CN108279146A - A kind of pre-treating method for zinc oxide-based ceramic composition test - Google Patents
A kind of pre-treating method for zinc oxide-based ceramic composition test Download PDFInfo
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- CN108279146A CN108279146A CN201810087189.0A CN201810087189A CN108279146A CN 108279146 A CN108279146 A CN 108279146A CN 201810087189 A CN201810087189 A CN 201810087189A CN 108279146 A CN108279146 A CN 108279146A
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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
- G01N1/34—Purifying; Cleaning
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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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Abstract
The invention discloses a kind of standardization pre-treating methods for zinc oxide-based ceramic composition test, including study cleaning, polishing, secondary cleaning, six procedure of drying, crushing and alkali soluble, in specific every procedure, the component for clearly limiting ceramics, the composition for removing dirty solvent, dosage, time, the size and quality of study, polishing and abrasive media, the granularity of crushing, aqueous slkali concrete component matches and concentration, realizes standardization and the high efficiency of pre-treatment, improves the precision of test.
Description
Technical field
The invention belongs to material analysis technical field of measurement and test, and zinc oxide-based ceramic composition test is used for more particularly, to one kind
Pre-treating method.
Background technology
Zinc oxide ceramics is using zinc oxide as a kind of semiconductive ceramic material made of principal crystalline phase addition dopant appropriate etc.
Material.With excellent nonlinear factor, pressure sensitive voltage range wide (zero a few volt to tens kilovolts), voltage temperature coefficient it is small, when
Between respond the features such as fast, leakage current is small.Primary raw material is zinc oxide, and dopant has bismuth oxide, cobalt oxide, strontium oxide strontia, titanium oxide
Deng.It is manufactured using general electronic ceramic process.It can be used for manufacturing voltage stabilizing element and overvoltage protection element in high-tension circuit (such as to collect
At the low-voltage piezoresistor in circuit), it can be also used as arrester.
Transparent conductive film be it is a kind of can a kind of conductive film with high transparency rate in visible-range again, mainly
There are metal membrane system, oxide membrane system, other compound membrane systems, macromolecule membrane system, compound film system etc..Metal membrane system electric conductivity
It is good, but transparent rate is poor.Transparent conductive film is mainly used for the window material of photoelectric device (such as LED, thin-film solar cells etc.)
Material.Doping zinc-oxide ceramics are a kind of important transparent conductive films, their energy gap is big, only absorb ultraviolet light, do not inhale
Visible light is received, therefore is referred to as " transparent ".Common doping zinc-oxide base ceramics include Al, Ga, In, Cr, Ti, Sn, Co etc. one
Kind or several doping, conductivity is 10-2Ω·cm-10-4Ω cm magnitudes, transmitance is generally in 65%-90%.
Preparing zinc oxide-based ceramic generally has dry and wet to be molded two classes.Dry-press process includes cold isostatic compaction, heat
Isostatic pressed, hot-forming etc., wet moulding include injection forming, injection moulding, note solidification forming etc..According to the difference of preparation process
The equipment used includes normal pressure-sintered stove, oxygen sintering furnace, vacuum sintering furnace, hot pressing furnace, hot isostatic pressing stove etc..
The composition test of zinc oxide ceramics includes principal component test (＜ 35%, doping component test) and impurity content test
(＜ 0.1%), according to different preparation processes, impurity component generally has the influences such as the beavy metal impurities such as Pb, Cd and Si, Fe electrical
The impurity of energy.Test method generally uses inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductive coupling etc.
Gas ions mass spectrography (ICP-MS) corresponds to precision about more than 50ppm and more than 1ppm respectively.However existing sample pre-treatment
There is the accurate measurement being difficult to realize to doped source and impurity content in method.
Invention content
In order to solve the above technical problems, being standardized to zinc oxide electronic ceramics sample the present invention provides a kind of
Method, realize to adulterate derived components and impurity content accurate measurement, be convenient for standardized management.
