CN106872317A - The preprocess method and measuring method of soft magnetic ferrite crystallite dimension measurement - Google Patents
The preprocess method and measuring method of soft magnetic ferrite crystallite dimension measurement Download PDFInfo
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- CN106872317A CN106872317A CN201710090422.6A CN201710090422A CN106872317A CN 106872317 A CN106872317 A CN 106872317A CN 201710090422 A CN201710090422 A CN 201710090422A CN 106872317 A CN106872317 A CN 106872317A
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- soft magnetic
- magnetic ferrite
- crystallite dimension
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 54
- 238000005259 measurement Methods 0.000 title claims abstract description 31
- 238000005530 etching Methods 0.000 claims abstract description 69
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000005498 polishing Methods 0.000 claims abstract description 21
- 238000000227 grinding Methods 0.000 claims abstract description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 16
- 238000009835 boiling Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 31
- 235000011187 glycerol Nutrition 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 8
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Chinese gallotannin Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 8
- 239000011521 glass Substances 0.000 description 3
- 238000004626 scanning electron microscopy Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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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
- G01N15/02—Investigating particle size or size distribution
-
- 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
- G01N1/32—Polishing; Etching
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to the preprocess method and measuring method of a kind of measurement of soft magnetic ferrite crystallite dimension.Preprocess method is mainly included the following steps that：Hydrochloric acid and nitric acid are mixed and stirred for uniformly, obtaining etching solution；Etching solution is placed in etching container and heated；The surface to be etched of soft magnetic ferrite sample upwards and is put into boiling in etching solution；Take out and rinsed with water；And the surface to etching sample is dried, and obtains etching sample.Soft magnetic ferrite surface after to grinding and polishing is etched, and soft magnetic ferrite can be made to polish the crystal boundary on section clearly, can read the accurate grain boundary number with straight line intersection；The crystallite dimension of soft magnetic ferrite is measured using the measuring method including the preprocess method, measurement result close to actual value can be made, at the same avoid for draw actual value and the high SEM of deployment cost.
Description
Technical field
The present invention relates to field of measuring technique, more particularly to a kind of pre- place of soft magnetic ferrite crystallite dimension measurement
Reason method and measuring method.
Background technology
Soft magnetic ferrite has relatively low fissipation factor, high magnetic permeability and high impedance/frequency characteristic, is widely used in
The production of current transformer, earth leakage protective device, insulating transformer and signal and pulse transformer etc..The crystal grain of soft magnetic ferrite
Size has conclusive influence to performances such as its initial permeability, coercivity and switch times, therefore is needed in production process
Strictly to control its crystallite dimension.
After the method for measurement soft magnetic ferrite crystallite dimension is to its sealing and grinding and polishing at present, take up an official post in polishing section
Meaning picture straight line, the length of straight line is measured using microscope, then counts the number with the grain boundary of straight line intersection, is passed through
It is calculated the size of its crystal grain；But, the crystal boundary on polishing section is unintelligible, for counting the grain boundary with straight line intersection
Number can produce larger interference, easily cause read untrue, and then in later stage calculating process, cause the discreteness of data
Greatly so that test value has larger deviation with actual value.Another method is directly carried out using SEM
Measurement；This method measurement result is accurate, but SEM price is costly, generally require million yuans with
On, and SEM is higher to place, environment and equipment operator's level requirement, therefore surveyed using the method
When determining crystallite dimension, disposably put into larger, general enterprises Disposing rate is relatively low.
The content of the invention
Based on this, it is necessary to provide one kind can make measurement soft magnetic ferrite crystallite dimension result accurately and reliably and into
The preprocess method and measuring method of this relatively low soft magnetic ferrite crystallite dimension measurement.
A kind of preprocess method of soft magnetic ferrite crystallite dimension measurement, comprises the following steps：
Etching solution is prepared, hydrochloric acid and nitric acid are mixed and stirred for uniformly, obtaining the etching solution；
The etching solution is placed in etching container and heated；
The surface to be etched of soft magnetic ferrite sample upwards and is put into boiling in the etching solution；
Taken out after etching and rinsed with water；And
Dry tack free is carried out, etching sample is obtained.
