CN109143126A - A kind of preparation method of hard alloy coercive force or magnetic saturation standard sample - Google Patents
A kind of preparation method of hard alloy coercive force or magnetic saturation standard sample Download PDFInfo
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- CN109143126A CN109143126A CN201811100375.XA CN201811100375A CN109143126A CN 109143126 A CN109143126 A CN 109143126A CN 201811100375 A CN201811100375 A CN 201811100375A CN 109143126 A CN109143126 A CN 109143126A
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Abstract
The invention discloses the preparation methods of a kind of hard alloy coercive force or magnetic saturation standard sample, comprising: step S1 determines the definite value gradient of hard alloy coercive force or magnetic saturation standard sample；Step S2 prepares coercive force or magnetic saturation value in the hard alloy standard sample of identified definite value gradient scope respectively and carries out quality testing；Step S3 randomly selects standard sample and carries out uniformity testing；Step S4 after uniformity testing is qualified, randomly selects standard sample and transfers to m family's mechanism for testing test coercive force or magnetic saturation performance；M family laboratory measures in step S4 coercive force or magnetic saturation result are carried out Mathematical Statistics Analysis by step S5；Step S6, coercive force or magnetic saturation result based on mathematical statistics qualification determine hard alloy standard sample coercive force or magnetically saturated standard value.The standard sample can provide unified calibration standard for China's coercimeter and magnetic saturation.
Description
Technical field
The present invention relates to the preparation methods of a kind of hard alloy coercive force or magnetic saturation standard sample.
Background technique
Coercive (magnetic) power, magnetic saturation (cobalt magnetic) have important special role in the research and production of hard alloy, are
Guarantee the most scientific method of alloy mass at present.Therefore, coercive (magnetic) power, magnetic saturation (cobalt magnetic) parameter are widely used in hard
The technology controlling and process and quality of alloy control.In WC-Co hard alloy, coercive (magnetic) power, magnetic saturation (cobalt magnetic) are hard alloy
The main indicator of properties of product, can concentrated expression cemented carbide structure minor change, reflect alloy in carbon content variation,
The distribution situation of WC grain degree size and grain size, and can be come out with the relationship expression accurately measured.All the time, coercive force
Because instrument producer difference, measurement method are also not quite similar, the testing result of different experiments room exists certain for power meter and magnetic saturation instrument
Difference, especially domestic coercimeter measurement method mostly using relative manner, i.e., by measurement one group known to
The reference sample of its value establishes an experiment curv, further according to experiment curv test sample.Thus one, this group " its known value
Reference sample " correctness is just of crucial importance, be the legal foundation of detection data accuracy.However current hard alloy row
Industry standard sample ununified in terms of physical property detection (coercive force, magnetic saturation) carries out magnitude tracing, can not check
The accuracy of detection data, also can not monitoring instrument equipment stability.Therefore, coercive (magnetic) power and magnetic saturation (cobalt magnetic) are established
Standard sample is conducive to trace to the source transmitting and the calibration of measuring instrument of magnitude, is conducive to carbon amounts and work during CEMENTED CARBIDE PRODUCTION
Skill accurately controls, and is conducive to the comparison of laboratory monitoring detectability, is conducive to the operation test for testing indoor occupant.
Summary of the invention
The purpose of the present invention is to provide the preparation methods of a kind of hard alloy coercive force or magnetic saturation standard sample, full
The requirement that sufficient cemented carbide industry accurately detects coercive force or magnetic saturation.
The purpose of the present invention adopts the following technical scheme that realize:
A kind of hard alloy coercive force or magnetic saturation standard sample preparation method, comprising:
Step S1 determines the definite value gradient of hard alloy coercive force or magnetic saturation standard sample；
Step S2 prepares the hard alloy mark of coercive force or magnetic saturation in the definite value gradient scope determined by step S1
Quasi- sample carries out quality testing to hard alloy standard sample；
Step S3 randomly selects standard sample and carries out uniformity testing；
Step S4 after uniformity testing is qualified, randomly selects sample and transfers to m family's mechanism for testing test coercive force or magnetic full
And performance, m >=7, it is preferable that every mechanism for testing is to each sample test n times, n >=3, preferably 5；
M family laboratory measures in step S4 coercive force or magnetic saturation data are carried out Mathematical Statistics Analysis by step S5；
Step S6, coercive force or magnetic saturation data based on mathematical statistics qualification, determines hard alloy standard sample
Coercive force or magnetically saturated characteristic value and the uncertainty for determining characteristic value, and then determine the coercive force or magnetic of standard sample
The definite value of saturation.
