CN106045517A - Zinc selenide transparent nano-ceramic and preparation method thereof - Google Patents

Zinc selenide transparent nano-ceramic and preparation method thereof Download PDF

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CN106045517A
CN106045517A CN201610386957.3A CN201610386957A CN106045517A CN 106045517 A CN106045517 A CN 106045517A CN 201610386957 A CN201610386957 A CN 201610386957A CN 106045517 A CN106045517 A CN 106045517A
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acid
zinc
zinc selenide
transparent ceramic
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夏晨曦
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Abstract

The invention provides zinc selenide transparent nano-ceramic and a preparation method thereof, and belongs to the field of ceramic material production. The zinc selenide transparent nano-ceramic is mainly prepared from, by weight, 5-15 parts of zinc acetate, 5-15 parts of ferrous acetate, 10-20 parts of sodium selenide, 0.1-0.5 part of methacrylic acid, 0.5-2 parts of acetic acid, 1-5 parts of ammonium hydroxide, 20-40 parts of methyl alcohol, 0.5-5 parts of dispersing agent, 2-6 parts of pH regulator, 40-80 parts of absolute ethyl alcohol, 20-80 parts of deionized water and 1-5 parts of sintering aids. The prepared transparent ceramic is good in optical property, high in mechanical property and not prone to fragmentation.