Wherein in one embodiment, the preparation etching solution also includes the step of adding glycerine, specifically：By the salt
It is sour that uniform hydrochloric acid glycerite is mixed and stirred for the glycerine, to adding the nitric acid in the hydrochloric acid glycerite and stir
Mix uniform, obtain the etching solution.
Wherein in one embodiment, the density of the hydrochloric acid is 1.19g/mL, the consumption of the hydrochloric acid for 20mL~
30mL；The density of the nitric acid is 1.42g/mL, and the consumption of the nitric acid is 10mL.
Wherein in one embodiment, the consumption of the glycerine is more than 0mL and less than or equal to 30mL.
Wherein in one embodiment, the temperature of the heating is 65 DEG C~95 DEG C.
Wherein in one embodiment, the time of the boiling is 60min~120min.
Wherein in one embodiment, the soft magnetic ferrite is CuZnNi ferrites.
A kind of measuring method of soft magnetic ferrite crystallite dimension, comprises the following steps：
By grinding and polishing after soft magnetic ferrite sealing；
By the soft magnetic ferrite sample after grinding and polishing according to the pre- of described soft magnetic ferrite crystallite dimension measurement
Processing method is pre-processed, and obtains the etching sample；
The crystallite dimension of the measurement etching sample.
Wherein in one embodiment, the crystallite dimension of the measurement etching sample is specifically included：
It is any on the etching face of the etching sample to draw straightway, measure the length of straight line section and count and straight line
The number of the intersecting grain boundary of section, by the crystallite dimension for being calculated the soft magnetic ferrite.
Above-mentioned soft magnetic ferrite crystallite dimension measuring method, is carried out to the soft magnetic ferrite surface after sealing and grinding and polishing
Etching pretreatment, can etch the border of soft magnetic ferrite crystal grain to come, and grain size can be really presented；With it is solid
Seal and directly the method for setting-out measurement is compared after grinding and polishing, carrying out line measurement after being pre-processed through overetch again can be more precisely
The grain boundary number with straight line intersection is read, makes crystallite dimension measurement result more accurate, while avoiding to draw actual value
And the high SEM of deployment cost.Above-mentioned etching solution is prepared, preprocess method process is simple, right using the present invention
The crystallite dimension of soft magnetic ferrite is measured, and the result of acquisition is accurate and low cost.
Brief description of the drawings
Fig. 1 is the flow chart of the measuring method of the soft magnetic ferrite crystallite dimension of an implementation method；
Fig. 2 is the flow chart of the preprocess method of step S120 in Fig. 1；
Fig. 3 is the photo using its etching face after implementation method etching CuZnNi ferrites；
Fig. 4 is the photo of the CuZnNi ferrite grinding and polishing sections not etched.
Specific embodiment
For the ease of understanding the present invention, the present invention is described more fully below.Given in specific embodiment
Presently preferred embodiments of the present invention.But, the present invention can be realized in many different forms, however it is not limited to described herein
Embodiment.On the contrary, the purpose for providing these embodiments is to make the understanding to the disclosure more thorough comprehensive.
As shown in figure 1, a kind of measuring method of soft magnetic ferrite crystallite dimension, comprises the following steps：
Step S110, by grinding and polishing after soft magnetic ferrite sealing；In the present embodiment, soft magnetic ferrite is
CuZnNi ferrites；
Step S120, the soft magnetic ferrite sample after grinding and polishing is pre-processed, and obtains etching sample；
Step S130, the crystallite dimension of measurement etching sample；Specifically：It is any on the etching face of etching sample to draw straight line
Section, measures the length of straight line section and counts the number for intersecting grain boundary with straightway, by being calculated soft magnet oxygen
The crystallite dimension of body material.
