CN100398488C - Process for preparing magnesium aluminate spinel nano transparent ceramic - Google Patents
Process for preparing magnesium aluminate spinel nano transparent ceramic Download PDFInfo
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- CN100398488C CN100398488C CNB2006100223185A CN200610022318A CN100398488C CN 100398488 C CN100398488 C CN 100398488C CN B2006100223185 A CNB2006100223185 A CN B2006100223185A CN 200610022318 A CN200610022318 A CN 200610022318A CN 100398488 C CN100398488 C CN 100398488C
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- aluminate spinel
- magnesium aluminate
- spinel nano
- magnesium
- transparent ceramic
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Abstract
The invention discloses a preparing method of magnesium aluminate spinel nanometer transparent ceramic, which comprises the following steps: adopting high-purity magnesium aluminate spinel nanometer powder with purity more than 99% as raw material; moulding; sintering under high pressure at 500-700 Deg C for at least 20 min; obtaining the product.
Description
Technical field
The invention belongs to the crystalline ceramics field, particularly the preparation method of magnesium-aluminium spinel crystalline ceramics.
Background technology
Crystalline ceramics has be easy to do special-shaped device and the size of the good physicochemical property of high-temperature oxide monocrystalline and glass can do big two-fold advantage, so its Application Areas is more and more wider.The fervent expectation of people in recent years prepares the more pottery of excellent properties by the synthesis of nano pottery.
The U.S. just is devoted to develop transparent magnesia-alumina spinel (MgAl from the seventies in last century
2O
4) pottery, US3974249 in 1976 disclose a kind of preparation method of transparent spinel, but because of the restriction of method and technology, the material optical transmittance of preparation is lower.Continue after, US 4930731, US 4983555, US5244849 disclose the preparation method and the application thereof of transparent spinel again in succession, but aforesaid method passes through the hip treatment two-step approach after all adopting vacuum hotpressing or atmosphere sintering again, complex process not only, facility investment is big, and prepared transparent spinel do not have absorption peak at infrared band, causes range of application to be restricted.
Chinese patent ZL95117836.9 discloses a kind of transparent polycrystalline spinel (MgAl
2O
4) the preparation method, this method is added sintering agent LiF in the spinel powder, at 5～10MPa compacted under, Heating temperature is 1000～1100 ℃, is incubated 30 minutes, and (pressure is corresponding to rise to 40～50 tons to continue to be warming up to 1500～1700 ℃, φ 100mm mould), be incubated 2～5 hours, with 5 ℃/minute speed cooling, make transparent polycrystalline spinel then.Though above-mentioned preparation method has reduced the investment of equipment, obtained the higher transparent polycrystalline spinel of transmitance, sintering temperature height (1500～1700 ℃), the preparation method is still complicated, and prepared transparent spinel does not still have absorption peak at infrared band.
" Applied Physics Letters " discloses a kind of low temperature, ultra-high pressure sintering method (Lu Tiecheng of nano transparent ceramic in May, 2006, Chang Xianghui, Qi Jianqi, Luo Xiangjie, Low-temperaturehigh-pressure preparation of transparent nanocrystalline MgAl
2O
4Ceramics, Applied PhysicsLetters, Vol:88, No.23120,2006), this method is shaped to biscuit with the first pressing of magnesium aluminate spinel nano powder, under high pressure biscuit is carried out sintering with six-plane piercer then, about 600 ℃ of sintering temperatures, sintering time 20～30 minutes.Though this method provides a kind of different technical scheme of conceiving for the preparation crystalline ceramics, and prepared crystalline ceramics (MgAl
2O
4) two absorption peaks appear at infrared band, but the problem that exists is: prepared crystalline ceramics transmitance is lower, and (at wavelength is that the infrared band transmitance of 760～2200nm is less than 50%, at wavelength is that the visible light wave range transmitance of 500～760nm is less than 40%), macro-size little (less than 10 millimeters), cleavage block easily.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of improved magnesium aluminate spinel nano transparent ceramic is provided, this kind method not only technology is simple, and prepared infrared band has the crystalline ceramics (MgAl of absorption peak
2O
4) the transmitance raising, fragility reduces, and macro-size increases.
Technical scheme of the present invention: low temperature, ultra-high pressure sintering method to existing crystalline ceramics are improved, and replace six-plane piercer that molding biscuit is carried out sintering with belt type press.