Description

A kind of zinc selenide nano transparent ceramic and preparation method thereof
Technical field
The invention belongs to ceramic material production field, concretely relate to a kind of zinc selenide nano transparent ceramic and system thereof Preparation Method.
Background technology
General pottery is opaque, but optical ceramics is the most transparent, therefore claims crystalline ceramics.General pottery is opaque Reason be inside it, to there is impurity and pore, the former can absorbing light, the latter makes light produce scattering, so just the most impermeable clear.Cause If this selects high pure raw material, and gets rid of pore by process means it is possible to obtain crystalline ceramics.With zinc selenide for material system Standby crystalline ceramics can be used to make completely reflecting mirror, half-reflecting mirror, beam expanding lens, field flattening lens, mid-infrared eyeglass, far infrared Various planoconvex lenss on 10.6Um/CO2 high or low power laser instrument, convex-concave crescent moon cutting lens, gold-plated reflecting mirror, circular polarizer, Beam expanding lens, field flattening lens etc..It is the most all to use chemical gaseous phase depositing process synthesis of zinc selenide material, although its light Performance is good, but mechanical performance is poor.
Summary of the invention
For solving above-mentioned technical problem, the present invention provides a kind of zinc selenide nano transparent ceramic and preparation method thereof.To change The problem of zinc selenide nano transparent ceramic bad mechanical property prepared by kind prior art.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
A kind of zinc selenide nano transparent ceramic, mainly includes following raw material, by parts by weight meter: zinc acetate 5-15 part, acetic acid Asia Ferrum 5-15 part, sodium selenide 10-20 part, methacrylic acid 0.1-0.5 part, acetic acid 0.5-2 part, ammonia 1-5 part, methanol 20-40 part, Dispersant 0.5-5 part, pH adjusting agent 2-6 part, dehydrated alcohol 40-80 part, deionized water 20-80 part, sintering aid 1-5 part.
Preferably, in the preferred embodiment, described zinc acetate is two water and zinc acetate, and described Ferrous acetate is Four water and Ferrous acetate.
Preferably, in the preferred embodiment, described sintering aid is in terms of weight/mass percentage composition, by TEOS 0.01-0.1%、TiO2 0.01-0.05%、LiO 0.01-0.05%、BaO 0.1-1.5%、MgO 0.002-0.01%、CaO 0.5-2.5%、ZrO20.01-0.05%, SrO 0.1-0.5% forms.
Preferably, in the preferred embodiment, described dispersant is ethanedioic acid, malonic acid, 1,3-propanedicarboxylic acid, and oneself is two years old Acid, 1,5-pentanedicarboxylic acid., suberic acid, Azelaic Acid, the mixture of any two kinds in decanedioic acid.
Present invention also offers the preparation method of a kind of zinc selenide nano transparent ceramic, comprise the following steps:
(1) described zinc acetate, described Ferrous acetate, described sodium selenide are dissolved in described deionized water and the solution of described methanol In, with 30-50r/min mix and blend 10-30min, obtain mother solution；
(2) described polymethylacrylic acid is added in described mother solution, described acetic acid and described ammonia are configured to mixed solution, slow Slowly it is added drop-wise in described mother solution, is warming up to 40-60 DEG C simultaneously and stirs 30-60min with 50-80r/min, after being added dropwise to complete, adding Enter described dispersant, described pH adjusting agent stirs；
(3) stand 12-18h, go out precipitate with 800-1200rpm centrifugation, described precipitate is anti-with described dehydrated alcohol Multiple cleaning, the most in a vacuum furnace, keeping temperature is 45-65 DEG C of drying, obtains nano-powder raw material；
(4) described nano-powder raw material and described sintering aid mix homogeneously are put in compression mold, at 50MPa-100MPa Pressure under compressing, at 1000-1150 DEG C after molding, vacuum is 0.5-4 × 10-3Sinter under the conditions of MPa, obtain zinc selenide Nano transparent ceramic.
Preferably, in the preferred embodiment, described rate of titration is 3-7ml/min;The pH value of regulation solution For 10.5-11.5.
Preferably, in the preferred embodiment, described in step (3), in vacuum drying oven, gas can be vacuum, nitrogen Gas or noble gas.
Beneficial effects of the present invention: zinc selenide nano transparent ceramic provided by the present invention not only has the most optical Can, also there is stronger mechanical performance.The present invention uses coprecipitation during powder material producing, various by solution Chemical reaction directly obtains the nano-powder material that chemical composition is homogeneous, granularity is little and is evenly distributed.Preparation technology of the present invention letter Single, the cycle is short, is suitable for producing in enormous quantities.
Below in conjunction with specific embodiment, technical scheme of the present invention is further described.
Embodiment 1:
A kind of zinc selenide nano transparent ceramic, mainly includes following raw material, by parts by weight meter: zinc acetate 5 parts, Ferrous acetate 5 Part, sodium selenide 10 parts, methacrylic acid 0.1 part, acetic acid 0.5 part, ammonia 1 part, methanol 20 parts, dispersant 0.5 part, pH adjusting agent 2 parts, dehydrated alcohol 40 parts, deionized water 20 parts, sintering aid 1 part.
Zinc acetate is two water and zinc acetate, and Ferrous acetate is four water and Ferrous acetate.
Sintering aid in terms of weight/mass percentage composition, by TEOS 0.01%, TiO2 0.01%, LiO 0.01%, BaO 0.1%, MgO 0.002%、CaO 0.5%、ZrO20.01%, SrO 0.1% forms.
Dispersant is the mixture of ethanedioic acid and malonic acid.
