CN105510302A - Migration processing method of cubic boron nitride abrasive metal impurity and detection method - Google Patents
Migration processing method of cubic boron nitride abrasive metal impurity and detection method Download PDFInfo
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Abstract
The invention provides a migration processing method of cubic boron nitride abrasive metal impurity. The method is characterized in that hydrochloric acid, nitric acid, hydrofluoric acid and perchloric acid are combined and heated for dissolving the metal impurity on surface of a cubic boron nitride abrasive to obtain a metal impurity migration solution. According to the method, migration of the metal impurity of the cubic boron nitride abrasive can be carried out as soon as possible. The invention also provides a method for detecting the metal impurity of the cubic boron nitride abrasive. The method mainly employs a plasma emission spectrum method for detecting the metal impurity migration solution prepared by the above method. The employed migration processing method can reduce viscosity of the used solution, and reduces damage on digestion equipment during a detection process.
Description
Technical field
The invention belongs to superhard material field, particularly relate to a kind of emigration processing method and detection method of cubic boron nitride abrasive materials metallic impurity.
Background technology
The hardness of cubic boron nitride abrasive materials is high, and chemical stability is good.Existing synthetic technology will use complicated metal alloy system as catalyst, and the parcel catalyst inevitably made in cubic boron nitride abrasive materials more or less remains by this, and to the bonding properties of itself and bonding agent, thermal stability etc. can produce considerable influence.The purification in later stage, the steps such as cleaning all can have an impact to the purity of product.Thus the assessment of impurity analysis to material quality and production technology of superhard material cubic boron nitride has very important significance.
Mainly utilize the digesting equipment such as autoclave, Hyperfrequency waves eliminating stove to remove the metallic impurity of cubic boron nitride in prior art, but obtain to clear up effect all undesirable.This is mainly because the content of the metallic impurity on highly purified cubic boron nitride abrasive materials surface is inherently in trace rank, adopt traditional sour Acid system then will commonly use the not easily volatile acid such as phosphoric acid, sulfuric acid, because the viscosity ratio of such acid is comparatively large, boiling point is higher, burden can be caused heavier to digesting equipment.So, for cubic boron nitride abrasive materials this kind of material, also do not have at present effectively to melt method, need development research.
Summary of the invention
In view of this, necessary emigration processing method and the detection method that a kind of cubic boron nitride abrasive materials metallic impurity are provided of the present invention, can by the migration possible as early as possible of cubic boron nitride abrasive materials metallic impurity, and the emigration processing method adopted can reduce the viscosity of used solution, reduce in testing process the damage that digesting equipment causes.
For this reason, technical scheme provided by the invention mainly first utilizes the dissolubility of metallic impurity in acid, by low viscosity, proportion is little, surface tension is little, residual less, the easily acid mixture system cubic boron nitride abrasive material that transfer is complicated carries out acid treatment, dissolve soluble metal impurity and the part cubic boron nitride on cubic boron nitride abrasive materials surface, and leaching is in solution system, thus make the migration of metallic impurity on cubic boron nitride abrasive materials surface in solution system.Technical scheme provided by the invention also comprises further using plasma atomic emission spectrometry and carries out quantitative test to moving to the total metallic impurity of solution system.Technical scheme provided by the invention is specific as follows:
An emigration processing method for cubic boron nitride abrasive materials metallic impurity, it comprises: the metallic impurity on associating hydrochloric acid, nitric acid, hydrofluorite and perchloric acid heating for dissolving cubic boron nitride abrasive materials surface, obtain migration of metallic impurity liquid.
Based on above-mentioned, it comprises and first in described cubic boron nitride abrasive materials, adds described hydrochloric acid and described nitric acid, and 90 ~ 200 DEG C of heating for dissolving, obtained easy molten metallic solution; In described easy molten metallic solution, add described perchloric acid and described hydrofluorite, the silicide in cubic boron nitride abrasive materials described in 90 ~ 200 DEG C of heating for dissolving, form molten silicon solution; The temperature of described molten silicon solution is maintained 100 ~ 250 DEG C, and constant temperature is until described perchloric acid smoked to the greatest extent, cools, obtains indissoluble dirt solution; In described indissoluble dirt solution, add the solvable residue of described dissolving with hydrochloric acid, prepare described migration of metallic impurity liquid.
