CN105403442A - Dissolving method for component detection of nanometer zirconia - Google Patents
Dissolving method for component detection of nanometer zirconia Download PDFInfo
- Publication number
- CN105403442A CN105403442A CN201510866140.1A CN201510866140A CN105403442A CN 105403442 A CN105403442 A CN 105403442A CN 201510866140 A CN201510866140 A CN 201510866140A CN 105403442 A CN105403442 A CN 105403442A
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- CN
- China
- Prior art keywords
- nanometer
- nanometer zirconia
- dissolving method
- zirconia
- powder
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Classifications
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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
-
- 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
Abstract
The invention belongs to the field of analytical chemistry and particularly relates to a dissolving method for component detection of nanometer zirconia. Nanometer zirconia powder is a powder material which is prepared from Y2O3 and partially-stable ZrO2 nanometer granules through spray granulation and sintering and is suitable for plasma spray, and according to the crystal structure, the tetragonal phase is larger than or equal to 95%, and the monoclinic phase is smaller than or equal to 5% (the monoclinic phase cannot be detected by X rays). Compared with a common thermal barrier coating, nanometer zirconia as a novel thermal spray material has lower heat conductivity and is applied to aero-engines more and more widely. The components of the powder are complex, and existing related detection standards for testing are not available. The dissolving method of nanometer zirconia is provided for accurately detecting the components of a nanometer zirconia composite, and thus the industry physicochemical detection technology is enriched.
Description
Technical field
The invention belongs to analytical chemistry field, be specifically related to a kind of dissolving method detected for nano zircite component.
Background technology
Nano zirconium oxide powder is Y
2o
3partially stabilized ZrO
2the powder body material of the applicable plasma spraying that nano particle is obtained after mist projection granulating sintering, crystal structure is: Tetragonal>=95%, monoclinic phase≤5% (X ray can't detect monoclinic phase).Nano zircite, as Novel hot sprayed on material, compared with general thermal barrier coating, has lower temperature conductivity, more and more extensive in aeromotor application.This powder constitution is comparatively complicated, and does not have existing coherent detection standard to test.
Carrying out such sample processing method at present has two kinds: one to be process with the acid mixture of hydrofluoric acid containing in confined conditions, two is carry out high-temperature fusion with alkaline matters such as boric acid sodium salt, potassium pyrophosphates (sodium), the first molten sample loading mode has when analyzing for some single element fast, simple advantage, but when multicomponent is analyzed, there is the undissolvable defect of Partial Elements, and hydrofluorite is comparatively large to glass container and environmental pollution, need pay special attention to during use.Relative alkali fusion process will be simply many, as long as choosing is to flux, will carry out normal running and just can obtain dissolving complete, limpid bright solution.(Na is had with the basic solvent that alkaline matter carries out high-temperature fusion conventional
2cO
3, K
2cO
3, KOH, potassium pyrophosphate (sodium), borate) etc., flux at high temperature melting together with sample, sample is converted into can water-soluble or sour compound.
Whether completely sample dissolution is the basis that chemical analysis accurately detects, and the composition due to nano zircite is made up of multiple oxide, can not complete the dissolving of nano zirconium oxide powder material by the sample dissolution technology of routine.Classical zr element method of testing adopts mandelic acid gravimetric method, as in zircon ore concentrate in YB876-76 " zircon ore concentrate analytical approach ", the mensuration of zirconium dioxide (hafnium) adopts mandelic acid gravimetric method.And to zirconia in nano zircite, the detection of hafnia can not apply mechanically above-mentioned standard completely, reason is that in YB876-76 " zircon ore concentrate analytical approach ", zircon ore concentrate complicated is (mainly siliceous, the compositions such as calcium), at mensuration zirconia, a large amount of step is adopted to be separated during hafnia, and nano zircite composition is simpler, impurity composition is few, if adopt YB876-76 " zircon ore concentrate analytical approach " completely, not only can not dissolved samples (the method adopt NaOH molten sample) completely, and it is many owing to adding reagent, running program complexity also can impact test result.
Summary of the invention
Technical matters to be solved by this invention is: in order to accurately detect the component of nano zirconium oxide composite material, propose a kind of dissolving method of nano zircite.
Technical scheme of the present invention is: a kind of dissolving method detected for nano zircite component, get sal tartari, sodium carbonate and boric acid by weight 1:1:1 and form mixed flux, 1:15 gets nano zircite sample and mixed flux and is placed in platinum crucible in mass ratio, keep furnace temperature in 980 DEG C ± 10 DEG C calcination 30min, take off cooling, add the hydrochloric acid of 50% concentration, heating makes dry thing in platinum ware dissolve, and dilute with water.
The invention has the beneficial effects as follows: proposed dissolving method is determined to sodium rice zirconia composition, has filled up blank.To carrying out of compound substance ingredient analysis, enrich industry physico-chemical examination technique.
