CN114112794A - Measuring device and measuring method for shear viscosity of chalcogenide glass - Google Patents
Measuring device and measuring method for shear viscosity of chalcogenide glass Download PDFInfo
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- CN114112794A CN114112794A CN202111465609.2A CN202111465609A CN114112794A CN 114112794 A CN114112794 A CN 114112794A CN 202111465609 A CN202111465609 A CN 202111465609A CN 114112794 A CN114112794 A CN 114112794A
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- 239000005387 chalcogenide glass Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000011521 glass Substances 0.000 claims abstract description 56
- 238000012360 testing method Methods 0.000 claims abstract description 43
- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- 239000010453 quartz Substances 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000001125 extrusion Methods 0.000 claims abstract description 18
- 230000006835 compression Effects 0.000 claims description 9
- 238000007906 compression Methods 0.000 claims description 9
- 239000006060 molten glass Substances 0.000 claims description 6
- 238000010008 shearing Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 abstract description 9
- 238000000354 decomposition reaction Methods 0.000 abstract description 5
- 230000036541 health Effects 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 7
- 238000013461 design Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 230000004297 night vision Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000005304 optical glass Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000005906 dihydroxylation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 238000001931 thermography Methods 0.000 description 1
- 238000000411 transmission spectrum Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
- G01N11/12—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by measuring rising or falling speed of the body; by measuring penetration of wedged gauges
Abstract
The invention relates to a measuring device and a measuring method for shear viscosity of chalcogenide glass, wherein the measuring device comprises a heating system, a measuring system and a measuring device, wherein the heating system comprises a container and a heating device for heating the container; the squeezing system is arranged in the container and is used for squeezing the glass sample in the container; the measuring system comprises a communicating pipe, a first pressure sensor and a second pressure sensor; one end of the communicating pipe is communicated with the lower part of the container, and a first pressure sensor and a second pressure sensor are arranged below the communicating pipe at intervals. The invention sets the testing environment of the glass sample as a closed quartz container, solves the problems of oxidation and decomposition of the glass sample in the testing process, and avoids the problem of damage of volatile matters to the health of a tester in the testing process because the testing sample is in the sealed environment. The device can be used for repeated tests for many times, and the extrusion system is arranged, so that the requirement of high-temperature viscosity test can be met.
Description
Technical Field
The invention belongs to the technical field of optical material testing, and particularly relates to a measuring device and a measuring method for shear viscosity of chalcogenide glass.
Background
Chalcogenide glass is used as an infrared optical material, has the advantages of wide transmission spectrum range in an infrared band, stable photo-thermal property, excellent chemical stability, continuously adjustable performance, low preparation cost, easy processing, complementarity with infrared crystal materials such as monocrystalline germanium and the like in certain performance, and the like, in the design of an infrared optical component, the chalcogenide glass with low thermal difference coefficient and the crystal material with high thermal difference coefficient are combined and applied to an infrared optical system, so that the selection range of the infrared optical material can be greatly enriched, the flexibility of system design is increased, the system structure is simplified, more importantly, the imaging quality of the system under different environments (-55 ℃ -130 ℃) can be obviously improved, the temperature adaptability of optical systems such as infrared thermal imaging and the like is improved, the athermalization design requirement of the system is met, therefore, chalcogenide glass is regarded as a new generation of temperature self-adaptive infrared optical system core lens material, the infrared sensor can be widely applied to military (night vision gun aiming, infrared shoulder-carrying missile, fighter plane night vision cruise and the like) and civil (automobile night vision, security monitoring and the like) infrared systems, and has huge market prospect.
However, chalcogenide glass is non-oxide glass, the glass structure mainly comprises bridge sulfur bonds, the strength is far lower than that of bridge oxygen bonds, and the stability of the network structure directly influences the physical and chemical properties of the glass in various aspects. The internal structural stability, the thermal property and the mechanical property of chalcogenide glass and the forming of glass seriously restrict the application of chalcogenide glass in the photoelectric industry, so that the research on the viscosity-temperature characteristic of chalcogenide glass has great significance on the improvement of the production efficiency and the quality of glass elements.
