CN102976389A - Modified yttrium oxide powder and preparation method thereof - Google Patents
Modified yttrium oxide powder and preparation method thereof Download PDFInfo
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- CN102976389A CN102976389A CN2012105471026A CN201210547102A CN102976389A CN 102976389 A CN102976389 A CN 102976389A CN 2012105471026 A CN2012105471026 A CN 2012105471026A CN 201210547102 A CN201210547102 A CN 201210547102A CN 102976389 A CN102976389 A CN 102976389A
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Abstract
The invention discloses a modified yttrium oxide having hydration resistance and a preparation method thereof. The surface of the yttrium oxide powder is sequentially coated with organic carboxylic acid and non-ionic surfactant, wherein the organic carboxylic acid is stearic acid or adipic acid; and the non-ionic surfactant is polyoxyethylene oleyl alcohol ether type, ethoxylated methyl glucoside stearate type or tween 80 (polyoxyethylene sorbitan monooleate) type surfactant. According to the invention, the preparation process is simple; and the prepared modified yttrium oxide powder has excellent hydration resistance, can be well soaked with water and can remain stable without being subjected to hydrolysis reaction in a humid environment at a temperature of 60 DEG C or below.
Description
Technical field
The present invention relates to a kind of modified oxidized yttrium powder and preparation method thereof, be specifically related to modified oxidized yttrium powder of a kind of anti-aquation and preparation method thereof.
Background technology
Yttrium oxide has high fusing point (2430 ℃), (0.23 ~ 8 μ m) wave band has high transmitance from the ultraviolet to the mid and far infrared, is mainly used in window and nose cone, microwave base plate, insulating support, infrared generator shell, Infrared Lens and other window pyrometer etc. of infra-red missile.In recent years, because good light transmission and the application thereof of yttrium oxide, yttrium oxide transparent ceramic causes people's extensive concern.
Yttrium oxide transparent ceramic often adopts dry-pressing and the static pressure method moulding such as cold rolling, and these two kinds of forming methods are suitable for preparing the sample of simple shape.Wet moulding can prepare the ceramic body of shape matching complexity, but the report for preparing yttrium oxide transparent ceramic about wet moulding seldom.Major cause is because yttrium oxide powder and water have higher reactive behavior, easy deliquescence in air, the easy and living reaction of steeping in water for reconstitution generates the yttrium hydroxide compound in water, affect the surface properties of yttrium oxide powder, the water base yttrium oxide slurry that preparation performance is good is relatively more difficult.Therefore, yttria surfaces being carried out anti-hydration process tool is of great significance.
Summary of the invention
To the objective of the invention is the defective that exists in the prior art in order solving, a kind of modified oxidized yttrium with anti-hydratability and preparation method thereof to be provided.
In order to achieve the above object, the invention provides a kind of modified oxidized yttrium powder, this yttrium oxide powder surface is wrapped up organic carboxyl acid and nonionic surface active agent successively; Organic carboxyl acid is stearic acid or hexanodioic acid, preferred stearic acid; Nonionic surface active agent is for being Brij92 type, ethoxylation methyl glucoside stearate type, tween 80 (polyoxyethylene sorbitol acid anhydride list olein) type tensio-active agent, preferred Brij92 type tensio-active agent.
The present invention also provides the preparation method of above-mentioned modified oxidized yttrium powder, may further comprise the steps:
(1) yttrium oxide powder and organic carboxyl acid are immersed in the organic solution, and ceaselessly stirred 2 ~ 4 hours, then left standstill 1～2 hour; Organic solution is easily evaporation and the large solvent of surface tension of low temperature, is selected from ether, toluene, dimethylbenzene, methyl alcohol, Virahol or its mixing solutions, and preferred volume ratio is the dimethylbenzene of 75.5:24.5 and the mixing solutions of methyl alcohol; Per 100 gram yttrium oxide powders need add the organic carboxyl acid of 5 ~ 10ml, and preferred addition is 8ml, and the consumption of described organic solution is that per 100 gram yttrium oxide powders add 100～300ml, and preferable amount is that every gram yttrium oxide powder adds 200ml;
(2) add nonionic surface active agent in the organic solution after leaving standstill in the step (1), 60～80 ℃ of lower heated and stirred 3～7 hours, filter, get pressed powder; The consumption of described nonionic surface active agent is that per 100 gram yttrium oxide powders add 6～10ml, and preferable amount is that every gram yttrium oxide powder adds 8ml;
(3) with filtering the pressed powder oven dry under 80～100 ℃ that makes in the step (2), namely get modified oxidized yttrium powder.
Organic carboxyl acid such as stearic acid in the step (1), adipic acid etc., main preferred stearic acid; Stir and adopt the planetary mills high-speed stirring, rotating speed is 188r/min, and the time is 2 ~ 4 hours.