The complete technical solution of the present invention includes：
A kind of standardization pre-treating method for zinc oxide-based ceramic composition test, including study clean, polish, is secondary
Cleaning, drying, crushing and six procedure of alkali soluble, the specific practice per procedure include：
(1) Ga doping zinc-oxide ceramics studies are taken, using go dirty solvent to study carry out ultrasonic cleaning, the decontamination
The concrete component of solvent is ethyl alcohol：Acetone：Go to stain oil=6:2:1.5, above group is divided into volume ratio；Study with go making for dirty solvent
With than for 50g studies：It is 2 minutes that 350ml, which removes dirty solvent, ultrasonic cleaning time,；
(2) after the study drying that cleaning finishes, it is (10-15) mm* (10-15) mm* to be handled study using SiC sand paper
The quality of the cube rule sample of (10-15) mm, each sample is 4-15g；
(3) obtained each sample after polishing carries out ultrasonic cleaning using what 100ml removed dirty solvent to study, described
It is ethyl alcohol to go the concrete component of dirty solvent：Acetone：Go to stain oil=6:2:1.5, above group is divided into volume ratio；The ultrasonic cleaning time
It is 3 minutes；
(4) sample that cleaning finishes is dried 2 hours in air dry oven or vacuum drying chamber at 80 DEG C；
(5) drying finishes sample and is crushed 0.5-2 hours in tungsten carbide mortar, is repeatedly sieved, and final size reaches 40-
80 mesh；
(6) broken powder is completely dissolved using the mixed solution of a concentration of 2mol/L, the mixed solution is by hydroxide
Potassium, sodium peroxide, lithium metaborate, lithium tetraborate composition, the concentration of four kinds of components is 2mol/L, and specific dosage is hydroxide
Potassium：Sodium peroxide：Lithium metaborate：Lithium tetraborate=1.5：2：1:1, above is volume ratio, and it is small that 0.5-2 is dissolved under ultrasonic wave
When, obtain the clear transparent solutions for the ICP tests that can be used for zinc oxide electronic ceramics.
The present invention compared with the existing technology the advantages of be：
1. compared with the existing technology, it is proposed that before a kind of standardization tested specific to zinc oxide electronic ceramics
Reason method realizes standardization and the height of cleaning by the component for clearly limiting ceramics, the composition for removing dirty solvent, dosage, time
Effectization makes dirty solvent be utilized to greatest extent, is both fully cleaned to sample, in turn avoids the excessive use of solvent, makes
At wasting and pollute the environment.
2. the specified in more detail size and quality of study, facilitates and clean in next step and broken standardization.
3. being directed to zinc oxide electronic ceramics, specifically define that most suitable polishing and abrasive media, hardness make enough
Polishing and grinding process are completed in short period, and is avoided that and is mixed into impurity, cause measurement result inaccurate.
4. defining the granularity of crushing in detail, coordinates subsequent aqueous slkali concrete component proportioning and concentration, make sample powder
It can fully dissolve at the appointed time, improve dissolved efficiency.
Description of the drawings
Fig. 1 is the flow diagram of published method of the present invention.
Specific implementation mode
The present invention will be further described with reference to the accompanying drawings and detailed description.
As shown in Figure 1, the invention discloses a kind of standardization pre-treating method for zinc oxide-based ceramic composition test,
Including study cleaning, polishing, secondary cleaning, six procedure of drying, crushing and alkali soluble, the specific practice per procedure includes：
(1) Ga doping zinc-oxide ceramics studies are taken, using go dirty solvent to study carry out ultrasonic cleaning, the decontamination
The concrete component of solvent is ethyl alcohol：Acetone：Go to stain oil=6:2:1.5, above group is divided into volume ratio；Study with go making for dirty solvent
With than for 50g studies：It is 2 minutes that 350ml, which removes dirty solvent, ultrasonic cleaning time,；
(2) after the study drying that cleaning finishes, the cube for the use of SiC sand paper being 10mm*10mm*10mm by study processing
The quality of regular sample, each sample is 5.6g；
(3) obtained each sample after polishing carries out ultrasonic cleaning using what 100ml removed dirty solvent to study, described
It is ethyl alcohol to go the concrete component of dirty solvent：Acetone：Go to stain oil=6:2:1.5, above group is divided into volume ratio；The ultrasonic cleaning time
It is 3 minutes；
(4) sample that cleaning finishes is dried 2 hours in air dry oven or vacuum drying chamber at 80 DEG C；
(5) drying finishes sample and is crushed 1 hour in tungsten carbide mortar, and granularity reaches 60 mesh；
(6) broken powder is completely dissolved using the mixed solution of a concentration of 2mol/L, the mixed solution is by hydroxide
Potassium, sodium peroxide, lithium metaborate, lithium tetraborate composition, the concentration of four kinds of components is 2mol/L, and specific dosage is hydroxide
Potassium：Sodium peroxide：Lithium metaborate：Lithium tetraborate=1.5：2：1:1, above is volume ratio, dissolves 1 hour, obtains under ultrasonic wave
The clear transparent solutions tested to the ICP that can be used for zinc oxide electronic ceramics.