According to the preferred embodiment of the present invention, according to the product characteristic of hard alloy, the coercive force one of hard alloy
As within the scope of 3-40KA/m, determine that the definite value gradient of the coercive force is divided into 4 gradients, respectively first gradient as a result,
(HC-1): 5KA/m is hereinafter, the second gradient (HC-2): 9-12KA/m, 3rd gradient (HC-3): 19-22KA/m and 4th gradient
(HC-4): 36-40KA/m.
According to the preferred embodiment of the present invention, according to the product characteristic of hard alloy, the magnetic saturation of hard alloy is general
Within the scope of 0-25%Co, the magnetically saturated definite value gradient is divided into 3 gradients, respectively first gradient (COM-1): 1%
Co is hereinafter, the second gradient (COM-2): 10-14%Co, 3rd gradient (COM-3): 22-26%Co.
According to the preferred embodiment of the present invention, in the coercive force or magnetically saturated definite value gradient for determining hard alloy
Afterwards, different raw materials is chosen respectively prepares the hard alloy mark of coercive force or magnetic saturation in identified definite value gradient scope
Quasi- sample.
According to the preferred embodiment of the present invention, which kind of raw material is selected to prepare the hard with different hc values
Alloy standard sample, and which kind of raw material is selected to prepare the side of the hard alloy standard sample with different magnetic saturation performances
Method is well-known to those skilled in the art.
According to the preferred embodiment of the present invention, the material composition for preparing hard alloy standard sample is substantially following several
Kind:
HC-1: main component 80wt%WC and 20wt%Co；
HC-2: main component 88wt%%WC and 12wt%Co；
HC-3: main component 93.5wt%WC and 6wt%Co；
HC-4: main component 90.8wt%WC, 8wt%Co；The VC and Cr of surplus3C2；
COM-1: main component 87.0-89.0wt%WC and surplus Ni+Cr and micro Co；
COM-2: main component 88%wt%WC and 12wt%Co；
COM-3: main component 72wt%WC and 28wt%Co.
According to the preferred embodiment of the present invention, the method for preparing hard alloy standard sample is those skilled in the art institute
Well known preparation process is made.In general, the technique for preparing hard alloy standard sample includes: raw material mixing, compacting and sintering etc.
Step.
According to the preferred embodiment of the present invention, quality testing includes physical property and institutional framework detection in step S2；
Preferably, physical property includes coercive force, magnetic saturation, hardness and density, and institutional framework includes heterogeneous microstructure and defect.
According to the preferred embodiment of the present invention, it is randomly selected in the step S3It was carried out with last standard sample equal
Test of homogeneity, N are the sum of standard sample.
According to the preferred embodiment of the present invention, when carrying out uniformity testing in step s3, using GB/T3848-2017
" hard alloy coercive (magnetic) power measuring method " measures hc values, GB/T23369-2009 " hard alloy magnetic saturation (MS)
The standard test method of measurement " measurement magnetic saturation (cobalt magnetic) value.
According to the preferred embodiment of the present invention, the uniform of coercive force and magnetic saturation sample is judged using variance test method
Property checks whether qualification.
According to the preferred embodiment of the present invention, in step S4, m family's mechanism for testing is that the country is recognized with laboratory
Can or qualification certification qualification laboratory.
According to the preferred embodiment of the present invention, in step s 4, m=7.
According to the preferred embodiment of the present invention, in the step S4, each standard sample carries out n times test, and n >=3 are excellent
It is selected as 5.Using the average value of n times measurement result as the test result of the sample.
According to the preferred embodiment of the present invention, in step S4, using GB/T3848-2017 " hard alloy coercive (magnetic)
Power measuring method " test coercive force, using " the code test side of hard alloy magnetic saturation (MS) measurement GB/T23369-2009
Method " test magnetic saturation.
According to the preferred embodiment of the present invention, the Mathematical Statistics Analysis includes uniformity testing, test of outlier, just
State distribution inspection and equally accurate are examined.
