CN105954144A - Density measurement equipment and method for variable-temperature metal - Google Patents

Abstract

The invention discloses density measurement equipment and method for variable-temperature metal. The density measurement equipment comprises an image acquisition system and a sample test system, wherein a CCD (charge coupled device) camera and a laser source of the image acquisition system are distributed at two ends of a furnace body respectively, and the CCD camera, laser source and the furnace body are mounted on the same track; the CCD camera is connected with a video controller which is connected with a computer and image processing software; a sample table and a heating element are mounted in the middle of the furnace body, and optical windows are mounted at two ends of the furnace body; a gas inlet and a gas outlet are formed in two sides of the furnace body respectively, and the gas outlet is connected with a vacuum pump; a thermocouple is arranged in the furnace body and connected with a temperature controller. During detection, a sample is heated to a required measurement temperature through the temperature controller, sample images are acquired and analyzed through the image acquisition system and the image processing software, the volume of the measured sample is obtained, and the density of the sample at the temperature is obtained through calculation. The operation is simple, the data are precise, and the measurement object range is wide.

Description

A kind of alternating temperature density metal measures equipment and measuring method thereof

Technical field

The invention belongs to density measure technical field, a kind of alternating temperature density metal measures equipment And measuring method, measure the density of metal under different temperatures fast and accurately, be suitable for most metal (including alloy) is in solid-state or the density measurement of molten state.

Background technology

Density is the important physical amount of quantitative description substance characteristics, has reacted material because of intermolecular force difference And the coherent condition presented, the subjects such as physics, metallurgy and materialogy are all had great importance.For liquid For state metal, density is to study the important parameter of the performances such as its structure, surface tension, viscosity and diffusion. Along with temperature raises, metal and alloy all can occur solid-state phase changes, when continuing to rise high-temperature to fusing point, can send out Raw solid-liquid transformation.All of solid-solid changes and solid-liquid transformation is all along with the transformation of volume transformation, i.e. density, And then affect the performance of material and device.Therefore, either for commercial Application or scientific research, Accurate density data is all indispensable important physical amount.

At present, there are many methods can measure the density of normal temperature metal, but for alternating temperature, particularly Metal under high temperature and high-melting-point, the density of high chemically active liquid metal, also lack and survey fast and accurately Metering method.

Summary of the invention

In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of alternating temperature density metal measurement and set Standby and measuring method, after sample is heated to the temperature measured, soft by image capturing system and image procossing The image of sample is acquired and analyzes by part, obtains the volume of sample, thus is calculated sample and exists Density at a temperature of Gai, accuracy is high, simple to operate.

The technical scheme that the present invention is used for achieving the above object is as follows:

A kind of alternating temperature density metal measures equipment, including image capturing system and sample test system；Wherein swash Radiant, CCD camera, Video Controller and computer and image processing software constitute image capturing system； Body of heater and attachment device thereof constitute sample test system；CCD camera and LASER Light Source are arranged in body of heater respectively Two ends, three is installed on same track；CCD camera is connected with Video Controller, Video Controller with Computer and image processing software are connected；

Sample stage is installed in the middle part of body of heater, in body of heater one week equipped with heating element heater；

Described body of heater two ends are respectively arranged with optical window, arrange cooling water pipeline around optical window；

Described body of heater is respectively provided on two sides with air inlet and gas outlet in order to control atmosphere in body of heater, and gas outlet is with true Empty pump is connected；Temperature in described body of heater is controlled by thermocouple by temperature controller.

Measure the density measuring method of equipment based on above-mentioned alternating temperature density metal, be under vacuum, pass through Temperature controller heats the sample to temperature to be measured, and gathers sample image by image capturing system, Process sample image by image processing software, be calculated sample volume.Solid state density measurement requirement sample Being shaped as cylinder, liquidus density is measured sample shape not requirement.

Specifically, the density measuring method of equipment is measured based on above-mentioned alternating temperature density metal, including following step Rapid:

Step 1, weighing sample quality, be designated as m；

Step 2, sample it is placed in substrate and is positioned on sample stage, closing body of heater, it is ensured that be true in body of heater Sky, and it is filled with noble gas；

Step 4, start-up temperature controller, heating sample is allowed to warm to temperature required, after temperature stabilization, Open LASER Light Source, CCD camera, Video Controller and computer and image processing software record sample drawing Picture；

Step 5, process image with image processing software, first substrate and edge are edited, then place The image managed is divided into i discoid figure according to 1 pixels tall, if each disc radius is r_i, highly For h, then the volume of disk is obtained by formula (1):

$V_i={\mathrm{\πr}}_i^{2}h---\left(1\right)$

May determine that 1 relation between pixel and h with a standard sample, then sample volume can be by public affairs Formula (2) obtains:

$V={\mathrm{\Σ}}_{i=1}^{i=i}{\mathrm{\πr}}_i^{2}h,---\left(2\right)$

Step 6, according to formula (3), with what the sample quality m recorded in step 1 and step 5 recorded Sample volume V, obtains the density of sample

ρ=m/V (3).