The preparation method of magnesium aluminate spinel nano transparent ceramic of the present invention is a raw material with the magnesium aluminate spinel nano powder of purity＞99%, may further comprise the steps:
(1) powder moulding
Purity is packed in the mould greater than 99% magnesium aluminate spinel nano powder, under normal temperature, 5～20MPa pressure, be shaped to biscuit in 1～5 minute;
(2) high-pressure sinter
Biscuit is put into belt type press, sintering under 2～5GPa pressure, sintering temperature is 500～700 ℃, sintering time was at least 20 minutes, promptly made magnesium aluminate spinel nano transparent ceramic.
The magnesium aluminate spinel nano powder of the described raw material of aforesaid method---purity＞99%, be prepared from by analytical pure (＞99%) magnesium salts and aluminium salt, the proportioning of magnesium salts and aluminium salt is metering in 1: 2 by the mol ratio of Mg and Al, the preparation method adds deionized water with magnesium salts and aluminium salt to form mixing solutions (add-on of deionized water does not have strict demand, flooded magnesium salts and aluminium salt gets final product), then mixing solutions is put into process furnace, be heated to 1100～1150 ℃ of roastings at normal pressure with 5～10 ℃/minute speed, after this temperature is incubated 2 hours at least, make it to naturally cool to room temperature, obtain pure white fluffy magnesium-aluminium spinel (MgAl
2O
4) powder, grind the back with the sub-sieve screening, promptly obtain MgAl
2O
4Nano-powder.Described magnesium salts is MgSO
4Or Mg (NO
3)
2Or MgCO
3, described aluminium salt is NH
4Al (SO
4)
2Or Al (NO
3)
3Or NH
4Al (CO
3)
2
The raw material (the magnesium aluminate spinel nano powder of purity＞99%) that the method for the invention is used also can adopt the bimetal hydroxides and oxides ultrafine powders, and concrete technology is seen Chinese patent ZL 95117836.9.
The present invention has following beneficial effect:
1, need not add sintering agent in the magnesium aluminate spinel nano powder, both can simplify technology, can reduce cost again.
2, molding biscuit is directly put into the belt type press sintering, promptly makes magnesium aluminate spinel nano transparent ceramic, and technology is very simple.
3, sintering temperature low (500～700 ℃), sintering time short (being at least 20 minutes), but saves energy.
4, with respect to existing low temperature, ultra-high pressure sintering method, prepared infrared band has the transparency of the magnesium aluminate spinel nano transparent ceramic of two absorption peaks to be significantly improved, wavelength be the infrared band transmitance of 760～2200nm greater than 70%, wavelength is that the visible light wave range transmitance of 500～760nm is greater than 50% (see figure 2).
5, prepared magnesium aluminate spinel nano transparent ceramic fragility reduces, and ceramic cleavage block phenomenon is obviously improved.
6, prepared magnesium aluminate spinel nano transparent ceramic macro-size increases, and its macro-size can reach more than 30 millimeters.
7, prepared magnesium aluminate spinel nano transparent ceramic has an absorption peak respectively near the infrared band wavelength is 1430nm and 1970nm, thereby its range of application expansion, in fields such as infrared acquisition and infrared photographies wide application prospect is arranged.
Description of drawings
Fig. 1 is the magnesium aluminate spinel nano transparent ceramic (MgAl with the method for the invention preparation
2O
4) photo, this photo is the grid substrate photographs that magnesium-aluminum spinel ceramic is placed on literal, showing the transparency of magnesium-aluminum spinel ceramic.
Fig. 2 is the magnesium aluminate spinel nano transparent ceramic (MgAl with the method for the invention preparation
2O
4) transmittance curve, this transmittance curve is that 2 millimeters magnesium-aluminium spinel is measured with thickness, testing tool is ultraviolet/visible/infrared spectrophotometer, model Lambda 950, produced by PerkinElmer company.
Fig. 3 is the magnesium aluminate spinel nano transparent ceramic (MgAl of the method for the invention preparation
2O
4) transmission electron micrograph, this picture shows that the average grain size of described crystalline ceramics is less than 100 nanometers, the testing tool model is JEOL 3011.
