CN106645008B - New surface layer oxygen, nitrogen, protium detection method in high-temperature alloy material High speed finish machining - Google Patents
New surface layer oxygen, nitrogen, protium detection method in high-temperature alloy material High speed finish machining Download PDFInfo
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 238000001514 detection method Methods 0.000 title claims abstract description 74
- 239000000956 alloy Substances 0.000 title claims abstract description 66
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 56
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000001301 oxygen Substances 0.000 title claims abstract description 51
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 51
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 title claims abstract description 48
- 241000720974 Protium Species 0.000 title claims abstract description 48
- 238000003754 machining Methods 0.000 title claims abstract description 45
- 239000002344 surface layer Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000012545 processing Methods 0.000 claims abstract description 13
- 238000004458 analytical method Methods 0.000 claims abstract description 12
- 238000000611 regression analysis Methods 0.000 claims abstract description 12
- 238000007689 inspection Methods 0.000 claims abstract description 9
- 238000009472 formulation Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 230000027734 detection of oxygen Effects 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000005538 encapsulation Methods 0.000 claims abstract description 4
- 238000005520 cutting process Methods 0.000 claims description 13
- 230000035515 penetration Effects 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 description 21
- 238000012360 testing method Methods 0.000 description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 10
- 229910052739 hydrogen Inorganic materials 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 230000001419 dependent effect Effects 0.000 description 5
- 238000003908 quality control method Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- NAWXUBYGYWOOIX-SFHVURJKSA-N (2s)-2-[[4-[2-(2,4-diaminoquinazolin-6-yl)ethyl]benzoyl]amino]-4-methylidenepentanedioic acid Chemical compound C1=CC2=NC(N)=NC(N)=C2C=C1CCC1=CC=C(C(=O)N[C@@H](CC(=C)C(O)=O)C(O)=O)C=C1 NAWXUBYGYWOOIX-SFHVURJKSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- OLBVUFHMDRJKTK-UHFFFAOYSA-N [N].[O] Chemical compound [N].[O] OLBVUFHMDRJKTK-UHFFFAOYSA-N 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 239000002173 cutting fluid Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000013100 final test Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000010275 isothermal forging Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- 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
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- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
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Abstract
New surface layer oxygen, nitrogen, protium detection method in a kind of high-temperature alloy material High speed finish machining, comprising: step 1. formulates High speed finish machining technique and detection frequency to the part of high-temperature alloy material;New surface layer can be generated on part with the phased separation of chip during High speed finish machining, using remove in part chip as detect sample;Step 2. according to the technological requirements processes part, and is collected using the detection frequency of formulation to the chip removed in process as detection sample, by the encapsulation of each detection sample, the inspection of collection;Step 3. carries out the content detection of oxygen, nitrogen, protium with infrared-thermal conductivity combination method to each detection sample respectively;Step 4. carries out comprehensive analysis processing with content data of the regression analysis to the oxygen of each detection sample detected, nitrogen, protium, the content data of the comprehensive whole oxygen of detection sample, nitrogen, protium is obtained, and then obtains the content data of the oxygen on the new surface layer of part, nitrogen, protium.
Description
Technical field
It is new in specifically a kind of high-temperature alloy material High speed finish machining the present invention relates to the detection method of material surface quality
Surface layer oxygen, nitrogen, protium detection method.
Background technique
High-temperature alloy material refer at 600~1200 DEG C or more and certain stress condition under long service high-temperature metal material
Material has excellent high temperature strength, the comprehensive performances such as inoxidizability, corrosion and heat resistant, fatigue behaviour and fracture toughness, has become
For the irreplaceable critical material of military, civilian gas-turbine unit (such as aero-engine) hot end part.Due to combustion gas whirlpool
The applied high temperature alloy part of turbine is on active service under 600~1200 DEG C of high temperature and complex stress environment for a long time, work
Inclement condition, thus to the reliability requirement of its work height, its every physical-mechanical properties is required very strict.
