CN102381841B - Yellow green luminescent glass ceramic material and preparation method thereof - Google Patents

Yellow green luminescent glass ceramic material and preparation method thereof Download PDF

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CN102381841B
CN102381841B CN 201010269710 CN201010269710A CN102381841B CN 102381841 B CN102381841 B CN 102381841B CN 201010269710 CN201010269710 CN 201010269710 CN 201010269710 A CN201010269710 A CN 201010269710A CN 102381841 B CN102381841 B CN 102381841B
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luminescent glass
green colour
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CN102381841A (en
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周明杰
马文波
翁方轶
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Oceans King Lighting Science and Technology Co Ltd
Shenzhen Oceans King Lighting Engineering Co Ltd
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Abstract

The invention belongs to the field of luminescent material, and discloses a yellow green luminescent glass ceramic material and a preparation method thereof. General chemical formula of the yellow green luminescent glass ceramic material is aCaO-bMgO-cSiO2-dEu2O3, in which a, b, c and d are mole fractions and a+b+c+d is equal to 100; numeric areas of a, b, c and d are respectively 30<=a<=50, 10<=b<=30, 30<=c<=50 and 0.1<=d<=1. The yellow green luminescent glass ceramic material provided by the invention has strong bandwidth excitation spectrum from ultraviolet to blue area and can emit strongyellow green light under excitation of ultraviolet or blue light.

Description

A kind of yellow-green colour luminescent glass ceramic material and preparation method thereof
Technical field
The present invention relates to field of light emitting materials, relate in particular to a kind of yellow-green colour luminescent glass ceramic material.The invention still further relates to a kind of yellow-green colour luminescent glass ceramic preparation methods.
Background technology
Development along with semiconductor lighting technology (LED), be supposed to as realizing reduce power consumption, long lifetime, the luminescent device of future generation of high light efficiency and high-color rendering, especially now commercialization technical scheme for luminescent device that semiconductor light-emitting elements and phosphor are combined caused widely and paid close attention to, carried out a large amount of research and development for this reason.Usually, as the primary light of luminous element emission, use be from the short UV light to the blue light, thereby the visible light then by primary light excitation wavelength transition material emission long wavelength is combined into white light.
This luminescent material for conversion from short wavelength to long wavelength is normally based on the luminescent material of powder.Therefore must cooperate organism (silica gel or Resins, epoxy) when in use.Present business-like most of White-light LED illumination device adopts is that blue-light LED chip cooperates and is subjected to blue-light excitedly can send gold-tinted or fluorescent material green, orange light.This class fluorescent material has higher luminous efficiency, and preparation method's maturation.But the light source device that this method is made has following defective: the Resins, epoxy that (1) is used for encapsulation is easily aging, and reduce device lifetime; (2) complex process, cost is higher; (3) chromaticity coordinates instability, the easy drift of white light etc.
Than powder body material, can realize that under blue light or ultraviolet excitation luminous glass-ceramic then has significant advantage: (1) has good light transmittance; (2) good chemical stability and thermostability; (3) preparation technology is simple, and is with low cost; (4) make bulk and different shapes easily; (5) can the displaced loop epoxy resins, because these characteristics can realize that the luminous glass of high-performance is suitable as the luminescence medium material of LED lighting field very much.But, being subjected to the restriction of glass preparation condition and glass structure, a lot of luminescent active ion luminous intensities in glass are very weak, even not luminous.
Summary of the invention
In order to address the above problem, the invention provides a kind of yellow-green colour luminescent glass ceramic material, its chemical general formula is: aCaO-bMgO-cSiO 2-dEu 2O 3Wherein, a, b, c, d are molfraction and a+b+c=100; The span of a, b, c, d is respectively: 30≤a≤50,10≤b≤30,30≤c≤50,0.1≤d≤1; Preferably, the span of a, b, c, d is respectively: 40≤a≤50,20≤b≤30,35≤c≤45,0.3≤d≤0.5.