Embodiment
Detect zirconium dioxide and hafnium oxide
Take 0.2 gram of (accurately to 0.1mg) nano zircite sample in giving in the platinum crucible being first equipped with 2 grams of mixed fluxs, add 1 gram of mixed flux again, in 980 DEG C ± 10 DEG C calcination 30min, take off cooling, add the hydrochloric acid of 10mL50% concentration, heating makes dry thing in platinum ware dissolve, and moves in 250mL beaker with water, and rare to 100mL.Add 3 phenolphthalein solutions, drip ammoniacal liquor to solution and to redden look, excessive several, be heated to boil, take off.Filter with middling speed quantitative filter paper while hot, and with micro-ammonia of PH=8 water washing beaker hot in nature, then wash 5 times, precipitation is put back in former beaker together with filter paper, add 25mL hydrochloric acid, heating for dissolving precipitates and smashs filter paper to pieces, is diluted with water to 100mL, be heated to boil, take off, add 50mL mandelic acid solution, continue to be heated to boil, move in boiling water bath and be incubated 2h (if be not incubated in boiling water bath, then will place more than 20h).Filter, with acidic cleaning liquid washing precipitation 6 ~ 8 times with middling speed quantitative filter paper.Precipitation is placed on calcination in the porcelain crucible of constant weight together with filter paper, ashing, 900 DEG C ± 10 DEG C calcinations to constant weight, weighs.
In sample, zirconium dioxide, hafnium oxide resultant provide by following formula:
c％＝(m1-m2)÷mo×100
In formula: the content of zirconium dioxide and hafnium oxide in c%-sample;
The quality (g) of m1-precipitation and crucible
M1---the quality (g) of empty crucible;
The quality (g) of mo---sample.
Claims (1)
1. the dissolving method detected for nano zircite component, it is characterized in that: get sal tartari, sodium carbonate and boric acid by weight 1:1:1 and form mixed flux, 1:15 gets nano zircite sample and mixed flux and is placed in platinum crucible in mass ratio, keep furnace temperature in 980 DEG C ± 10 DEG C calcination 30min, take off cooling, add the hydrochloric acid of 50% concentration, heating makes dry thing in platinum ware dissolve, and dilute with water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510866140.1A CN105403442A (en) | 2015-12-01 | 2015-12-01 | Dissolving method for component detection of nanometer zirconia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510866140.1A CN105403442A (en) | 2015-12-01 | 2015-12-01 | Dissolving method for component detection of nanometer zirconia |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105403442A true CN105403442A (en) | 2016-03-16 |
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|---|---|---|---|
| CN201510866140.1A Pending CN105403442A (en) | 2015-12-01 | 2015-12-01 | Dissolving method for component detection of nanometer zirconia |
Country Status (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110441123A (en) * | 2019-08-13 | 2019-11-12 | 湖北大学 | A kind of zirconio material digestion procedure |
| CN106745023B (en) * | 2016-12-02 | 2021-07-02 | 河南理工大学 | Compound hafnium sodium borate luminescent crystal material, preparation method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011252710A (en) * | 2010-05-31 | 2011-12-15 | Tosoh Analysis And Research Center Co Ltd | Analyzing method of impurity in hardly soluble sample |
| CN102564834A (en) * | 2011-12-19 | 2012-07-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Digestion method of metallurgical materials and detection method |
| EP2031365A4 (en) * | 2006-05-26 | 2012-12-05 | Jx Nippon Mining & Metals Corp | Zirconium crucible for analytical sample melting, method of preparing analytical sample and method of analysis |
| CN103091155A (en) * | 2013-01-10 | 2013-05-08 | 成都光明光电股份有限公司 | Method for dissolving high purity zirconia |
-
2015
- 2015-12-01 CN CN201510866140.1A patent/CN105403442A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2031365A4 (en) * | 2006-05-26 | 2012-12-05 | Jx Nippon Mining & Metals Corp | Zirconium crucible for analytical sample melting, method of preparing analytical sample and method of analysis |
| JP2011252710A (en) * | 2010-05-31 | 2011-12-15 | Tosoh Analysis And Research Center Co Ltd | Analyzing method of impurity in hardly soluble sample |
| CN102564834A (en) * | 2011-12-19 | 2012-07-11 | 攀钢集团攀枝花钢铁研究院有限公司 | Digestion method of metallurgical materials and detection method |
| CN103091155A (en) * | 2013-01-10 | 2013-05-08 | 成都光明光电股份有限公司 | Method for dissolving high purity zirconia |
Non-Patent Citations (1)
| Title |
|---|
| 梁献雷 等: "电感耦合等离子体原子发射光谱法测定高铬质耐火材料中次量及微量成分", 《分析试验室》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745023B (en) * | 2016-12-02 | 2021-07-02 | 河南理工大学 | Compound hafnium sodium borate luminescent crystal material, preparation method and application |
| CN110441123A (en) * | 2019-08-13 | 2019-11-12 | 湖北大学 | A kind of zirconio material digestion procedure |
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Application publication date: 20160316 |