CN110044763A - Method for detecting content of nitric acid insoluble substances in high-purity silver ingot - Google Patents
Method for detecting content of nitric acid insoluble substances in high-purity silver ingot Download PDFInfo
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- CN110044763A CN110044763A CN201910369497.7A CN201910369497A CN110044763A CN 110044763 A CN110044763 A CN 110044763A CN 201910369497 A CN201910369497 A CN 201910369497A CN 110044763 A CN110044763 A CN 110044763A
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- silver ingot
- nitric acid
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- purity silver
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 187
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 187
- 239000004332 silver Substances 0.000 title claims abstract description 187
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title abstract description 10
- 239000000126 substance Substances 0.000 title abstract description 5
- 238000001514 detection method Methods 0.000 claims abstract description 66
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 238000010309 melting process Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000007770 graphite material Substances 0.000 claims description 15
- 239000004575 stone Substances 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 15
- 239000002699 waste material Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract 1
- 238000005259 measurement Methods 0.000 description 13
- 238000012360 testing method Methods 0.000 description 7
- 238000005070 sampling Methods 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- 235000013399 edible fruits Nutrition 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 229910052745 lead Inorganic materials 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 239000012982 microporous membrane Substances 0.000 description 4
- 229910052711 selenium Inorganic materials 0.000 description 4
- 229910052714 tellurium Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000011978 dissolution method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010946 fine silver Substances 0.000 description 3
- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000009182 swimming Effects 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
- G01N15/0606—Investigating concentration of particle suspensions by collecting particles on a support
- G01N15/0618—Investigating concentration of particle suspensions by collecting particles on a support of the filter type
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G01N33/202—Constituents thereof
- G01N33/2028—Metallic constituents
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N2015/0042—Investigating dispersion of solids
- G01N2015/0061—Investigating dispersion of solids in solids, e.g. petrography
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Abstract
The application discloses a method for detecting the content of nitric acid insoluble substances in a high-purity silver ingot, belongs to the technical field of impurity detection, and solves the problems that the detection cost is high and the detection is inaccurate easily caused by the existing method for detecting the content of the nitric acid insoluble substances in the high-purity silver ingot, the mass percentage content of silver in the high-purity silver ingot is not less than 99.99 percent, and the detection method comprises the following steps: melting a high-purity silver ingot in a protective gas atmosphere, and moving the high-purity silver ingot intermittently in the melting process; cooling after the melting is finished to obtain a discharged silver ingot, wherein a foreign object area and a mirror surface bright area are formed on the upper surface of the discharged silver ingot; and determining the content of the nitric acid insoluble substances in the high-purity silver ingot according to the ratio of the area of the foreign material area to the mass of the high-purity silver ingot. The detection method is simple and convenient, and waste of silver ingots is prevented.
Description
Technical field
This application involves defects inspecting technical fields, and in particular to the detection of nitric acid insolubles content in a kind of high-purity silver ingot
Method.
Background technique
In GB/T 4135-2016 " silver ingot " national standard, by impurity content Cu, Pb, Fe, Sb, Se, Te, Bi, Pd in silver ingot
It is provided with impurity summation, silver ingot is divided into IC-Ag99.99, IC-Ag99.95 and IC-Ag99.90 further according to impurity summation
IC-Ag99.99 is known as high-purity silver ingot in the application by three trades mark.
But many enterprises are when buying high-purity silver ingot, just for these elements of Cu, Pb, Fe, Sb, Se, Te, Bi, Pd into
Row detection, comes into operation if detecting qualification, has ignored the defects inspecting in high-purity silver ingot insoluble in nitric acid.Further divide thus
Analysis dissolves high-purity silver ingot drill hole sampling using pure nitric acid is analyzed, and by silver nitrate solution filtering with microporous membrane, finds micropore
Occurs the foreign matter of grey or yellow on filter membrane.And as control, it is micro- after the pure nitric acid filtering with microporous membrane of the analysis of equivalent
Foreign matter is not found on the filter membrane of hole.In response to this, it can reason out in high-purity silver ingot there are nitric acid insoluble matter, influence high purity silver
The purity of ingot.Impurity summation in the high-purity silver ingot of IC-Ag99.99 is subtracted into Cu, Pb, Fe, Sb, Se, Te, Bi, Pd these impurity member
The content requirement of element, it can be deduced that nitric acid insoluble matter impurity content does not allow more than 0.0014%, and (14ppm, ppm are million points
Rate), if the content of nitric acid insoluble matter is more than 14ppm, impurity summation will be unsatisfactory for GB/T 4135-2016 " silver ingot " national standard
Requirement.