In general, in order to make high temperature alloy part can satisfy technical requirements, high temperature alloy part mostly uses finish forge, whole
The near-net-shape methods such as body essence casting, monocrystalline essence casting, isothermal forging, hot isostatic pressing or powder metallurgy process are fabricated blank, high
Temperature alloy blank must it is machined after can finished product, the machining of high temperature alloy blank is that High speed finish machining is handled.High temperature
Alloy part, because of violent plastic deformation and strong friction, can generate a large amount of cutting heat, in addition high temperature in machining
The thermal coefficient of alloy material is natively very low, so that the cutting temperature in narrow cutting zone easily be made to increase, reaches as high as
1000℃.Under such hot environment, the elements such as oxygen, nitrogen, hydrogen in surrounding medium are just easy to intrusion high temperature alloy zero
(cutting interface is the release surface of part and chip, and release surface makes part and chip generate new table respectively at the cutting interface of part
Layer) in, so that the new surface layer of the tool surface in cutting zone, part be made to generate alternate brittlement phase respectively, alternate brittlement phase will add
Acute materials microstructure stress concentration, can not only induce cutter crack, even tipping the phenomenon that, but also high temperature can be deteriorated
The mechanical behavior under high temperature and resistance to corrosion of alloy part.
It can be seen that how to control the content of the oxygen in high-temperature alloy material, nitrogen, protium, it is directly related to high temperature conjunction
The processing technology and mechanical property of golden material.Currently, the content control to oxygen, nitrogen, protium in high-temperature alloy material, mainly
Realization is reduced by strictly screening the means such as raw material, raising vacuum degree in high-temperature alloy material smelting or cast sections,
The content of the oxygen in high-temperature alloy material, nitrogen, protium is set to be reduced to acceptable level.However, oxygen in high-temperature alloy material,
The content control mode of nitrogen, protium can not be suitable for oxygen, nitrogen, the hydrogen on the new surface of high-temperature alloy material after High speed finish machining
The content of element controls, this is because: the residual gas such as oxygen, nitrogen, hydrogen are used as harmful element in high-temperature alloy material, with height
Main intensified element (such as Cr, Al, Ti and Nb element) in temperature alloy material has very strong affinity, in processing environment
Oxygen, nitrogen, protium are easily invaded during High speed finish machining in the new surface layer of high-temperature alloy material, removal residual gas nitrogen,
Oxygen, hydrogen are by no means easy, this is also at present not by oxygen, nitrogen, the protium on the new surface layer of high-temperature alloy material after High speed finish machining
Content, bring reason for it within high-temperature alloy material quality control on the surface scope into.
If bringing the content of the oxygen on the new surface layer of high-temperature alloy material after High speed finish machining, nitrogen, protium into high temperature
Within the control scope of alloy material surface quality, then the oxygen being related to in high-temperature alloy material, nitrogen, protium is needed to contain
Amount is detected, and then formulates the control program to processing environment according to testing result, final to realize high-temperature alloy material surface
Nitrogen, oxygen, protium content control, that is, realize high-temperature alloy material surface quality control.
Currently, the detection of oxygen, nitrogen, protium content in high-temperature alloy material is mainly real with infrared-thermal conductivity combination method
Existing.The working principle of infrared-thermal conductivity combination method is substantially are as follows: the detection sample of a known weight is placed on graphite crucible
In, it is then melted in electrode furnace under helium protection, oxygen is restored by carbon, with CO and CO2Form release, helium carrier gas will discharge
Analysis gas out flows through mass flow controller after copper oxide furnace, stably enters various detection cells;Rare-earth oxidation copper
CO is converted by CO2, infrared detector quantitative detection CO2Content;Nitrogen is decomposed and with N2Form release, by thermal conductivity detector
Detection;Hydrogen is thermal decomposited and with H2Form release is overheated rare-earth oxidation copper and is oxidized to H2O, steam are examined by dedicated infrared detection pond
Survey, after be converted to hydrogen content.Infrared-thermal conductivity the combination method has the spies such as detection limit is low, high sensitivity, stability is good, can trace to the source
Point, and fully achieved automation and made detection speed fast, it can satisfy wanting for the quality inspection timeliness in actual production
It asks.
