CN113248136A - Glass for neutron scattering device and preparation method thereof - Google Patents
Glass for neutron scattering device and preparation method thereof Download PDFInfo
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- CN113248136A CN113248136A CN202110598940.5A CN202110598940A CN113248136A CN 113248136 A CN113248136 A CN 113248136A CN 202110598940 A CN202110598940 A CN 202110598940A CN 113248136 A CN113248136 A CN 113248136A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
- C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
- C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B9/00—Blowing glass; Production of hollow glass articles
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
Abstract
The invention discloses glass for a neutron scattering device and a preparation method thereof, wherein the glass comprises the following components in percentage by weight: 15-25 wt% of BaO; 3-8 wt% of CaO; al (Al)2O310~18wt%;SiO250~65wt%;MgO 0~5wt%;R20-15 wt% of O; wherein R is2O is Li2O、Na2O and K2At least one of O. The preparation method comprises the following steps: mixing the raw materials according to the weight ratio, heating to 1400 ℃ and 1800 ℃, and preserving heat to obtain liquid glass; and carrying out forming treatment on the liquid glass, and then carrying out annealing treatment to obtain the glass for the neutron scattering device. BaO, CaO and Al of the invention2O3、SiO2The four are mutually matched, so that the transmittance can reachOr higher, and a glass softening point below 1050 ℃; the method is simple to operate, does not need special equipment or harsh forming conditions, and is easy for large-scale production.
Description
Technical Field
The invention relates to a glass material and a preparation method thereof, in particular to glass for a neutron scattering device and a preparation method thereof.
Background
China spallation neutron source is from the construction of Lawnian province in Guangdong Dongguan city in 2011, and successful targeting is performed in 2017 in 8 months to obtain neutron beam, which also marks that China has a spallation neutron source. Neutron detection is widely applied to the fields of nuclear reaction team devices, particle physics, military mine detection and nuclear explosion monitoring, cosmic ray detection, environmental radiation detection, material detection, medical inspection and the like. The glass articles required for neutron scattering experiments are an important component in the sample environment, including: observation window, vacuum container, gas-tight container, optics (prism, reflector, refractor). The glass material which requires high neutron transmittance for neutron scattering glass products is also a hardware basis of modern physical experiment design.
At present, all countries in the world still use GE180 glass raw materials of the last century 50 years, which can not meet modern requirements, and all large neutron sources seek substitutes and simultaneously meet the requirements of plastic glass container materials for neutron ray and light transmission. There are also studies on the use of a particulate physical test ceramic filler of glass encapsulating gas for improving the mechanical strength and insulation properties of glassware and preventing warping due to glass surface tension during sintering. The mechanism of neutron penetration through glass materials is complex, wherein the neutron energy of the elements with small atomic number of the materials is greatly reduced through elastic scattering, and meanwhile, the elements with small atomic number are easy to absorb by radiation capture reaction. In addition, since iron, manganese, chromium, boron, cadmium, and iron elements are activated or undergo isotopic changes upon neutron irradiation to absorb a large amount of neutrons, such elements cannot be contained in high-transmittance neutron glass.
Disclosure of Invention
The purpose of the invention is as follows: provides glass for a neutron scattering device with high neutron ray transmittance and strong low-temperature plasticity;
the second purpose of the invention is to provide a preparation method of the glass for the neutron scattering device.
The technical scheme is as follows: the glass for the neutron scattering device comprises the following components in percentage by weight: 15-25 wt% of BaO; 3-8 wt% of CaO; al (Al)2O3 10~18wt%;SiO2 50~65wt%;MgO 0~5wt%;R20-15 wt% of O; wherein R is2O is Li2O、Na2O and K2At least one of O.
Wherein when R is2O is Li2O、Na2O and K2When two or more of O are used, the two or more components may be mixed in any mass ratio.
Preferably, the glass for a neutron scattering device has a softening point of less than 1050 ℃.
The preparation method of the glass for the neutron scattering device comprises the following steps:
(1) mixing the raw materials according to the weight ratio, heating to 1400 ℃ and 1800 ℃, and preserving heat to obtain liquid glass;
(2) and carrying out forming treatment on the liquid glass, and then carrying out annealing treatment to obtain the glass for the neutron scattering device.
Preferably, in the step (2), the temperature of the annealing treatment is 600-780 ℃.
Preferably, in the step (4), the temperature is kept for 30-120min after annealing, and then furnace cooling is carried out.
Preferably, in the step (1), the heat preservation time is 4-12 h.