According to the standard GBT10247-1988, the current viscosity measurement methods are mainly the capillary method, the falling sphere method, the rotation method and the vibration method. The high temperature viscometer of rotation method mainly measures the viscosity value through the torque that the continuous rotation of the rotor that soaks in the measured liquid formed, and the torque is proportional with the rotor that soaks in the sample by the drag that the stickness was drawn and is formed, therefore also is proportional with the viscosity, surveys the viscosity characteristic of fuse-element with the rotor under high temperature state promptly, and this needs the instrument to have characteristics such as accurate control to the temperature and accurate measurement to the viscosity. The capillary method is suitable for testing kinematic viscosity, and selected glass capillary viscometers are a flat-open Virgiz viscometer, a Cannon-Fensk viscometer, a Ubbelott viscometer and a counter-flow Cannon-Fensk viscometer. However, these glass containers are open, and thus the reaction of infrared chalcogenide optical glass components with air and the decomposition and volatilization at high temperature cannot be avoided. Chalcogenide glass is easily oxidized and decomposed when heated. The problems that the repeatability of a test result is not high, the high-temperature viscosity cannot be tested, and volatile matters damage the health of a tester in the test process can occur when the common optical glass viscosity test method is adopted to measure the chalcogenide glass.
Disclosure of Invention
The invention mainly aims to provide a measuring device for the shear viscosity of chalcogenide glass, and aims to solve the technical problems that chalcogenide glass is easy to oxidize and decompose in a test engineering, the repeatability of a test result is not high, the high-temperature viscosity cannot be tested, and volatile matters damage the health of a tester in the test process.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a measuring device for the shear viscosity of chalcogenide glass comprises:
a heating system comprising a container and heating means for heating the container;
the squeezing system is arranged in the container and is used for squeezing the glass sample in the container;
the measuring system comprises a communicating pipe, a first pressure sensor and a second pressure sensor;
one end of the communicating pipe is communicated with the lower part of the container, and a first pressure sensor and a second pressure sensor are arranged below the communicating pipe at intervals.
Further, still include:
and the sample collecting system comprises a collecting box connected to the other end of the communicating pipe and used for collecting samples after the test is finished.
The heating device comprises an electric furnace wire arranged at the lower part of the container.
The extrusion system comprises a pressure head, the end face of the pressure head, which is contacted with the glass sample, is of a plane structure, and the gap between the periphery of the pressure head and the inner wall of the container is 0-1.0 mm.
The communicating pipe is a cuboid quartz tube, and a thermocouple is arranged on the communicating pipe.
The container and the pressure head are made of quartz.
The collecting box is provided with an exhaust hole.
The invention also provides a method for measuring the shear viscosity of the chalcogenide glass by using the measuring device for the shear viscosity of the chalcogenide glass, which comprises the following steps of:
heating a glass sample in a container, and heating the glass sample to a test temperature;
secondly, preserving the heat for 30-50 minutes, and applying given pressure to a pressure head to enable the molten glass to overcome internal friction resistance and generate viscous flow;
recording the descending speed v of the pressure head, the compression time t from the beginning to the end of compression and the pressure value P when the glass sample flows through the first pressure sensor1And a pressure value P when passing through the second pressure sensor2Recording the temperature T of the glass sample measured by the thermocouple;
the shearing force of the glass sample between the two pressure sensors at the temperature T is as follows:
h is the internal height of the cuboid quartz tube, and L is the distance between the first pressure sensor and the second pressure sensor;
the shear rate was:
wherein W is the internal width of the cuboid quartz tube, and r is the radius of the pressure head;
the shear viscosity of the sample, as defined by the shear viscosity, is:
the descending speed v is 0.01-1 m/h.