Another object of the present invention is to provide a kind of yellow-green colour luminescent glass ceramic preparation methods, preparation flow is as follows:
Step S1, according to chemical general formula aCaO-bMgO-cSiO 2-dEu 2O 3In each component mole number, take by weighing source compound, the source compound of MgO, the SiO of CaO 2Raw material and Eu 2O 3Source compound, mix, grind to form mixed powder; Wherein, a, b, c, d are molfraction and a+b+c=100; The span of a, b, c, d is respectively: 30≤a≤50,10≤b≤30,30≤c≤50,0.1≤d≤1;
Step S2, place 1100～1300 ℃ of following precalcinings to handle 1～6h described mixed powder, be cooled to room temperature, grinding then;
Under step S3, the reducing atmosphere, the mixed powder after the above-mentioned precalcining is placed 1200～1300 ℃ of reduction processing 2～4h down again, be cooled to room temperature then;
Step S4, add the finings Sb of 1%～5% (weight) in the above-mentioned reduction mixed powder later 2O 3, mix, grind the back in 1500～1650 ℃ of insulation fusion 1～4h down, then the glass melt of fusing is poured fast into preheating temperature and be in 200～500 ℃ the copper material mould and be shaped, obtain the glass precursor;
Step S5, carry out crystallization again after described forerunner's glass annealing handled and handle, obtain described yellow-green colour luminescent glass ceramic material.
Preferably, the span of a, b, c, d is respectively: 40≤a≤50,20≤b≤30,35≤c≤45,0.3≤d≤0.5.
Among the above-mentioned steps S5, the temperature of described anneal is 400`700 ℃, and the annealing soaking time is 2～4 hours; Described crystallization is handled and is comprised: under the reducing atmosphere, and 800 ℃～1300 ℃ 1～10 hour crystallization of insulation processing down.
Compared with prior art, the present invention has the following advantages:
Yellow-green colour luminescent glass ceramic material provided by the present invention has strong broadband excitation spectrum in ultraviolet to blue light region, and can launch strong yellow green light under the exciting of UV-light or blue light.
Description of drawings
Fig. 1 is preparation technology's schema of yellow-green colour luminescent glass ceramic material of the present invention;
Fig. 2 is emmission spectrum figure and the exciting light spectrogram of the yellow-green colour luminescent glass ceramic material of embodiment 6, wherein, and curve a-excitation spectrum; Curve b-emission spectrum.
Embodiment
The invention provides a kind of yellow-green colour luminescent glass ceramic material, its chemical general formula is: aCaO-bMgO-cSiO 2-dEu 2O 3Wherein, a, b, c, d are molfraction and a+b+c=100; The span of a, b, c, d is respectively: 30≤a≤50,10≤b≤30,30≤c≤50,0.1≤d≤1; Preferably, the span of a, b, c, d is respectively: 40≤a≤50,20≤b≤30,35≤c≤45,0.3≤d≤0.5.
Above-mentioned yellow-green colour luminescent glass ceramic preparation methods, as shown in Figure 1, preparation flow is as follows:
Step S1, according to chemical general formula aCaO-bMgO-cSiO 2-dEu 2O 3In each component mole number, take by weighing source compound, the source compound of MgO, the SiO of CaO 2Raw material and Eu 2O 3Source compound, mix, grind to form mixed powder; Wherein, a, b, c, d are molfraction and a+b+c=100; The span of a, b, c, d is respectively: 30≤a≤50,10≤b≤30,30≤c≤50,0.1≤d≤1
Step S2, place 1100～1300 ℃ of following precalcinings to handle 1～6h described mixed powder, be cooled to room temperature, grinding then;
Under step S3, the reducing atmosphere, the mixed powder after the above-mentioned precalcining is placed 1200～1300 ℃ of reduction processing 2～4h down again, be cooled to room temperature then;
Step S4, add the finings Sb of 1%～5% (weight) in the above-mentioned reduction mixed powder later 2O 3, mix, grind the back in 1500～1650 ℃ of insulation fusion 1～4h down, then the glass melt of fusing is poured fast into preheating temperature and be 200～500 ℃ copper material but be not limited to and be shaped in the mould of copper material, obtain the glass precursor;
Step S5, carry out crystallization again after described forerunner's glass annealing handled and handle, obtain described yellow-green colour luminescent glass ceramic material.
Preferably, the span of a, b, c, d is respectively: 40≤a≤50,20≤b≤30,35≤c≤45,0.3≤d≤0.5.