The present embodiment additionally provides the preparation method of a kind of zinc selenide nano transparent ceramic, comprises the following steps:
(1) zinc acetate, Ferrous acetate, sodium selenide are dissolved in the solution of deionized water and methanol, with 30r/min mix and blend 10min, obtains mother solution；
(2) polymethylacrylic acid is added in mother solution, acetic acid and ammonia is configured to mixed solution, is slowly dropped in mother solution, Being warming up to 40 DEG C simultaneously and stir 30min with 50r/min, after being added dropwise to complete, addition dispersant, pH adjusting agent stir；
(3) stand 12h, go out precipitate with 800rpm centrifugation, precipitate dehydrated alcohol is cleaned repeatedly, then in vacuum In stove, keeping temperature is 45 DEG C of drying, obtains nano-powder raw material；
(4) nano-powder raw material and sintering aid mix homogeneously are put in compression mold, be pressed under the pressure of 50MPa Type, at 1000 DEG C after molding, vacuum is 0.5 × 10-3Sinter under the conditions of MPa, obtain zinc selenide nano transparent ceramic.
Rate of titration is 3ml/min;The pH value of regulation solution is 10.5.
In step (3), in vacuum drying oven, gas is nitrogen.
Embodiment 2:
A kind of zinc selenide nano transparent ceramic, mainly includes following raw material, by parts by weight meter: zinc acetate 15 parts, Ferrous acetate 15 parts, sodium selenide 20 parts, methacrylic acid 0.5 part, acetic acid 2 parts, ammonia 5 parts, methanol 40 parts, dispersant 5 parts, pH adjusting agent 6 Part, dehydrated alcohol 80 parts, deionized water 80 parts, sintering aid 5 parts.
Zinc acetate is two water and zinc acetate, and Ferrous acetate is four water and Ferrous acetate.
Sintering aid in terms of weight/mass percentage composition, by TEOS 0.1%, TiO2 0.05%, LiO 0.05%, BaO 1.5%, MgO 0.01%、CaO 2.5%、ZrO20.05%, SrO 0.5% forms.
Dispersant is the mixture of ethanedioic acid and adipic acid.
The present embodiment additionally provides the preparation method of a kind of zinc selenide nano transparent ceramic, comprises the following steps:
(1) zinc acetate, Ferrous acetate, sodium selenide are dissolved in the solution of deionized water and methanol, with 50r/min mix and blend 30min, obtains mother solution；
(2) polymethylacrylic acid is added in mother solution, acetic acid and ammonia is configured to mixed solution, is slowly dropped in mother solution, Being warming up to 60 DEG C simultaneously and stir 60min with 80r/min, after being added dropwise to complete, addition dispersant, pH adjusting agent stir；
(3) stand 18h, go out precipitate with 1200rpm centrifugation, precipitate dehydrated alcohol is cleaned repeatedly, then very In empty stove, keeping temperature is 65 DEG C of drying, obtains nano-powder raw material；
(4) nano-powder raw material and sintering aid mix homogeneously are put in compression mold, be pressed under the pressure of 100MPa Type, at 1150 DEG C after molding, vacuum is 4 × 10-3Sinter under the conditions of MPa, obtain zinc selenide nano transparent ceramic.
Rate of titration is 7ml/min;The pH value of regulation solution is 11.5.
In step (3), in vacuum drying oven, gas is noble gas.
Embodiment 3:
A kind of zinc selenide nano transparent ceramic, mainly includes following raw material, by parts by weight meter: zinc acetate 10 parts, Ferrous acetate 10 parts, sodium selenide 15 parts, methacrylic acid 0.3 part, acetic acid 1.25 parts, ammonia 3 parts, methanol 30 parts, dispersant 2.7 parts, pH adjust Joint agent 4 parts, dehydrated alcohol 60 parts, deionized water 50 parts, sintering aid 3 parts.
Zinc acetate is two water and zinc acetate, and Ferrous acetate is four water and Ferrous acetate.
Sintering aid in terms of weight/mass percentage composition, by TEOS 0.055%, TiO2 0.03%, LiO 0.03%, BaO 0.8%, MgO 0.006%、CaO 1.5%、ZrO20.03%, SrO 0.3% forms.
Dispersant is ethanedioic acid, the mixture of malonic acid.
The present embodiment additionally provides the preparation method of a kind of zinc selenide nano transparent ceramic, comprises the following steps:
(1) zinc acetate, Ferrous acetate, sodium selenide are dissolved in the solution of deionized water and methanol, with 40r/min mix and blend 20min, obtains mother solution；
(2) polymethylacrylic acid is added in mother solution, acetic acid and ammonia is configured to mixed solution, is slowly dropped in mother solution, Being warming up to 50 DEG C simultaneously and stir 45min with 65r/min, after being added dropwise to complete, addition dispersant, pH adjusting agent stir；
(3) stand 15h, go out precipitate with 1000rpm centrifugation, precipitate dehydrated alcohol is cleaned repeatedly, then very In empty stove, keeping temperature is 55 DEG C of drying, obtains nano-powder raw material；
(4) nano-powder raw material and sintering aid mix homogeneously are put in compression mold, be pressed under the pressure of 75MPa Type, at 1075 DEG C after molding, vacuum is 2.3 × 10-3Sinter under the conditions of MPa, obtain zinc selenide nano transparent ceramic.
Rate of titration is 5ml/min;The pH value of regulation solution is 11.
In step (3), vacuum drying oven is vacuum, without other gas.
The zinc selenide nano transparent ceramic preparing embodiment 1-3 is finished to the thin slice of 2mm, 3-15 μm transmitance and Mechanical performance is tested, and test result is as shown in table 1:
Table 1
Embodiment Transmitance, % Impact strength, J/cm2
Embodiment 1 65.4 0.92
Embodiment 2 68.2 1.05
Embodiment 3 73.5 1.12
As known from Table 1, the zinc selenide nano transparent ceramic transmitance that the present invention prepares is all more than 65%, and impact strength all exists 0.9J/cm2Above.By contrast find the zinc selenide nano transparent ceramic that embodiment 3 prepares have concurrently excellent optical property and Stronger mechanical performance.