However, infrared-thermal conductivity combination method is higher to the specification requirement of inspection detection sample, the generally indicated weight of precision processing
For the cylindrical body of 1g.If the high temperature alloy part after high speed or ultrahigh speed finishing is made into standard detection sample, need to carry out
All multi-process such as wire cutting, polishing, cleaning, long period can not meet the timeliness requirement of actual production;In addition, plus
The oxygen, nitrogen, the protium that invade in work environment are mainly enriched in the new surface layer of high temperature alloy part, and Dispersed precipitate is not closed in high temperature
The inside of metal parts can be such that final testing result seriously loses if high temperature alloy part to be fabricated to the detection sample of standard
Very.
Summary of the invention
Technical purpose of the invention is: in view of the above shortcomings of the prior art, providing a kind of easy to operate, simple side
Just, new surface layer oxygen in the high-temperature alloy material High speed finish machining that detection cycle is short, timeliness is good, testing result accuracy is high, nitrogen,
The rapid detection method of protium.
Mentality of designing of the invention is mainly: the forming process on the i.e. new surface layer of part machined surface-is exactly chip in fact
With the separation process of part base solid, oxygen, nitrogen, hydrogen when high-temperature alloy material carries out High speed finish machining cutting, in processing environment
Element is invaded simultaneously in the release surface (i.e. their respective new surface layer) of high temperature alloy part and chip, therefore, the new table of chip
Layer in oxygen, nitrogen, protium content theoretically in the new surface layer of high temperature alloy part oxygen, nitrogen, protium content be
It is identical;Moreover, high temperature alloy part is when carrying out High speed finish machining cutting, the cutting depth of use be it is smaller, so
The thickness of the chip of formation is than relatively thin, in this way it is to be understood that the oxygen on the new surface layer of chip, nitrogen, hydrogen are more inside chip
Distribution is dissipated, that is, the oxygen on new surface layer, nitrogen, hydrogen are in the Dispersed precipitate of high temperature alloy inside parts;Described before comprehensive, the present invention is to divide
, as detection sample, new table of the high-temperature alloy material through generating in High speed finish machining is realized from the chip on high temperature alloy part
Layer in oxygen, nitrogen, protium content it is timely, quickly and accurately detect.
The present invention realizes its technical purpose the technical scheme adopted is that new in a kind of high-temperature alloy material High speed finish machining
Surface layer oxygen, nitrogen, protium detection method, including the following steps:
Step 1. formulates High speed finish machining technique and detection frequency to the part of high-temperature alloy material;In High speed finish machining mistake
New surface layer can be generated on part with the phased separation of chip in journey, using remove in part chip as detect sample;
Step 2. requires to carry out part High speed finish machining according to the technique of formulation, and with the detection frequency of formulation to high speed
The chip removed in finishing passes is collected as detection sample, by the encapsulation of each detection sample, the inspection of collection;
Step 3. carries out the content detection of oxygen, nitrogen, protium with infrared-thermal conductivity combination method to each detection sample respectively;
Step 4. is carried out comprehensive with content data of the regression analysis to the oxygen of each detection sample detected, nitrogen, protium
Analysis processing is closed, obtains the content data of the comprehensive whole oxygen of detection sample, nitrogen, protium, and then obtain high-temperature alloy material
The content data of part oxygen, nitrogen, protium on new surface layer in High speed finish machining;The analysis of the regression analysis, which is handled, to be calculated
Model are as follows:
Y=β0+β1x1+β2x2+...+βmxm+ε;
In formula, y is the comprehensive whole content data of variable-corresponding element;
x1、x2、...、xmFor independent variable-High speed finish machining technological parameter;
β0、β1、β2、...、βmFor regression coefficient;
ε is accidental error.