With reference to Fig. 2, the preprocess method in above-mentioned steps S120 is comprised the following steps：
Step S121, prepares etching solution, and hydrochloric acid and nitric acid are mixed and stirred for uniformly, obtaining etching solution；Wherein, hydrochloric acid is close
It is 1.19g/mL to spend, and the consumption of hydrochloric acid is 20mL~30mL；The density of nitric acid is 1.42g/mL, and the consumption of nitric acid is 10mL；This
Outward, in the present embodiment, preparing etching solution also includes the step of adding glycerine, specifically：Hydrochloric acid is mixed and stirred with glycerine
Uniform hydrochloric acid glycerite is mixed, to adding nitric acid in hydrochloric acid glycerite and stirring, etching solution is obtained；Wherein, glycerine
Consumption is more than 0mL and less than or equal to 30mL；
Step S122, etching solution is placed in etching container and heated；Preferably, the temperature of heating is 65 DEG C~95 DEG C；
Step S123, upwards and boiling in etching solution is put into by the surface to be etched of soft magnetic ferrite sample；Preferably,
The time of boiling is 60min~120min；
Step S124, takes out after etching and is rinsed with water；And
Step S125, carries out dry tack free, obtains etching sample.
Specific examples below is that the present invention is further described, rather than limitation of the present invention.
Embodiment 1
A kind of measuring method of CuZnNi ferrite crystal grains size comprises the following steps：
1st, by CuZnNi ferrites sealing and grinding and polishing；
2nd, prepare etching solution, by 20mL density for 1.19g/mL hydrochloric acid with 10mL density for 1.42g/mL nitric acid mixes,
And stir；
3rd, etching solution is placed in glass beaker, and is put into thermostat water bath and is heated to 95 DEG C；By CuZnNi ferrites
The surface to be etched of sample is upward and is put into boiling 120min in etching solution；It is rapid to take out and with flowing originally after the completion of etching
Water is rinsed；Surface is dried rapidly with hot blast after the completion of flushing, obtains etching sample；The photo of CuZnNi ferrite etching faces
As shown in Figure 3；
4th, it is any on the etching face of etching sample to draw straightway, measure the length of straight line section and count and straightway
The number of intersecting grain boundary, by being calculated the ferritic crystallite dimensions of CuZnNi.
Embodiment 2
A kind of measuring method of CuZnNi ferrite crystal grains size comprises the following steps：
1st, by CuZnNi ferrites sealing and grinding and polishing；
2nd, etching solution is prepared, by 30mL density for the hydrochloric acid of 1.19g/mL mixes with 30mL glycerine, and is stirred, obtain salt
Acid glycerol solution；It is 1.42g/mL nitric acid and stirs to addition 10mL density in hydrochloric acid glycerite；
3rd, etching solution is placed in glass beaker, and is put into thermostat water bath and is heated to 65 DEG C；By CuZnNi ferrites
The surface to be etched of sample is upward and is put into boiling 90min in etching solution, obtains etching sample；The step of after the completion of etching and embodiment
1 is identical.
Embodiment 3
A kind of measuring method of CuZnNi ferrite crystal grains size comprises the following steps：
1st, by CuZnNi ferrites sealing and grinding and polishing；
2nd, etching solution is prepared, by 25mL density for the hydrochloric acid of 1.19g/mL mixes with 15mL glycerine, and is stirred, obtain salt
Acid glycerol solution；It is 1.42g/mL nitric acid and stirs to addition 10mL density in hydrochloric acid glycerite；
3rd, etching solution is placed in glass beaker, and is put into thermostat water bath and is heated to 80 DEG C；By CuZnNi ferrites
The surface to be etched of sample is upward and is put into boiling 100min in etching solution, obtains etching sample；The step of after the completion of etching and implementation
Example 1 is identical.
