CN102910911A - Test rod and preparation method thereof - Google Patents
Test rod and preparation method thereof Download PDFInfo
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- CN102910911A CN102910911A CN2012103523914A CN201210352391A CN102910911A CN 102910911 A CN102910911 A CN 102910911A CN 2012103523914 A CN2012103523914 A CN 2012103523914A CN 201210352391 A CN201210352391 A CN 201210352391A CN 102910911 A CN102910911 A CN 102910911A
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Abstract
The invention discloses a test rod for measuring melting and growing rate of silicon crystal, which is characterized by comprising the components by mass: 0-100% of silicon nitride with purity of 90-99.95%, 0-100% of silicon carbide with purity of 90-99.95%, 0-25% of silicon powder with purity of 90-99.9999999% and 0-8% of sintering aid. The invention also discloses a preparation method of the test rod. By adopting the test rod disclosed by the invention, the shortcomings in the prior art that the quartz rod is easy to deform, easy to adhere with silicone fluid and easy to be corroded by the silicone fluid are overcome, the corrosion resistance and measuring accuracy are improved, the service life of the test rod is prolonged, and the probability of great economic loss caused by the influence on the quality of the silicon crystal due to rupture of the test rod is reduced.
Description
Technical field
The present invention relates to the fields of measurement of the fusing of silicon material or silicon crystal growth, relate in particular to a kind of test rod and preparation method thereof.
Background technology
Silicon crystal material is widely used in photovoltaic solar, liquid-crystal display and semiconductor applications.The polycrystalline silicon ingot casting technology that adopt are come growing silicon crystal more at present, in this process of growth, need regularly monitor the brilliant speed of length of polysilicon.Simultaneously, adopt in the process of directional solidification method growing silicon single crystal, need the melting rate of strict control silicon material, thereby also need measure the melting rate of silicon material.
One of technology is at present, quartz pushrod is inserted in the container of built-in silicon liquid, contacts with solid-liquid interface, records the height of this moment test rod.After the unit time, again measure, and record this constantly height of test rod.Obtain growth velocity or the melting rate of silicon material in the unit time by calculating the two difference of altitude.In addition, this technology also is applicable to judge whether fine melt of silicon material, the situation such as melted silicon liquid level behind the fine melt.But, adopt quartz pushrod test silicon liquid height, have a plurality of shortcomings: the first, quartz pushrod is flexible or tensile deformation at high temperature, affects measuring accuracy.Polycrystalline silicon ingot or purifying furnace operation top temperature is 1560 ℃ ± 15 ℃, and the phenomenons such as distortion very easily appear in quartz pushrod in this temperature range, cause measuring error large, affect data gathering.In addition, lay in the method for seeded growth silicon ingot the bottom, and the distortion of quartz pushrod can cause the fusing thickness measuring out of true of seed crystal, affects the silicon crystal quality.The second, work-ing life is short, is disposable use substantially.If quartz pushrod uses repeatedly by force, easily cause the quartz pushrod fracture, and then cause silicon ingot to be bonded on the container even cracking, lose thereby cause than large economy.The 3rd, quartz pushrod and melted silicon wetting property are strong, cause silicon liquid easily to stick on the quartz pushrod, affect measuring accuracy.
Two of technology are at present, adopt infrared range-measurement system to obtain solid-liquid interface.Light source emission infrared light, infrared light is met the object back reflection, is received by the receiver, and calculates distance with this, obtains the solid-liquid interface particular location.Shortcoming is that equipment cost is high, and testing precision is poor, and several millimeters error is generally arranged.
Summary of the invention
Technical problem to be solved by this invention is, provides not yielding under a kind of high temperature, and the life-span is long, infiltrates weak test rod with silicon liquid, can measure easily, over and over again the situation of the fusing of silicon material and silicon crystal growth.
In order to solve the problems of the technologies described above, the invention provides a kind of test rod, each component of described test rod and mass percent are: silicon nitride 0% ~ 100%, silicon carbide 0% ~ 100%, silica flour 0% ~ 25%, sintering aid 0% ~ 8%, the purity of described silicon nitride is 90% ~ 99.95%, the purity of described silicon carbide is 90% ~ 99.95%, and the purity of described silica flour is 90% ~ 99.9999999%.
