CN105776259A - Production method for high-purity magnesium fluoride polycrystals for ultraviolet-level single crystal growth - Google Patents
Production method for high-purity magnesium fluoride polycrystals for ultraviolet-level single crystal growth Download PDFInfo
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- CN105776259A CN105776259A CN201610073771.2A CN201610073771A CN105776259A CN 105776259 A CN105776259 A CN 105776259A CN 201610073771 A CN201610073771 A CN 201610073771A CN 105776259 A CN105776259 A CN 105776259A
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- C01F5/00—Compounds of magnesium
- C01F5/26—Magnesium halides
- C01F5/28—Fluorides
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- C—CHEMISTRY; METALLURGY
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- C01P2006/80—Compositional purity
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Abstract
The invention relates to a production method for high-purity magnesium fluoride polycrystals for ultraviolet-level single crystal growth.The production method includes the following steps that a high-purity magnesium fluoride powder material is prepared; 2, two-high graphite is adopted to be prepared into a graphite crucible according to a conventional process; 3, the high-purity magnesium fluoride powder material is pre-pressed; 4, the pressed high-purity magnesium fluoride blocky material is placed in the graphite crucible, the graphite crucible is placed in a heating furnace to be heated, and a magnesium fluoride blocky material is obtained; 5, after the material is heated at the temperature of 400-1,300 DEG C, the material is naturally cooled along with the furnace and then taken out, and the magnesium fluoride polycrystals with the purity larger than or equal to 99.99% are obtained.Magnesium sulfate heptahydrate is adopted as a raw material, ammonium hydroxide is adopted as a precipitator, a high-purity magnesium hydrate powder precursor is synthesized, high-purity magnesium fluoride powder is obtained after a fluorination reaction, the content of impurities is effectively reduced, and therefore the problem that in the prior art, the purity of magnesium fluoride is not high due to the high content of impurities of Al, Ca, Fe, Mn, Ni and Zn is solved.
Description
Technical field
The present invention relates to Condensed Matter Physics, artificial optical crystal Afluon (Asta) production technical field, particularly relate to the production method of a kind of UV grade crystal growth high purity magnesium fluoride polycrystalline.
Background technology
High purity magnesium fluoride polycrystalline material has good polarization and infrared transmission performance, especially on 1 ~ 7 μm of infrared band, transmitance reaches more than 90%, it is widely used in the vacuum coating of optical element anti-reflection film, antireflective film, meanwhile, is also the basic material of growth UV grade Afluon (Asta) monocrystalline.Therefore, produce the high purity magnesium fluoride polycrystalline without hydrolysis, oxide-free impurity, be very necessary and important to the technique for vacuum coating of optical component and the Afluon (Asta) monocrystalline of growth UV grade.
The existing Afluon (Asta) polycrystal manufacture without hydrolysis, oxide-free impurity substantially adopts two kinds of methods: one is that anhydrous hydrogen fluoride is passed into heating furnace, carries out gas phase fluorination and the protection of fluorine element；Two is add a certain amount of PbF in magnesium fluoride powder material, NaF or LiF.Method one, because using anhydrous hydrogen fluoride gas, to install hydrofluoric absorption equipment additional so follow-up and add chemicals, also to use platinum crucible, environmental risk and security risk big, and equipment investment is big.Method two, because adding other fluorides, waits in the high-purity fluorine magnesium that coexists and introduces impurity, reduce the purity of magnesium fluoride material itself；It addition, the tail end at vacuum drying oven extract system still needs to install absorption plant additional.
Summary of the invention
The technical problem to be solved is to provide that a kind of cost is low, the production method of the UV grade crystal growth high purity magnesium fluoride polycrystalline of easy enforcement.