By the technical scheme, the invention at least has the following advantages:
according to the invention, after the infrared chalcogenide glass sample is heated to the test temperature in the cavity, the given pressure is applied to the quartz pressure head to enable the molten glass in the quartz container to overcome the internal friction resistance to generate viscous flow, and the shear viscosity of the glass sample can be calculated according to the shear stress and the shear rate of the glass sample in the test system. The test environment of the glass sample is set to be a closed quartz container, so that the problems of oxidation and decomposition of the glass sample in the test process are solved, and the problem of damage of volatile matters to the health of a tester in the test process is avoided because the test sample is in a sealed environment. The device can be used for repeated tests for many times, and the extrusion system is arranged, so that the requirement of high-temperature viscosity test can be met.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a schematic structural diagram of a measuring apparatus for measuring shear viscosity of chalcogenide glass according to an embodiment of the present invention.
In the figure:
1, container; 2, glass samples; 3, communicating pipes; 4 a first pressure sensor; 5 a second pressure sensor; 6, a collection box; 7, a pressure head; 8, a thermocouple; 9 air exhaust holes.
Detailed Description
To further explain the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the embodiments, structures, features and effects of the present invention will be made with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
As shown in fig. 1, a measuring apparatus for shear viscosity of chalcogenide glass includes:
a heating system comprising a container 1 and heating means for heating the container 1;
a squeezing system arranged in the container 1 and used for squeezing the glass sample 2 in the container 1;
the measuring system comprises a communicating pipe 3, a first pressure sensor 4 and a second pressure sensor 5;
one end of the communicating pipe 3 is communicated with the lower part of the container 1, and a first pressure sensor 4 and a second pressure sensor 5 are arranged below the communicating pipe 3 at an interval L.
By adopting the measuring device, the glass sample is in a fully-closed state and is not in contact with gas, the influence on the test result caused by the oxidation and decomposition of chalcogenide glass in the test process is avoided, the glass sample in the quartz container is heated, when the glass sample is heated to the test temperature, the molten glass in the lower die cavity overcomes the internal friction resistance to generate viscous flow by applying given pressure to the upper die, the pipe flow phenomenon is formed, and the shear viscosity of the glass sample can be calculated according to the shear stress and the shear rate of the glass sample in the test system. The invention adopts a modular structure and has the advantages of simple maintenance, strong real-time performance, low operation cost and monitoring data sharing.
Further, still include:
the sample collecting system comprises a collecting box 6 which is connected to the other end of the communicating pipe 3 and used for collecting samples after the test is finished.
Preferably, the heating means comprise an electric furnace wire arranged in the lower part of the container 1.
The temperature control part of the invention adopts a high-precision digital temperature controller, a solid-state relay, a K-type thermocouple closed-loop control and a self-tuning PID to carry out real-time control; the PID control algorithm is a control algorithm which combines three links of proportion, integral and differentiation into a whole, is the most mature technology and the most widely applied control algorithm in a continuous system, wherein parameter setting of the PID controller is the core content of control system design, and the proportional coefficient, the integral time and the differential time of the PID controller are determined according to the characteristics of a controlled process, so that the control algorithm is mature.
The heating device adopts an electric furnace wire for heating, and the maximum testing temperature can reach 900 ℃.
Preferably, the pressing system comprises a pressing head 7, the end face of the pressing head 7, which is contacted with the glass sample, is of a plane structure, and the clearance between the periphery of the pressing head 7 and the inner wall of the container 1 is 0-1.0 mm. Namely, the circular diameter of the pressure head is slightly smaller than the inner diameter of the quartz mold cavity, and is preferably less than or equal to 1.0 mm. The indenter seals the glass sample and applies pressure to the heated glass sample to cause the glass sample to flow.
The extrusion system comprises an inlet high-precision turbine worm, a linear guide post secondary hanging rack, a three-jaw chuck and the like, wherein the extrusion system is controlled by an operation panel instruction to be issued to a programming control driver, and then a micro-stepping motor drives a pressure head to complete extrusion according to the instruction; the existing components can be adopted for realizing the extrusion work, and the extrusion device is a mature extrusion mode.