Among the above-mentioned steps S5, the temperature of described anneal is 400～700 ℃, and the annealing soaking time is 2～4 hours; Described crystallization is handled and is comprised: under the reducing atmosphere, and 800 ℃～1300 ℃ 1～10 hour crystallization of insulation processing down.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Embodiment 1
30CaO-20MgO-50SiO 2-0.1Eu 2O 3Take by weighing calcium carbonate (CaCO respectively 3) 16.29g, magnesium oxide (MgO) 4.37g, silicon-dioxide (SiO 2) 16.3g, europiumsesquioxide (Eu 2O 3) 0.18g.After load weighted raw material ground and mixed in mortar is even, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1100 degrees centigrade of calcinings of high temperature box furnace 1 hour, and the powder raw material after will calcining is then put into the full and uniform grinding of corundum mortar; Powder body material after grinding is placed tube furnace again, at 5% (volume ratio, down together) H 2With 95% (volume ratio, down together) N 2Under the reducing atmosphere of gas mixture again with powder body material in 1200 ℃ down calcining close the tube furnace power supply after 2 hours, turn off 5%H after cooling to room temperature with the furnace 2And 95%N 2Gas mixture; The adding weight percent is 1% finings antimonous oxide (Sb in the powder body material after will reducing subsequently 2O 3) 0.30g and place the full and uniform grinding of corundum mortar; Powder body material after grinding is packed in the corundum crucible, and the corundum crucible that powder body material will be housed puts into a big corundum crucible, the gap between two crucibles is filled up with graphite block, covers big crucible with the first plate of corundum; Again big corundum crucible is placed High Temperature Furnaces Heating Apparatus when the room temperature, and furnace temperature is risen to 1500 ℃ gradually, be incubated 1 hour; At last the glass melt of fusing is poured in the copper mold of 200 ℃ of preheatings fast and be shaped; The forerunner's glass that obtains is put into 700 ℃ of insulations of resistance furnace annealing in 2 hours to eliminate internal stress; Glass after the annealing continues at 5%H 2And 95%N 2Be heated to 800 ℃ of heat tracings under the gas mixture reducing atmosphere and made it to take place crystallization in 1 hour, obtain glass-ceramic.
Embodiment 2
50CaO-10MgO-40SiO 2-1Eu 2O 3Take by weighing calcium carbonate (CaCO respectively 3) 25.34g, magnesium oxide (MgO) 2.03g, silicon-dioxide (SiO 2) 13.78g, europiumsesquioxide (Eu 2O 3) 1.78g.After load weighted raw material ground and mixed in mortar is even, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1300 degrees centigrade of calcinings of high temperature box furnace 6 hours, and the powder raw material after will calcining is then put into the full and uniform grinding of corundum mortar; Powder body material after grinding is placed tube furnace again, at 5%H 2And 95%N 2Under the reducing atmosphere of gas mixture again with powder body material in 1300 ℃ down calcining close the tube furnace power supply after 4 hours, turn off 5%H after cooling to room temperature with the furnace 2And 95%N 2Gas mixture; The adding weight percent is 5% finings antimonous oxide (Sb in the powder body material after will reducing subsequently 2O 3) 1.50g and place the full and uniform grinding of corundum mortar; Powder body material after grinding is packed in the corundum crucible, and the corundum crucible that powder body material will be housed puts into a big corundum crucible, the gap between two crucibles is filled up with graphite block, covers big crucible with the first plate of corundum; Again big corundum crucible is placed High Temperature Furnaces Heating Apparatus when the room temperature, and furnace temperature is risen to 1550 ℃ gradually, be incubated 4 hours; At last the glass melt of fusing is poured in the copper mold of 300 ℃ of preheatings fast and be shaped; The forerunner's glass that obtains is put into 600 ℃ of insulations of resistance furnace annealing in 2 hours to eliminate internal stress; Glass after the annealing continues at 5%H 2And 95%N 2Be heated to 1000 ℃ of heat tracings under the gas mixture reducing atmosphere and made it to take place crystallization in 10 hours, obtain glass-ceramic.