Exceptional value refers in one group of measured value and the deviation of average value is more than the measured value of twice of standard deviation, with average value
Deviation is more than the measured value of three times standard deviation, the referred to as exceptional value of Height Anomalies.
The method of test of outlier includes that Grubbs (Grubbs) is examined and Charles Dixon (Dixon) inspection.
Equal precision measurement refers in entire measurement process, if influencing and determining whole factors (condition) of error size
Remain constant, such as by the same gauger, with same instrument, same measurement method, in identical environmental condition
Under, to the same measurement method for being measured and carrying out that measurement is repeated several times.It is extremely difficult in practice to accomplish to influence and determine error size
Whole factors (condition) remain constant, therefore can only be that be approximately considered be equal precision measurement under normal circumstances.
Normal distribution-test includes that K-S (Kolmogorov-Smirnov) is examined, Lilliefors is examined, AD is examined
(Anderson-Darling inspection), W examine (Shapiro-Wilk inspection), Ryan-Joiner to examine.
According to the preferred embodiment of the present invention, be calculated as follows standard sample coercive force or magnetically saturated feature
Value:
Wherein, m is the number of mechanism for testing,Indicate measurement of i-th mechanism for testing to the standard sample of same gradient
Average value；Indicate the coercive force or magnetic saturation characteristic value of hard alloy standard sample.
According to the preferred embodiment of the present invention, describedRefer to i-th mechanism for testing to the standard sample of same gradient
Measurement average value.The average value read group total arithmetic overall average that m family's mechanism for testing is measured, as hard alloy standard sample
The coercive force of product or magnetically saturated characteristic value.
According to the preferred embodiment of the present invention, the uncertainty includes A class uncertainty uA, B class uncertainty uB、
Uncertainty u caused by inhomogeneitieslWith uncertainty u caused by unstabilityr。
According to the preferred embodiment of the present invention, A class uncertainty uAWith the standard deviation of single measurementIt indicates,
Wherein,It is average to the measurement of the measurement average value of the standard sample of same gradient to represent i-th mechanism for testing
Value；The coercive force or magnetic saturation characteristic value of hard alloy standard sample are represented, m indicates the number of mechanism for testing.
According to the preferred embodiment of the present invention, by the analysis to determination influences factor, B class uncertainty is estimated,
It is denoted as uB。
According to the preferred embodiment of the present invention, uncertainty caused by the inhomogeneities of standard sample generally uses sample
Mean squares between groups root error u in grouplTo indicate:
Wherein, n represents every mechanism for testing to the testing time of each standard sample, Q1Sum of square of deviations between representative group, Q2
Sum of square of deviations in representative group, v1Freedom degree between representative group, v2The representative group internal degree of freedom.
According to the preferred embodiment of the present invention, uncertainty caused by the unstability of standard sample is using in sample sets
Mean squares between groups root error urTo indicate:
Wherein, n represents every mechanism for testing to the testing time of each standard sample, Q1Sum of square of deviations between representative group, Q2
Sum of square of deviations in representative group, v1Freedom degree between representative group, v2The representative group internal degree of freedom.
Combined standard uncertainty are as follows:
Multiple laboratories are used with the solid non-ferrous metal standard sample of a variety of method definite values, usual B class uncertainty
uBWith uncertainty u caused by unstabilityrNegligible, then the uncertainty of this standard sample development process includes: that A class is not true
Uncertainty caused by fixed degree (i.e. single measurement standard deviation) and inhomogeneities.
Calculate expanded uncertainty U:U=kuc
Take fiducial probability for 95%, k=2, then
U=kuc=2 × uc
According to the preferred embodiment of the present invention, the uncertainty are as follows:
Wherein, U indicates uncertainty, Q1Sum of square of deviations between representative group, Q2Sum of square of deviations in representative group, v1Represent group
Between freedom degree, v2The representative group internal degree of freedom,The coercive force of expression hard alloy standard sample or magnetically saturated characteristic value,
I-th mechanism for testing is represented to the measurement average value of the standard sample of same gradient, m is the number of mechanism for testing, and n is every survey
Testing time of the test-run a machine structure to each standard sample.
According to the preferred embodiment of the present invention, the standard value are as follows:
I be coercive force or magnetically saturated standard value,Indicate coercive force or the magnetic saturation of hard alloy standard sample
Characteristic value, U indicate uncertainty.