Since the Impurity Distribution in silver ingot is not visibly homogeneous, if drill hole sampling detection sampling is less, cannot accurately survey
Out in high-purity silver ingot nitric acid insoluble matter content, so that the requirement for whether meeting national standard to the impurity summation of high-purity silver ingot cannot be into
Row accurately judgement.If but the detection of the nitric acid insolubles content of high-purity silver ingot, be all high-purity silver ingot nitric acid with 5kg or more
The method of dissolution largely uses nitric acid it will cause detection process, while high-purity silver ingot can not put into again after being dissolved and make
With can make that testing cost is extremely high in this way.
There is no the detection method for nitric acid insolubles content, all kinds of texts in national standard GB/T 4135-2016 " silver ingot " at present
Offer in patent also without reference to.
Summary of the invention
The embodiment of the present application solves existing by providing a kind of detection method of nitric acid insolubles content in high-purity silver ingot
The problem of the detection method testing cost height of impurity and testing result inaccuracy in silver ingot, the detection method of the application it is simple,
While directly detecting nitric acid insolubles content in high-purity silver ingot, reduce the use of nitric acid, avoids the waste of silver ingot.
In order to achieve the above objectives, the application mainly provides the following technical solutions:
The embodiment of the present application provides a kind of detection method of nitric acid insolubles content in high-purity silver ingot, high-purity silver ingot
The mass percentage of middle silver is not less than 99.99%, and described detection method includes the following steps:
High-purity silver ingot is melted under protective gas atmosphere, in melting process by high-purity intermittent movement of silver ingot；
Cooling after melting to obtain silver ingot of coming out of the stove, the upper surface of the silver ingot of coming out of the stove forms foreign matter area and bright in mirror surface
Area；
Nitric acid insoluble matter in high-purity silver ingot is determined according to the ratio of the area in the foreign matter area and the quality of high-purity silver ingot
Content.
Preferably, the detection method further include: determine the high purity silver ingot shape of known nitric acid insolubles content at foreign matter
The area in area, known high-purity silver ingot quality and nitric acid insolubles content between linear relationship, further according to the linear pass
System determines the content of nitric acid insoluble matter in high-purity silver ingot to be measured.
Preferably, the silver ingot of coming out of the stove with a thickness of 13-15mm.
Preferably, determining high-purity silver ingot according to the area in the foreign matter area and the ratio of the area for silver ingot upper surface of coming out of the stove
The content of middle nitric acid insoluble matter.
Preferably, the upper surface of the silver ingot of coming out of the stove is rectangle.
Preferably, the melting temperature is 1000-1200 DEG C.
Preferably, the melting temperature is 1100 ± 10 DEG C.
Preferably, the melting time is 1-3h.
Preferably, the intermittent movement uses single traveling time for 20-40min, the mobile speed of single is 4-
6cm/min, single intermittent time are the mode of 20-40s.
Preferably, being melted in high temperature furnace for high-purity silver ingot carries out, the intermittent movement of high-purity silver ingot is
High-purity silver ingot is put into graphite material boat, is pushed to graphite material boat from high temperature furnace entrance is intermittent by the push rod in high temperature furnace
High temperature outlet of still.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
The embodiment of the present application by changing the conventional method for detecting silver ingot impurity with nitric acid dissolution method, do not need to silver ingot into
Row dissolution, it is only necessary to silver ingot be melted, can simply and intuitively determine that nitric acid insolubles content is in high-purity silver ingot detected
The no requirement for meeting national standard avoids the use of nitric acid, while the silver ingot of coming out of the stove after detection can come into operation again, solve
The excessively high problem of cost caused by nitric acid dissolution method, for drill hole sampling, the testing result of the application detection method more may be used
It leans on.Production phase due to whether meeting national standard to nitric acid insolubles content in high-purity silver ingot judges, does not need higher
Detection accuracy, it is only necessary to judge in high-purity silver ingot nitric acid insolubles content whether in 14ppm or less, the embodiment of the present application
Detection method only can quickly and intuitively judge that nitric acid is not in high-purity silver ingot by measurement area on the basis of silver ingot melts
Whether the content of molten object is qualified, reduces operating procedure, improves detection efficiency.