Meanwhile the preparation method of Ga doping zinc-oxides ceramics is in step (1)：
The material powder of corrresponding quality is weighed with numerical digit electronic balance, and is mixed to get composite granule, in the composite granule
Including ZnO powders and doped source, the mass fraction of ZnO powders is 72% in the mixed powder, and doped source mass fraction is
28%, the doped source component is according to molar ratio computing2O3:Ga2O3:MgO:TiO2:ZrO2:Bi2O3=1.2:1.5:0.8:
1.2:0.3；
Above-mentioned composite granule purity is 99.99% or more, 0.8 μm of composite granule average grain diameter, and D50 grain sizes are 0.5 μm；
By pure water, polyacrylic acid, N-N ' bismethacrylamides with 100：3.5：1.2 weight ratio fully dissolving group
At premixed liquid.
The JA-281 of noresidue after the sintering of 0.05wt% is done into dispersant, premixed liquid is added.
The composite granule of 50wt% is added in premixed liquid and is placed in ball milling 30 minutes in ball mill, it then again will be remaining multiple
It closes powder and is put into ball mill and continue ball milling 40 hours, slurry does ball-milling medium with zirconia ball in the ball mill.It is prepared by ball milling
Go out the slurry that powder volume content is 55%, i.e., the solid concentration 55% of material powder in slurry adjusts slurry with pure ammonium hydroxide
PH value obtains the high fluidity slurry that viscosity is 60-65mPas or so to 9.5.The n-octyl alcohol for adding 0.3wt% is organic de-
‰ ammonium persulfate initiator of infusion and 0.1wt, negative pressure stirring degassing 15 minutes, are poured into mold in running gate system.
The mold equipped with slurry is put into 50 DEG C of air -ovens after casting mold, heating promotes gel monomers crosslinking curing.
Wet green body demoulding, 30 hours dry under 65 DEG C and 80% damp condition after solidification, to obtain the flawless oxidation of high intensity
Zinc biscuit of ceramics.
Biscuit is heated in ventilating air stove and carries out degumming, furnace temperature is risen to 300 DEG C first, heating rate is not higher than 1
DEG C/min, and keep the temperature and be not less than 2 hours, be then warming up to 650 DEG C, and keep the temperature and be not less than 5 hours, heating rate not higher than 1 DEG C/
min.It cools to room temperature with the furnace, obtains the blank after degumming.
Blank after degumming is positioned in ventilating air stove and is sintered, furnace temperature is risen to 800 DEG C first, heating rate
It not higher than 1 DEG C/min, and keeps the temperature and is not less than 2 hours, be then warming up to 1020 DEG C, and keep the temperature and be not less than 5 hours, heating rate is not
Higher than 1 DEG C/min.It cools to room temperature with the furnace, sintered body is polished, produce zinc oxide voltage stabilizing original paper.It is opposite with drainage actual measurement
Density is 98.7%, and it is 2 × 10 to cut sample and survey ceramic body resistivity-3Ω cm, microstructure is uniform, and there is no vacuum-sinterings to be led
The ceramic oxygen lack problem of cause.
In another preferred embodiment, running gate system of the invention further includes gel casting forming mold, institute
The mold stated includes inner core, and external mold, mold chassis fastens external mold bolt, fastens inner core bolt, external mold sealing ring, inner core sealing
Circle, bottom eject percussion hammer, filter screen, filter screen handle.External mold is placed on mold chassis, there is external mold sealing ring on contact surface,
External mold is fixed with chassis by fastening bolt, ensures no leakage.Inner core is inserted in mold center chassis, there is inner core sealing on contact surface
Circle, inner core are fixed with chassis by fastening bolt, ensure no leakage.The inner wall of external mold, the outer wall of inner core and mold chassis with
The space that its non-intersection is formed injects aqueous slurries in die cavity as die cavity, forms earthenware green compact.It generally can also be
Handle is designed on external mold, is carried convenient for mold.Core designs are hollow structure, and interior design handle further decreases weight, just
In operations such as core pullings.There is screw thread on bottom percussion hammer surface, is rotatably mounted on mold chassis, is used for the ejection of inner core.Filter screen
In use, investing the outer wall of external mold and inner core, manual or motor drives filter screen handle to propose to starch by filter screen after casting complete
Material.Especially, during filter screen is lifted out slurry, the speed of lifting is determined by following formula：
In formula, V is pull rate, and a is speed correction factor, and value range 5-20, H are filter screen during lifting
The ratio of place height and mold height, value range 0<H<1, X is solid rate, value range 10<X<90, b be solid phase
Rate modified index, value range 0-2, ν are the viscosity of slurry, and unit mPas, c are viscosity modified index, value range
For 0-2.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention, every according to the present invention
Technical spirit changes any simple modification, change and equivalent structure made by above example, still falls within skill of the present invention
In the protection domain of art scheme.