The relative amount that the magnetic Binder Phase such as cobalt in sample, iron, nickel can be measured by magnetic saturation measurement, since hard closes
Magnetic saturation standard sample product examine of the golden industry mostly using percentage cobalt content (i.e. cobalt magnetic) measurement data as judging basis, in the present invention
Measured data is subject to cobalt magnetic measurement data, and magnetic saturation is cobalt magnetic value in the present invention.
The development of coercive (magnetic) power, magnetic saturation (cobalt magnetic) standard sample of the present invention has effectively ensured analysis detection result
Reliability can provide unified calibration standard for China's coercimeter, solve to detect knot between different experiments room for a long time
The otherness of fruit, and can check the accuracy of coercimeter, the stability of magnetic saturation instrument and evaluation detection method.
Specific embodiment
The present invention is described in detail with reference to embodiments, but the present invention is not limited by following embodiments.
Embodiment 1
(1) determine that coercive force definite value gradient design is 4 gradients, the respectively first ladder according to hart metal product characteristic
(HC-1): 5KA/m is spent hereinafter, the second gradient (HC-2): 9-12KA/m, 3rd gradient (HC-3): 19-22KA/m and 4th gradient
(HC-4): 36-40KA/m.I.e. 4 standard samples are a set of.
According to hart metal product characteristic determine magnetic saturation (cobalt magnetic) definite value gradient design be 3 gradients, respectively first
Gradient (COM-1): 1%Co is hereinafter, the second gradient (COM-2): 10-14%Co, 3rd gradient (COM-3): 22-26%Co.I.e. 3
A standard sample is a set of.
(2) the coercive force standard sample of different gradients is prepared with following raw material respectively:
HC-1: main component 80wt%WC and 20wt%Co；
HC-2: main component 88wt%WC and 12wt%Co；
HC-3: main component 93.5wt%WC and 6wt%Co；
HC-4: main component 90.8wt%WC, 8wt%Co；The VC and Cr of surplus3C2。
The magnetic saturation standard sample of different gradients is prepared with following raw material respectively:
COM-1: main component 87.0-89.0wt%WC and surplus Ni+Cr and micro Co；
COM-2: main component 88wt%WC and 12wt%Co；
COM-3: main component 72wt%WC and 28wt%Co.
Physical property, institutional framework and characteristic value detection are carried out to obtained standard sample.
Physical property detection includes: coercive force, magnetic saturation, hardness and density.
Institutional framework detection includes: heterogeneous microstructure and defect.
By this laboratory test, the average value of the coercive force standard sample of different gradients be respectively 3.70KA/m,
The average value of 9.90KA/m, 21.9KA/m, 38.6KA/m, magnetic saturation (cobalt magnetic) standard sample of different gradients are respectively 0.16%
Co, 11.38%Co, 24.15%Co meet design requirement.
(3) for coercive force standard sample, randomly select 10 sets totally 40 samples using GB/T3848-2017 " hard
Alloy coercive (magnetic) power measuring method " measurement hc values progress uniformity initial survey.It is random to select for magnetic saturation standard sample
Take 8 sets totally 24 samples using GB/T23369-2009 " standard test method of hard alloy magnetic saturation (MS) measurement " measurement magnetic
It is saturated (cobalt magnetic) value and carries out uniformity initial survey.
When carrying out coercive force or magnetic saturation is tested, each sample carries out 5 measurements under duplicate experiment condition, and
It is for statistical analysis using data of the variance test method to test, judge that the uniformity testing of coercive force and magnetic saturation sample is
No qualification.
In uniformity testing, sum of square of deviations calculation formula is as follows between group:
Wherein, Q1Sum of square of deviations between representative group,The testing mean of i-th of standard sample is represented,Represent same ladder
Hard alloy standard sample overall average is spent, a represents the number of standard sample, and b represents the pendulous frequency of same standard sample.
Sum of square of deviations calculation formula is as follows in group:
Wherein, Q2Sum of square of deviations in representative group, LijTest result of i-th of standard sample in jth time test is represented,Represent the testing mean of i-th of standard sample；A represents the number of standard sample, and b represents the measurement time of same standard sample
Number.
Freedom calculation formula is as follows:
v1=a-1；v2=a (b-1)
Wherein, v1Freedom degree between representative group, v2The representative group internal degree of freedom, a represent the number of standard sample, and b represents same mark
The pendulous frequency of quasi- sample.