Based on above-mentioned, it comprises 0.2 ~ 5g cubic boron nitride abrasive materials is placed in teflon crucible, add high purity water to soak, then the concentrated hydrochloric acid of 1 ~ 10ml and the red fuming nitric acid (RFNA) of 1 ~ 10ml is added successively, at 90 ~ 200 DEG C of heated sealed 1 ~ 3h, then be cooled to room temperature, obtain described easy molten metallic solution; In described easy molten metallic solution, add the hydrofluorite that the perchloric acid of 1 ~ 10ml and 1 ~ 10ml massfraction are greater than 40%, 90 ~ 200 DEG C of heated sealed 1 ~ 3h, thus form described molten silicon solution; By the uncovered placement of described molten silicon solution, and be heated to 100 ~ 250 DEG C, constant temperature 1 ~ 3h, treat that perchloric acid smoked to the greatest extent, cooling, obtains indissoluble dirt solution; The concentrated hydrochloric acid adding 1 ~ 10ml in described indissoluble dirt solution dissolves solvable residue, prepares described migration of metallic impurity liquid.
Wherein, why concentrated hydrochloric acid, red fuming nitric acid (RFNA), hydrofluorite will seal in the process of heating is because they are all effumability acid solutions, heated sealed is conducive to ensureing cubic boron nitride abrasive materials and the duration of contact of acid, and the metallic impurity in cubic boron nitride abrasive materials can be made to dissolve fully completely.In the present invention, the mass percentage concentration of described concentrated hydrochloric acid is not less than 35%; The mass percentage concentration of described red fuming nitric acid (RFNA) is not less than 65%; Described perchloric acid is the pure level of top grade, and its mass percent is 70% ~ 72%.
Based on above-mentioned, described high-purity resistivity of water >=18.2M Ω cm.
Based on above-mentioned, described hydrochloric acid, described nitric acid, described hydrofluorite and described perchloric acid add the liquid-transfering gun got and all adopt plastics matter rifle head.
The present invention also provides a kind of detection method of cubic boron nitride abrasive materials metallic impurity, and it comprises:
Migration impurity adopts said method to process described cubic boron nitride abrasive materials, by cubic boron nitride abrasive materials migration of metallic impurity in solution, and obtained described migration of metallic impurity liquid;
Defects inspecting using plasma emission spectrometry detects analyzes described migration of metallic impurity liquid.
Based on above-mentioned, in the step of described defects inspecting, adopt inductive coupling plasma emission spectrograph to detect and analyze described migration of metallic impurity liquid, wherein, described inductive coupling plasma emission spectrograph adopts HF acid resistant device, and running parameter is: RF power 1000 ~ 1400W, secondary air speed 0.3 ~ 0.6L/min, nebulizer pressure 0.1 ~ 0.3Mpa, nebulizer flow 0.3 ~ 0.6L/min, pump speed 50 ~ 100rpm, pump 4 ~ 7s stabilization time and observed altitude 10.0 ~ 13.5mm.
The purity of above-mentioned cubic boron nitride abrasive materials is higher, impurities element own is all in trace rank, the emigration processing method associating nitric acid of cubic boron nitride abrasive materials metallic impurity provided by the invention, hydrochloric acid, hydrofluorite, perchloric acid processes, the dissolving power of increase system, not only can dissolve the metallic impurity that cubic boron nitride surface is soluble in acid, the silicide on cubic boron nitride surface can also be dissolved, organism and part cubic boron nitride, thus the metallic impurity on cubic boron nitride surface are farthest moved in solution, obtain placing for a long time and metastable migration of metallic impurity liquid, for the composition of subsequent detection metallic impurity and content ready, be conducive to the research that a series of chemical analysis aspect carried out by cubic boron nitride abrasive material, the cubic boron nitride abrasive materials that purity is higher can also be obtained.