For solving the problems referred to above, the production method of a kind of UV grade crystal growth high purity magnesium fluoride polycrystalline of the present invention, comprise the following steps:
(1) prepare high purity magnesium fluoride powder material:
1. purification of sulphuric acids magnesium solution is prepared:
The hydrolysis of Magnesium sulfate heptahydrate pure water is formed the magnesium sulfate solution that mass concentration is 20% ~ 30%, and the heating of this magnesium sulfate solution adds oxalic acid after 60 DEG C ~ 80 DEG C, filters, obtain filtrate after stirring reaction 3 ~ 5h；Described filtrate is sequentially added into hydrogen peroxide, sodium hydroxide that mass concentration is 30%, and is stirred well to uniformly, through staticly settling 12 ~ 24h, extract supernatant, obtain purification of sulphuric acids magnesium solution；The quality of described oxalic acid is the 0.5 ~ 1.5% of described magnesium sulfate solution quality；The quality of described hydrogen peroxide is the 3% ~ 5% of described magnesium sulfate solution quality；The quality of described sodium hydroxide is the 1% ~ 2% of described magnesium sulfate solution quality；
2. magnesium hydroxide presoma is prepared:
Described purification of sulphuric acids magnesium solution is heated after 30 DEG C ~ 50 DEG C, by the 1.1 ~ 1.5 of its quality times add mass concentration be 20% ammonia carry out complete reaction after, it is filtrated to get magnesium hydroxide hydrate by centrifugation, this magnesium hydroxide hydrate, after pure water to sulfate radical-free remains, obtains magnesium hydroxide presoma；
3. magnesium fluoride powder is prepared:
The reactor be lined with politef adds the analytical pure Fluohydric acid. that mass concentration is 40%, is subsequently adding described magnesium hydroxide presoma and is stirred, after the reaction of fluorine element after centrifugal filtration, obtain magnesium fluoride powder；The mass ratio of described magnesium hydroxide presoma and described Fluohydric acid. is 1:1.5 ~ 2；
4. high purity magnesium fluoride powder is prepared:
Described magnesium fluoride powder is loaded corundum crucible calcine, obtain the magnesium fluoride powder of purity >=99.99%；
(2) the two high graphite techniques routinely adopting high-purity high-density make high purity graphite crucible, and arrange Multi-layer graphite in vacuum drying oven and carbon felt is thermally shielded；
(3) described high purity magnesium fluoride powder material is carried out pre-stamped, the high purity magnesium fluoride bulk material after being suppressed.
(4) the high purity magnesium fluoride bulk material after described compacting is put in the graphite crucible of described step (2) gained, and together put in heating furnace, be 1 × 10 in vacuum-1Heat 10 ~ 36h when Pa, temperature are 100 DEG C ~ 400 DEG C, obtain the Afluon (Asta) bulk material that moisture is 1 ~ 1.5%；
(5) it is 1 × 10 by magnesium fluoride powder material that described moisture is 1 ~ 1.5% in vacuum-3Heat when Pa, temperature are 400 DEG C ~ 1300 DEG C, after 36 ~ 100h, take out after material is with stove natural cooling, obtain the Afluon (Asta) polycrystalline of purity >=99.99%.
Described step 1. in pure electrical conductivity of water≤1 μ S/cm.
Described step 3. middle fluorine element reaction condition refers to that temperature is 60 ~ 80 DEG C, and the time is 1 ~ 3h.
Described step 4. middle calcination condition refers to that temperature is 100 DEG C ~ 400 DEG C, and the time is 5 ~ 10h.
Described step (3) in pre-stamped condition refer to the material after compacting, it is possible to be bulk can also be graininess.As such, it is possible to release powder body material to fly upward problem in vacuum drying oven.
The present invention compared with prior art has the advantage that
1, the present invention is with Magnesium sulfate heptahydrate for raw material, ammonia is precipitant, synthesize high purity magnesium hydrate powder body presoma, high purity magnesium fluoride powder is obtained after the reaction of fluorine elementization, effectively reduce impurity content, thus solving the Afluon (Asta) problem that purity that is that cause is not high because impurity A l, Ca, Fe, Mn, Ni, Zn content is more in prior art.
2, the high purity magnesium fluoride powder in side of the present invention through inductive coupling plasma emission spectrograph ICP detect (referring to table 1), its impurity A l, Ca, Fe, Mn, Ni and Zn mass ratio respectively at below 9ppm, total mass ratio is below 100ppm.