Preferably, in the step (1), the raw material is CaCO3、BaCO3、SiO2、MgCO3、Al2O3And R2CO3。
Preferably, in the step (1), bubbles are discharged by stirring with a quartz rod during heating.
Has the advantages that: compared with the prior art, the invention has the following advantages: (1) the high-transmittance glass of the invention has good transmittance to neutron radiation: the glass network structure and the chemical composition can allow uncharged neutrons to efficiently penetrate through the glass network structure, so that the glass network structure has good transmittance on the neutrons; the glass contains multiple components, such as BaO and Al2O3、SiO2Or MgO, R2O (R is Li, Na and K) and elements (iron, manganese, chromium, boron, cadmium, rolling and the like) with strong neutron capture capacity are not contained in the component, and experiments prove that the glass pair with the thickness of 2mm is suitable for glass pairs with the thickness of 2mmThe neutron transmittance is more than 90%. (2) The neutron high-transmittance glass discussed in the invention has good processability, and the softening point of the glass is below 1050 ℃, which is superior to quartz glass.
Drawings
FIG. 1 is a graph showing the results of neutron transmittance tests on glass in example 2 of the present invention.
Detailed Description
The present invention is described in further detail below.
Example 1
As 99% industrial pure CaCO399% of industrial pure BaCO399% industrial pure SiO299% of industrially pure MgCO399% of industrially pure Al2O3Chemically pure R2CO3The glass material prepared by using the raw materials comprises the following components: 19 wt% of BaO; 6 wt% of CaO; al (Al)2O315wt%;SiO260 wt%. The preparation method comprises the following steps:
(1) the glass material comprises the following components: adding the raw materials corresponding to the oxides into a stirrer, and uniformly mixing to obtain a glass raw material;
(2) adding the glass raw material obtained in the step (1) into a quartz crucible, heating the crucible to 1800 ℃, preserving heat for 5 hours at a high-temperature stage, and simultaneously stirring by using a quartz rod in the heating process;
(3) draining the glass liquid obtained in the step (2) into a grinding tool to be blown and drawn into a glass tube;
(4) and (4) annealing the glass tube formed in the step (3) to 780 ℃, preserving heat for 30 minutes, and cooling along with the furnace to obtain the glass material of the neutron scattering device.
The main properties of the glass material prepared in this example are shown in table 1.
Example 2
According to BaO 16 wt%; CaO 7 wt%; al (Al)2O3 14wt%;SiO2 61wt%;Na2O2 wt% of the stoichiometric batch.
The specific preparation process is basically the same as that of the embodiment 1, except that in the step (2), the crucible is heated to 1600 ℃, and is subjected to heat preservation for 8 hours and then is blown and drawn into a glass tube; and (3) annealing treatment is carried out for 60 minutes at 730 ℃ after the glass tube is formed in the step (3), so as to obtain the glass material of the neutron scattering device, and the neutron transmittance is shown in figure 1 through experimental tests.
The main properties of the glass material prepared in this example are shown in table 1.
Example 3
According to BaO 17 wt%; 4 wt% of CaO; al (Al)2O3 13wt%;SiO2 65wt%;Na2O1 wt% of the stoichiometric batch.
The specific preparation process is basically the same as that of the example 1, except that in the step (2), the crucible is heated to 1550 ℃, the temperature is kept for 6 hours, the crucible is blown and drawn into a glass tube, the glass rod is formed in the step (3), then annealing treatment is carried out, the temperature is kept for 60 minutes at 700 ℃, and furnace cooling is carried out, so that the glass material of the neutron scattering device is obtained.
The main properties of the glass material prepared in this example are shown in table 1.
Example 4
According to BaO 19 wt%; CaO 7 wt%; al (Al)2O3 16wt%;SiO2 55wt%;MgO 1wt%;K2O2 wt% of the stoichiometric batch.
The specific preparation process is basically the same as that of the example 1, except that in the step (2), the crucible is heated to 1550 ℃, the temperature is kept for 4 hours, the crucible is blown and drawn into a glass tube, and after the glass rod is formed in the step (3), the glass rod is annealed at 700 ℃ for 60 minutes to obtain the glass material of the neutron scattering device.
The main properties of the glass material prepared in this example are shown in table 1.
Example 5
According to 15 wt% of BaO; 5 wt% of CaO; al (Al)2O3 10wt%;SiO2 65wt%;MgO 0wt%;Na2O 2wt%;K2O3 wt% of the stoichiometric batch.
