CN100494959C - Method for preparing X-ray austenite measuring and caliberating sample - Google Patents
Method for preparing X-ray austenite measuring and caliberating sample Download PDFInfo
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- CN100494959C CN100494959C CNB2005100237785A CN200510023778A CN100494959C CN 100494959 C CN100494959 C CN 100494959C CN B2005100237785 A CNB2005100237785 A CN B2005100237785A CN 200510023778 A CN200510023778 A CN 200510023778A CN 100494959 C CN100494959 C CN 100494959C
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Abstract
The present invention relates to material analyzing and measuring technology. The preparation process of X-ray measuring and calibrating austenite sample includes the following steps: screening of austenite powder and ferrite powder; mixing austenite powder and ferrite powder in absolute alcohol in certain volume ratio mechanically; hot pressing the mixture powder into block material at high temperature and vacuum state; and machining calibrated sample with the block material and annealing in vacuum furnace. The measuring and calibrating austenite sample is used in calibrating X-ray diffraction system, and has its austenite content maintained stably for long period to ensure the reliable measurement result.
Description
Technical field
That the present invention relates to is a kind of preparation method of calibration sample, specifically, is a kind of preparation method of X ray austenite measuring and caliberating sample.Be used for the material analysis technical field of measurement and test.
Background technology
Before carrying out the measurement of X ray austenite, at first detect the calibration sample of known austenite content, whether normal with the tester system.Therefore, select suitable calibration sample most important to whole surveying work.The austenite measurement belongs to the X ray quantitative analysis tech, comprises internal standard method, K value method and intensity factor method, and simple X ray austenite measuring and caliberating sample preparation method is with some standard substance grind into powders.So far, still do not have ripe austenite measuring and caliberating sample preparation method, can not guarantee the reliability of X ray austenite measurement result.
Find by prior art documents, (the scientific and technological publishing house in Liaoning in " mechanical engineering material manual testing " that mechanical industry science and technology and quality supervision department write, 1999, the 400-402 page or leaf), calibration sample of having introduced the X ray quantitative test and preparation method thereof is: 1, select suitable standard substance such as SiO
22, with the standard substance grind into powder; 3, these powder are mixed in the testing sample, with this as calibration sample.Its weak point is: because the preparation method of this class calibration sample is too simple, and in actual X ray quantitative test process, must mix it in testing sample, the work of specified rate analysis to measure is made troubles, and can not guarantee the reliability of measurement result.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of preparation method of X ray austenite measuring and caliberating sample is provided, make its calibration sample of preparing, be convenient to execute-in-place, can farthest guarantee the reliability of X ray austenite measurement result.
The present invention is achieved by the following technical solutions, and concrete steps of the present invention are as follows:
(1) particle to austenite powder and ferrite dust screens, utilize the sieve of aperture 5 μ m to screen and limit powder full-size, utilize the sieve of aperture 2 μ m to screen and limit the powder minimum dimension, remove oversize or too small powder particle, particle size distribution is controlled at 2 μ m～5 mu m ranges.
Its principle of work is that in X ray austenite measuring process, particle size is one of key factor that influences measuring accuracy.The elimination of big particle makes the debye ring of each family of crystal planes continuous.Therefore, when detector swept away each diffraction ring, the diffraction peak intensity fluctuation was little, and the diffraction peak shape is good, thereby makes measured diffraction integral intensity accurate, and this accurately measures the precondition of austenite content just.Having limited particle size can not be too small, mainly is for fear of the diffraction peak phenomenon of disperse too, also helps improving the quality of X-ray diffraction peak shape, thereby improves the measuring accuracy of austenite content.Facts have proved that particle size distribution is controlled at 2 μ m～5 mu m ranges, promptly each particle is equivalent to about 10
5The stack of layer atom, both guaranteed that the debye diffraction ring of particle is continuous this moment, do not have the diffraction diffusing phenomenon again, so this range of size relatively is suitable for X ray quantitative test work.
(2) mix powder,, utilize mechanical system, in anhydrous alcohol solution, the austenite powder is mixed equably with ferrite dust according to austenite volume fraction (being the number percent that the volume of austenite powder accounts for austenite powder and ferrite dust volume).