Preferably, detection frequency >=3 time formulated in step 1.The quality for the detection sample collected in step 2 >=
1g。
The method have the benefit that:
Above-mentioned detection method for oxygen of the high-temperature alloy material in the new surface layer generated in High speed finish machining process, nitrogen,
The content detection of protium and propose, the chip of high temperature alloy part is located away from using under High speed finish machining as infrared-thermal conductivity
The detection sample of combination method, the detection sample can not only really react the oxygen, nitrogen, protium on the new surface layer of high-temperature alloy material
Content data, and the molding of the detection sample can substantially shorten the sample preparation time, so not only effectively reduce sample preparation at
Originally, timeliness requirement when and meeting actual production to quality control;
Meanwhile above-mentioned detection method integrates detection data obtained in detection sample with corresponding regression analysis
Analysis processing, thus comprehensively, the content stablizing, accurately and reliably obtain the oxygen on the new surface layer of high-temperature alloy material, nitrogen, protium
Data, testing result accuracy is high, and authenticity is good;
In conclusion the present invention has, easy to operate, simple and convenient, detection cycle is short, timeliness is good, testing result is accurate
Spend height, good economy performance, it is reliable and practical the features such as;In addition, the high temperature after High speed finish machining can be closed by above-mentioned detection method
The oxygen on the golden new surface layer of material, nitrogen, protium content bring within the quality control on the surface scope of high-temperature alloy material, thus
Extension from surface layer internally is realized to the concern of high-temperature alloy material surface quality, while to other materials under high-temperature long life
Quality control on the surface have directive property meaning.
Detailed description of the invention
Fig. 1 is flow diagram of the invention.
Fig. 2 is the design of part schematic diagram that the present invention is applied to test example.
Fig. 3 is the side view of Fig. 2.
Specific embodiment
The present invention is high-temperature alloy material (such as high-temperature alloy material applied to aero-engine hot-end component) in height
In fast finishing passes, the detection method of content of the oxygen in new surface layer (face), nitrogen, protium is generated.It is shown in Figure 1, this hair
It is bright to include the following steps:
Step 1. according to the characteristic of high-temperature alloy material, to the part of high-temperature alloy material formulate High speed finish machining technique and
Detect frequency, it is desirable that detection frequency >=3 time of formulation;With the phased separation of chip and in part during High speed finish machining
On can generate new surface layer, using remove in part chip as detect sample;
Step 2. requires to carry out part High speed finish machining according to the technique of formulation, and with the detection frequency of formulation to high speed
The chip removed in finishing passes is collected as detection sample: collection movement is completed under shutdown status, collected
Detection sample be usually most newly generated chip, it is desirable that collection detection sample quality >=1g;By each detection sample of collection
The encapsulation of this loading hermetic bag, inspection;
Step 3. carries out the content detection of oxygen, nitrogen, protium with infrared-thermal conductivity combination method to each detection sample respectively, i.e.,
Corresponding calibration, detection are carried out by its demarcation flow according to detecting instrument of each detection sample to infrared-thermal conductivity combination method, until
All detection finishes the detection sample of each frequency time;Each detection data is recorded respectively;
Step 4. is carried out comprehensive with content data of the regression analysis to the oxygen of each detection sample detected, nitrogen, protium
Analysis processing is closed, obtains the content data of the comprehensive whole oxygen of detection sample, nitrogen, protium, and then obtain high-temperature alloy material
The content data of part oxygen, nitrogen, protium on new surface layer in High speed finish machining;The analysis of the regression analysis, which is handled, to be calculated
Model are as follows:
Y=β0+β1x1+β2x2+...+βmxm+ε;
In formula, y is the comprehensive whole content data of variable-corresponding element;
x1、x2、...、xmFor independent variable-High speed finish machining technological parameter;
β0、β1、β2、...、βmFor regression coefficient;
ε is accidental error.
In above-mentioned steps 4, the theoretical basis of regression analysis is least square method and statistical principle, i.e., according to one
Or the change conditions prediction of one group of independent variable has the future value of certain stochastic variable of correlativity with it.In scientific experimentation, often
The multi-group data of the multiple variables often obtained according to actual measurement, finds out approximate functional relation between variable, i.e. analysis processing calculates
Model.