The specific preparation process is basically the same as that of the embodiment 1, except that in the step (2), the crucible is heated to 1550 ℃, the temperature is kept for 6 hours, the crucible is blown and drawn into a glass tube, and annealing treatment is carried out after the step (3) to form glass, and the temperature is kept for 30 minutes at 660 ℃ to obtain the glass material of the neutron scattering device.
The main properties of the glass material prepared in this example are shown in table 1.
Example 6
According to BaO 17 wt%; 5 wt% of CaO; al (Al)2O3 16wt%;SiO259 wt%; MgO 3 wt% of the stoichiometric batch.
The specific preparation process is basically the same as that of the example 1, except that in the step (2), the crucible is heated to 1600 ℃, the temperature is kept for 10 hours, then the crucible is blown and drawn into a glass tube, and after the glass tube is formed in the step (3), annealing treatment is carried out at 750 ℃ for 30 minutes to obtain the glass material of the neutron scattering device.
The main properties of the glass material prepared in this example are shown in table 1.
Example 7
According to BaO 18 wt%; 3 wt% of CaO; al (Al)2O3 14wt%;SiO2 50wt%;MgO 2wt%;Li2O 5wt%;Na2O 5wt%;K2O5 wt% of a stoichiometric batch.
The specific preparation process is basically the same as that of the example 1, except that in the step (2), the crucible is heated to 1400 ℃, the temperature is kept for 9 hours, then the crucible is blown and drawn into a glass tube, and after the glass tube is formed in the step (3), annealing treatment is carried out at 600 ℃ for 60 minutes to obtain the glass material of the neutron scattering device.
The main properties of the glass material prepared in this example are shown in table 1.
Example 8
According to 15 wt% of BaO; CaO 7 wt%; al (Al)2O3 16wt%;SiO2 55wt%;MgO 3wt%;Na2O 7wt%;K2O3 wt% of the stoichiometric batch.
The specific preparation process is basically the same as that of the example 1, except that in the step (2), the crucible is heated to 1450 ℃, the temperature is kept for 6 hours, the crucible is blown and drawn into a glass tube, and annealing treatment is carried out after the glass is formed in the step (3) and the temperature is kept for 30 minutes at 680 ℃ to obtain the glass material of the neutron scattering device.
Example 9
According to BaO 17 wt%; 5 wt% of CaO; al (Al)2O3 14wt%;SiO2 56wt%;MgO 5wt%;Li2O3 wt% of the stoichiometric batch.
The specific preparation process is basically the same as that of the example 1, except that in the step (2), the crucible is heated to 1500 ℃, the temperature is kept for 6 hours, the crucible is blown and drawn into a glass tube, and after the glass tube is formed in the step (3), annealing treatment is carried out at 680 ℃ for 60 minutes to obtain the glass material of the neutron scattering device.
The main properties of the glass material prepared in this example are shown in table 1.
Example 10
According to BaO 25 wt%; 3 wt% of CaO; al (Al)2O3 18wt%;SiO2 50wt%;MgO 0wt%;Li2O 1wt%;Na2O3 wt% of the stoichiometric batch. The specific preparation process is basically the same as that of the example 1, except that in the step (2), the crucible is heated to 1500 ℃, the temperature is kept for 6 hours, the crucible is blown and drawn into a glass tube, and annealing treatment is carried out after the glass is formed in the step (3) and the temperature is kept for 30 minutes at 650 ℃ to obtain the glass material of the neutron scattering device.
The main properties of the glass material prepared in this example are shown in table 1.
Comparative examples 1 to 5
The preparation processes of comparative examples 1 to 5 are the same as those of example 1, the specific components are different from those of example 1, and the specific components and properties of comparative examples 1 to 5 are shown in Table 2.
Comparative example 6
Is ampoule glass commonly used in laboratories.
From examples 1 to 10, the present invention provides a neutron transmittanceOr higher, and a glass softening point of 1050 ℃ or lower, can meet the application requirements of the glass product required by neutron scattering experiments, such as application requirements of an observation window, a vacuum container, a gas sealing container and an optical device.
Wherein the glass materials prepared in examples 9 and 10 have properties consistent with those of examples 1-8 above, and a neutron transmittance greater than that of examplesThe application requirement of the neutron scattering device can be met, because the content of the silicon dioxide of the network forming body is reduced, and the content of the magnesium oxide of the network outer body is higher, so that the neutron transmittance is reduced.
TABLE 1 Performance parameters of the examples
The main properties of the glass materials prepared in the comparative examples are shown in Table 2.