Detailed description of the invention
Fig. 1 is the measurement effect in foreign matter area and silver ingot upper surface area ratio of coming out of the stove in the detection method of one embodiment of the application
Figure；
Fig. 2 is that foreign matter area and the measurement for silver ingot upper surface area ratio of coming out of the stove are imitated in the detection method of the another embodiment of the application
Fruit figure；
Fig. 3 is that foreign matter area and the measurement for silver ingot upper surface area ratio of coming out of the stove are imitated in the detection method of the another embodiment of the application
Fruit figure；
Fig. 4 is that foreign matter area and the measurement for silver ingot upper surface area ratio of coming out of the stove are imitated in the detection method of the another embodiment of the application
Fruit figure；
Fig. 5 is that foreign matter area and the measurement for silver ingot upper surface area ratio of coming out of the stove are imitated in the detection method of the another embodiment of the application
Fruit figure；
Fig. 6 is that foreign matter area and the measurement for silver ingot upper surface area ratio of coming out of the stove are imitated in the detection method of the another embodiment of the application
Fruit figure.
Specific embodiment
Understanding for the ease of those skilled in the art to application scheme, combined with specific embodiments below to the application side
Case is further elaborated, it should be understood that the embodiment of the present application is the explanation to application scheme, not as to the application
The restriction of protection scope.
Applicant has found through lot of experiments, by the separately sampled 0.1kg of high-purity silver ingot that a block specifications are 30kg,
0.5kg, 1kg, 2kg, 4kg, 5kg, 6kg, 7kg, sampled deviation of weight are detected as follows respectively all within 10g: being used
Nitric acid sample dissolution, after filtering with microporous membrane silver nitrate solution, by miillpore filter impurity and filter membrane dry together, weigh
Weight difference before and after miillpore filter use determines the content of nitric acid insoluble matter impurity, and obtained data are as shown in table 1:
Table 1
Find out from above data, when sampling is in 5kg or more, detection data is relatively stable, can more accurately determine height
Nitric acid insolubles content in fine silver ingot can be more in conjunction with these Element detection data of Cu, Pb, Fe, Sb, Se, Te, Bi, Pd
Accurately determine whether the purity of high-purity silver ingot meets national standard.It is all to use if the detection of nitric acid insoluble matter in high-purity silver ingot
The method of high-purity silver ingot nitric acid dissolution of 5kg or more, it will cause detection process largely to use nitric acid, while high-purity silver ingot exists
It can not come into operation again after being dissolved, can make that testing cost is extremely high in this way.
Applicant it is also found that: high-purity silver ingot is sampled, is dissolved through research using nitric acid, after filtering with microporous membrane silver nitrate,
Nitric acid insoluble matter and filter membrane are dried, detected using scanning electron microscope, the main component of discovery nitric acid insoluble matter is aluminium oxide, oxidation
Silicon and tin oxide etc..
According to the property of above-mentioned impurity, the embodiment of the present application proposes nitric acid insolubles content in a set of high-purity silver ingot of measurement
Method, it is specific as follows:
The detection method of nitric acid insolubles content in a kind of high-purity silver ingot, wherein mass percentage silver-colored in high-purity silver ingot
Not less than 99.99%, detection method includes the following steps for this:
High-purity silver ingot is melted under protective gas atmosphere, in melting process by the intermittent movement of high-purity silver ingot；
Cooling obtains silver ingot of coming out of the stove after melting, and the upper surface of the silver ingot of coming out of the stove forms foreign matter area and specular light clear zone；
The content of nitric acid insoluble matter in high-purity silver ingot is determined according to the ratio of the area in foreign matter area and high-purity silver ingot quality.
