CN100590084C - Quartz rod production method - Google Patents
Quartz rod production method Download PDFInfo
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- CN100590084C CN100590084C CN200610144810A CN200610144810A CN100590084C CN 100590084 C CN100590084 C CN 100590084C CN 200610144810 A CN200610144810 A CN 200610144810A CN 200610144810 A CN200610144810 A CN 200610144810A CN 100590084 C CN100590084 C CN 100590084C
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- quartz
- silica tube
- heavy wall
- quartz pushrod
- wall silica
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B17/00—Forming molten glass by flowing-out, pushing-out, extruding or drawing downwardly or laterally from forming slits or by overflowing over lips
- C03B17/04—Forming tubes or rods by drawing from stationary or rotating tools or from forming nozzles
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/04—Re-forming tubes or rods
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- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
Abstract
There's provided a way to produce quartz sticks: smelting the quartz sand to prepare hollow quartz columns by plasms body flame; by mechanical cold work to prepare quartz ampoule with thick walls; producing the quartz sticks by intermediate frequency heating quadric-forming technology absence of contact. The quartz ampoule with thick walls is hanged in the intermediate frequency stove so as to cause underpressure in the quartz ampoule then the producers can melt and shrink the ampoule as well as producing the quartz sticks at the same time. The quartz sticks in the invention has high purity, low hydroxyl radical content, high measurement precision, high appearance quality without flaws which can be used in high technology domain.
Description
Technical field
The present invention relates to the production method of quartz ware, particularly a kind of production method of quartz pushrod.
Background technology
The prior art of producing quartz pushrod at present mainly contains two kinds: continuous smelting single stage method and oxyhydrogen flame two step method.Wherein, the characteristics of continuous smelting one-step technology are to utilize continuous induction melting furnace fusing of margin fossil English powder limit to draw quartz pushrod.As shown in Figure 1; at first with in the crucible of quartz sand in feed bin adds continuous induction melting furnace; in stove, feed shielding gas; heating then; 1900 ℃-2000 ℃ of Heating temperatures, be heated to the quartz sand molten state after, begin to draw material by fire door; draw quartz pushrod, draw in the process of quartz pushrod pull-rod limit, limit and in continuous induction melting furnace, add quartz sand and continuously draw quartz pushrod.The shortcoming of this method is: 1. owing to do well heater and crucible with tungsten order material, silica glass is had pollution, cause the purity of quartz pushrod low; 2. prevent the tungsten and molybdenum material oxidation with hydrogen shield, so quartz pushrod contains great amount of hydroxy group, hydroxy radical content is about 150ppm, does not accomplish low hydroxyl, causes the heat resistance of quartz pushrod poor; 3. because space between the raw material and the bubble inclusion in the raw material can't in time be got rid of, cause outward appearance bubble, the colo(u)r streak of quartz pushrod many.The quartz pushrod that this method is produced is subjected to certain restriction in application facet.
Formerly the oxyhydrogen flame two step method of technology is produced quartz pushrod, the first step: do thermal source with vertical lump maker with oxyhydrogen flame, 1850 ℃ of temperature---1950 ℃ quartz sand being founded becomes quartz wool and sticks together, as shown in Figure 2, quartz sand enters duration and degree of heating from tremie pipe, founds into quartz wool through oxyhydrogen flame and sticks together; Second step: will stick together only through the quartz of mechanical workout and draw material, the quartz pushrod of drawing all size, 1900 ℃ of-2000 ℃ of (see figure 3)s of Heating temperature after being heated to the softening temperature of silica glass by resistance furnace.Quartz wool sticks together and to stick together only all be solid in this method.The shortcoming of this method is: 1. make thermal source quartz pushrod hydroxy radical content height with oxyhydrogen flame, greater than about 200ppm, the quartz pushrod heat resistance that hydroxy radical content is high is poor; 2. because resistance furnace graphite crucible sticks together only with quartz and directly contacts, the quartz pushrod surface quality is had pollution, macroscopic irregularitys such as bubble, gas line, ditch rib are arranged, the quartz pushrod that makes this method produce is restricted in application facet equally.