Claims (8)
1. a kind of standardization pre-treating method for zinc oxide-based ceramic composition test, which is characterized in that cleaned including study,
Polishing, secondary cleaning, six procedure of drying, crushing and alkali soluble,
(1) zinc oxide electronic ceramics study is taken, using alcohol, acetone, stain oil is removed etc. and goes the one or more of dirty solvent to sample
Carry out routine or ultrasonic cleaning；
(2) after the study drying that cleaning finishes, diamond, silicon carbide, alundum wheel or sand paper or other abrasive medias are used
It is the regular shapes such as cube or cylinder by study processing；
(3) sample after polishing using alcohol, acetone, remove stain oil etc. and go dirty solvent it is one or more of to sample carry out it is conventional or
Ultrasonic cleaning；
(4) sample that cleaning finishes dries 0.5-5hr in air dry oven or vacuum drying chamber in 50-200 DEG C of range；
(5) drying finishes sample and is crushed in hard alloy mortar, and repeated multiple times, granularity reaches 40-80 mesh；
(6) sodium hydroxide of the concentration not less than 0.5mol/L, potassium hydroxide, sodium peroxide, sodium carbonate, lithium metaborate, four are used
Broken powder is completely dissolved by lithium borate or a variety of mixed solutions, is obtained clear transparent solutions and be can be used for zinc oxide electronic ceramics
ICP is tested.
2. standardization pre-treating method described in claim 1, which is characterized in that the zinc oxide ceramics is Ga doping oxidations
Zinc ceramics.
3. standardization pre-treating method described in claim 1, which is characterized in that in the step (1), remove the tool of dirty solvent
Body group is divided into ethyl alcohol：Acetone：Go to stain oil=6:2:1.5, above group is divided into volume ratio；Study is with the use ratio of dirty solvent is removed
50g studies：It is 2 minutes that 350ml, which removes dirty solvent, ultrasonic cleaning time,.
4. standardization pre-treating method described in claim 1, which is characterized in that in the step (2), use SiC sand paper
The quality of the cube rule sample for being (10-15) mm* (10-15) mm* (10-15) mm by study processing, each sample is 4-
15g。
5. standardization pre-treating method described in claim 1, which is characterized in that in the step (3), obtained after polishing
Each sample carries out ultrasonic cleaning using what 100ml removed dirty solvent to study, and the concrete component for removing dirty solvent is second
Alcohol：Acetone：Go to stain oil=6:2:1.5, above group is divided into volume ratio；The ultrasonic cleaning time is 3 minutes.
6. standardization pre-treating method described in claim 1, which is characterized in that in the step (4), clean the sample finished
Product are dried 2 hours in air dry oven or vacuum drying chamber at 80 DEG C.
7. standardization pre-treating method described in claim 1, which is characterized in that in the step (5), drying finishes sample
It crushes 0.5-2 hours in tungsten carbide mortar, is repeatedly sieved, final size reaches 40-80 mesh.
8. standardization pre-treating method described in claim 1, which is characterized in that in the step (6), use is a concentration of
Broken powder is completely dissolved by the mixed solution of 2mol/L, the mixed solution by potassium hydroxide, sodium peroxide, lithium metaborate,
Lithium tetraborate forms, and the concentration of four kinds of components is 2mol/L, and specific dosage is potassium hydroxide：Sodium peroxide：Lithium metaborate：Four
Lithium borate=1.5：2：1:1, it is above to obtain can be used for zinc oxide electronic ceramics 0.5-2 hours under ultrasonic wave for volume ratio
The clear transparent solutions of ICP tests.
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