Table 1 is the impurity element result (ppm) of the ICP detection of the high purity magnesium fluoride powder that embodiment 1 ~ 3 prepares
| Fe | Mn | Al | Ni | Zn | Ca | |
| Embodiment 1 | 8 | 7 | 6 | 3 | 6 | 9 |
| Embodiment 2 | 5 | 4 | 3 | 2 | 3 | 5 |
| Embodiment 3 | 3 | 2 | 1 | 1 | 1 | 2 |
3, the present invention is provided with Multi-layer graphite and carbon felt in vacuum drying oven, thus reaching effectively insulation and heat insulation purpose.
4, magnesium fluoride powder material is carried out pre-stamped by the present invention, thus avoiding subsequent handling dusty material under vacuum to fly upward phenomenon, has ensured the use of vacuum equipment.
5, magnesium fluoride powder is dried initially with the mode of coarse vacuum and anhydrates point by the present invention, then in high vacuum conditions to its water that decrystallizes, so that final products reach the purpose without hydrolysis, oxide-free impurity.
6, the Afluon (Asta) polycrystalline material function admirable (referring to table 2) adopting the inventive method to obtain, can be used for the vacuum coating of optical element anti-reflection film, antireflective film；Meanwhile, also it is the basic material growing UV grade Afluon (Asta) monocrystalline.
Table 2 is the testing result of the Afluon (Asta) polycrystalline product that embodiment 1 ~ 3 prepares
| Fe | Mn | Al | Ni | Zn | Ca | MgO | |
| Embodiment 1 | 5 | 4 | 3 | 2 | 1 | 9 | Do not detect |
| Embodiment 2 | 3 | 2 | 2 | 2 | 1 | 9 | Do not detect 2--> |
| Embodiment 3 | 2 | 2 | 1 | 1 | 0 | 5 | Do not detect |
7, raw material of the present invention is easy to get, with low cost, it is easy to implement.
Detailed description of the invention
1 one kinds of UV grade crystal growth production methods of high purity magnesium fluoride polycrystalline of embodiment, comprise the following steps:
(1) prepare high purity magnesium fluoride powder material:
1. purification of sulphuric acids magnesium solution is prepared:
Being hydrolyzed by the pure water of 100 kilograms of Magnesium sulfate heptahydrate electrical conductivity≤1 μ S/cm and form the magnesium sulfate solution that mass concentration is 20%, the heating of this magnesium sulfate solution adds oxalic acid after 60 DEG C, filters after stirring reaction 3h, removes calcium oxalate and obtains filtrate；Filtrate is sequentially added into hydrogen peroxide, sodium hydroxide that mass concentration is 30%, and is stirred well to uniformly, through staticly settling 12h, to remove the metal impurities such as ferrum, manganese, nickel, aluminum, extract supernatant, obtain purification of sulphuric acids magnesium solution.
Wherein: the quality of oxalic acid is the 0.5% of magnesium sulfate solution quality；The quality of hydrogen peroxide is the 3% of magnesium sulfate solution quality；The quality of sodium hydroxide is the 1% of magnesium sulfate solution quality.
2. magnesium hydroxide presoma is prepared:
By the heating of purification of sulphuric acids magnesium solution to after 30 DEG C, add after the ammonia that mass concentration is 20% carries out complete reaction by the 1.1 of its quality times, filter by centrifugation and remove ammonium sulfate liquid, obtain magnesium hydroxide hydrate.This magnesium hydroxide hydrate is through pure water, with BaClAfter remaining to sulfate radical-free for indicator detection, obtain magnesium hydroxide presoma.
3. magnesium fluoride powder is prepared:
The reactor be lined with politef adds the analytical pure Fluohydric acid. that mass concentration is 40%, it is subsequently adding magnesium hydroxide presoma to be stirred, carry out fluorine element reaction when temperature is 60 DEG C, remove the hydrofluoric acid solution containing silicon through centrifugal filtration after 1h, obtain magnesium fluoride powder.
Wherein: the mass ratio of magnesium hydroxide presoma and Fluohydric acid. is 1:1.5.
4. high purity magnesium fluoride powder is prepared:
Magnesium fluoride powder is loaded corundum crucible, calcines 10h when temperature is 100 DEG C ~ 200 DEG C, obtain the magnesium fluoride powder of purity >=99.99%.
(2) two high graphite techniques routinely make high purity graphite crucible, and arrange Multi-layer graphite and carbon felt outside this high purity graphite crucible.