Nonionic surface active agent is the Brij92 type in the step (2), ethoxylation methyl glucoside stearate type, tween 80 type (polyoxyethylene sorbitol acid anhydride list olein), preferred Brij92 type; Add the thermal recovery ultra thermostat, 60 ~ 80 ℃ of heating in water bath of constant temperature utilize electric blender to stir 3～7 hours.
Step (3) adopts first organic solvent that powder is repeatedly cleaned before powder is dried, and preferred alcohol solution (dehydrated alcohol) cleans 2 ~ 4 times.Adopt vacuum drying box to dry after cleaning, storing temperature is 80 ~ 100 ℃, and the time is 2 ~ 5 hours.
The present invention has the following advantages compared to existing technology: utilize surface adsorption technique, at first so that organic carboxyl acid is adsorbed on the yttrium oxide powder surface, thereby the prevention water molecules contacts with yttria surfaces, simultaneously wrap up again one deck nonionogenic tenside at powder surface, both improved the powder hydration resistance, so that powder can well infiltrate with water, and organic carboxyl acid and nonionic surface active agent at high temperature easily decompose, and do not affect original performance of yttrium oxide again.Preparation technology of the present invention is simple, the modified oxidized yttrium powder hydration resistance that makes is outstanding, can well infiltrate with water, and in wet environment below 60 ℃, keep the stable hydrolysis reaction that do not occur, can effectively solve the difficulty that yttrium oxide powder brings in storage, transportation and follow-up technological process, and provide support for the water base yttrium oxide slurry of preparation high solids content.
Description of drawings
Fig. 1 soaks the modified oxidized yttrium powder of the present invention and starting powder under 60 ℃, the pH value time history plot of water in the water;
Fig. 2 soaks the modified oxidized yttrium powder of the present invention and starting powder 10min, the temperature variant graphic representation of pH value of water in the water.
Among the figure, 1-starting powder, the modified oxidized yttrium powder of 2-.
Embodiment
Below in conjunction with specific embodiment the modified oxidized yttrium of the present invention is elaborated.
Embodiment one
(1) stearic acid of 50g yttrium oxide powder and 5ml is immersed in the 50ml ethanolic soln, and ceaselessly stirred 4 hours, then left standstill 1 hour;
(2) in the mixture of step (1), add 3ml tween 80 type nonionic surface active agent, in 80 ℃ of stirring in water bath heating 3 hours, filter;
(3) yttrium oxide powder that leaches in the step (2) is cleaned 4 times with dehydrated alcohol;
(4) 100 ℃ of oven dry of the yttrium oxide powder after will cleaning are 2 hours, namely obtain the exsertile modified oxidized yttrium powder of hydration resistance.
Embodiment two
(1) 100g yttrium oxide powder and 5ml adipic acid are immersed in the mixing solutions of 200ml dimethylbenzene and methyl alcohol (volume ratio 75.5:24.5), and ceaselessly stirred 2 hours, then left standstill 2 hours;
(2) in said mixture, add 10ml Brij92 type nonionic surface active agent, in 60 ℃ of stirring in water bath heating 7 hours, filter;
(3) yttrium oxide powder that leaches in the step (2) is cleaned 4 times with dehydrated alcohol;
(4) 80 ℃ of oven dry of the yttrium oxide powder after will cleaning are 5 hours, namely obtain the exsertile modified oxidized yttrium powder of hydration resistance.
Embodiment three
(1) stearic acid of 100g yttrium oxide powder and 8ml is immersed in the mixing solutions of 300ml dimethylbenzene and methyl alcohol (volume ratio 75.5:24.5), and ceaselessly stirred 4 hours, then left standstill 2 hours;
(2) in said mixture, add 8ml tween 80 type nonionic surface active agent, in 60 ℃ of stirring in water bath heating 5 hours, filter;
(3) yttrium oxide powder that leaches in the step (2) is cleaned 4 times with dehydrated alcohol;
(4) 80 ℃ of oven dry of the yttrium oxide powder after will cleaning are 5 hours, namely obtain the exsertile modified oxidized yttrium powder of hydration resistance.
Effect embodiment
The modified oxidized yttrium powder of embodiment three preparation is immersed in the water, under 60 ℃, soaks starting powder in the contrast water, observe the pH value of water over time, as shown in Figure 1.As shown in Figure 1, undressed starting powder 1 is with the growth of soak time, aquation gradually, and the pH value increases thereupon; Modified oxidized yttrium powder 2 through anti-hydration process soaks through long-time in water, and its pH remains unchanged substantially.
The modified oxidized yttrium powder of embodiment three preparations is immersed in 10min in the water, soaks starting powder in the contrast water, under differing temps, observe the pH value of water, as shown in Figure 2.As shown in Figure 2, undressed starting powder 1 is with the rising of soaking temperature, and extent of hydration increases gradually, and the pH value increases thereupon; Modified oxidized yttrium powder 2 has better stability below 60 ℃, and aquation does not occur.