Its principle of work is, when the austenite volume fraction of five kinds of calibration sample is respectively 10%, 20%, 30%, 40%, 50%, utilize above-mentioned five kinds of calibration sample, demarcate the X-ray diffraction system, its calibration result data are comprehensive, and help guaranteeing the measuring accuracy of instrument system.Austenite volume fraction or 10%, or 20%, or 30%, or 40%, or 50%, its reason is to meet engineering custom on the one hand, and main is because these data are spacedly distributed and are integer, carry out regretional analysis calculate time ratio be easier to and standard error little.In addition, have only the austenite powder is evenly mixed with ferrite dust, just can guarantee in effective penetration volume of X ray, poly-partially phenomenon does not separately all appear in two kinds of powder in the calibration sample, reduced the stochastic error of diffract spectral line, made measurement result reliable more and have a good repeatability.Mixing powder in anhydrous alcohol, mainly is to occur the heating phenomenon in mixed powder process, prevents that the material of austenite powder and ferrite dust from changing.
(3) hot-forming, 10
-3In the Pa vacuum mixed-powder is heated, heating-up temperature is 800 ℃, and austenite powder and ferrite dust is hot-forming, obtains voidage less than 3% block materials.
Its principle of work is, with particle powder hot-forming be block materials, belong to PM technique.Because 10
-3Heat in the Pa vacuum environment, can prevent effectively that two kinds of powder are oxidized, thereby guarantee that X ray austenite measuring and caliberating sample material is constant.Adopting hot-forming mode, mainly is to consider that ruckbildung all takes place for austenite powder and ferrite dust under 800 ℃ of states of temperature, can make between two kinds of powder this moment in conjunction with good, reduces voidage, improves the strength of materials of calibration sample.
(4) processing is handled, and utilizes above-mentioned block materials to be processed into the X ray austenite measuring and caliberating sample, 10
-3Carry out abundant heating anneal in the Pa vacuum drying oven and handle 650 ℃ of annealing temperatures, annealing time 2 hours.
Its principle of work is, process calibration sample after, handle through abundant heating anneal, can effectively reduce the level of unrelieved stress in the X ray austenite measuring and caliberating sample, and realize the stabilization of its materials microstructure.In addition, in vacuum drying oven, carry out heating anneal and handle, can avoid X ray austenite measuring and caliberating sample generation oxidative phenomena.No matter heating anneal is the reduction of unrelieved stress in the X ray austenite measuring and caliberating sample during handling, and perhaps the stabilization of materials microstructure all is thermodynamics rules of following the power exponent mode.Practice confirms, adopts the annealing process of 650 ℃ of above temperature and time 2 hours, can fully eliminate the unrelieved stress in the calibration sample
Owing to tiny austenite powder and ferrite dust are hot pressed into block materials, thereby have limited the material granule size and eliminated the texture phenomenon, guaranteed the authenticity of austenite measurement result, be not subjected to the restriction of various measuring conditions.Austenite in the calibration sample is a kind of stainless steel material, and ferrite is that pure iron also has stronger corrosion resistance, and the block materials of two kinds of powder has and is difficult for getting rusty and advantage such as surface aesthetic.This calibration sample size is less to be very light in weight, so easy to carry.Standard specimen has been removed unrelieved stress in the material effectively, and has been realized the stabilization of institutional framework through the vacuum high-temperature annealing in process, so the austenite content stable for extended periods of time, helps improving the reliability of measurement result.
The invention has the beneficial effects as follows: the X ray austenite measuring and caliberating sample that the present invention is prepared, be used to demarcate the X-ray diffraction system, guarantee the works fine state of instrument.Particle size in the restriction calibration sample is eliminated texture, is difficult for getting rusty, and is easy to carry, surface aesthetic, and the austenite content stable for extended periods of time has improved the measurement result reliability.
Description of drawings
Fig. 1 is an austenite X-ray diffraction spectral line in the calibration sample material
Fig. 2 is a ferrite X-ray diffraction spectral line in the calibration sample material
Fig. 3 is the shape and the size of calibration sample
Fig. 4 is that calibration sample austenite actual content and austenite are measured content
Fig. 5 is the relation of calibration sample austenite content and room temperature standing time
Embodiment
Provide following examples in conjunction with content of the present invention:
(1) powder particle size screening
Select austenite powder and ferrite dust, utilize the sieve of aperture 5 μ m to screen and limit powder full-size, utilize the sieve of aperture 2 μ m to screen and limit the powder minimum dimension, make the particle size distribution of acquisition be controlled at 2 μ m～5 mu m ranges.
(2) mix powder
Austenite powder and ferrite dust are put into anhydrous alcohol, utilize mechanical system, two kinds of powder are mixed equably.The austenite volume fraction is 10%, 20%, 30%, 40% and 50%, the calibration sample of a series of austenite contents that obtain.