Further, above-mentioned disposal route provided by the invention first adds hydrochloric acid and nitric acid carries out heating for dissolving process, add perchloric acid again and hydrofluorite carries out heating for dissolving process, finally add hydrochloric acid again, the trace metal impurity on cubic boron nitride abrasive materials surface can be impelled to dissolve as much as possible, peel off with cubic boron nitride.This is because: the volatility of hydrochloric acid and nitric acid is good, and the many trace elements in cubic boron nitride abrasive materials can be converted into the nitrate of high-dissolvability by the metal of the molten overwhelming majority of energy, and subsidiary ion ratio is less.HF can molten Si, and the hydrochloric acid of molten metal and nitric acid can be combined cubic boron nitride surface can be made farthest to be cleared up, and is farthest migrated in solution system by metallic impurity ion.Perchloric acid boiling point is higher than hydrochloric acid, and nitric acid and HF, low boiling acid is driven in higher boiling acid in heating process, especially avoids HF on the impact of sampling device.Add perchloric acid, also can clear up organism, avoid organism on the impact of measured value.Finally add hydrochloric acid, improve solution system acid, increase system dissolving power, dissolve solvable residue.
The detection method of cubic boron nitride abrasive materials metallic impurity provided by the invention, the acid mixture of the nitric acid adopted, hydrochloric acid, hydrofluorite and perchloric acid prepares migration of metallic impurity liquid, the viscosity ratio of the acid mixture of nitric acid, hydrochloric acid, hydrofluorite and perchloric acid compared with low, proportion is little, surface tension is little, residual few, damage can not be brought to checkout equipment, the H using viscosity ratio larger can be avoided
3pO
4and H
2sO
4, thus avoid damage detection device; In addition, because the metallic impurity on cubic boron nitride abrasive materials surface move in described migration of metallic impurity liquid as much as possible, exact composition and the content of metallic impurity can be obtained, be conducive to cubic boron nitride abrasive material and carry out various research.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
The embodiment of the present invention provides a kind of disposal route of cubic boron nitride migration of metallic impurity, the steps include: accurately to take cubic boron nitride testing sample about 0.2 ~ 5g in teflon crucible, soak with a small amount of high purity water, under being placed in fuming cupboard, add 1 ~ 10ml concentrated hydrochloric acid successively, with 1 ~ 10ml red fuming nitric acid (RFNA), be placed on electric hot plate, 90 ~ 200 DEG C of lid lid heating 1 ~ 3h.After being cooled to room temperature, add 1 ~ 10ml perchloric acid and 1 ~ 10ml hydrofluorite, lid lid, 90 ~ 200 DEG C of heating 1 ~ 3h.Then take off crucible cover, be warming up to 100 ~ 250 DEG C, keep temperature 1 ~ 3h, treat that described perchloric acid smoked to the greatest extent, takes off cooling.Add concentrated hydrochloric acid described in 1 ~ 10ml, dissolved metal ions, obtain migration of metallic impurity liquid.
The embodiment of the present invention also provides a kind of detection method of cubic boron nitride metallic impurity, and the migration of metallic impurity liquid that this detection method uses above-described embodiment to provide, as liquid sample to be measured, specifically comprises the following steps:
Sample blank liquid is done according to the method for the described migration of metallic impurity liquid of above-mentioned preparation.Then, leave standstill described migration of metallic impurity liquid and sample blank liquid respectively, pipette respective supernatant and transfer in corresponding volumetric flask, use dust technology constant volume, shake up, carry out mark, obtained sample liquid to be measured and blank liquid to be measured.
Adopt the tenor in inductive coupling plasma emission spectrograph (being called for short ICP ~ OES) working sample solution, concrete steps are: the mixed standard solution of compound concentration gradient, production standard curve.The concentration of first getting 0.5ml is the standard stock solution hybrid standard of 1000ppm (national non-ferrous metal and electronic material Institute of Analysis), is placed in 50ml volumetric flask, uses dust technology constant volume, obtain the hybrid standard of 10ppm.Mixed mark 0ml, 0.25ml, 0.5ml, 1.0ml and 2.5ml of getting 10ppm are more respectively placed in 50ml volumetric flask, with the dust technology constant volume of same concentrations, obtain the standard solution of 0ppm, 0.05ppm, 0.1ppm, 0.2ppm and 0.5ppm.Above-mentioned standard solution is imported in ICP ~ OES instrument, is entering atomizer forward slip value.The each element response be measured to according to known content and the inductive coupling plasma emission spectrograph of element each in standard solution draws the standard working curve of each element respectively, then the response of working sample solution and blank solution element, calculate the concentration value of blank solution element and the concentration value of sample solution element according to standard working curve, thus obtain the content of each metallic element in sample.