Respectively the modified oxidized yttrium powder of embodiment one and embodiment two preparations is immersed in the water below 60 ℃, all can keeps stable preferably, illustrate that the modified oxidized yttrium powder for preparing by the present invention has stronger hydration resistance.
Claims (7)
1. modified oxidized yttrium powder, it is characterized in that: described yttrium oxide powder surface is wrapped up organic carboxyl acid and nonionic surface active agent successively; Described organic carboxyl acid is stearic acid or hexanodioic acid; Described nonionic surface active agent is for being Brij92 type, ethoxylation methyl glucoside stearate type, tween 80 type tensio-active agent.
2. modified oxidized yttrium powder according to claim 1, it is characterized in that: described organic carboxyl acid is stearic acid; Described nonionic surface active agent is Brij92 type tensio-active agent.
3. preparation method of modified oxidized yttrium powder as claimed in claim 1 or 2 is characterized in that: may further comprise the steps:
(1) described yttrium oxide powder and described organic carboxyl acid are immersed in the organic solution, and ceaselessly stirred 2 ~ 4 hours, then left standstill 1～2 hour; Described organic solution is selected from ether, toluene, dimethylbenzene, methyl alcohol, Virahol or its mixing solutions; The consumption of described organic carboxyl acid is that per 100 gram yttrium oxide powder add 5 ~ 10ml, and the consumption of described organic solution is that per 100 gram yttrium oxide powders add 100～300ml;
(2) add nonionic surface active agent in the organic solution after leaving standstill in the step (1), 60～80 ℃ of lower heated and stirred 3～7 hours, filter, get pressed powder; The consumption of described nonionic surface active agent is that per 100 gram yttrium oxide powders add 6～10ml;
(3) with filtering the pressed powder oven dry under 80～100 ℃ that makes in the step (2), namely get described modified oxidized yttrium powder.
4. the preparation method of modified oxidized yttrium powder according to claim 3 is characterized in that: per 100 gram yttrium oxide powders need add the organic carboxyl acid of 8ml in the described step (1), and the consumption of described organic solution is that per 100 gram yttrium oxide powders add 200ml; The consumption of nonionic surface active agent is that per 100 gram yttrium oxide powders add 8ml in the described step (2).
5. the preparation method of modified oxidized yttrium powder according to claim 3 is characterized in that: organic solution is the mixing solutions of dimethylbenzene and methyl alcohol in the described step (1); The volume ratio of described dimethylbenzene and methyl alcohol is 75.5:24.5.
6. the preparation method of modified oxidized yttrium powder according to claim 3 is characterized in that: to before the pressed powder oven dry, adopt first organic solvent to clean 2～4 times in the described step (3); Described organic solvent adopts dehydrated alcohol.
7. the preparation method of modified oxidized yttrium powder according to claim 3 is characterized in that: drying time is 2～5 hours in the described step (3).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110204334A (en) * | 2019-05-29 | 2019-09-06 | 常州大学 | A kind of high-compactness Zirconium oxide powder injection moulding PP Pipe Compound and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20120270050A1 (en) * | 2009-04-23 | 2012-10-25 | Anderson Scott L | Functionally Coated Non-Oxidized Particles and Methods for Making the Same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20120270050A1 (en) * | 2009-04-23 | 2012-10-25 | Anderson Scott L | Functionally Coated Non-Oxidized Particles and Methods for Making the Same |
Non-Patent Citations (2)
| Title |
|---|
| 姚义俊等: "表面涂覆氮化铝粉末的抗水化性", 《硅酸盐学报》, vol. 38, no. 5, 31 May 2010 (2010-05-31), pages 913 - 917 * |
| 靳玲玲等: "氧化钇粉体的抗水化处理研究", 《人工晶体学报》, vol. 38, 31 August 2009 (2009-08-31), pages 321 - 323 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204334A (en) * | 2019-05-29 | 2019-09-06 | 常州大学 | A kind of high-compactness Zirconium oxide powder injection moulding PP Pipe Compound and preparation method thereof |
| CN110204334B (en) * | 2019-05-29 | 2021-12-21 | 常州大学 | Special material for high-density zirconium oxide powder injection molding and preparation method thereof |
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Effective date of registration: 20161227 Address after: 225400 Jiangsu Province, Taixing City Industrial Park Xiangrong Road No. 18 Patentee after: JIANGSU QIANJING INFORMATION TECHNOLOGY CO., LTD. Address before: 210044 Nanjing City, Pukou Province, Nanjing Road, No. 219, No. six, No. Patentee before: Nanjing IT Engineering Univ. |
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Effective date of registration: 20180117 Address after: 210044 Nanjing Ning Road, Jiangsu, No. six, No. 219 Patentee after: Nanjing University of Information Science and Technology Address before: 225400 Jiangsu Province, Taixing City Industrial Park Xiangrong Road No. 18 Patentee before: JIANGSU QIANJING INFORMATION TECHNOLOGY CO., LTD. |
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