Embodiment
Embodiment 1
The processing step of present embodiment is as follows:
(1) preparation magnesium aluminate spinel nano powder
With analytical pure MgSO
47H
2O (purity 〉=99.0%) and NH
4Al (SO
4)
212H
2O (purity 〉=99.5%) is a raw material, MgSO
47H
2O and NH
4Al (SO
4)
212H
2The proportioning of O is pressed the mol ratio metering in 1: 2 of Mg and Al.With the MgSO that measures
47H
2O and NH
4Al (SO
4)
212H
2O puts into container, and (add-on of deionized water does not have strict demand, floods MgSO to add deionized water and stirring formation mixing solutions
47H
2O and NH
4Al (SO
4)
212H
2O gets final product), mixing solutions is positioned in the retort furnace after with the quartz curette splendid attire, be heated to 1150 ℃ of roastings at normal pressure with 5 ℃/minute, insulation is 4 hours under this temperature, makes it to naturally cool to room temperature then, obtains pure white fluffy MgAl
2O
4Powder grinds the back with the sub-sieve screening, promptly obtains purity greater than 99% magnesium-aluminium spinel (MgAl
2O
4) nano-powder;
(2) powder moulding
The magnesium aluminate spinel nano powders of 10 gram steps (1) preparations are packed in the steel die, and pressurize promptly may be molded to biscuit in 3 minutes under the pressure of normal temperature, 10MPa;
(3) high-pressure sinter
Biscuit is put into belt type press, at 5 minutes pressure is risen to 4GPa, elevated temperature slowly when keeping this pressure rose to 500 ℃ at 5 minutes with temperature, 500 ℃ of sintering 20 minutes, cooled the temperature to room temperature then at 5 minutes, 5 minutes with pressure drop to normal pressure, promptly make magnesium aluminate spinel nano transparent ceramic, the photo after this is ceramic polished as shown in Figure 1, transmittance curve as shown in Figure 2, the projection electron microscope picture is as shown in Figure 3.
(1) preparation magnesium aluminate spinel nano powder
With analytical pure MgSO
47H
2O (purity 〉=99.0%) and NH
4Al (CO
3)
2(purity 〉=99.5%) is raw material, MgSO
47H
2O and NH
4Al (CO
3)
2Proportioning be metering in 1: 2 by the mol ratio of Mg and Al.With the MgSO that measures
47H
2O and NH
4Al (CO
3)
2Put into container, (add-on of deionized water does not have strict demand, floods MgSO to add deionized water and stirring formation mixing solutions
47H
2O and NH
4Al (CO
3)
2Get final product), mixing solutions is positioned in the retort furnace after with the quartz curette splendid attire, be heated to 1150 ℃ of roastings at normal pressure with 10 ℃/minute, insulation is 2 hours under this temperature, makes it to naturally cool to room temperature then, obtains pure white fluffy MgAl
2O
4Powder grinds the back with the sub-sieve screening, promptly obtains purity greater than 99% magnesium-aluminium spinel (MgAl
2O
4) nano-powder;
(2) powder moulding
The magnesium aluminate spinel nano powders of 10 gram steps (1) preparations are packed in the steel die, and pressurize promptly may be molded to biscuit in 5 minutes under the pressure of normal temperature, 5MPa;
(3) high-pressure sinter
Biscuit is put into belt type press, at 3 minutes pressure is risen to 3GPa, elevated temperature slowly when keeping this pressure, at 3 minutes temperature is risen to 700 ℃, 700 ℃ of sintering 30 minutes, cooled the temperature to room temperature then at 3 minutes, 3 minutes with pressure drop to normal pressure, promptly make magnesium aluminate spinel nano transparent ceramic.
Embodiment 3
(1) preparation magnesium aluminate spinel nano powder
With analytical pure Mg (NO
3)
2(purity 〉=99.0%) and NH
4Al (SO
4)
212H
2O (purity 〉=99.5%) is a raw material, Mg (NO
3)
2And NH
4Al (SO
4)
212H
2The proportioning of O is metering in 1: 2 by the mol ratio of Mg and Al.With the Mg (NO that measures
3)
2And NH
4Al (SO
4)
212H
2O puts into container, and (add-on of deionized water does not have strict demand, floods Mg (NO to add deionized water and stirring formation mixing solutions
3)
2And NH
4Al (SO
4)
212H
2O gets final product), mixing solutions is positioned in the retort furnace after with the quartz curette splendid attire, be heated to 1150 ℃ of roastings at normal pressure with 8 ℃/minute, insulation is 6 hours under this temperature, makes it to naturally cool to room temperature then, obtains pure white fluffy MgAl
2O
4Powder grinds the back with the sub-sieve screening, promptly obtains purity greater than 99% magnesium-aluminium spinel (MgAl
2O
4) nano-powder;
(2) powder moulding
The magnesium aluminate spinel nano powders of 10 gram steps (1) preparations are packed in the steel die, and pressurize promptly may be molded to biscuit in 2 minutes under the pressure of normal temperature, 15MPa;
(3) high-pressure sinter
Biscuit is put into belt type press, at 5 minutes pressure is risen to 5GPa, elevated temperature slowly when keeping this pressure, at 5 minutes temperature is risen to 600 ℃, 600 ℃ of sintering 25 minutes, cooled the temperature to room temperature then at 5 minutes, 5 minutes with pressure drop to normal pressure, promptly make magnesium aluminate spinel nano transparent ceramic.