The evolution process of the analysis processing computation model of regression analysis is specific as follows:
One, regression analysis basic principle
If variable y and m independent variable (x1,x2,...,xm) there are linear relationship (referred to as regression equations), see formula (1) institute
Show:
Y=β0+β1x1+β2x2+...+βmxm+ε (1);
In formula, y is the comprehensive whole content data of variable-corresponding element;
x1、x2、...、xmFor independent variable-High speed finish machining technological parameter;
β0、β1、β2、...、βmFor regression coefficient;
ε is accidental error;
In formula (1), the reckoning of regression coefficient, evolution process are as follows:
-- it is located in n group observation data, xjIt is x in the observation of i-thij, then have multiple linear regression mathematical model, see
Shown in formula (2):
yi=β0+β1xi1+β2xi2+...+βmxim+εiI=1,2 ..., n (2);
In formula (2), εiFor the accidental error of i-th observation;
-- set β1,β2,...,βmCorresponding least-squares estimation value is b1,b2,...,bm, the then observation y of yiSee formula
(3) shown in:
yi=b0+b1xi1+b2xi2+...+bmxim+eiI=1,2 ..., n (3);
In formula (3), eiFor error εiEstimated value, that is, residual error;
-- set yiEstimated value beThen have shown in formula (4):
-- as residual error eiQuadratic sum Q when reaching minimum, observation yiWith estimated valueIt is fitted preferably to get such as following formula
(5):
-- b is determined by the differential method1,b2,...,bm, i.e. solving equations formula (6):
Abbreviation, which arranges, to obtain such as following formula (7):
It enables:
-- equation group formula (7) is write as matrix form, is seen as shown in following formula (8):
(X'X) (8) b=X'Y;
In formula (8), X' is the transposed matrix of X;
-- if note formula (7) coefficient matrices A, right end constant term are B, then have A=X'X, B=X'Y;If A full rank, i.e. A-1
In the presence of then just like following formula (9):
B=A-1B=(X'X)-1X'Y (9);
-- regression equation (4) must then solve;
Two, regression equation significance tests
For milling test data, each value y of dependent variable yi(i=1,2 ..., n) has fluctuation, whole n times
The total deviation size of observation can be used total sum of squares of deviations to indicate, see as shown in following formula (10):
In formula (10), LyyFor total deviation, that is, total sum of squares of deviations;
N is test level number;
I is independent variable quantity;
yiFor the observation of independent variable y;
For yiAverage value;
For yiEstimated value;
Q is residual sum of squares (RSS), and freedom degree p=n-m-1 includes test error and other factors;
U is regression sum of square, and freedom degree p=m reflects that independent variable itself changes caused fluctuation;
The inspection of F method of inspection can be used in overall regression effect;Rule of thumb first assume confidence alpha, F can be obtained by looking into F distribution tableα
The value of (m, n-m-1), if F value is greater than Fα(m, n-m-1), then it represents that popualtion regression significant effect;In addition, phase relation can also be used
Number R measures regression effect, R2=U/ (Q+U) is more intended to 1, indicates that the correlation between dependent variable and independent variable is closer.