Embodiment 3
40CaO-30MgO-30SiO 2-0.8Eu 2O 3Take by weighing calcium carbonate (CaCO respectively 3) 21.90g, magnesium oxide (MgO) 6.57g, silicon-dioxide (SiO 2) 11.17g, europiumsesquioxide (Eu 2O 3) 1.54g.After load weighted raw material ground and mixed in mortar is even, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1200 degrees centigrade of calcinings of high temperature box furnace 3 hours, and the powder raw material after will calcining is then put into the full and uniform grinding of corundum mortar; Powder body material after grinding is placed tube furnace again, at 5%H 2And 95%N 2Under the reducing atmosphere of gas mixture again with powder body material in 1200 ℃ down calcining close the tube furnace power supply after 3 hours, turn off 5%H after cooling to room temperature with the furnace 2And 95%N 2Gas mixture; The adding weight percent is 3% finings antimonous oxide (Sb in the powder body material after will reducing subsequently 2O 3) 0.90g and place the full and uniform grinding of corundum mortar; Powder body material after grinding is packed in the corundum crucible, and the corundum crucible that powder body material will be housed puts into a big corundum crucible, the gap between two crucibles is filled up with graphite block, covers big crucible with the first plate of corundum; Again big corundum crucible is placed High Temperature Furnaces Heating Apparatus when the room temperature, and furnace temperature is risen to 1500 ℃ gradually, be incubated 2 hours; At last the glass melt of fusing is poured in the copper mold of 500 ℃ of preheatings fast and be shaped; The forerunner's glass that obtains is put into 400 ℃ of insulations of resistance furnace annealing in 2 hours to eliminate internal stress; Glass after the annealing continues at 5%H 2And 95%N 2Be heated to 900 ℃ of heat tracings under the gas mixture reducing atmosphere and made it to take place crystallization in 5 hours, obtain glass-ceramic.
Embodiment 4
40CaO-25MgO-35SiO 2-0.6Eu 2O 3Take by weighing calcium carbonate (CaCO respectively 3) 21.35g, magnesium oxide (MgO) 5.34g, silicon-dioxide (SiO 2) 12.70g, europiumsesquioxide (Eu 2O 3) 1.13g.After load weighted raw material ground and mixed in mortar is even, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1250 degrees centigrade of calcinings of high temperature box furnace 4 hours, and the powder raw material after will calcining is then put into the full and uniform grinding of corundum mortar; Powder body material after grinding is placed tube furnace again, at 5%H 2And 95%N 2Under the reducing atmosphere of gas mixture again with powder body material in 1250 ℃ down calcining close the tube furnace power supply after 2.5 hours, turn off 5%H after cooling to room temperature with the furnace 2And 95%N 2Gas mixture; The adding weight percent is 2% finings antimonous oxide (Sb in the powder body material after will reducing subsequently 2O 3) 0.60g and place the full and uniform grinding of corundum mortar; Powder body material after grinding is packed in the corundum crucible, and the corundum crucible that powder body material will be housed puts into a big corundum crucible, the gap between two crucibles is filled up with graphite block, covers big crucible with the first plate of corundum; Again big corundum crucible is placed High Temperature Furnaces Heating Apparatus when the room temperature, and furnace temperature is risen to 1580 ℃ gradually, be incubated 3 hours; At last the glass melt of fusing is poured in the copper mold of 300 ℃ of preheatings fast and be shaped; The forerunner's glass that obtains is put into 650 ℃ of insulations of resistance furnace annealing in 2 hours to eliminate internal stress; Glass after the annealing continues at 5%H 2And 95%N 2Be heated to 1100 ℃ of heat tracings under the gas mixture reducing atmosphere and made it to take place crystallization in 6 hours, obtain glass-ceramic.