To note here is that: since nitric acid insoluble matter fusing point is high, after high-purity silver ingot melts in high temperature furnace, silver-colored molten slurry is viscous
Degree reduces, so nitric acid insoluble matter floats under the action of wetability and density contrast.Simultaneously in melting process by high-purity silver ingot
Intermittent movement, under the effect of inertia of intermittent promotion and stopping, the nitric acid insoluble matter for swimming in silver-colored molten slurry surface is assembled
Collection is in side.At that same temperature, tension is substantially suitable everywhere on silver-colored molten slurry surface, so nitric acid insoluble matter is on silver-colored molten slurry surface
Extravagant thickness is also more uniform.When the solidification of silver-colored molten slurry, nitric acid insoluble matter thickness is more uniformly deposited on the upper of silver ingot of coming out of the stove
Surface, the upper surface for silver ingot of coming out of the stove form the specular light clear zone of free from admixture and the foreign matter area containing nitric acid insoluble matter.Due to containing
Have the thickness in the foreign matter area of nitric acid insoluble matter certain, thus formed foreign matter area area in high-purity silver ingot nitric acid insoluble matter it is exhausted
It is directly proportional to content, it thus can determine the high purity silver ingot shape of known nitric acid insolubles content at the area in foreign matter area, known high-purity
Linear relationship between the quality and nitric acid insolubles content of silver ingot, then according to the linear relationship, it is to be measured high-purity by measuring
Silver ingot forms the area in foreign matter area and the ratio of high-purity silver ingot quality to be measured, it may be determined that nitric acid insoluble matter in high-purity silver ingot to be measured
Content.The detection method of the embodiment of the present application does not need to dissolve silver ingot, it is only necessary to melt silver ingot, just can detect height
Whether nitric acid insolubles content meets the requirement of national standard in fine silver ingot；In addition, the embodiment of the present application nitre in carrying out high-purity silver ingot
When the detection of acid non-soluble substance, the use of nitric acid is avoided, while the silver ingot of coming out of the stove after detection can come into operation again, solve
The excessively high problem of cost caused by nitric acid dissolution method, for drill hole sampling, the testing result of the embodiment of the present application detection method
It is more accurate.
The accurate detection of the content of nitric acid insoluble matter in high-purity silver ingot has may be implemented in above scheme, and can reduce
The waste of silver ingot；Preferred embodiment is provided on the basis of herein below:
Preferably, above-mentioned silver ingot of coming out of the stove with a thickness of 13-15mm.It is detected using the detection method of the embodiment of the present application high
In fine silver ingot when the content of nitric acid insoluble matter, since the quality of high-purity silver ingot is different, nitric acid insoluble matter is absolute in high-purity silver ingot
Content is different, different in the area that silver ingot upper surface of coming out of the stove forms foreign matter area, it is understood that there may be silver ingot of coming out of the stove is completely covered in foreign matter area
The case where upper surface, so that the thickness of nitric acid insoluble matter is not able to maintain stabilization in foreign matter area, so that the embodiment of the present application
Detection method is not applicable.The application, can in conjunction with the application detection method according to the substantially content of nitric acid insoluble matter in high-purity silver ingot
The factors such as the range of detection have obtained the thickness range for silver ingot of coming out of the stove in the application detection method, when silver ingot of coming out of the stove with a thickness of
When 13-15mm, the upper surface for silver ingot of coming out of the stove exists simultaneously foreign matter area and specular light clear zone, and high-purity silver ingot of any quality can be adopted
With the content of the detection method detection nitric acid insoluble matter of the application.It is carried out in addition, high-purity silver ingot is generally placed into graphite material boat
High-temperature fusion can quickly calculate the surface area for silver ingot of coming out of the stove by the thickness for silver ingot of coming out of the stove and the quality for silver ingot of coming out of the stove, by
The size of graphite material boat needed for known to this improves detection efficiency and detection success rate so as to avoid duplicate detection operation.
It should be noted that this programme is come out of the stove, the thickness of silver ingot refers to the thickness that silver ingot is cylindrical body of coming out of the stove, and measures for convenience, at this
In some embodiments of application, silver ingot of coming out of the stove is cuboid or square, it is of course also possible to be other cylinders.
Preferably, determining high-purity silver ingot according to the area in above-mentioned foreign matter area and the ratio of the area for silver ingot upper surface of coming out of the stove
The content of middle nitric acid insoluble matter.In the present solution, when the thickness for silver ingot of coming out of the stove keeps a timing, the face in foreign matter area on silver ingot of coming out of the stove
Long-pending and the ratio between silver ingot upper surface area of coming out of the stove is directly proportional to the mass percentage of nitric acid insoluble matter in high-purity silver ingot, thus can be true
High-purity silver ingot of fixed known nitric acid insolubles content after melting, form the area in foreign matter area and come out of the stove silver ingot upper surface area it
Than the corresponding relationship of the mass percentage with nitric acid insoluble matter, then according to the corresponding relationship, by measuring high-purity silver ingot to be measured
Form the area in foreign matter area and the ratio between silver ingot upper surface area of coming out of the stove, it may be determined that nitric acid insoluble matter contains in high-purity silver ingot to be measured
Amount.
Applicant after having conducted extensive research and testing, obtained the application detection method measurement foreign matter area area and
The corresponding relationship of the content of nitric acid insoluble matter in the ratio and high-purity silver ingot of silver ingot upper surface area of coming out of the stove.