The main ingredient of described test rod is: silicon nitride and/or silicon carbide.
When described test rod main ingredient was silicon nitride, each component of described test rod and mass percent were: silicon nitride 85% ~ 99%, silica flour 0% ~ 10%, sintering aid 1% ~ 5%.
When described test rod main ingredient was silicon carbide, each component of described test rod and mass percent were: silicon carbide 80% ~ 99%, silica flour 0% ~ 12%, sintering aid 1% ~ 8%.
When described test rod main ingredient was silicon nitride and silicon carbide, each component of described test rod and mass percent were: silicon nitride 1% ~ 20%, silicon carbide 50% ~ 90%, silica flour 0% ~ 25%, sintering aid 1% ~ 8%.
Wherein, the cross section circumscribed circle diameter of described test rod is 5 ~ 30mm, and length is 300 ~ 2400mm.
Wherein, described sintering aid comprises one or more in yttrium oxide, magnesium oxide, Cs2O, silicon-dioxide, aluminium sesquioxide or the carbon dust.Described sintering aid is present in the finished product for reducing fusing point and bonded particulate.
Wherein, the particle diameter of described silicon nitride is 0.1 ~ 10 μ m, and the particle diameter of described silicon carbide is 0.1 ~ 10 μ m, and the particle diameter of described silica flour is 0.01 ~ 20 μ m.
Accordingly, the invention discloses a kind of preparation method of above-mentioned test rod:
Take by weighing each component raw material of test rod, mixing granulation, compression molding is packed base substrate in the protective gas atmosphere sintering furnace into, and normal pressure-sintered under 1300～2200 ℃ of temperature, high-temperature holding time 0.5～15h prepares described test rod.
Wherein, described raw material also comprises binding agent, and described binding agent comprises a kind of of polyvinyl alcohol, tetrafluoroethylene or Xylo-Mucine.Described binding agent increases the flowability of powder and the compactness of product in pressing process, there are not or seldom exist this component in pyrolytic decomposition, volatilization in the sintering process of finished product in the product.
Wherein, described granulation particle diameter is 16 ~ 160 mesh sieves, and described forming method is included in compression moulding under 25 ~ 500MPa pressure.
Adopt test rod of the present invention, it is yielding to have overcome the prior art quartz pushrod, easily and the shortcoming of silicon liquid adhesion, improved measuring accuracy, prolonged the work-ing life of test rod, reduced test rod and caused the unusual probability of silicon crystal production because of fracture, thereby reduced financial loss.
Embodiment
Embodiment 1
A kind of preparation method of test rod:
Get purity and be 99.95% silicon nitride, purity is that 99% yttrium oxide and purity are 99% polyvinyl alcohol, respectively by mass percentage example 95%, 4.5% and each component of 0.5% weighing.Wherein, the particle diameter of silicon nitride is 0.1 ~ 10 μ m.
With the above-mentioned raw materials mixing granulation, granulation is controlled between 16 ~ 160 mesh sieves, after the preforming tool of packing into.Under 25MPa pressure, carry out premolding, the isostatic pressing mold of then work in-process being packed into, isostatic pressing under 200MPa pressure carries out surperficial repaired biscuit after the demoulding, and base substrate is trimmed to right cylinder.Base substrate is packed in the atmosphere sintering furnace, and the nitrogen atmosphere protection is lower normal pressure-sintered, and sintering temperature is 1750 ℃, and soaking time is 2h.Gained finished product test rod diameter 9mm after the sharp processing, length 400mm, density 3.3g/cm
3
Embodiment 2
A kind of preparation method of test rod:
Get purity and be 99.7% silicon carbide, purity is 99% aluminium sesquioxide, and purity is that 99% yttrium oxide and purity are 99% tetrafluoroethylene, respectively by mass percentage example 98%, 1%, 0.5% and 0.5% each component of weighing.Wherein, the carborundum powder particle diameter is 0.1 ~ 10 μ m.