Embodiment 4
(1) preparation magnesium aluminate spinel nano powder
With analytical pure MgCO
3(purity 〉=99.0%) and Al (NO
3)
3(purity 〉=99.5%) is raw material, MgCO
3And Al (NO
3)
3Proportioning be metering in 1: 2 by the mol ratio of Mg and Al.With the MgCO that measures
3And Al (NO
3)
3Put into container, (add-on of deionized water does not have strict demand, floods MgCO to add deionized water and stirring formation mixing solutions
3And Al (NO
3)
3Get final product), mixing solutions is positioned in the retort furnace after with the quartz curette splendid attire, be heated to 1150 ℃ of roastings at normal pressure with 6 ℃/minute, insulation is 4 hours under this temperature, makes it to naturally cool to room temperature then, obtains pure white fluffy MgAl
2O
4Powder grinds the back with the sub-sieve screening, promptly obtains purity greater than 99% magnesium-aluminium spinel (MgAl
2O
4) nano-powder;
(2) powder moulding
The magnesium aluminate spinel nano powders of 10 gram steps (1) preparations are packed in the steel die, and pressurize promptly may be molded to biscuit in 1 minute under the pressure of normal temperature, 20MPa;
(3) high-pressure sinter
Biscuit is put into belt type press, at 3 minutes pressure is risen to 2GPa, elevated temperature slowly when keeping this pressure, in 3 minutes, temperature is risen to 500 ℃, 500 ℃ of sintering 20 minutes, cooled the temperature to room temperature then at 3 minutes, 3 minutes with pressure drop to normal pressure, promptly make magnesium aluminate spinel nano transparent ceramic.
The belt type press that uses in the foregoing description, 2 * 3500 tons of model DS are the commercial goods; The used pressurizing device of powder moulding is a screw block.
Claims (3)
1. the preparation method of a magnesium aluminate spinel nano transparent ceramic is raw material with purity greater than 99% magnesium aluminate spinel nano powder, it is characterized in that may further comprise the steps:
(1) powder moulding
Purity is packed in the mould greater than 99% magnesium aluminate spinel nano powder, under normal temperature, 5～20MPa pressure, be shaped to biscuit in 1～5 minute;
(2) high-pressure sinter
Biscuit is put into belt type press, sintering under 2～5GPa pressure, sintering temperature is 500～700 ℃, sintering time was at least 20 minutes, promptly made magnesium aluminate spinel nano transparent ceramic.
2. the preparation method of magnesium aluminate spinel nano transparent ceramic according to claim 1, it is characterized in that described magnesium aluminate spinel nano powder is prepared from by analytical pure magnesium salts and aluminium salt, the proportioning of magnesium salts and aluminium salt is metering in 1: 2 by the mol ratio of Mg and Al, the preparation method adds deionized water formation mixing solutions with magnesium salts and aluminium salt, then mixing solutions is put into process furnace and be heated to 1100～1150 ℃ of roastings with 5～10 ℃/minute speed, after this temperature is incubated 2 hours at least, make it to naturally cool to room temperature, promptly make the magnesium aluminate spinel nano powder.
3. the preparation method of magnesium aluminate spinel nano transparent ceramic according to claim 2 is characterized in that described magnesium salts is MgSO
4Or Mg (NO
3)
2, described aluminium salt is NH
4Al (SO
4)
2Or Al (NO
3)
3Or NH
4Al (CO
3)
2
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| CN106630996A (en) * | 2016-12-12 | 2017-05-10 | 天津津航技术物理研究所 | Preparation method of gel injection molding MgAl2O4 biscuit |
| CN111807828A (en) * | 2020-07-07 | 2020-10-23 | 上海衡益特陶新材料有限公司 | Preparation method of low-cost magnesia-alumina spinel transparent ceramic product |
| CN112415637B (en) * | 2020-11-24 | 2022-05-10 | 中国科学院上海硅酸盐研究所 | Super-thick ceramic lens, manufacturing method of super-thick ceramic lens and laser lighting device |
| CN114195505A (en) * | 2021-11-25 | 2022-03-18 | 天津津航技术物理研究所 | Ceramic with red fluorescence property and preparation method thereof |
| CN114538913B (en) * | 2022-02-17 | 2023-05-02 | 大连海事大学 | Pure-phase nano MgAl with high sintering activity 2 O 4 Powder and preparation method and application thereof |
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2006
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