By taking nitric acid dissolves high-purity silver ingot of 5 ± 0.1kg as an example, high-purity silver ingot is obtained using filtering-drying-weighing method
The content of middle nitric acid insoluble matter, the application can determine containing for nitric acid insoluble matter in high-purity silver ingot more than 14ppm corresponding thereto
Measure unqualified, data are as shown in table 2:
Table 2.
Above-described embodiment does not need to dissolve silver ingot, it is only necessary to silver ingot melted, it is insoluble containing nitric acid by measurement
The area ratio in the foreign matter area of object and silver ingot upper surface of coming out of the stove, just can simply and intuitively determine in high-purity silver ingot detected
Whether nitric acid insolubles content meets the requirement of national standard；Due to being wanted to whether nitric acid insolubles content in high-purity silver ingot meets national standard
The judgement asked does not need higher detection accuracy, it is only necessary to judge in high-purity silver ingot nitric acid insolubles content whether 14ppm with
Lower, the detection method of the embodiment of the present application only can be quickly and intuitive by measurement area on the basis of silver ingot melts
Judge whether the content of nitric acid insoluble matter in high-purity silver ingot is qualified, reduces operating procedure, improves detection efficiency.
In some embodiments of the present application, the upper surface of above-mentioned silver ingot of coming out of the stove is rectangle.To note here is that: it comes out of the stove
When silver ingot upper surface is rectangle, measurement area ratio only needs measured length ratio, so that measuring simpler convenience, should manage
Solution, the embodiment of the present application is not especially limited the upper surface shape for silver ingot of coming out of the stove, as long as facilitating reference area ratio, at this
In some other embodiments of application, the shape for silver ingot of coming out of the stove can also be trapezoidal, round etc..
In some embodiments of the present application, the area ratio in the foreign matter area containing nitric acid insoluble matter and silver ingot upper surface of coming out of the stove
Measurement method be to measure foreign matter area and the length ratio of silver ingot of coming out of the stove.It should be appreciated that for the length for how measuring foreign matter area, this
Application is not especially limited, preferably, the measurement of length mode in foreign matter area is to pass through in some embodiments of the present application
The extreme length and shortest length in foreign matter area are measured, then is averaged to obtain the length in foreign matter area.
In some embodiments of the present application, the measurement of length mode in foreign matter area is the length measured at foreign matter area 5-10
Degree, then the length for taking its average value to obtain foreign matter area, director's 5-10 degree include the extreme length and shortest length in foreign matter area.This
Although the shape in it is noted that foreign matter area is irregular, from the melting of intermittent movement and the formation in foreign matter area
For principle, shape takes the average value of a few director's degree as its length close to rectangle, convenient and accurate.
In some embodiments of the present application, high-purity silver ingot melting temperature is 1000-1200 DEG C, and preferred molten temperature is
1100±10℃.Melting time is 1-3h.
In some embodiments of the present application, the intermittent movement of high-purity silver ingot uses single traveling time for 20-
40min, the mobile speed of single are 4-6cm/min, and the single intermittent time is the mode of 20-40s, i.e., high-purity silver ingot is with 4-6cm/
The every mobile 20-40min of the speed of min stops mobile 20-40s, then repeats to move.
In some embodiments of the present application, being melted in high temperature furnace for high-purity silver ingot is carried out, high-purity silver ingot it is intermittent
Mobile is that high-purity silver ingot is put into graphite material boat, by the push rod in high temperature furnace that graphite material boat is intermittent from high temperature furnace entrance
It is pushed to high temperature outlet of still.
In some embodiments of the present application, protective gas atmosphere when high-purity silver ingot melts is chemically inert guarantor
Gas is protected, the specific type of protective gas can be not especially limited for inert gases, the application such as nitrogen, helium.
Embodiment 1
(1) the high-purity silver ingot of 5 ± 0.1kg is fitted into graphite material boat；
(2) by equipped with high-purity silver ingot graphite material boat be put into 1100 DEG C and have nitrogen atmosphere protect high temperature furnace in, high temperature
The length of the effective warm area of furnace is 750cm；
(3) the graphite material boat equipped with high-purity silver ingot is elapsed to high temperature furnace by the push rod in high temperature furnace from high temperature furnace entrance
Mouthful, driving velocity 5cm/min, the every promotion 30min of push rod stop pushing 30s, then proceed to push forward；
(4) when reaching high temperature outlet of still, the appearance for silver ingot upper surface of coming out of the stove in graphite material boat is observed, is measured with ruler,
Such as Fig. 5, the total length for silver ingot of coming out of the stove is about 20cm, wherein the length in the foreign matter area containing nitric acid insoluble matter is about 10cm, is contained
The foreign matter area of nitric acid insoluble matter accounts for about the 50% of the gross area for silver ingot upper surface of coming out of the stove, can be sentenced by the corresponding relationship in table 2
The content of nitric acid insoluble matter is qualified in fixed high-purity silver ingot.