(3) high purity magnesium fluoride powder material is carried out pre-stamped, high purity magnesium fluoride bulk material after being suppressed or granular material.
(4) the high purity magnesium fluoride powder material after suppressing 10 kilograms is put in the graphite crucible of step (2) gained, and together puts in heating furnace, is 1 × 10 in vacuum-1Heat 36h when Pa, temperature are 300 DEG C, obtain the magnesium fluoride powder material that moisture is 1.5%.
(5) it is 1 × 10 by magnesium fluoride powder material that moisture is 1.5% in vacuum-3Heat when Pa, temperature are 1100 DEG C, after 100h, take out after material is with stove natural cooling, obtain the Afluon (Asta) polycrystalline of 8.9 kilograms of purity >=99.99%.
2 one kinds of UV grade crystal growth production methods of high purity magnesium fluoride polycrystalline of embodiment, comprise the following steps:
(1) prepare high purity magnesium fluoride powder material:
1. purification of sulphuric acids magnesium solution is prepared:
Being hydrolyzed by the pure water of 100 kilograms of Magnesium sulfate heptahydrate electrical conductivity≤1 μ S/cm and form the magnesium sulfate solution that mass concentration is 25%, the heating of this magnesium sulfate solution adds oxalic acid after 70 DEG C, filters after stirring reaction 4h, removes calcium oxalate and obtains filtrate；Filtrate is sequentially added into hydrogen peroxide, sodium hydroxide that mass concentration is 30%, and is stirred well to uniformly, through staticly settling 18h, to remove the metal impurities such as ferrum, manganese, nickel, aluminum, extract supernatant, obtain purification of sulphuric acids magnesium solution.
Wherein: the quality of oxalic acid is the 1.0% of magnesium sulfate solution quality；The quality of hydrogen peroxide is the 4% of magnesium sulfate solution quality；The quality of sodium hydroxide is the 1.5% of magnesium sulfate solution quality.
2. magnesium hydroxide presoma is prepared:
By the heating of purification of sulphuric acids magnesium solution to after 40 DEG C, add after the ammonia that mass concentration is 20% carries out complete reaction by the 1.2 of its quality times, filter by centrifugation and remove ammonium sulfate liquid, obtain magnesium hydroxide hydrate.This magnesium hydroxide hydrate is through pure water, with BaClAfter remaining to sulfate radical-free for indicator detection, obtain magnesium hydroxide presoma.
3. magnesium fluoride powder is prepared:
The reactor be lined with politef adds the analytical pure Fluohydric acid. that mass concentration is 40%, it is subsequently adding magnesium hydroxide presoma to be stirred, carry out fluorine element reaction when temperature is 70 DEG C, remove the hydrofluoric acid solution containing silicon through centrifugal filtration after 2h, obtain magnesium fluoride powder.
Wherein: the mass ratio of magnesium hydroxide presoma and Fluohydric acid. is 1:1.75.
4. high purity magnesium fluoride powder is prepared:
Magnesium fluoride powder is loaded corundum crucible, calcines 8h when temperature is 200 DEG C ~ 300 DEG C, obtain the magnesium fluoride powder of purity >=99.99%.
(2) adopt two high graphite techniques routinely to make graphite crucible, and Multi-layer graphite and carbon felt are set in vacuum drying oven.
(3) high purity magnesium fluoride powder material is carried out pre-stamped, high purity magnesium fluoride bulk material after being suppressed or granular material.
(4) the high purity magnesium fluoride powder material after suppressing 10 kilograms is put in the graphite crucible of step (2) gained, and together puts in heating furnace, is 1 × 10 in vacuum-1Heat 10h when Pa, temperature are 350 DEG C, obtain the magnesium fluoride powder material that moisture is 1.2%.
(5) it is 1 × 10 by magnesium fluoride powder material that moisture is 1.2% in vacuum-3Heat when Pa, temperature are 1200 DEG C, after 36h, take out after material is with stove natural cooling, obtain the Afluon (Asta) polycrystalline of 8.7 kilograms of purity >=99.99%.