With the above-mentioned raw materials mixing granulation; granulation is controlled between 16 ~ 160 mesh sieves; the isostatic pressing mold of packing into; isostatic pressing under 220MPa pressure carries out surperficial repaired biscuit after the demoulding, base substrate is trimmed to right cylinder; base substrate is packed in the atmosphere sintering furnace; the argon atmospher protection is lower normal pressure-sintered, and sintering temperature is 2000 ℃, and soaking time is 30min.Gained finished product test rod diameter 9mm after the sharp processing, length 500mm, density 3.1g/cm
3
Embodiment 3
A kind of preparation method of test rod:
Get purity and be 99.7% silicon carbide, purity is 99.95% silicon nitride, and purity is that 99,995% silica flour and purity are 99% Xylo-Mucine, respectively example 55%, 19%, 25% by mass percentage, and each component of 1% weighing.Wherein, the particle diameter of carborundum powder is 0.1 ~ 10 μ m, and the particle diameter of silica flour is 0.01 ~ 20 μ m.
With above-mentioned batching mixing granulation, granulation is controlled between 16 ~ 160 mesh sieves, after the preforming tool of packing into.Carry out premolding under 25MPa pressure, carry out isostatic pressing under 240MPa pressure, carry out surperficial repaired biscuit after the demoulding, base substrate is trimmed to right cylinder.Base substrate is packed in the atmosphere sintering furnace, and the nitrogen atmosphere protection is lower normal pressure-sintered, and sintering temperature is 1450 ℃, and soaking time is 15h.Gained finished product test rod diameter 9mm after the sharp processing, length 2100mm, density 2.7g/cm
3
Effect embodiment
For verification test rod performance, get embodiment 1 prepared test rod and be installed in the polycrystalline silicon ingot casting furnace apparatus.Fully during melting, whole test rod does not contact with the silicon material silicon material.Treat the complete melting of silicon material, test rod inserted silicon liquid certain depth, keep 1min, after it improved break away from silicon liquid certain altitude.Keep at high temperature about 30h of test rod, go out ingot after, the taking-up test rod.
Carry out the test rod after primary effect embodiment tests, compare with quartz pushrod, concrete advantage is as follows:
Test rod is without the obviously distortion of bending or stretching, and high thermal resistance is better;
Test rod noresidue silicon liquid sign proves the not wetting property of itself and silicon liquid;
Carry out repeatedly the test rod after effect embodiment tests, compare with quartz pushrod, concrete advantage is as follows:
Adopt quartz pushrod to carry out above-mentioned effect embodiment and test reduced 4.4% behind ingot casting 5 stoves, test behind ingot casting 5 stoves in the reduced 0.1% and adopt the nitrogenize silicon rod to carry out above-mentioned effect embodiment;
Be test 30 times, ingot casting 7 stoves the work-ing life of quartz pushrod.And the work-ing life of nitrogenize silicon rod is for testing ingot casting 200 stoves 900 times.
To sum up, the test rod high thermal resistance of the embodiment of the invention is strong, and a little less than infiltrating with silicon liquid, anti-silicon corrosion is strong.Simultaneously, it is yielding also to have overcome the prior art quartz pushrod, easily with the shortcoming of silicon liquid adhesion, has improved measuring accuracy, has prolonged the work-ing life of test rod, has reduced test rod and has ruptured and cause the unusual probability of silicon crystal production, thereby reduced financial loss.
Claims (10)
1. test rod, the fields of measurement that is used for the fusing of silicon material or silicon crystal growth, it is characterized in that, each component of described test rod and mass percent are: silicon nitride 0% ~ 100%, silicon carbide 0% ~ 100%, silica flour 0% ~ 25%, sintering aid 0% ~ 8%, the purity of described silicon nitride is 90% ~ 99.95%, and the purity of described silicon carbide is 90% ~ 99.95%, and the purity of described silica flour is 90% ~ 99.9999999%.
2. a kind of test rod as claimed in claim 1 is characterized in that, each component of described test rod and mass percent are: silicon nitride 85% ~ 99%, silica flour 0% ~ 10%, sintering aid 1% ~ 5%.