The invention can meet the requirement of high-temperature viscosity test of glass by arranging the extrusion system, can repeatedly measure, seals a test sample and avoids the oxidation and decomposition of chalcogenide glass in the test engineering.
Preferably, the communicating pipe 3 is a rectangular parallelepiped quartz pipe, and the thermocouple 8 is provided on the communicating pipe 3.
The measuring system of the invention consists of an inlet pressure sensor and a pressure display controller, wherein the pressure display controller displays the pressure at two ends in real time, and a K-type thermocouple monitors the actual temperature of a sample during testing at any time.
Preferably, the material of the container 1 and the pressure head 7 is quartz. The container and the pressure head are both made of quartz materials with smooth surfaces and subjected to dehydroxylation;
preferably, the collection tank 6 is provided with an exhaust hole 9. The vent hole 9 is arranged to exhaust the gas in the glass sample after the test is finished.
The invention also provides a measuring method of the shear viscosity of the chalcogenide glass, which comprises the following steps:
heating a glass sample in a container, and heating the glass sample to a test temperature; rate of temperature rise vLifting of wineV is more than or equal to 200 ℃/hLifting of wine≥80℃/h；
Secondly, preserving heat to enable the glass sample to reach thermal balance, wherein the heat preservation time is not less than 30 minutes, then placing an extrusion system in place, and applying a load to carry out extrusion operation on the glass sample; namely, a given pressure is applied to the pressure head to ensure that the molten glass overcomes the internal friction resistance to generate viscous flow; the extrusion process is controlled by an extrusion mechanism and a measuring system together, the extrusion feeding speed is controlled to be 0.01-1m/h, the uniform speed is adjustable, and the numerical value of the extrusion loading pressure is displayed in real time; and the high-precision turbine scroll bar, the two linear guide rail hangers and the pressure head jointly complete the flow of the sample in the horizontal direction.
Recording the descending speed v and the compression time t of the pressure head and the pressure value P when the glass sample flows through the first pressure sensor1And a pressure value P when passing through the second pressure sensor2Recording the temperature T of the glass sample measured by the thermocouple; the time from the start of the ram movement to the stop of the ram movement is the compression time t.
The shearing force of the glass sample between the two pressure sensors at the temperature T is as follows:
h is the internal height of the cuboid quartz tube, and L is the distance between the first pressure sensor and the second pressure sensor;
the shear rate was:
wherein W is the internal width of the cuboid quartz tube, and r is the radius of the pressure head;
the shear viscosity of the sample, as defined by the shear viscosity, is:
the descending speed v is 0.01-1 m/h.
The extrusion system also comprises a high-temperature-resistant and acid-alkali-resistant stainless steel charging barrel for containing a glass sample to be heated, the heating device is a heating furnace with an electric furnace wire, the quartz container is placed on the bracket, and the heating furnace is placed below the bracket and used for heating the quartz container.
The invention is further illustrated by the following specific examples of the invention:
example 1
Method for testing high temperature viscosity of glass:
firstly, pulling out a quartz pressure head, adding IRG206 chalcogenide glass into a quartz container, heating a glass sample in the quartz container, and heating at a temperature rise rate vLifting of wineHeating the glass sample to a test temperature T of 551 ℃ at 150 ℃/h;
secondly, preserving the heat for 40 minutes, and then applying given pressure to a pressure head to enable the molten glass to generate viscous flow;
recording the descending speed v of the pressure head to be 1m/h, wherein the compression time t from the beginning of compression to the end of compression is 0.05 hour, namely the time from the beginning of the movement to the stop of the movement of the pressure head is 0.05 hour, and the pressure value P of the glass sample when flowing through the first pressure sensor1Is 1.3X 108Pa and a pressure value P when flowing through the second pressure sensor2Is 2.0X 109Pa, recording the temperature T of the glass sample measured by the thermocouple as 551K;
the shearing force of the glass sample between the two pressure sensors at the temperature T is as follows:
wherein H is the internal height of the cuboid quartz tube and is 0.02m, and L is the distance between the first pressure sensor and the second pressure sensor and is 0.1 m;
the shear rate was:
wherein W is the internal width of the cuboid quartz tube and is 0.05m, and r is the radius of a pressure head and is 0.2 m; the shear viscosity of the sample, as defined by the shear viscosity, is:
Example 2
Essentially the same test method as in example 1, except that:
the test temperature T is 573K;
heat preservation for 30 minutes, rate of temperature rise vLifting of wineIs 200 ℃/h;
the specific measurement parameters are detailed in table 1.