Embodiment 2
(1) the high-purity silver ingot of 5 ± 0.1kg is fitted into graphite material boat；
(2) by equipped with high-purity silver ingot graphite material boat be put into 1100 DEG C and have nitrogen atmosphere protect high temperature furnace in, high temperature
The length of the effective warm area of furnace is 750cm；
(3) the graphite material boat equipped with high-purity silver ingot is elapsed to high temperature furnace by the push rod in high temperature furnace from high temperature furnace entrance
Mouthful, driving velocity 5cm/min, the every promotion 30min of push rod stop pushing 30s, then proceed to push forward；
(4) when reaching high temperature outlet of still, the appearance for silver ingot upper surface of coming out of the stove in graphite material boat is observed, is measured with ruler,
Such as Fig. 6, the total length for silver ingot of coming out of the stove is about 20cm, wherein the length in the foreign matter area containing nitric acid insoluble matter is about 15cm, is contained
The foreign matter area of nitric acid insoluble matter accounts for about the 75% of the gross area for silver ingot upper surface of coming out of the stove, can be sentenced by the corresponding relationship in table 2
The content of nitric acid insoluble matter is unqualified in fixed high-purity silver ingot.
Finally, it is stated that above embodiments are only to illustrate the technical solution of the application rather than limit, although referring to compared with
The application is described in detail in good embodiment, those skilled in the art should understand that, it can be to the skill of the application
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical scheme, should all be covered at this
In the scope of the claims of application.
Claims (10)
1. the detection method of nitric acid insolubles content in a kind of high-purity silver ingot, in high-purity silver ingot, silver-colored mass percentage is not
Less than 99.99%, which is characterized in that described detection method includes the following steps:
High-purity silver ingot is melted under protective gas atmosphere, in melting process by high-purity intermittent movement of silver ingot；
Cooling after melting to obtain silver ingot of coming out of the stove, the upper surface of the silver ingot of coming out of the stove forms foreign matter area and specular light clear zone；
The content of nitric acid insoluble matter in high-purity silver ingot is determined according to the ratio of the area in the foreign matter area and high-purity silver ingot quality.
2. detection method according to claim 1, which is characterized in that the detection method further include: determine known nitric acid
The high purity silver ingot shape of insolubles content is between the area in foreign matter area, the quality and nitric acid insolubles content of known high-purity silver ingot
Linear relationship, the content of nitric acid insoluble matter in high-purity silver ingot to be measured is determined further according to the linear relationship.
3. detection method according to claim 1, which is characterized in that the silver ingot of coming out of the stove with a thickness of 13-15mm.
4. detection method according to claim 1, which is characterized in that according to the area in the foreign matter area and come out of the stove on silver ingot
The ratio of the area on surface determines the content of nitric acid insoluble matter in high-purity silver ingot.
5. detection method according to claim 1, which is characterized in that the upper surface of the silver ingot of coming out of the stove is rectangle.
6. detection method according to claim 1, which is characterized in that the melting temperature is 1000-1200 DEG C.
7. detection method according to claim 6, which is characterized in that the melting temperature is 1100 ± 10 DEG C.
8. detection method according to claim 1, which is characterized in that the melting time is 1-3h.
9. detection method according to claim 1, which is characterized in that the intermittent movement use single traveling time for
20-40min, the mobile speed of single are 4-6cm/min, and the single intermittent time is the mode of 20-40s.
10. detection method according to claim 1, which is characterized in that high-purity silver ingot be melted in high temperature furnace into
Row, the intermittent movement of high-purity silver ingot are that high-purity silver ingot is put into graphite material boat, by the push rod in high temperature furnace by stone
Ink boat is pushed to high temperature outlet of still from high temperature furnace entrance is intermittent.
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| CN110608971A (en) * | 2019-10-15 | 2019-12-24 | 克拉玛依友诚实验检测分析有限责任公司 | Indoor detection method for acid insoluble substances in sulfonated asphalt |
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| DE102019120763A1 (en) | 2020-11-12 |
| DE102019120763B4 (en) | 2022-05-12 |
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