Summary of the invention:
The objective of the invention is to invent a kind of method, with preparation purity height, hydroxy radical content is low, dimensional precision is high, visual appearance does not have fault well quartz pushrod.The method that the present invention produces quartz pushrod comprises the steps:
1. using plasma flame heating, quartz sand founded to be become hollow quartz wool and sticks together;
2. hollow quartz wool is sticked together and be cold worked into quartz by machinery and stick together only (also claiming the heavy wall silica tube);
3. adopt Frequency Induction Heating, contactless trombone slide mode that the heavy wall silica tube is drawn quartz pushrod.
The temperature of above-mentioned steps 1 ionic medium body flame is 2000～3000 ℃, preferred 2500 ℃, makes the quartz wool that makes not have bubble in sticking together as far as possible.Can adopt the horizontal lump maker of plasma to prepare quartz wool sticks together, as shown in Figure 4, utilize the higher frequency electromagnetic field to make working gas (pressurized air, oxygen, nitrogen, argon gas etc.) ionization produce plasma flame, quartz sand sticks together being injected in the quartz wool of making hollow on the basic pipe under the heating of plasma flame by tremie pipe simultaneously.The present invention of this technology is referred to as plasma body solid phase external sediment technology.
Above-mentioned steps 2 sticks together quartz wool to become inside and outside highly polished quartz to stick together only by cold worked methods such as mechanical grinding, boring, honing, cylindrical processing.
Above-mentioned steps 3 specifically can comprise the following steps:
3-1. in the intermediate frequency furnace burner hearth, port feeds nitrogen or rare gas element from it with heavy wall silica tube vertical lifting;
Begin fusion 3-2. be warming up to heavy wall silica tube lower port, treat after the closure of lower end nitrogen or rare gas element to be switched in the outer burner hearth of access tube;
3-3. take out from heavy wall silica tube upper port and to manage interior gas, make the air pressure in the heavy wall silica tube be lower than the outer air pressure of pipe;
3-4. the heavy wall silica tube of lower end contraction on melting is drawn into quartz pushrod.
Wherein, usually in step 3-2 earlier with heavy wall silica tube pre-heating temperature elevation to 1100 ℃-1500 ℃, keep behind the 40-60min again secondary temperature elevation to 1780 ℃-2000 ℃ to make heavy wall silica tube lower end begin fusion, treat after the closure of lower end nitrogen or rare gas element to be switched in the outer burner hearth of access tube.The purpose of preheating is to prevent that silica tube from owing to violent the intensification bursts, just reaching its fused temperature behind the secondary temperature elevation.Treat that taper that heavy wall silica tube lower end is melt into draws partly profile symmetrically time of material, take out from heavy wall silica tube upper port and manage interior gas, make in the heavy wall silica tube centre hole and form negative pressure.Rare gas element described in the step 3-1 is commonly used argon gas; In the process of step 3-4 drawing silica tube, can be furnished with the non-contact type laser measuring apparatus, quartz pushrod is carried out diameter measurement, adjust pulling rate by the closed-loop control of on-line measurement simultaneously, to guarantee the precision of quartz pushrod size.
The general contactless tubing machine of intermediate frequency furnace that adopts of step 3 in actually operating; with heavy wall silica tube vertical lifting in burner hearth; the upper port of heavy wall silica tube and exhaust system and nitrogen or protection of inert gas system link; when in the heavy wall silica tube, feeding nitrogen or rare gas element at the beginning; because the lower end of silica tube is open; nitrogen or indifferent gas cognition are full of whole intermediate frequency furnace burner hearth; heavy wall silica tube centre hole is the same with the outer air pressure of pipe; treat that heavy wall silica tube lower end begins fusion; variation in diameter and when being taper and flowing out fire door vertically downward; the lower end of heavy wall silica tube has just been sealed; at this moment switch nitrogen or rare gas element; in the outer burner hearth of it access tube; when drawing of taper expects that partly its profile symmetrically; open the exhaust system of heavy wall silica tube upper port; air pressure in the heavy wall silica tube is lower than the outer air pressure of pipe like this, makes the silica tube contraction on melting to be drawn into quartz pushrod.