3 one kinds of UV grade crystal growth production methods of high purity magnesium fluoride polycrystalline of embodiment, comprise the following steps:
(1) prepare high purity magnesium fluoride powder material:
1. purification of sulphuric acids magnesium solution is prepared:
Being hydrolyzed by the pure water of 100 kilograms of Magnesium sulfate heptahydrate electrical conductivity≤1 μ S/cm and form the magnesium sulfate solution that mass concentration is 30%, the heating of this magnesium sulfate solution adds oxalic acid after 80 DEG C, filters after stirring reaction 5h, removes calcium oxalate and obtains filtrate；Filtrate is sequentially added into hydrogen peroxide, sodium hydroxide that mass concentration is 30%, and is stirred well to uniformly, through staticly settling 24h, to remove the metal impurities such as ferrum, manganese, nickel, aluminum, extract supernatant, obtain purification of sulphuric acids magnesium solution.
Wherein: the quality of oxalic acid is the 1.5% of magnesium sulfate solution quality；The quality of hydrogen peroxide is the 5% of magnesium sulfate solution quality；The quality of sodium hydroxide is the 2% of magnesium sulfate solution quality.
2. magnesium hydroxide presoma is prepared:
By the heating of purification of sulphuric acids magnesium solution to after 50 DEG C, add after the ammonia that mass concentration is 20% carries out complete reaction by the 1.3 of its quality times, filter by centrifugation and remove ammonium sulfate liquid, obtain magnesium hydroxide hydrate.This magnesium hydroxide hydrate is through pure water, with BaClAfter remaining to sulfate radical-free for indicator detection, obtain magnesium hydroxide presoma.
3. magnesium fluoride powder is prepared:
The reactor be lined with politef adds the analytical pure Fluohydric acid. that mass concentration is 40%, it is subsequently adding magnesium hydroxide presoma to be stirred, carry out fluorine element reaction when temperature is 80 DEG C, remove the hydrofluoric acid solution containing silicon through centrifugal filtration after 3h, obtain magnesium fluoride powder.
Wherein: the mass ratio of magnesium hydroxide presoma and Fluohydric acid. is 1:2.
4. high purity magnesium fluoride powder is prepared:
Magnesium fluoride powder is loaded corundum crucible, calcines 5h when temperature is 300 DEG C ~ 400 DEG C, obtain the magnesium fluoride powder of purity >=99.99%.
(2) adopt two high graphite techniques routinely to make graphite crucible, and Multi-layer graphite is set in vacuum drying oven and carbon felt is thermally shielded.
(3) high purity magnesium fluoride powder material is carried out pre-stamped, high purity magnesium fluoride bulk material after being suppressed or granular material.
(4) the high purity magnesium fluoride bulk material after suppressing 10 kilograms is put in the graphite crucible of step (2) gained, and together puts in heating furnace, is 1 × 10 in vacuum-1Heat 23h when Pa, temperature are 400 DEG C, obtain the Afluon (Asta) bulk material that moisture is 1%.
(5) it is 1 × 10 by magnesium fluoride powder material that moisture is 1% in vacuum-3Heat when Pa, temperature are 850 DEG C, after 68h, take out after material is with stove natural cooling, obtain the Afluon (Asta) polycrystalline of 8.3 kilograms of purity >=99.99%.