Wherein, selected sour kind will with mark liquid medium close to just drawing good actual value, the medium of standard stock solution used to be mass percentage concentration be 8% nitric acid and mass percentage concentration be the HF of 1%.Through dilution, the concentration gradient medium obtained and constant volume dust technology used are close to consistent.So, treat that test sample is consistent with standard solution media environment, ensure Matrix Match.
Described ICP ~ OES apparatus selection HF acid resistant device is as instrument hardware, and its running parameter is as described in Table 1:
The running parameter of table 1ICP ~ OES instrument
| RF power | Assisted gas flow velocity | Nebulizer pressure | Nebulizer flow | Pump speed | Pump stabilization time | Observed altitude | Flush time | Multiplicity |
| 1150 W | 0.5 L/min | 0.2 Mpa | 0.5 L/min | 50～100 rpm | 5 s | 12.0 mm | 40 s | 2 |
The selection of spectral line is as shown in table 2:
The spectral line of each metallic element of table 2
| Element | Al | Co | Fe | Li | Mg | Mn | Ni | Ta |
| Wavelength/nm | 396.152{85} | 228.616{447} | 238.204{141} | 670.784{50} | 279.553{120} | 257.610{131} | 231.604{445} | 240.063{140} |
With specific embodiment more, technical scheme provided by the invention will be further illustrated below.
Step 1. accurately takes testing sample 1#, 2#, 3#, 4#, 5#, 6# are about 0.5g in teflon crucible, soak, under being placed in fuming cupboard with a small amount of high purity water, draw 3ml top grade pure hydrochloric acid with liquid-transfering gun, the pure nitric acid of 2ml top grade adds crucible, is placed on electric hot plate, 115 DEG C of lid lid heating 1h.After being cooled to room temperature, add the pure perchloric acid of 2ml top grade and the pure hydrofluorite of 3ml top grade, lid lid, 115 DEG C of heating 2h.Then take off crucible cover, be warming up to 205 DEG C, keep temperature to be about 1h, treat that perchloric acid smoked to the greatest extent, takes off cooling.Add 2ml top grade pure hydrochloric acid, dissolved metal ions, obtain 6 kinds of migration of metallic impurity liquid.Sample blank is done according to identical method.Leave standstill, get supernatant with plastic dropper, transfer in plastics volumetric flask, with 2% dust technology constant volume, shake up, carry out mark, to be measured.
Step 2.ICP ~ OES working sample GOLD FROM PLATING SOLUTION belongs to content, the steps include:
The mixed standard solution of compound concentration gradient, production standard curve.The concentration of first getting 0.5ml is the standard stock solution hybrid standard of 1000ppm (national non-ferrous metal and electronic material Institute of Analysis), is placed in 50ml volumetric flask, with the dust technology constant volume of 2%, obtains the hybrid standard of 10ppm.Mixed mark 0ml, 0.25ml, 0.5ml, 1.0ml and 2.5ml of getting 10ppm are more respectively placed in 50ml volumetric flask, with 2% dust technology constant volume, obtain the standard solution of 0ppm, 0.05ppm, 0.1ppm, 0.2ppm and 0.5ppm.Above-mentioned standard solution is imported in ICP ~ OES instrument, the each element response be measured to according to known content and the inductive coupling plasma emission spectrograph of element each in standard solution draws the standard working curve of each element respectively, then the response of working sample solution and blank solution element, calculate the concentration value of blank solution element and the concentration value of sample solution element according to standard working curve, thus obtain the content of each metallic element in sample.
Following table be this method measurement result and with the contrasting of outer inspection result:
From upper table comparing result, the measured value of this method measured value and Wai Jian unit meets better.
Therefore, disposal route provided by the invention is easy to operation, completes the task of cubic boron nitride abrasive materials surface impurity migration at low cost; Above-mentioned Comparison between detecting methods provided by the invention is simple, is easy to operation, and the evaluation detecting numerical value cubic boron nitride material quality is significant.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or carry out equivalent replacement to portion of techniques feature; And not departing from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope of request of the present invention protection.