(3) hot-forming
In 800 ℃ of temperature and 10
-3In the Pa vacuum environment, mixed-powder is through hot-briquetting modeling process, obtained voidage less than 3% block materials, between two kinds of powder in conjunction with good.As shown in Figure 1 and Figure 2, austenite and ferrite X-ray diffraction spectral line in the calibration sample material show and eliminate the thick and texture of particle in the material.
(4) processing is handled
Above-mentioned block materials is processed as shown in Figure 3 calibration sample.10
-3Carry out heating anneal in the Pa vacuum drying oven and handle, 650 ℃ of annealing temperatures and time 2 hours, finally eliminated the unrelieved stress in the calibration sample, and made the institutional framework sufficient stabilization of material.
(5) austenite is measured
By the X-ray diffraction system, measure the austenite content in each calibration sample, instrument parameter is: tube voltage 25kV, tube current 5mA, collimator diameter 2mm, Cr target K
aRadiant rays.Utilize austenitic (220) crystallography face and ferritic (211) crystallography face to measure, measurement result shows that the strictness of calibration sample austenite actual content and austenite measurement content is consistent as shown in Figure 4.
(6) estimation of stability
With above-mentioned calibration sample, under room temperature state, placed for 1 year, regularly carry out austenite and measure, the result is as shown in Figure 5.Show among the figure that the repeated experiments error of data confirms that the austenite content of calibration sample can stable for extended periods of time within ± 1%.
Claims (6)
1, a kind of preparation method of X ray austenite measuring and caliberating sample is characterized in that, concrete steps are as follows:
(1) powder particle size screening: the particle to austenite powder and ferrite dust screens, and the powder particle size that makes acquisition is in 2 μ m～5 mu m ranges;
(2) mix powder: according to the austenite volume fraction, utilize mechanical system, in anhydrous alcohol solution, the austenite powder is mixed equably with ferrite dust;
(3) hot-forming: in a vacuum mixed-powder is heated, austenite powder and ferrite dust is hot-forming, obtain block materials;
(4) processing is handled: utilize above-mentioned block materials to be processed into the X ray austenite measuring and caliberating sample, carry out abundant heating anneal and handle in vacuum drying oven.
2, the preparation method of X ray austenite measuring and caliberating sample according to claim 1 is characterized in that, described austenite volume fraction or 10%, or 20%, or 30%, or 40%, or 50%.
3, the preparation method of X ray austenite measuring and caliberating sample according to claim 1 is characterized in that, the vacuum described in (3) step is hot-forming, and its vacuum tightness is 10
-3Pa.
4, the preparation method of X ray austenite measuring and caliberating sample according to claim 1 is characterized in that, describedly in a vacuum mixed-powder is heated, and its heating-up temperature is 800 ℃.
5, the preparation method of X ray austenite measuring and caliberating sample according to claim 1 is characterized in that, the voidage of described block materials is less than 3%.
6, the preparation method of X ray austenite measuring and caliberating sample according to claim 1 is characterized in that, described vacuum drying oven, and its pressure is 10
-3Pa, annealing temperature is 650 ℃, the time of annealing is 2 hours.
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| CNB2005100237785A CN100494959C (en) | 2005-02-03 | 2005-02-03 | Method for preparing X-ray austenite measuring and caliberating sample |
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| CN102680502B (en) * | 2012-04-27 | 2014-04-09 | 中国航空工业集团公司北京航空材料研究院 | Method for measuring metal bar textures |
| CN102706708B (en) * | 2012-06-06 | 2014-12-10 | 沈阳飞机工业（集团）有限公司 | Calibration test cube manufacturing method for X-ray residual stress testing system |
| CN104062310B (en) * | 2014-05-23 | 2017-09-05 | 武汉钢铁有限公司 | The method of residual austenite content in accurate measurement ferrous materials |
| CN106033037B (en) * | 2015-03-18 | 2018-07-20 | 中国科学院金属研究所 | A kind of residual stress standard specimen preparation method |
| JP7059974B2 (en) * | 2019-03-25 | 2022-04-26 | 新東工業株式会社 | Manufacturing method of reference piece for X-ray residual stress measurement and reference piece for X-ray residual stress measurement |
| CN110609048A (en) * | 2019-09-19 | 2019-12-24 | 西安交通大学 | Calibration method based on monochromatic X-ray diffraction |
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Assignee: Shanghai Mingjia Metal Technology Co.,Ltd. Assignor: Shanghai Jiao Tong University Contract record no.: 2010310000134 Denomination of invention: Method for preparing X-ray austenite measuring and caliberating sample Granted publication date: 20090603 License type: Exclusive License Open date: 20050803 Record date: 20100802 |
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