3. a kind of test rod as claimed in claim 1 is characterized in that, each component of described test rod and mass percent are: silicon carbide 80% ~ 99%, silica flour 0% ~ 12%, sintering aid 1% ~ 8%.
4. a kind of test rod as claimed in claim 1 is characterized in that, each component of described test rod and mass percent are: silicon nitride 1% ~ 20%, silicon carbide 50% ~ 90%, silica flour 0% ~ 25%, sintering aid 1% ~ 8%.
5. a kind of test rod as claimed in claim 1 is characterized in that, the cross section circumscribed circle diameter of described test rod is 5 ~ 30mm, and length is 300 ~ 2400mm.
6. a kind of test rod as claimed in claim 1 is characterized in that, described sintering aid comprises one or more in yttrium oxide, magnesium oxide, Cs2O, silicon-dioxide, aluminium sesquioxide or the carbon dust.
7. a kind of test rod as claimed in claim 1 is characterized in that, the particle diameter of described silicon nitride is 0.1 ~ 10 μ m, and the particle diameter of described silicon carbide is 0.1 ~ 10 μ m, and the particle diameter of described silica flour is 0.01 ~ 20 μ m.
8. preparation method such as each described test rod of claim 1～7; it is characterized in that; take by weighing each component raw material of test rod; mixing granulation, compression molding is packed base substrate in the protective gas atmosphere sintering furnace into; under 1300～2200 ℃ of temperature; normal pressure-sintered, high-temperature holding time 0.5～15h prepares described test rod.
9. a kind of preparation method as claimed in claim 8 is characterized in that, described raw material also comprises binding agent, and described binding agent comprises a kind of of polyvinyl alcohol, tetrafluoroethylene or Xylo-Mucine.
10. a kind of preparation method as claimed in claim 8 is characterized in that, described granulation particle diameter is 16 ~ 160 mesh sieves, and described forming method is included in compression moulding under 25 ~ 500MPa pressure.
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| CN2012103523914A CN102910911A (en) | 2012-09-20 | 2012-09-20 | Test rod and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012103523914A CN102910911A (en) | 2012-09-20 | 2012-09-20 | Test rod and preparation method thereof |
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| CN102910911A true CN102910911A (en) | 2013-02-06 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107399978A (en) * | 2017-08-02 | 2017-11-28 | 嵊州市万智网络科技有限公司 | A kind of acid/alkali-corrosion-resistant building block and preparation method thereof |
| CN115417674A (en) * | 2022-10-14 | 2022-12-02 | 郴州市拓道新材料科技有限公司 | Wear-resistant silicon nitride/silicon carbide composite ceramic and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201395646Y (en) * | 2009-03-11 | 2010-02-03 | 周宇 | Silicon nitride ceramic integral crucible |
| CN102408242A (en) * | 2011-08-19 | 2012-04-11 | 武汉科技大学 | Composite ceramic cushion block for hot rolling walking beam reheating furnace and preparation method thereof |
-
2012
- 2012-09-20 CN CN2012103523914A patent/CN102910911A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201395646Y (en) * | 2009-03-11 | 2010-02-03 | 周宇 | Silicon nitride ceramic integral crucible |
| CN102408242A (en) * | 2011-08-19 | 2012-04-11 | 武汉科技大学 | Composite ceramic cushion block for hot rolling walking beam reheating furnace and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107399978A (en) * | 2017-08-02 | 2017-11-28 | 嵊州市万智网络科技有限公司 | A kind of acid/alkali-corrosion-resistant building block and preparation method thereof |
| CN115417674A (en) * | 2022-10-14 | 2022-12-02 | 郴州市拓道新材料科技有限公司 | Wear-resistant silicon nitride/silicon carbide composite ceramic and preparation method and application thereof |
| CN115417674B (en) * | 2022-10-14 | 2023-06-09 | 湖南省拓道新材料科技有限公司 | Wear-resistant silicon nitride/silicon carbide composite ceramic and preparation method and application thereof |
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Application publication date: 20130206 |