Claims (7)
1. an emigration processing method for cubic boron nitride abrasive materials metallic impurity, it comprises the metallic impurity on associating hydrochloric acid, nitric acid, hydrofluorite and perchloric acid heating for dissolving cubic boron nitride abrasive materials surface, obtains migration of metallic impurity liquid.
2. the emigration processing method of cubic boron nitride abrasive materials metallic impurity according to claim 1, it is characterized in that: it comprises and first in described cubic boron nitride abrasive materials, adds described hydrochloric acid and described nitric acid, and 90 ~ 200 DEG C of heating for dissolving, obtained easy molten metallic solution; In described easy molten metallic solution, add described perchloric acid and described hydrofluorite, the silicide in cubic boron nitride abrasive materials described in 90 ~ 200 DEG C of heating for dissolving, form molten silicon solution; The temperature of described molten silicon solution is maintained 100 ~ 250 DEG C, and constant temperature is until described perchloric acid smoked to the greatest extent, cools, obtains indissoluble dirt solution; In described indissoluble dirt solution, add the solvable residue of described dissolving with hydrochloric acid, prepare described migration of metallic impurity liquid.
3. the emigration processing method of cubic boron nitride abrasive materials metallic impurity according to claim 2, it is characterized in that: it comprises 0.2 ~ 5g cubic boron nitride abrasive materials is placed in teflon crucible, add high purity water to soak, then the concentrated hydrochloric acid of 1 ~ 10ml and the red fuming nitric acid (RFNA) of 1 ~ 10ml is added successively, at 90 ~ 200 DEG C of heated sealed 1 ~ 3h, then be cooled to room temperature, obtain described easy molten metallic solution; The massfraction adding 1 ~ 10ml in described easy molten metallic solution is perchloric acid and 1 ~ 10ml massfraction hydrofluorite of being greater than 40% of 70% ~ 72%, 90 ~ 200 DEG C of heated sealed 1 ~ 3h, thus forms described molten silicon solution; By the uncovered placement of described molten silicon solution, and be heated to 100 ~ 250 DEG C, constant temperature 1 ~ 3h, treat that perchloric acid smoked to the greatest extent, cooling, obtains indissoluble dirt solution; The concentrated hydrochloric acid adding 1 ~ 10ml in described indissoluble dirt solution dissolves solvable residue, prepares described migration of metallic impurity liquid.
4. the emigration processing method of cubic boron nitride abrasive materials metallic impurity according to claim 3, is characterized in that: described high-purity resistivity of water >=18.2M Ω cm.
5. the emigration processing method of the cubic boron nitride abrasive materials metallic impurity according to any one of Claims 1 to 4, is characterized in that: described hydrochloric acid, described nitric acid, described hydrofluorite and described perchloric acid add the liquid-transfering gun got and all adopt plastics matter rifle head.
6. a detection method for cubic boron nitride abrasive materials metallic impurity, it comprises:
Migration impurity adopts the emigration processing method of the cubic boron nitride abrasive materials metallic impurity described in any one of Claims 1 to 5 to obtain described migration of metallic impurity liquid;
Defects inspecting using plasma emission spectrometry detects analyzes described migration of metallic impurity liquid.
7. the detection method of cubic boron nitride abrasive materials metallic impurity according to claim 6, it is characterized in that: in the step of described defects inspecting, adopt inductive coupling plasma emission spectrograph to detect and analyze described migration of metallic impurity liquid, wherein, described inductive coupling plasma emission spectrograph adopts HF acid resistant device, running parameter is: RF power 1000 ~ 1400W, secondary air speed 0.3 ~ 0.6L/min, nebulizer pressure 0.1 ~ 0.3Mpa, nebulizer flow 0.3 ~ 0.6L/min, pump speed 50 ~ 100rpm, pump 4 ~ 7s stabilization time and observed altitude 10.0 ~ 13.5mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114427996A (en) * | 2020-09-25 | 2022-05-03 | 中国石油化工股份有限公司 | Method for dissolving rhodium in rhodium-containing waste liquid and application thereof |
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