CN101915685A - Method for preparing standard sample for detecting impact toughness of superhard material - Google Patents
Method for preparing standard sample for detecting impact toughness of superhard material Download PDFInfo
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- CN101915685A CN101915685A CN 201010223289 CN201010223289A CN101915685A CN 101915685 A CN101915685 A CN 101915685A CN 201010223289 CN201010223289 CN 201010223289 CN 201010223289 A CN201010223289 A CN 201010223289A CN 101915685 A CN101915685 A CN 101915685A
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Abstract
The invention relates to a method for preparing a standard sample for detecting the impact toughness of a superhard material. In the method, a standard sample granule with uniform granularity, purity and crystalform integrity is selected through three-stage separation of granularity screening, purity magnetic separation and crystalform integrity separation. By using the method to prepare the standard sample for detecting the impact toughness of a superhard material, the transfer comparison quality of an impact toughness detection quantity valve of the superhard material can be effectively improved, thereby the requirement on the detection of the product produced on a large scale from the superhard material is met. The method has the advantages of reasonable design, simple and convenient operation and strong reliability.
Description
Technical field
The invention belongs to superhard material Performance Detection technical field, particularly a kind of method for preparing standard sample for detecting impact toughness of superhard material.
Background technology
In technique known, impact flexibility (TI, TTI) is the main performance index of superhard materials such as adamas, cubic boron nitride.Synthesizing superhard material impact toughness detects the method that adopts usually: in 2ct sample to be tested and a steel ball (φ 8) impulse test of packing into pipe, add a cover the back clamping on the impact flexibility tester.Open and to measure not percentage of damage after the impact flexibility tester impacts certain number of times, this not percentage of damage after the standard sample correction, be the notched bar impact strength of sample.But; same batch superhard material sample; in the different experiments chamber or the not percentage of damage of on same breadboard different impact flexibility testers, measuring often have certain difference; must after the standard sample for detecting impact toughness correction, just can calculate the notched bar impact strength of comparative sense, so standard sample for detecting impact toughness is to carry out impact toughness of superhard material transmission of quantity value and mass ratio basis.Owing to reasons such as synthesis material, equipment, technologies, cause the aspects such as overall dimensions, crystal shape and integrality, composition degree of purity of same batch the different single crystal grains of superhard material all to have in various degree difference.We can say and from hundreds of millions of single crystal grains, to select two sizes, shape, the on all four particle of degree of purity.The key of preparation superhard material standard sample is to adopt various sorting technology means, crystal grain that make to form the superhard material standard sample has aspect mainly enough close at particle size, shape and integrality, degree of purity etc., thus the sampling error when reducing to detect.
Summary of the invention
The purpose of this invention is to provide a kind of complete homogeneity of granularity, degree of purity and crystalline form that can guarantee standard sample for detecting impact toughness of superhard material, method for preparing standard sample for detecting impact toughness of superhard material easy and simple to handle.
Realize that the technical scheme that purpose of the present invention is taked is: this method is to carry out according to the following steps:
1) granularity screening: selecting size of mesh for use is the electrical forming testing sieve of 425 μ m, 384 μ m, and the superhard material particle that the screening of superhard material particulate material is got under the 425 μ m testing sieves sieve, 384 μ m testing sieves sieve is standby;
2) degree of purity magnetic separation: the superhard material particle that filters out is poured in the magnetic separator hopper, start magnetic separator and carry out the repeated multiple times magnetic separation, select the superhard material particle that accounts for total magnetic separation quality 5% high magnetic at every turn, and measure the magnetic susceptibility value of the high magnetic superhard material particle select and select the magnetic susceptibility value of surplus superhard material particle to compare with the superhard material magnetic susceptibility meter, if the magnetic susceptibility of 5% high magnetic superhard material particle is greater than selecting 3 times of surplus superhard material granulated magnetic rate, the 5% high magnetic superhard material particle that then will select is thrown aside, to selecting surplus superhard material particle to carry out the repetition magnetic separation, magnetic susceptibility until 5% high magnetic superhard material particle is less than or equal to till 3 times that select surplus superhard material granulated magnetic rate, and leave and take and select surplus superhard material particle as superhard material particulate samples to be selected this moment.
3) crystalline form integrality sorting: will send in the superhard material type selecting machine hopper through the superhard material particulate samples to be selected that magnetic separation is selected, and adjustment superhard material type selecting machine blanking velocity, type selecting plate angle of inclination and oscillation intensity parameter, start superhard material type selecting machine and carry out the sorting of crystalline form integrality, sub-elect the crystalline form integrality the good superhard material particle with crystalline form integrality difference is thrown aside at every turn, select and account for total sorting quality 50% crystalline form of this time alternative superhard material particulate samples medium than integrality, repeat sorting once more, be divided into and select 3 times, sub-elect for the third time and account for the more complete medium superhard material particulate samples to be selected of total sorting quality 50% crystalline form of this time and be standard sample for detecting impact toughness of superhard material.