Embodiment 5
25CaO-30MgO-45SiO 2-0.4Eu 2O 3Take by weighing calcium carbonate (CaCO respectively 3) 13.75g, magnesium oxide (MgO) 6.64g, silicon-dioxide (SiO 2) 14.86g, europiumsesquioxide (Eu 2O 3) 0.77g.After load weighted raw material ground and mixed in mortar is even, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1250 degrees centigrade of calcinings of high temperature box furnace 2 hours, and the powder raw material after will calcining is then put into the full and uniform grinding of corundum mortar; Powder body material after grinding is placed tube furnace again, at 5%H 2And 95%N 2Under the reducing atmosphere of gas mixture again with powder body material in 1200 ℃ down calcining close the tube furnace power supply after 3.5 hours, turn off 5%H after cooling to room temperature with the furnace 2And 95%N 2Gas mixture; The adding weight percent is 4% finings antimonous oxide (Sb in the powder body material after will reducing subsequently 2O 3) 1.20g and place the full and uniform grinding of corundum mortar; Powder body material after grinding is packed in the corundum crucible, and the corundum crucible that powder body material will be housed puts into a big corundum crucible, the gap between two crucibles is filled up with graphite block, covers big crucible with the first plate of corundum; Again big corundum crucible is placed High Temperature Furnaces Heating Apparatus when the room temperature, and furnace temperature is risen to 1650 ℃ gradually, be incubated 4 hours; At last the glass melt of fusing is poured in the copper mold of 350 ℃ of preheatings fast and be shaped; The forerunner's glass that obtains is put into 600 ℃ of insulations of resistance furnace annealing in 2 hours to eliminate internal stress; Glass after the annealing continues at 5%H 2And 95%N 2Be heated to 1300 ℃ of heat tracings under the gas mixture reducing atmosphere and made it to take place crystallization in 5 hours, obtain glass-ceramic.
Embodiment 6
40CaO-20MgO-40SiO 2-0.5Eu 2O 3Take by weighing calcium carbonate (CaCO respectively 3) 21.33g, magnesium oxide (MgO) 4.29g, silicon-dioxide (SiO 2) 12.80g, europiumsesquioxide (Eu 2O 3) 0.93g.After load weighted raw material ground and mixed in mortar is even, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1300 degrees centigrade of calcinings of high temperature box furnace 4 hours, and the powder raw material after will calcining is then put into the full and uniform grinding of corundum mortar; Powder body material after grinding is placed tube furnace again, at 5%H 2And 95%N 2Under the reducing atmosphere of gas mixture again with powder body material in 1300 ℃ down calcining close the tube furnace power supply after 2 hours, turn off 5%H after cooling to room temperature with the furnace 2And 95%N 2Gas mixture; The adding weight percent is 1% finings antimonous oxide (Sb in the powder body material after will reducing subsequently 2O 3) 0.30g and place the full and uniform grinding of corundum mortar; Powder body material after grinding is packed in the corundum crucible, and the corundum crucible that powder body material will be housed puts into a big corundum crucible, the gap between two crucibles is filled up with graphite block, covers big crucible with the first plate of corundum; Again big corundum crucible is placed High Temperature Furnaces Heating Apparatus when the room temperature, and furnace temperature is risen to 1600 ℃ gradually, be incubated 2 hours; At last the glass melt of fusing is poured in the copper mold of 300 ℃ of preheatings fast and be shaped; The forerunner's glass that obtains is put into 550 ℃ of insulations of resistance furnace annealing in 2 hours to eliminate internal stress; Glass after the annealing continues at 5%H 2And 95%N 2Be heated to 1250 ℃ of heat tracings under the gas mixture reducing atmosphere and made it to take place crystallization in 10 hours, obtain glass-ceramic.Fig. 2 excites and emission spectrum for this fact Example.Find out that from spectrogram the wavelength region of excitation spectrum is 250～500 nanometers, peak wavelength is to be fit to very much blue-light LED chip near 457 nanometers excite; The wavelength region of emission spectrum is 500～650 nanometers, and peak wavelength is near the emission 537 nanometers.The yellow green light of emission just can generate white light with the blue light that excites according to suitable mixed.