Claims (7)

1. a zinc selenide nano transparent ceramic, it is characterised in that mainly include following raw material, by parts by weight meter: zinc acetate 5-15 part, Ferrous acetate 5-15 part, sodium selenide 10-20 part, methacrylic acid 0.1-0.5 part, acetic acid 0.5-2 part, ammonia 1-5 Part, methanol 20-40 part, dispersant 0.5-5 part, pH adjusting agent 2-6 part, dehydrated alcohol 40-80 part, deionized water 20-80 part, burning Knot auxiliary agent 1-5 part.
Zinc selenide nano transparent ceramic the most according to claim 1, it is characterised in that: described zinc acetate is two water and acetic acid Zinc, described Ferrous acetate is four water and Ferrous acetate.
Zinc selenide nano transparent ceramic the most according to claim 1, it is characterised in that: described sintering aid is with percent mass Content meter, by TEOS 0.01-0.1%, TiO2 0.01-0.05%, LiO 0.01-0.05%, BaO 0.1-1.5%, MgO 0.002-0.01%、CaO 0.5-2.5%、ZrO20.01-0.05%, SrO 0.1-0.5% forms.
Zinc selenide nano transparent ceramic the most according to claim 1, it is characterised in that: described dispersant is ethanedioic acid, third Diacid, 1,3-propanedicarboxylic acid, adipic acid, 1,5-pentanedicarboxylic acid., suberic acid, Azelaic Acid, the mixture of any two kinds in decanedioic acid.
5. the preparation method of the zinc selenide nano transparent ceramic as described in any one of claim 1-4, it is characterised in that bag Include following steps:
(1) described zinc acetate, described Ferrous acetate, described sodium selenide are dissolved in described deionized water and the solution of described methanol In, with 30-50r/min mix and blend 10-30min, obtain mother solution；
(2) described polymethylacrylic acid is added in described mother solution, described acetic acid and described ammonia are configured to mixed solution, slow Slowly it is added drop-wise in described mother solution, is warming up to 40-60 DEG C simultaneously and stirs 30-60min with 50-80r/min, after being added dropwise to complete, adding Enter described dispersant, described pH adjusting agent stirs；
(3) stand 12-18h, go out precipitate with 800-1200rpm centrifugation, described precipitate is anti-with described dehydrated alcohol Multiple cleaning, the most in a vacuum furnace, keeping temperature is 45-65 DEG C of drying, obtains nano-powder raw material；
(4) described nano-powder raw material and described sintering aid mix homogeneously are put in compression mold, at 50MPa-100MPa Pressure under compressing, at 1000-1150 DEG C after molding, vacuum is 0.5-4 × 10-3Sinter under the conditions of MPa, obtain zinc selenide Nano transparent ceramic.
The preparation method of zinc selenide nano transparent ceramic the most according to claim 5, it is characterised in that: described rate of titration For 3-7ml/min;The pH value of regulation solution is 10.5-11.5.
The preparation method of zinc selenide nano transparent ceramic the most according to claim 5, it is characterised in that: institute in step (3) Stating gas in vacuum drying oven can be vacuum, nitrogen or noble gas.
CN201610386957.3A 2016-06-02 2016-06-02 Zinc selenide transparent nano-ceramic and preparation method thereof Pending CN106045517A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060275196A1 (en) * 2005-03-28 2006-12-07 The Research Foundation Of State University Of New York Synthesis of nanostructured materials using liquid crystalline templates
CN1978378A (en) * 2005-12-01 2007-06-13 中国科学院福建物质结构研究所 Mid-infrared laser nano transparent ceramic material iron-doped zinc selenide
CN101855187A (en) * 2007-09-14 2010-10-06 宾夕法尼亚州立大学研究基金会 The manufacture method of crystalline ceramics
CN101920942A (en) * 2010-09-20 2010-12-22 东华大学 Method for controlling synthesis of zinc selenide multi-morphological nano material
CN103159189A (en) * 2013-04-03 2013-06-19 南京理工大学 Synthesis method of ZnSe hollow microspheres by alcohol thermal reduction

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060275196A1 (en) * 2005-03-28 2006-12-07 The Research Foundation Of State University Of New York Synthesis of nanostructured materials using liquid crystalline templates
CN1978378A (en) * 2005-12-01 2007-06-13 中国科学院福建物质结构研究所 Mid-infrared laser nano transparent ceramic material iron-doped zinc selenide
CN101855187A (en) * 2007-09-14 2010-10-06 宾夕法尼亚州立大学研究基金会 The manufacture method of crystalline ceramics
CN101920942A (en) * 2010-09-20 2010-12-22 东华大学 Method for controlling synthesis of zinc selenide multi-morphological nano material
CN103159189A (en) * 2013-04-03 2013-06-19 南京理工大学 Synthesis method of ZnSe hollow microspheres by alcohol thermal reduction

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《简明化学试剂手册》编写组: "《简明化学试剂手册》", 31 January 1991, 上海科学技术出版社 *

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