Comparing the properties of the glass materials prepared in comparative examples 1-3 with those of examples 1-3, comparative examples 1-3 have a glass softening point of 1050 ℃ or higher, a general glass processability, and a neutron transmittance of 1050 ℃ or lowerIn addition, the glass materials prepared in comparative examples 4 to 5 have properties, compared with those of the above examples 1 to 3, and comparative examples 4 to 5 have glass softening points of 900 ℃ or less, poor glass processability, and neutron of glassTransmittance of less than or equal toComparative example 6 is an ampoule glass having a neutron transmittance of only a small amount of boron in the composition
TABLE 2 comparative Performance parameters
Note: the test method of the embodiment of the invention comprises the following steps: the sample uses TG-DCS to test the glass sample Ts, an Archimedes method is adopted to test the volume density of the test sample, and a neutron spectrometer is adopted to test the neutron transmittance of the glass.
Claims (9)
1. The glass for the neutron scattering device is characterized by comprising the following components in percentage by weight: 15-25 wt% of BaO; 3-8 wt% of CaO; al (Al)2O3 10~18wt%;SiO2 50~65wt%;MgO 0~5wt%;R20-15 wt% of O; wherein R is2O is Li2O、Na2O and K2At least one of O.
3. The glass for a neutron scattering device according to claim 1, wherein the glass for a neutron scattering device has a softening point of less than 1050 ℃.
4. A method for producing a glass for a neutron scattering device according to claim 1, comprising the steps of:
(1) mixing the raw materials according to the weight ratio, heating to 1400 ℃ and 1800 ℃, and preserving heat to obtain liquid glass;
(2) and carrying out forming treatment on the liquid glass, and then carrying out annealing treatment to obtain the glass for the neutron scattering device.
5. The method for preparing glass for a neutron scattering device according to claim 4, wherein the temperature of the annealing treatment in the step (2) is 600-800 ℃.
6. The method for preparing glass for a neutron scattering device according to claim 4, wherein in the step (4), the temperature is kept for 30-120min after annealing, and then the glass is cooled along with a furnace.
7. The method for producing glass for a neutron scattering device according to claim 4, wherein the holding time in step (1) is 4 to 12 hours.
8. The method of claim 4, wherein the raw material used in the step (1) is CaCO3、BaCO3、SiO2、MgCO3、Al2O3And R2CO3。
9. The method of manufacturing glass for a neutron scattering device according to claim 4, wherein in the step (1), the bubbles are discharged by stirring with a quartz rod during heating.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4238705A (en) * | 1979-09-12 | 1980-12-09 | General Electric Company | Incandescent lamp seal means |
JPH09255354A (en) * | 1996-03-18 | 1997-09-30 | Asahi Glass Co Ltd | Glass composition for substrate |
JPH09255356A (en) * | 1996-03-18 | 1997-09-30 | Asahi Glass Co Ltd | Glass composition for substrate |
CN101189702A (en) * | 2005-06-09 | 2008-05-28 | 肖特股份公司 | Lamp device with an outer bulb in particular a high-pressure discharge lamp |
JP2008308376A (en) * | 2007-06-15 | 2008-12-25 | Central Glass Co Ltd | Substrate glass for display device |
CN101835718A (en) * | 2007-10-25 | 2010-09-15 | 旭硝子株式会社 | Glass composition for substrate and method for producing the same |
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Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4238705A (en) * | 1979-09-12 | 1980-12-09 | General Electric Company | Incandescent lamp seal means |
JPH09255354A (en) * | 1996-03-18 | 1997-09-30 | Asahi Glass Co Ltd | Glass composition for substrate |
JPH09255356A (en) * | 1996-03-18 | 1997-09-30 | Asahi Glass Co Ltd | Glass composition for substrate |
CN101189702A (en) * | 2005-06-09 | 2008-05-28 | 肖特股份公司 | Lamp device with an outer bulb in particular a high-pressure discharge lamp |
JP2008308376A (en) * | 2007-06-15 | 2008-12-25 | Central Glass Co Ltd | Substrate glass for display device |
CN101835718A (en) * | 2007-10-25 | 2010-09-15 | 旭硝子株式会社 | Glass composition for substrate and method for producing the same |
Non-Patent Citations (2)
Title |
---|
Y.SAKAGUCHI等: "Research on glass cells for 3He neutron spin filters", 《PHYSICA B》 * |
弗吉尼亚大学: "http://www.phys.virginia.edu/~wat4y/", 《必应搜索》 * |
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