Embodiment 7
30CaO-30MgO-40SiO 2-0.3Eu 2O 3Take by weighing calcium carbonate (CaCO respectively 3) 16.67g, magnesium oxide (MgO) 6.71g, silicon-dioxide (SiO 2) 13.35g, europiumsesquioxide (Eu 2O 3) 0.58g.After load weighted raw material ground and mixed in mortar is even, pack in the corundum crucible, the corundum crucible with cover that will install raw material is then put into 1200 degrees centigrade of calcinings of high temperature box furnace 5 hours, and the powder raw material after will calcining is then put into the full and uniform grinding of corundum mortar; Powder body material after grinding is placed tube furnace again, at 10%H 2And 90%N 2Under the reducing atmosphere of gas mixture again with powder body material in 1250 ℃ down calcining close the tube furnace power supply after 2.5 hours, turn off 10%H after cooling to room temperature with the furnace 2And 90%N 2Gas mixture; The adding weight percent is 3% finings antimonous oxide (Sb in the powder body material after will reducing subsequently 2O 3) 0.90g and place the full and uniform grinding of corundum mortar; Powder body material after grinding is packed in the corundum crucible, and the corundum crucible that powder body material will be housed puts into a big corundum crucible, the gap between two crucibles is filled up with graphite block, covers big crucible with the first plate of corundum; Again big corundum crucible is placed High Temperature Furnaces Heating Apparatus when the room temperature, and furnace temperature is risen to 1650 ℃ gradually, be incubated 2 hours; At last the glass melt of fusing is poured in the copper mold of 250 ℃ of preheatings fast and be shaped; The forerunner's glass that obtains is put into 600 ℃ of insulations of resistance furnace annealing in 2 hours to eliminate internal stress; Glass after the annealing continues at 10%H 2And 90%N 2Be heated to 1300 ℃ of heat tracings under the gas mixture reducing atmosphere and made it to take place crystallization in 8 hours, obtain glass-ceramic.
Should be understood that above-mentioned statement at preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, scope of patent protection of the present invention should be as the criterion with claims.

Claims (8)

1. yellow-green colour luminescent glass ceramic material, its chemical general formula is: aCaO-bMgO-cSiO 2-dEu 2O 3Wherein, a, b, c, d are molfraction and a+b+c=100; The span of a, b, c, d is respectively: 40≤a≤50,20≤b≤30,35≤c≤45,0.3≤d≤0.5.
2. a yellow-green colour luminescent glass ceramic preparation methods is characterized in that, comprises the steps:
According to chemical general formula aCaO-bMgO-cSiO 2-dEu 2O 3In each component mole number, take by weighing source compound, the source compound of MgO, the SiO of CaO 2Raw material and Eu 2O 3Source compound, mix, grind to form mixed powder; Wherein, a, b, c, d are molfraction and a+b+c=100; The span of a, b, c, d is respectively 40≤a≤50,20≤b≤30,35≤c≤45,0.3≤d≤0.5;
Place 1100～1300 ℃ of following precalcinings to handle described mixed powder, be cooled to room temperature, grinding then;
Under the reducing atmosphere, the mixed powder after the above-mentioned precalcining is placed 1200～1300 ℃ of reduction processing down again, be cooled to room temperature then;
Add weight ratio in the above-mentioned reduction mixed powder later and be 1%～5% finings, mix, grind the back in 1500～1650 ℃ of insulation fusion 1～4h down, the glass melt of fusing is poured into fast be shaped in the mould then, obtain the glass precursor;
Handle carrying out crystallization again after described forerunner's glass annealing processing, obtain described yellow-green colour luminescent glass ceramic material.
3. yellow-green colour luminescent glass ceramic preparation methods according to claim 2 is characterized in that, the described mixed powder precalcining treatment time is 1～6h.
4. yellow-green colour luminescent glass ceramic preparation methods according to claim 2 is characterized in that, the described mixed powder reduction treatment time is 2～4h.
5. yellow-green colour luminescent glass ceramic preparation methods according to claim 2 is characterized in that, in the described glass precursor preparation process, described finings is Sb 2O 3Comprise also described mould carried out thermal pretreatment that preheating temperature is 200～500 ℃.
6. according to claim 2 or 5 described yellow-green colour luminescent glass ceramic preparation methods, it is characterized in that described mould is copper mould.
7. yellow-green colour luminescent glass ceramic preparation methods according to claim 2 is characterized in that, the temperature of described anneal is 400～700 ℃, and the annealing soaking time is 2～4 hours.
8. yellow-green colour luminescent glass ceramic preparation methods according to claim 2 is characterized in that, described crystallization is handled and comprised: under the reducing atmosphere, and 800 ℃～1300 ℃ 1～10 hour crystallization of insulation processing down.
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