Method for preparing standard sample for detecting impact toughness of superhard material of the present invention, by granularity, degree of purity and three grades of sortings of crystalline form integrality, guaranteed the standard sample for detecting impact toughness of superhard material performance parameter homogeneity, thereby can improve impact toughness of superhard material effectively and detect the value transfer comparison quality, satisfy the needs that the superhard material mass production of products detects, this method is reasonable in design, and is easy and simple to handle, good reliability.
Embodiment
Method for preparing standard sample for detecting impact toughness of superhard material of the present invention, be by the inventor on the basis of summing up the long-term practice experience, and obtain by great deal of experimental.This method at granularity, degree of purity and three main performance index of crystalline form integrality of impact toughness of superhard material strong correlation, by screening, magnetic separation and type selecting three road sortings, reject the nonuniformity sample, select standard sample the most with consistency, thereby guaranteed the reliability of impact toughness of superhard material detection reference.Method for preparing standard sample for detecting impact toughness of superhard material of the present invention is to carry out according to the following steps:
The first step, the granularity screening: selecting size of mesh for use is the electrical forming testing sieve of 425 μ m, 384 μ m, and the superhard material particle that the screening of superhard material particulate material is got under the 425 μ m testing sieves sieve, 384 μ m testing sieves sieve is standby.
In technical field of superhard material, granularity is 40/45 superhard material certified products, according to the GB/T6406 regulation, the granular mass number percent of particle diameter between 255 μ m～645 μ m is not less than 99.4%, and the granular mass number percent of particle diameter between 360 μ m～455 μ m is not less than 90.0%; According to the ISO6106 regulation, the granular mass number percent of particle diameter between 255 μ m～645 μ m is not less than 99.4%, and the granular mass number percent of particle diameter between 360 μ m～455 μ m is not less than 93.0%.And this method is not used the last test sieve (aperture 455 μ m) of 40/45 granularity of this sizing correspondence and the following test sieve (aperture 360 μ m) of 40/45 granularity, and be to use the following test sieve (aperture 425 μ m) of 35/40 granularity and going up of 45/50 granularity to examine test sieve (aperture 384 μ m), the particle of sample particle diameter between 360 μ m～455 μ m that screening obtains is 100.0%, and mainly concentrate between 384 μ m～425 μ m, thereby the consistance of particle size increases greatly.
Second step, degree of purity magnetic separation: 1. the superhard material particle that filters out is poured in the magnetic separator hopper, started magnetic separator; 2. adjusting the magnetic separator electric current starts from scratch and increases on magnetic separator rotation magnetic roller gradually and sense magnetic-particle in the superhard material particle can be kicked up to the magnetic force of material; 3. adjust sub-material nose angle degree to the highly higher high magnetic material of kicking up on the magnetic separator account for the magnetic separation gross mass 5% till, 5% high magnetic superhard material particle with select surplus part superhard material particle to insert respectively in the different charging baskets; 4. high magnetic superhard material particle with select surplus superhard material particle mixing separately; 5. measure high magnetic superhard material granulated magnetic rate value and select surplus superhard material granulated magnetic rate value with the superhard material magnetic susceptibility meter respectively.If 6. high magnetic superhard material granulated magnetic rate value is greater than 3 times of the magnetic susceptibility value of selecting surplus superhard material particle, then will select surplus superhard material particle repeating step 1.～5. to carry out final election, magnetic susceptibility until 5% high magnetic superhard material particle is less than or equal to till 3 times that select surplus superhard material granulated magnetic rate, and leave and take and select surplus superhard material particle as superhard material particulate samples to be selected this moment.
The assay method of superhard material magnetic susceptibility is that 20 gram superhard material samples are packed on the magnetic susceptibility meter in the special-purpose coupon, and coupon is inserted on the magnetic susceptibility meter, presses the measurement key, and magnetic susceptibility meter is the magnetic susceptibility value of show sample.The size of superhard material magnetic susceptibility value has reflected that the sample particle on average feels the power of magnetic energy power, and impurity such as superhard material iron content what have reflected indirectly.In the superhard material of producing with same batch of starting material, identical device and technology, the magnetic susceptibility value is impure few more in the bright granule crystal of novel more, and quality grade is high more.In producing, the superhard material sorting often pays close attention to the average magnetic susceptibility value of different quality grade products particle in the same large quantities of products.This method is mainly paid close attention to is the consistance of magnetic susceptibility of forming the superhard material particle of standard sample, does not pay close attention to the concrete average magnetic susceptibility value of material.