Normalized set formula is as follows:
Take level of significance α=0.05, freedom degree ν1,ν2, examine tables of critical values to check in F from Fα.Compare F and Fα:
F < F0.05, the results showed that sample homogeneity is examined qualified.
(4) 20 domestic 7 laboratories of coercive force standard sample commission are counted by 5 sets and carries out coercive force test, by 5 sets
It counts 15 domestic 7 laboratories of magnetic saturation standard sample commission and carries out magnetic saturation test, every laboratory is to 5 sets of coercive forces
Power standard sample and 5 sets of magnetic saturation standard samples are tested, and using GB/T3848-2017, " hard alloy coercive (magnetic) power is surveyed
Determine method " test coercive force, using GB/T23369-2009 " standard test method of hard alloy magnetic saturation (MS) measurement "
Test magnetic saturation.5 independent test results are quoted to each sample in every laboratory, and 10 groups (every group 5 × 4) are obtained
(certain mechanism for testing have multiple groups test equipment to coercive force data, and thus, every set standard sample can be into same mechanism for testing
The independent test of row multiple groups, provides multiple groups test result), obtain 7 groups of (every group 5 × 3) a magnetic saturation data.
(5) test of outlier is carried out to every group of determination data using Dixon method, there are 3 groups of coercive force data is exceptional value
Not to adopt, remaining 7 groups of hc values or magnetic saturation value use Dixon method to carry out test of outlier to every group of determination data,
R1, r5 are respectively less than f(0.05,5)0.71, it is no different constant value, so data retain.
It is tested with normality of the Shapiro-Wilk test to each cell mean, calculation formula are as follows:
In formula, k value range is 1-h；N is pendulous frequency, when n is even number, h=n/2；H=(n-1)/2 when n is odd number；
aKIt is particular value related with n and k, it can be by being checked in Shapiro-Wilk test table；Xn+1-kRepresent the (n+1)th-k measurement knots
Fruit；XkRepresent kth time measurement result；；Represent measurement average value.As W > W (n, P), then receive determination data as normal state point
Cloth, W (n, P) are numerical value related with measurement number and fiducial probability.
In the present invention, n=7, as a result, h=6/2=3；Table look-up to obtain a1=0.6233, a2=0.2413, a3=0.1401,
W(7,0.05)=0.803, it is computed W and is all larger than W(7,0.05), 5 cell mean data fit normal distributions, every group of 35 coercive forces
Power, magnetic saturation test data meet normal distribution.
Consistency between each cell mean is examined using Ge Labu (Grubbs) method.It is average by every group 7 of determination data
Value forms one group of new data by sequence arrangement from small to large:
X1≤X2≤......≤Xn
Find out its average valueAnd standard deviation S, Counting statistics amount G1And Gn:
Under 95% fiducial probability, the tables of critical values for looking into Grubbs Law obtains G(0.05,7)=2.020
G1, GnRespectively less than G(0.05,7)Value, therefore obtain check conclusion: the average value of each group of data is without outlier.
Using Cochran (Cochran) method examine average value between whether equally accurate, look into Cochran (Cochran) method check table
Obtain C(0.95,5,7)=0.4307, C(0.99,5,7)=0.5080, Counting statistics amount CmaxRespectively less than C(0.99,5,7), therefore obtain inspection knot
By: 5 sets there was no significant difference between totally 20 coercive force samples and the test data average value of 15 magnetic saturation samples, belongs to
Equal precision measurement.
The overall average of each average value is the best estimate of the standard value of this magnetic property standard sample.It is calculated as follows:
M is the number of mechanism for testing,Indicate i-th mechanism for testing to the measurement average value of same gradient standard sample；The coercive force of expression hard alloy standard sample or magnetically saturated characteristic value.
The composition of standard uncertainty
The uncertainty of standard sample standard value forms: caused by A class uncertainty, B class uncertainty, inhomogeneities not
Uncertainty caused by degree of certainty and unstability.
The standard deviation of the A class uncertainty single measurement of standard sampleIt indicates.