The present invention has a following beneficial effect:

(1) measuring equipment simple to operate, test accuracy is high, limits sample seldom；

(2) temperature range is wide, can measure the density of (metal is from solid-state to liquid) from room temperature to high temperature, because of This is possible not only to measure low melting point liquid metal, it is also possible to measure high-melting-point, high chemically active metal；Suitable Extensive by object range, may be used for most metals (including alloy).

Accompanying drawing explanation

Fig. 1 is the structural representation that alternating temperature density metal of the present invention measures equipment；

Fig. 2 is that the embodiment of the present invention 1 is by measuring image (the a-sample Sb that device measuring density obtains₂Te₃, B-sample Ge₂Sb₂Te₅)。

Label in figure: 1-CCD photographing unit, 2-optical window, 3-cooling water pipeline, 4-air inlet, 5-temperature Controller, 6-thermocouple, 7-gas outlet, 8-vacuum pump, 9-LASER Light Source, 10-aluminum alloy rail, 11-stove Body, 12-heating element heater, 13-sample stage, 14-computer and image processing software, 15-Video Controller.

Detailed description of the invention

Below example will be in conjunction with two kinds of high-melting-points, high chemically active alloy Sb₂Te₃600 DEG C of solid-states and Ge₂Sb₂Te₅At the density measure example of 700 DEG C of liquid, the present invention will be further described, but the present invention is not It is confined to specific embodiment.

Fig. 1 is the structural representation that alternating temperature density metal of the present invention measures equipment；With reference to shown in Fig. 1, measure Equipment image capturing system mainly by CCD camera 1, LASER Light Source 9, body of heater 11, Video Controller 15, Computer and image processing software 14；Wherein LASER Light Source 9, CCD camera 1, Video Controller 15 and Computer and image processing software 14 constitute image capturing system, body of heater 11 and attachment device thereof and constitute sample Test system；Attachment device herein refer to the sample stage 13 in body of heater, temperature controller 5, thermocouple 6, Heating element heater 12, optical window 2, cooling water pipeline 3, air inlet 4, gas outlet 7 and vacuum pump 8.

Body of heater 11 is arranged around body of heater built with heating element heater 12, heating element heater for one week；Pacify in the middle part of described body of heater Equipped with sample stage 13, sample stage is placed testing sample；Described body of heater two ends are respectively provided with optical window 2, Cooling water pipeline 3 is had around optical window；Described body of heater be respectively provided on two sides with air inlet 4 and gas outlet 7 in order to Controlling atmosphere in body of heater, gas outlet 7 is connected with vacuum pump 8；Temperature in described body of heater is by temperature controller 5 Controlled by thermocouple 6.

CCD camera 1 and LASER Light Source 9 are arranged and described body of heater two ends respectively, and three is installed on same On aluminum alloy rail 10.CCD camera is connected with Video Controller 15, Video Controller 15 and computer and Image processing software 14 is connected.

Embodiment 1

Inventive samples Sb₂Te₃Sb by purity 99.9%₂Te₃Powder fusion metallurgy forms, Ge₂Sb₂Te₅By 99.9% Sb₂Te₃Powder and 99.9% GeTe powder fusion metallurgy form.By Sb₂Te₃Powder loads internal diameter 6.5mm Quartz ampoule in, be smelted into bar-shaped Sb under vacuo₂Te₃Sample.Rod-like samples is cut into height 10mm Left and right cylindrical sample, with sand paper upper and lower surface be polished to #2000 and keep upper and lower surface parallel.For Ge₂Sb₂Te₅Sample shape not requirement.

Utilize the measurement device measuring Sb of the present invention₂Te₃And Ge₂Sb₂Te₅Alloy density, step is as follows:

Alloy sample is placed on sample stage 13；Under vacuum, by temperature controller 5 by Sb₂Te₃ And Ge₂Sb₂Te₅Alloy sample is separately heated to 600 and 700 DEG C；By image capturing system, gather Sb₂Te₃ And Ge₂Sb₂Te₅Alloy image；Sb is processed by image processing software₂Te₃And Ge₂Sb₂Te₅Alloy image, It is calculated Sb₂Te₃And Ge₂Sb₂Te₅Alloy volume.