The 3rd step, crystalline form integrality sorting: the superhard material particulate samples of selecting through magnetic separation to be selected is sent in the superhard material type selecting machine hopper, open the type selecting machine and adjust type selecting machine blanking velocity, type selecting plate angle of inclination and oscillation intensity parameter, make sample particle fall on the type selecting plate of type selecting machine and from hopper equably and scatter, guarantee sample particle collisionless tumbling in the different hopper in type selecting plate below from the type selecting plate respectively at the type selecting plate.After finishing, type selecting discards the material in the hopper of left and right both sides, about 50% material in the middle of leaving and taking.Carry out three times type selecting so repeatedly altogether, promptly can be used as the standard sample that impact flexibility detects after 50% material that obtains for the third time mixes.
The sorting of crystalline form integrality is to utilize the superhard material sample through size sorting and magnetic sorting superhard material type selecting machine to select crystal shape to be the complete particle of perfectly round shape, crystal (crystal edge, crystal face) and to have prolate crystal shape, crystal (crystal edge, crystal face) that the particle of serious defect is arranged, obtain having slightly on crystal edge, the crystal face standard model of damaged fair average quality.
Below with granularity be 40/45, the medium superhard material product of quality grade is the preparation method of example description standard sample.
1, the method for separating of particle size: selecting size of mesh for use is the electrical forming testing sieve of 425 μ m, 384 μ m.Sieve is got 425 μ m testing sieve screen underflows, 384 μ m testing sieve screen overflows.
Illustrate: granularity is 40/45 superhard material specification product, stipulate according to GB/T6406, the particle of particle diameter between 255 μ m～645 μ m is not less than 99.4% (mass percent), and the particle of particle diameter between 360 μ m～455 μ m is not less than 90.0% (mass percent); According to the ISO6106 regulation, the particle of particle diameter between 255 μ m～645 μ m is not less than 99.4% (mass percent), and the particle of particle diameter between 360 μ m～455 μ m is not less than 93.0% (mass percent).This method is not used the last test sieve (aperture 455 μ m) of 40/45 granularity of this sizing correspondence and the following test sieve (aperture 360 μ m) of 40/45 granularity, and is to use the following test sieve (aperture 425 μ m) of 35/40 granularity and going up of 45/50 granularity to examine test sieve (aperture 384 μ m).The particle of sample particle diameter between 360 μ m～455 μ m that screening obtains is 100.0%, and mainly concentrates between 384 μ m～425 μ m, and the particle size consistance increases greatly.
2, granule interior degree of purity method for separating.The particle diameter that obtains through the sorting of particle size is concentrated on sample between 384 μ m～425 μ m, utilize magnetic separator that the particle of sense magnetic strong (being that the crystals ferrous contaminants is more) in the superhard material particle is selected, obtain the consistent sample of pure interior degree.
Magnetic selection method is: 1. material is poured in the magnetic separator hopper, started magnetic separator; 2. adjusting the magnetic separator electric current starts from scratch and increases on magnetic separator rotation magnetic roller gradually and sense magnetic-particle in the superhard material particle can be kicked up to the magnetic force of material; 3. sub-material nose angle degree to the highly higher high magnetic material of adjusting on the magnetic separator of kicking up accounts for till the material total amount 5%, 5% high magnetic material with in the other parts material inserts different charging baskets respectively; 4. high magnetic material and its clout mixing separately; 5. measure high magnetic material magnetic susceptibility value and its clout magnetic susceptibility value with the superhard material magnetic susceptibility meter respectively.If 1. 6. high magnetic material magnetic susceptibility value greater than 3 times of the magnetic susceptibility value of (or equaling) its clout, then repeated～5. till the magnetic susceptibility of 5% high magnetic material would not be higher than three times of remaining sample magnetic susceptibility.
Illustrate: the assay method of superhard material magnetic susceptibility is that 20 gram superhard material samples are packed on the magnetic susceptibility meter in the special-purpose coupon, and coupon is inserted on the magnetic susceptibility meter, presses the measurement key, and magnetic susceptibility meter is the magnetic susceptibility value of show sample.The size of superhard material magnetic susceptibility value has reflected that the sample particle on average feels the power of magnetic energy power, and impurity such as superhard material iron content what have reflected indirectly.In the superhard material of producing with same batch of starting material, identical device and technology, the magnetic susceptibility value is impure few more in the bright granule crystal of novel more, and quality grade is high more.The magnetic susceptibility value and the product quality grade of the superhard material crystal that different batches starting material and different technical parameters are produced do not have strict corresponding relationship.In producing, the superhard material sorting often pays close attention to the average magnetic susceptibility value of different quality grade products particle in the same large quantities of products.This method is mainly paid close attention to is the consistance (otherness) of magnetic susceptibility of forming the superhard material particle of standard sample, does not pay close attention to the concrete average magnetic susceptibility value of material.