By the analysis to determination influences factor, B class uncertainty is estimated, u is denoted asB。
Uncertainty caused by the inhomogeneities of standard sample generally uses Mean squares between groups root error u in sample setslCarry out table
Show:
Wherein, n represents every mechanism for testing to the testing time of each standard sample, Q1Sum of square of deviations between representative group, Q2
Sum of square of deviations in representative group, v1Freedom degree between representative group, v2The representative group internal degree of freedom.
Uncertainty caused by the unstability of standard sample generally uses Mean squares between groups root error u in sample setsrCarry out table
Show:
Wherein, n represents every mechanism for testing to the testing time of each standard sample, Q1Sum of square of deviations between representative group, Q2
Sum of square of deviations in representative group, v1Freedom degree between representative group, v2The representative group internal degree of freedom.
Calculate combined standard uncertainty:
Multiple laboratories are used with the solid non-ferrous metal standard sample of a variety of method definite values, the B class of normally result is not
Degree of certainty uBWith unstability uncertainty urNegligible, then the uncertainty of this standard sample development process includes: definite value process
Uncertainty caused by single measurement standard deviation and inhomogeneities.
Calculate expanded uncertainty U:
Wherein, U indicates uncertainty, Q1Sum of square of deviations between representative group, Q2Sum of square of deviations in representative group, v1Represent group
Between freedom degree, v2The representative group internal degree of freedom,The coercive force of expression hard alloy standard sample or magnetically saturated characteristic value,I-th mechanism for testing is represented to the measurement average value of the standard sample of same gradient, m is the number of mechanism for testing, and n is every
Testing time of family's mechanism for testing to each standard sample.
The standard value of this coercive force national standard sample is as follows:
The standard value of this magnetic saturation (cobalt magnetic) national standard sample is as follows:
It should be noted that embodiment described above for explaining only the invention, is not constituted to of the invention any
Limitation.By referring to exemplary embodiments, invention has been described, it should be appreciated that word used in it is descriptive
With explanatory vocabulary, rather than limited vocabulary.The present invention can be made within the scope of the claims by regulation
Modification, and the present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it relates to
And specific method, material and embodiment, it is not intended that the present invention is limited to particular case disclosed in it, on the contrary, this hair
It is bright to can be extended to other all methods and applications with the same function.
Claims (10)
1. the preparation method of a kind of hard alloy coercive force or magnetic saturation standard sample, comprising:
Step S1 determines the definite value gradient of hard alloy coercive force or magnetic saturation standard sample；
Step S2, prepare coercive force or magnetic saturation value in step sl determined by definite value gradient scope hard alloy standard
Sample carries out quality testing to hard alloy standard sample；
Step S3 randomly selects standard sample and carries out uniformity testing；
Step S4 after uniformity testing is qualified, randomly selects standard sample and transfers to m family's mechanism for testing test coercive force or magnetic full
And performance, m >=7, it is preferable that every mechanism for testing is to each sample test n times, n >=3, preferably 5；
M family laboratory measures in step S4 coercive force or magnetic saturation result are carried out Mathematical Statistics Analysis by step S5；
Step S6, the coercive force or magnetic saturation based on mathematical statistics qualification are as a result, determine that hard alloy coercive force or magnetic are full
With the characteristic value of standard sample and determine the uncertainty of characteristic value, so determine hard alloy standard sample coercive force or
Magnetically saturated standard value.
2. preparation method according to claim 1, which is characterized in that the definite value gradient of the coercive force includes 4 ladders
Degree, respectively first gradient: 5KA/m is hereinafter, the second gradient: 9-12KA/m, 3rd gradient: 19-22KA/m and 4th gradient:
36-40KA/m。
3. preparation method according to claim 1 or 2, which is characterized in that the magnetically saturated definite value gradient includes 3 ladders
Degree, respectively first gradient: 1%Co is hereinafter, the second gradient: 10-14%Co, 3rd gradient: 22-26%Co.
4. preparation method according to any one of claim 1-3, which is characterized in that quality testing includes object in step S2
Rationality can be with institutional framework detection；Preferably, physical property includes coercive force, magnetic saturation, hardness and density, institutional framework packet
Include heterogeneous microstructure and defect.
5. preparation method described in any one of -4 according to claim 1, which is characterized in that randomly selected in the step S3The above standard sample carries out uniformity testing, and N is the sum of standard sample.
6. preparation method according to any one of claims 1-5, which is characterized in that in step S4, using GB/T3848-
2017 " hard alloy coercive (magnetic) power measuring methods " test coercive force, and using GB/T23369-2009, " hard alloy magnetic is full
The standard test method of (MS) measurement " test magnetic saturation.