Example 3
Essentially the same test method as in example 1, except that:
the test temperature T is 643K;
heat preservation for 50 minutes, rate of temperature rise vLifting of wineIs 80 ℃/h;
the specific measurement parameters are detailed in table 1.
Calculating the shear viscosity eta of the sample according to the shear viscosity calculation formula1，η2，η3。
The specific test and calculation results for examples 1-3 are shown in Table 1 below.
TABLE 1
The measuring device can meet the requirements of high-temperature viscosity tests of different chalcogenide glasses.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A measuring device for the shear viscosity of chalcogenide glass is characterized by comprising:
a heating system comprising a container and heating means for heating the container;
the squeezing system is arranged in the container and is used for squeezing the glass sample in the container;
the measuring system comprises a communicating pipe, a first pressure sensor and a second pressure sensor;
one end of the communicating pipe is communicated with the lower part of the container, and a first pressure sensor and a second pressure sensor are arranged below the communicating pipe at intervals.
2. The device for measuring the shear viscosity of chalcogenide glass according to claim 1, further comprising:
and the sample collecting system comprises a collecting box connected to the other end of the communicating pipe and used for collecting samples after the test is finished.
3. The apparatus for measuring shear viscosity of chalcogenide glass according to claim 1 or 2, wherein the heating means comprises an electric furnace wire disposed at a lower portion of the container.
4. The device for measuring the shear viscosity of chalcogenide glass according to claim 3, wherein the extrusion system comprises a pressure head, the end face of the pressure head, which is in contact with the glass sample, is of a planar structure, and the clearance between the periphery of the pressure head and the inner wall of the container is 0-1.0 mm.
5. The device for measuring the shear viscosity of chalcogenide glass according to claim 4, wherein the communicating tube is a rectangular quartz tube, and a thermocouple is arranged on the communicating tube.
6. The device for measuring the shear viscosity of chalcogenide glass according to claim 5, wherein the container and the pressure head are made of quartz.
7. The device for measuring the shear viscosity of chalcogenide glass according to claim 2, wherein the collection box is provided with an exhaust hole.
8. The method for measuring the shear viscosity of chalcogenide glass by using the device for measuring the shear viscosity of chalcogenide glass according to any one of claims 1 to 7, comprising the steps of:
heating a glass sample in a container, and heating the glass sample to a test temperature;
secondly, preserving the heat for 30-50 minutes, and applying given pressure to a pressure head when the glass sample is heated to the testing temperature to enable the molten glass to overcome internal friction resistance and generate viscous flow;
recording the descending speed v of the pressure head, the compression time t from the beginning to the end of compression and the pressure value P when the glass sample flows through the first pressure sensor1And a pressure value P when passing through the second pressure sensor2Recording the temperature T of the glass sample measured by the thermocouple;
the shearing force of the glass sample between the two pressure sensors at the temperature T is as follows:
h is the internal height of the cuboid quartz tube, and L is the distance between the first pressure sensor and the second pressure sensor;
the shear rate was:
wherein W is the internal width of the cuboid quartz tube, and r is the radius of the pressure head;
the shear viscosity of the sample, as defined by the shear viscosity, is:
9. the method according to claim 8, wherein the descending speed v is 0.01 to 1 m/h; the heating rate of the glass sample in the heating container is 80-200 ℃/h.
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