Claims (5)
1. a UV grade crystal growth production method for high purity magnesium fluoride polycrystalline, comprises the following steps:
(1) prepare high purity magnesium fluoride powder material:
1. purification of sulphuric acids magnesium solution is prepared:
The hydrolysis of Magnesium sulfate heptahydrate pure water is formed the magnesium sulfate solution that mass concentration is 20% ~ 30%, and the heating of this magnesium sulfate solution adds oxalic acid after 60 DEG C ~ 80 DEG C, filters, obtain filtrate after stirring reaction 3 ~ 5h；Described filtrate is sequentially added into hydrogen peroxide, sodium hydroxide that mass concentration is 30%, and is stirred well to uniformly, through staticly settling 12 ~ 24h, extract supernatant, obtain purification of sulphuric acids magnesium solution；The quality of described oxalic acid is the 0.5 ~ 1.5% of described magnesium sulfate solution quality；The quality of described hydrogen peroxide is the 3% ~ 5% of described magnesium sulfate solution quality；The quality of described sodium hydroxide is the 1% ~ 2% of described magnesium sulfate solution quality；
2. magnesium hydroxide presoma is prepared:
Described purification of sulphuric acids magnesium solution is heated after 30 DEG C ~ 50 DEG C, by the 1.1 ~ 1.3 of its quality times add mass concentration be 20% ammonia carry out complete reaction after, it is filtrated to get magnesium hydroxide hydrate by centrifugation, this magnesium hydroxide hydrate, after pure water to sulfate radical-free remains, obtains magnesium hydroxide presoma；
3. magnesium fluoride powder is prepared:
The reactor be lined with politef adds the analytical pure Fluohydric acid. that mass concentration is 40%, is subsequently adding described magnesium hydroxide presoma and is stirred, after the reaction of fluorine element after centrifugal filtration, obtain magnesium fluoride powder；The mass ratio of described magnesium hydroxide presoma and described Fluohydric acid. is 1:1.5 ~ 2；
4. high purity magnesium fluoride powder is prepared:
Described magnesium fluoride powder is loaded corundum crucible calcine, obtain the magnesium fluoride powder of purity >=99.99%；
(2) the two high graphite techniques routinely adopting high-purity high-density make graphite crucible, and arrange Multi-layer graphite in vacuum drying oven and carbon felt is thermally shielded；
(3) described high purity magnesium fluoride powder material is carried out pre-stamped, high purity magnesium fluoride bulk material after being suppressed or granular material；
(4) the high purity magnesium fluoride bulk material after described compacting is put in the graphite crucible of described step (2) gained, and together put in heating furnace, heating 10 ~ 36h when vacuum be 1 × 10-1Pa, temperature is 100 DEG C ~ 400 DEG C, obtains the Afluon (Asta) bulk material that moisture is 1 ~ 1.5%；
(5), by the heating when vacuum be 1 × 10-3Pa, temperature is 400 DEG C ~ 1300 DEG C of magnesium fluoride powder material that described moisture is 1 ~ 1.5%, after 36 ~ 100h, take out after material is with stove natural cooling, obtain the Afluon (Asta) polycrystalline of purity >=99.99%.
2. the production method of a kind of UV grade crystal growth high purity magnesium fluoride polycrystalline as claimed in claim 1, it is characterised in that: described step 1. in pure electrical conductivity of water≤1 μ S/cm.
3. the production method of a kind of UV grade crystal growth high purity magnesium fluoride polycrystalline as claimed in claim 1, it is characterised in that: described step 3. middle fluorine element reaction condition refers to that temperature is 60 ~ 80 DEG C, and the time is 1 ~ 3h.
4. the production method of a kind of UV grade crystal growth high purity magnesium fluoride polycrystalline as claimed in claim 1, it is characterised in that: described step 4. middle calcination condition refers to that in vacuum be 1 × 10-3Pa, and temperature is 400 DEG C ~ 1300 DEG C, and the time is 36 ~ 100h.
5. the production method of a kind of UV grade crystal growth high purity magnesium fluoride polycrystalline as claimed in claim 1, it is characterized in that: described step (3) in pre-stamped condition refer to the material after compacting, for block or graininess, as such, it is possible to release powder body material to fly upward problem in vacuum drying oven.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107352562A (en) * | 2017-08-10 | 2017-11-17 | 青海盐湖工业股份有限公司 | A kind of preparation technology of magnesium fluoride |
| CN114804165A (en) * | 2022-04-02 | 2022-07-29 | 五矿铍业股份有限公司 | Method for preparing magnesium fluoride by purifying magnesium fluoride waste residue |
-
2016
- 2016-02-03 CN CN201610073771.2A patent/CN105776259A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107352562A (en) * | 2017-08-10 | 2017-11-17 | 青海盐湖工业股份有限公司 | A kind of preparation technology of magnesium fluoride |
| CN114804165A (en) * | 2022-04-02 | 2022-07-29 | 五矿铍业股份有限公司 | Method for preparing magnesium fluoride by purifying magnesium fluoride waste residue |
| CN114804165B (en) * | 2022-04-02 | 2024-04-26 | 五矿铍业股份有限公司 | Method for preparing magnesium fluoride by purifying magnesium fluoride waste residues |
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