7. preparation method according to claim 1 to 6, which is characterized in that the Mathematical Statistics Analysis includes equal
Test of homogeneity, test of outlier, normal distribution-test and equally accurate are examined.
8. preparation method described in any one of -7 according to claim 1, which is characterized in that hard alloy standard is calculated as follows
The coercive force of sample or magnetically saturated characteristic value:
M is the number of mechanism for testing,Indicate i-th mechanism for testing to the measurement average value of the standard sample of same gradient；
The coercive force of expression hard alloy standard sample or magnetically saturated characteristic value.
9. preparation method according to claim 1 to 8, which is characterized in that the uncertainty of the characteristic value
Are as follows:
Wherein, U indicates uncertainty, Q1Sum of square of deviations between representative group, Q2Sum of square of deviations in representative group, v1Between representative group certainly
By spending, v2The representative group internal degree of freedom,Indicate coercive force or magnetically saturated characteristic value,Every mechanism for testing is represented to same
The measurement average value of the standard sample of gradient, m are the number of mechanism for testing, and n is every mechanism for testing to each standard sample
Testing time.
10. preparation method according to claim 9, which is characterized in that the coercive force and magnetically saturated standard value are as follows:
Wherein, I be coercive force or magnetically saturated standard value,Indicate coercive force or the magnetic saturation of hard alloy standard sample
Characteristic value, U indicate uncertainty.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111650096A (en) * | 2020-04-24 | 2020-09-11 | 株洲硬质合金集团有限公司 | Fisher-type particle size standard sample and preparation method and application thereof |
| WO2021128520A1 (en) * | 2019-12-23 | 2021-07-01 | 郑州大学 | Magnetic moment correction method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103243253A (en) * | 2013-05-16 | 2013-08-14 | 成都斯锐特钨钢刀具有限公司 | Cemented carbide and preparation method thereof |
| CN102539207B (en) * | 2011-12-27 | 2013-11-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing standard sample for testing content of hard-alloy components and method for testing content of hard-alloy components |
| CN103674659A (en) * | 2013-12-27 | 2014-03-26 | 株洲硬质合金集团有限公司 | Preparation method of standard sample of free carbon of tungsten carbide powder |
| CN106153569A (en) * | 2016-07-08 | 2016-11-23 | 株洲硬质合金集团有限公司 | The preparation of refractory metal oxygen standard sample, application and the choosing method of sample niobium powder |
| CN107557639A (en) * | 2017-09-27 | 2018-01-09 | 武汉新锐合金工具有限公司 | A kind of three-phase structure hard alloy and preparation method thereof |
| WO2018143230A1 (en) * | 2017-01-31 | 2018-08-09 | 日立金属株式会社 | Method for producing r-t-b sintered magnet |
-
2018
- 2018-09-20 CN CN201811100375.XA patent/CN109143126A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539207B (en) * | 2011-12-27 | 2013-11-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing standard sample for testing content of hard-alloy components and method for testing content of hard-alloy components |
| CN103243253A (en) * | 2013-05-16 | 2013-08-14 | 成都斯锐特钨钢刀具有限公司 | Cemented carbide and preparation method thereof |
| CN103674659A (en) * | 2013-12-27 | 2014-03-26 | 株洲硬质合金集团有限公司 | Preparation method of standard sample of free carbon of tungsten carbide powder |
| CN106153569A (en) * | 2016-07-08 | 2016-11-23 | 株洲硬质合金集团有限公司 | The preparation of refractory metal oxygen standard sample, application and the choosing method of sample niobium powder |
| WO2018143230A1 (en) * | 2017-01-31 | 2018-08-09 | 日立金属株式会社 | Method for producing r-t-b sintered magnet |
| CN107557639A (en) * | 2017-09-27 | 2018-01-09 | 武汉新锐合金工具有限公司 | A kind of three-phase structure hard alloy and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021128520A1 (en) * | 2019-12-23 | 2021-07-01 | 郑州大学 | Magnetic moment correction method |
| CN111650096A (en) * | 2020-04-24 | 2020-09-11 | 株洲硬质合金集团有限公司 | Fisher-type particle size standard sample and preparation method and application thereof |
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