Comparative example 1~3
It is right respectively using the direct method of measurement, the SEM direct method of measurement and the method for the present invention after grinding and polishing
CuZnNi ferrites carry out crystallite dimension measurement, and the measurement result of three kinds of methods is as shown in table 1；Not etched soft magnetism after grinding and polishing
The photo of Ferrite Material grinding and polishing section is as shown in Figure 4.
The crystallite dimension measurement result of table 1
Result shows, using the grain size measurement result and scanning electron microscopy measurement result phase one of the inventive method
Cause, and the measurement result crystallite dimension of the microscope direct method of measurement is relatively low after grinding and polishing.That is the inventive method and scanning electron microscopy
Mirror method is better than the microscope direct method of measurement after grinding and polishing, and the alternative scanning electron microscopy of the inventive method.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Can not therefore be construed as limiting the scope of the patent.It should be pointed out that coming for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (9)
1. the preprocess method that a kind of soft magnetic ferrite crystallite dimension is measured, it is characterised in that comprise the following steps：
Etching solution is prepared, hydrochloric acid and nitric acid are mixed and stirred for uniformly, obtaining the etching solution；
The etching solution is placed in etching container and heated；
The surface to be etched of soft magnetic ferrite sample upwards and is put into boiling in the etching solution；
Taken out after etching and rinsed with water；And
Dry tack free is carried out, etching sample is obtained.
2. the preprocess method that soft magnetic ferrite crystallite dimension as claimed in claim 1 is measured, it is characterised in that described
Preparing etching solution also includes the step of adding glycerine, specifically：The hydrochloric acid and the glycerine are mixed and stirred for uniform salt
Acid glycerol solution, to adding the nitric acid in the hydrochloric acid glycerite and stirring, obtains the etching solution.
3. the preprocess method that soft magnetic ferrite crystallite dimension as claimed in claim 1 or 2 is measured, it is characterised in that
The density of the hydrochloric acid is 1.19g/mL, and the consumption of the hydrochloric acid is 20mL~30mL；The density of the nitric acid is 1.42g/mL,
The consumption of the nitric acid is 10mL.
4. the preprocess method that soft magnetic ferrite crystallite dimension as claimed in claim 2 is measured, it is characterised in that described
The consumption of glycerine is more than 0mL and less than or equal to 30mL.
5. the preprocess method that soft magnetic ferrite crystallite dimension as claimed in claim 1 or 2 is measured, it is characterised in that
The temperature of the heating is 65 DEG C~95 DEG C.
6. the preprocess method that soft magnetic ferrite crystallite dimension as claimed in claim 1 or 2 is measured, it is characterised in that
The time of the boiling is 60min~120min.
7. the preprocess method that soft magnetic ferrite crystallite dimension as claimed in claim 1 is measured, it is characterised in that described
Soft magnetic ferrite is CuZnNi ferrites.
8. a kind of measuring method of soft magnetic ferrite crystallite dimension, it is characterised in that comprise the following steps：
By grinding and polishing after soft magnetic ferrite sealing；
By the soft magnetic ferrite sample after grinding and polishing according to the soft magnetic ferrite any one of claim 1~7
The preprocess method of crystallite dimension measurement is pre-processed, and obtains the etching sample；
The crystallite dimension of the measurement etching sample.
9. the measuring method of soft magnetic ferrite crystallite dimension as claimed in claim 8, it is characterised in that the measurement institute
The crystallite dimension for stating etching sample is specifically included：
It is any on the etching face of the etching sample to draw straightway, measure the length of straight line section and count and straightway phase
The number of grain boundary is handed over, by the crystallite dimension for being calculated the soft magnetic ferrite.
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Cited By (1)
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| CN114578015A (en) * | 2022-04-12 | 2022-06-03 | 安徽龙磁金属科技有限公司 | Intelligent quality detection method for soft magnetic ferrite |
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| CN114578015B (en) * | 2022-04-12 | 2024-02-13 | 安徽龙磁金属科技有限公司 | Intelligent quality detection method for soft magnetic ferrite |
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