3, crystalline form integrality sorting.Utilizing the superhard material sample through size sorting and magnetic sorting superhard material type selecting machine to select crystal shape is the complete particle of perfectly round shape, crystal (crystal edge, crystal face) and has prolate crystal shape, crystal (crystal edge, crystal face) that the particle of serious defect is arranged, obtain having slightly on crystal edge, the crystal face standard model of damaged fair average quality.
The crystal perfection method for separating is: sample is poured in the superhard material type selecting machine hopper, open the type selecting machine and adjust type selecting machine blanking velocity, type selecting plate angle of inclination and oscillation intensity parameter, make sample particle fall on the type selecting plate of type selecting machine and from hopper equably and scatter, guarantee that sample particle is respectively from the type selecting plate in collisionless (different) hopper that tumbles under the type selecting plate at the type selecting plate.After finishing, type selecting discards the material (annotating: be recycled in the batch mixing) in the hopper of left and right both sides, about 50% material in the middle of leaving and taking.Carry out three times type selecting so repeatedly altogether.After mixing, 50% material that obtains for the third time promptly can be used as the standard sample that 40/45 granularity impact flexibility detects.
Claims (1)
1. method for preparing standard sample for detecting impact toughness of superhard material, it is characterized in that: it is to carry out according to the following steps:
1) granularity screening: selecting size of mesh for use is the electrical forming testing sieve of 425 μ m, 384 μ m, and the superhard material particle that the screening of superhard material particulate material is got under the 425 μ m testing sieves sieve, 384 μ m testing sieves sieve is standby;
2) degree of purity magnetic separation: the superhard material particle that filters out is poured in the magnetic separator hopper, start magnetic separator and carry out the repeated multiple times magnetic separation, select the superhard material particle that accounts for total magnetic separation quality 5% high magnetic at every turn, and measure the magnetic susceptibility value of the high magnetic superhard material particle select and select the magnetic susceptibility value of surplus superhard material particle to compare with the superhard material magnetic susceptibility meter, if the magnetic susceptibility of 5% high magnetic superhard material particle is greater than selecting 3 times of surplus superhard material granulated magnetic rate, the 5% high magnetic superhard material particle that then will select is thrown aside, to selecting surplus superhard material particle to carry out the repetition magnetic separation, magnetic susceptibility until 5% high magnetic superhard material particle is less than or equal to till 3 times that select surplus superhard material granulated magnetic rate, and leave and take and select surplus superhard material particle as superhard material particulate samples to be selected this moment;
3) crystalline form integrality sorting: will send in the superhard material type selecting machine hopper through the superhard material particulate samples to be selected that magnetic separation is selected, and adjustment superhard material type selecting machine blanking velocity, type selecting plate angle of inclination and oscillation intensity parameter, start superhard material type selecting machine and carry out the sorting of crystalline form integrality, sub-elect the crystalline form integrality the good superhard material particle with crystalline form integrality difference is thrown aside at every turn, select and account for total sorting quality 50% crystalline form of this time alternative superhard material particulate samples medium than integrality, repeat sorting once more, be divided into and select 3 times, sub-elect for the third time and account for the more complete medium superhard material particulate samples to be selected of total sorting quality 50% crystalline form of this time and be standard sample for detecting impact toughness of superhard material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104075920A (en) * | 2014-06-27 | 2014-10-01 | 中南钻石有限公司 | Preparation method of superhard material impact toughness testing standard samples |
| CN108267502A (en) * | 2016-12-30 | 2018-07-10 | 大众汽车自动变速器（大连）有限公司 | The eddy detection system and detection method of case depth |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01274046A (en) * | 1988-04-27 | 1989-11-01 | Kawasaki Steel Corp | Solidification of powder sample for instrumental analysis |
| CN101614641A (en) * | 2009-08-10 | 2009-12-30 | 南阳中南金刚石有限公司 | A kind of method for detecting impact toughness of artificial diamond |
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2010
- 2010-07-12 CN CN2010102232895A patent/CN101915685B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01274046A (en) * | 1988-04-27 | 1989-11-01 | Kawasaki Steel Corp | Solidification of powder sample for instrumental analysis |
| CN101614641A (en) * | 2009-08-10 | 2009-12-30 | 南阳中南金刚石有限公司 | A kind of method for detecting impact toughness of artificial diamond |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104075920A (en) * | 2014-06-27 | 2014-10-01 | 中南钻石有限公司 | Preparation method of superhard material impact toughness testing standard samples |
| CN108267502A (en) * | 2016-12-30 | 2018-07-10 | 大众汽车自动变速器（大连）有限公司 | The eddy detection system and detection method of case depth |
| CN108267502B (en) * | 2016-12-30 | 2022-06-17 | 大众汽车自动变速器（大连）有限公司 | Eddy current detection system and method for depth of hardened layer |
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