It is right below using high temperature alloy NiCr16TiAl as test example (design of part is as shown in Figures 2 and 3, has boss)
It carries out High speed finish machining, and the oxygen, nitrogen on new surface layer, the content of protium quickly detect in the process, with this in technology of the invention
Hold and in detail, clearly and completely illustrate, specifically includes following content:
-- experimental condition are as follows: used lathe is VDL-850D vertical machining centre;Used milling cutter is diameter 16mm, 2
The indexable slotting cutter of Zhuzhou diamond (blade material code name YBG202) of tooth;Based on machining condition see as shown in table 1 below;It cuts
Cut the boss upper surface that position is part;
With such experimental condition, High-speed Finish Milling processing is carried out to the boss upper surface of high temperature alloy NiCr16TiAl part;
Table 1
-- it shuts down and collects most newly generated chip, be packed into hermetic bag inspection, quality is not less than 1g;Dry cut is collected as far as possible
Bits, if containing cutting fluid, it is recommended that being handled with air gun drying;
-- detecting instrument used by infrared-thermal conductivity combination method is the ONH836 oxygen nitrogen hydrogen analysis of Leco Corporation, U.S. research and development
Instrument;According to each detection sample, detecting instrument is demarcated respectively by demarcation flow, is detected;Testing result is as shown in table 1;
-- using regression analysis to high temperature alloy NiCr16TiAl, during High speed finish machining the oxygen, nitrogen on new surface layer,
The content detection data of protium are analyzed and processed, and regression equation is shown in as shown in following formula (11):
Regression is examined as follows:
The F test value of surface layer oxygen element content O: F=100000000.00 > F0.03(10,1)=672.546 return effect
Fruit highly significant, R2=1 dependent variable and independent variable are closely related;
The F test value of surface layer nitrogen element content N: F=162440.5 > F0.03(10,1)=672.546, regression effect is non-
Chang Xianzhu, R2=1 dependent variable and independent variable are closely related;
The F test value of surface layer protium content H: F=100000000.00 > F0.03(10,1)=672.546 return effect
Fruit highly significant, R2=1 dependent variable and independent variable are closely related;
And then it obtains high temperature alloy NiCr16TiAl part oxygen, nitrogen, protium on new surface layer in High speed finish machining and contains
Measure data.
The above specific technical solution and specific example are only to illustrate the present invention, rather than its limitations;Although referring to above-mentioned
Invention is explained in detail for specific example and specific technical solution, those skilled in the art should understand that:
The present invention can still modify to above-mentioned specific technical solution or equivalent replacement of some of the technical features,
And these are modified or replaceed, the spirit and scope of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (3)
1. new surface layer oxygen, nitrogen, protium detection method in a kind of high-temperature alloy material High speed finish machining, including the following steps:
Step 1. formulates High speed finish machining technique and detection frequency to the part of high-temperature alloy material;During High speed finish machining
New surface layer can be generated on part with the phased separation of chip, using remove in part chip as detect sample;
Step 2. requires to carry out part High speed finish machining according to the technique of formulation, and with the detection frequency of formulation to detection sample
It is collected, by the encapsulation of each detection sample, the inspection of collection;
Step 3. carries out the content detection of oxygen, nitrogen, protium with infrared-thermal conductivity combination method to each detection sample respectively;
Step 4. carries out comprehensive point with content data of the regression analysis to the oxygen of each detection sample detected, nitrogen, protium
Analysis processing obtains the content data of the comprehensive whole oxygen of detection sample, nitrogen, protium, and then obtains high-temperature alloy material part
The content data of the oxygen, nitrogen, protium on new surface layer in High speed finish machining;The analysis of the regression analysis handles computation model
Are as follows:
Y=β0+β1x1+β2x2+...+βmxm+ε;
In formula, y is the comprehensive whole content data of variable-corresponding element;
x1、x2、...、xmFor independent variable-High speed finish machining technological parameter, including cutting speed, feed engagement, side penetration of a cutting tool
Amount, back engagement of the cutting edge, nose radius;
β0、β1、β2、...、βmFor regression coefficient;
ε is accidental error.
2. new surface layer oxygen, nitrogen, protium detection method in high-temperature alloy material High speed finish machining according to claim 1,
It is characterized in that: detection frequency >=3 time formulated in step 1.
3. new surface layer oxygen, nitrogen, protium detection method in high-temperature alloy material High speed finish machining according to claim 1,
It is characterized in that: the quality >=1g for the detection sample collected in step 2.
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JP2012136767A (en) * | 2010-12-28 | 2012-07-19 | Jfe Steel Corp | Method for estimating phosphorus concentration in converter |
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JP2012136767A (en) * | 2010-12-28 | 2012-07-19 | Jfe Steel Corp | Method for estimating phosphorus concentration in converter |
CN104764695A (en) * | 2015-03-26 | 2015-07-08 | 中国船舶重工集团公司第七二五研究所 | Method for determining oxygen/nitrogen/hydrogen content in interalloy for titanium alloys |
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