen-hydrogen analyzer in example 1 of the present invention.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In addition, for numerical ranges in the present disclosure, it is understood that each intervening value, to the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including but not limited to.
The particle size of the graphite powder used in the embodiment of the invention is 20-50 μm; the used tin and copper bath material is a tin sheet with the thickness of 0.5mm and copper scraps with the diameter of 0.2mm and the length of 1 mm.
Example 1
4 kinds of aluminum nitride ceramic block samples which are self-made in a certain laboratory are respectively numbered as a sample 1, a sample 2, a sample 3 and a sample 4, and then oxygen content is measured, and the method comprises the following steps:
(1) Preparing an instrument:
the instrument is a TCH600 oxygen-nitrogen-hydrogen analyzer of LECO company in America, and the lower electrode is a high-temperature electrode slice; before analysis, the instrument is preheated and carrier gas is introduced to make the temperature of the inlet catalyst and the inlet purifying agent reach 650 ℃, and oxygen content analysis is carried out after 3.5 hours of gas introduction. The carrier gas is high-purity helium, the working pressure of the carrier gas is 20psi, and the ventilation flow is 450 mL/min; the power gas is high-purity nitrogen, and the working pressure of the power gas is 40 psi; a high-purity high-temperature graphite crucible is prepared, the crucible type 'high temperature 782 and 720' is selected under the software 'system-furnace', and other parameters are in a default state.
(2) Establishment of an analysis method:
selecting a manual analysis mode, and delaying the analysis for 60 s; the furnace adopts a power control mode, the degassing power is 5.5kW, 2 times of degassing are carried out, the purging time is 20s, the degassing time is 15s, and the cooling time is 5 s; the analysis process adopts a step-by-step heating mode: the power of the first stage is 1.5kW and stays for 60s, the power of the second stage is 2.5kW and stays for 120s, and the power of the third stage is 4.8kW and stays for 60 s; the shortest analysis time of oxygen, nitrogen and hydrogen is 240s, the oxygen integration delay is 5s, and the comparator level is 1%; nitrogen integration delay 15s, comparator level 1%; the hydrogen integration is delayed by 10s and the comparator level is 20%.
(3) Air and water calibration
Performing blank analysis on the crucible, the graphite powder, the tin sheet and the copper scraps for 3 times by selecting the analysis method set in the step (2), and performing blank deduction operation; a single standard calibration of oxygen content was performed with LECO standard 502-874 (O content 0.0366% in 1g standard).
(4) Analyzing the sample:
crushing and grinding an aluminum nitride ceramic block sample containing 3% of sintering aid (yttrium pentoxide), and sieving the crushed and ground sample through a 200-mesh sieve to obtain powder with the particle size of less than or equal to 75 mu m. The additives, bath agents and samples were weighed with an electronic balance to the nearest 0.0001 g. 0.025g of sample, 0.025g of graphite powder, 0.5g of tin sheet and 0.5g of copper scraps are weighed and recorded and numbered. And (3) inputting the sample number and quality on a software analysis interface, and selecting the analysis method established in the step (2) for analysis operation. Placing the sample, the bath material and the graphite powder into a crucible after degassing the crucible, wherein the placing sequence is as follows: sample-graphite powder-tin flakes-copper flakes. After adding the graphite powder, shaking the crucible to completely cover the sample by the graphite powder; and horizontally placing the tin sheet, so that the graphite powder is below the tin sheet as much as possible, and the copper scraps are above the tin sheet. And in the analysis process, operation is carried out according to the prompt of the left lower foot of the computer screen until the analysis is finished. Checking the oxygen content of each section in a peak-splitting mode, deducting blanks from surface oxygen and crystal boundary oxygen, and calculating the crystal lattice oxygen content according to the intensity proportion of the crystal lattice oxygen. Each sample is subjected to 3 times of parallel analysis, and the average value of the lattice oxygen obtained by the 3 times of analysis is the final measured value; FIG. 1 is an oxygen content analysis chart of the 1 st analysis of sample 1 in example 1, and the results of the lattice oxygen measurement of 4 groups of aluminum nitride ceramic bulk samples are shown in Table 1.
TABLE 1
| Sample numbering | Oxygen content of crystal lattice% |
| Sample No. 1 | 0.1469 |
| Sample No. 2 | 0.0671 |
| Sample No. 3 | 0.0341 |
| Sample No. 4 | 0.0379 |
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (6)
1. A method for measuring the oxygen content of aluminum nitride crystal lattices is characterized by comprising the following steps: adding an aluminum nitride sample containing a sintering aid, graphite powder and a tin-copper binary bath material into a high-temperature resistant container, heating a mixture in the high-temperature resistant container in a segmented heating mode, determining oxygen released by the aluminum nitride sample in a segmented manner by using an infrared absorption spectroscopy, checking the oxygen content of each segment in a peak splitting manner, deducting blanks from surface oxygen and crystal boundary oxygen, and calculating the crystal lattice oxygen content according to the intensity proportion of the crystal lattice oxygen;
the aluminum nitride sample containing the sintering aid, the graphite powder and the tin-copper binary bath material are sequentially added into the furnace body in sequence.
2. The method for determining the oxygen content in the aluminum nitride crystal lattice according to claim 1, wherein the mass ratio of the aluminum nitride sample containing the sintering aid to the graphite powder is 1 (0.8-1.2); the mass ratio of the aluminum nitride sample containing the sintering aid to the tin-copper binary bath material is 1 (30-50), wherein the mass ratio of tin to copper is 1 (0.9-1.1).
3. The method for determining the oxygen content in the aluminum nitride crystal lattice according to claim 1, wherein the particle size of the aluminum nitride sample containing the sintering aid is 75 μm or less.
4. The method for determining the oxygen content of an aluminum nitride crystal lattice according to claim 1, wherein the high temperature resistant container is a high temperature graphite crucible.
5. The method for determining the oxygen content in the aluminum nitride crystal lattice according to claim 1, wherein the specific parameters of the segmented temperature rise mode are as follows: the first stage is as follows: staying for 40-60 s under the power of 1.4-1.6 kW; and a second stage: staying for 100-120 s under the power of 2.4-2.6 kW; and a third stage: the power is 4.5-5.0 kW, and the mixture stays for 60-70 s.
6. The method for determining the oxygen content in the aluminum nitride crystal lattice according to claim 1, wherein the oxygen released by the aluminum nitride sample in sections is sequentially carried by an inert carrier gas into an infrared absorption spectrum detector for detection.
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| US4429047A (en) * | 1981-08-28 | 1984-01-31 | Rca Corporation | Method for determining oxygen content in semiconductor material |
| JP2827703B2 (en) * | 1992-05-19 | 1998-11-25 | 信越半導体株式会社 | Method and apparatus for measuring interstitial oxygen concentration in silicon single crystal |
| JPH0749305A (en) * | 1993-08-04 | 1995-02-21 | Komatsu Electron Metals Co Ltd | Apparatus and method for measuring interstitial oxygen concentration in silicon single crystal |
| CN104034664A (en) * | 2014-05-30 | 2014-09-10 | 中国船舶重工集团公司第七二五研究所 | Method for determining oxygen content of flux-cored wire powder and soldering flux |
| CN104764695A (en) * | 2015-03-26 | 2015-07-08 | 中国船舶重工集团公司第七二五研究所 | Method for determining oxygen/nitrogen/hydrogen content in interalloy for titanium alloys |
| JP6717221B2 (en) * | 2017-02-13 | 2020-07-01 | 株式会社Sumco | Method for evaluating oxygen concentration in silicon crystal |
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