Specifically comprise the following steps that

Step 1, weighing 1.728g Sb₂Te₃With 2.437g Ge₂Sb₂Te₅Alloy sample quality, is designated as m；

Step 2, sample is placed in MgO substrate and is positioned on sample stage 13, close body of heater 11, close Close air inlet 4, open gas outlet 7 and vacuum pump 8 evacuation 20 minutes；

Step 3, closedown vacuum pump 8, open air inlet 4 and be passed through argon 10 minutes, be then switched off air inlet 4, Open gas outlet 7 and vacuum pump 8, evacuation again；

Step 4, start-up temperature controller 5 heat sample makes it be warming up to 600 DEG C and 700 DEG C respectively, treats temperature After degree is stable, open at LASER Light Source 9, CCD camera 1, Video Controller 15 and computer and image Reason software 14 records sample image, obtains two images as shown in Figure 2；

Step 5, the image obtained by image processing software process step 4, first compile substrate and edge Volume, then the image handled well is divided into several discoid figures according to 1 pixels tall, if each circle Dish radius is r_i, height is h, then the volume of disk is obtained by formula (1):

$V_i={\mathrm{\πr}}_i^{2}h,---\left(1\right)$

May determine that 1 relation between pixel and h with a standard sample, then sample volume can be by public affairs Formula (2) is calculated

$V={\mathrm{\Σ}}_{i=1}^{i=i}{\mathrm{\πr}}_i^{2}h,---\left(2\right)$

This example is 0.287cm³And 0.436cm³；

Step 6, with the sample volume V recorded in the sample quality m recorded in step 1 and step 5, can To obtain the density of sample, this example is 6.02g/cm³And 5.59g/cm³, the results are shown in Table shown in 1:

ρ=m/V (3).

Table 1

Sample	Sb2Te3	Ge2Sb2Te5
			Temperature and state	600 DEG C of solid-states	700 DEG C of liquid
Sample quality (g)	1.728	2.437
			Sample volume (cm3)	0.287	0.436
Density p (g/cm3)	6.02	5.59

Claims (5)

1. an alternating temperature density metal measures equipment, it is characterised in that include image capturing system and sample test System；Wherein LASER Light Source, CCD camera, Video Controller and computer and image processing software are constituted Image capturing system；Body of heater and attachment device thereof constitute sample test system；

CCD camera and LASER Light Source are arranged in body of heater two ends respectively, and three is installed on same track； CCD camera is connected with Video Controller, and Video Controller is connected with computer and image processing software；

Being provided with sample stage and heating element heater in the middle part of body of heater, described body of heater two ends are respectively arranged with optical window；

Described body of heater is respectively provided on two sides with air inlet and gas outlet, and gas outlet is connected with vacuum pump；

Arranging thermocouple in described body of heater, thermocouple connects temperature controller.

Alternating temperature density metal the most according to claim 1 measures equipment, it is characterised in that heating element heater edge Within in body of heater one week, arrange.

Alternating temperature density metal the most according to claim 1 measures equipment, it is characterised in that optical window week Cloth puts cooling water pipeline.

4. the density measuring method of equipment, its feature is measured based on the alternating temperature density metal described in claim 1 It is, comprises the following steps:

Step 1, weighing sample quality, be designated as m；

Step 2, sample it is placed in substrate and is positioned on sample stage, closing body of heater, it is ensured that be true in body of heater Sky, and it is filled with noble gas；

Step 4, start-up temperature controller, heating sample is allowed to warm to temperature required, after temperature stabilization, Open LASER Light Source, CCD camera, Video Controller and computer and image processing software record sample drawing Picture；

Step 5, process image with image processing software, first substrate and edge are edited, then place The image managed is divided into i discoid figure according to 1 pixels tall, if each disc radius is r_i, highly For h, then the volume of disk is obtained by formula (1):

V_i=π r_i ²h (1)

May determine that 1 relation between pixel and h with a standard sample, then sample volume can be by public affairs Formula (2) obtains:

$V={\mathrm{\Σ}}_{i=1}^{i=i}{\mathrm{\πr}}_i^{2}h,---\left(2\right)$

Step 6, according to formula (3), with what the sample quality m recorded in step 1 and step 5 recorded Sample volume V, obtains the density of sample

ρ=m/V (3).

Alternating temperature density metal measuring method the most according to claim 4, it is characterised in that when measuring metal Solid state density time require sample shape be cylinder, measure metal liquidus density time sample shape is not had Requirement.