The present invention adopts the post forming technology to prepare quartz pushrod, and the quartz pushrod purity height of being produced, hydroxy radical content is low, dimensional precision is high, visual appearance does not have fault well, is particularly suitable for making the quartz pushrod of diameter more than 5 millimeters, below 50 millimeters.Particularly, the present invention's method of producing quartz pushrod has following advantage:
1,2000～3000 ℃ plasma flame heating, abundant melt raw material makes the quartz wool that makes not have bubble substantially in sticking together;
2, with purified plasma body as thermal source, do not have the introducing of introduced contaminants, the silica glass of founding has the high characteristics of purity;
3, the working gas that produces plasma body during once shaped is generally exsiccant pressurized air, oxygen, nitrogen or argon gas, the silica glass of founding has the characteristics of low hydroxyl, adopt the heating in medium frequency mode during post forming, no hydrogen-oxygen source, thereby make the hydroxy radical content of the quartz glass bar that finally makes low, only about 20ppm, heat resistance is good;
4, intermediate frequency furnace well heater and quartz are contactless between sticking together only, and heating member graphite can not pollute silica glass, and pure introducing makes quartz pushrod purity height, and surface quality is good, does not have fault substantially;
5, the present invention prepares quartz pushrod by post forming, promptly silica glass has been carried out the secondary high temperature melting, makes the silica glass refining quality good, so the quartz pushrod visual appearance is good, and defectives such as no bubble, gas line.
6, on-line measurement control techniques makes the quartz pushrod dimensional precision very high.
Quartz pushrod of the present invention can satisfy the making requirement of semi-conductor industry with the large-sized rock quartz boat, and this quartz boat is used for High temperature diffusion and oxidation.Quartz pushrod of the present invention also can be applicable to other high-tech sector.
Description of drawings
Fig. 1 is the synoptic diagram that continuous induction melting furnace prepares quartz pushrod;
Fig. 2 is the synoptic diagram that the vertical preparation quartz wool of oxyhydrogen flame sticks together;
Fig. 3 is the synoptic diagram for preparing quartz pushrod with resistance furnace;
Fig. 4 prepares the synoptic diagram that quartz wool sticks together with the horizontal lump maker of plasma;
Fig. 5 is the synoptic diagram that the contactless trombone slide mode of intermediate frequency furnace prepares quartz pushrod.
Wherein:
1---continuous induction melting furnace electrode 2---crucible 3---quartz sand 4---lagging material
5---continuous induction melting furnace well heater 6---fire door 7---quartz pushrod 8---tremie pipes
9---duration and degree of heating 10---oxyhydrogen flame 11---the stuffed quartz hair sticks together 12---resistance furnace electrodes
13---stuffed quartz sticks together 14 only---graphite pot 15---resistance furnace well heater 16---quartz pushrods
17---tremie pipe 18---flame passes 19---hollow quartz wool sticks together 20---basis pipes
21---heavy wall silica tube 22---intermediate frequency furnace 23---laser diameter measuring instrument 24---quartz pushrods
Embodiment:
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in more detail.
The present invention uses the post forming technology and produces quartz pushrod.The first step: adopt the horizontal lump maker of plasma to prepare quartz wool and stick together, as shown in Figure 4, be under 2000～3000 ℃ plasma flame 18 heating in temperature, the quartz sand fusing of getting off by tremie pipe 17 also is injected in the quartz wool of making hollow on the basis pipe 20 and sticks together 19; Second step: as shown in Figure 5; 21 (also claiming the heavy wall silica tube) vertical lifting will stick together through the quartz of mechanical workout only in the burner hearth of intermediate frequency furnace 22; its upper port and an exhaust system and a nitrogen protecting system link; feed nitrogen from heavy wall silica tube 21 upper port that lift; beginning is warming up to 1100 ℃ of-1500 ℃ of preheatings one hour for the first time; begin secondary temperature elevation then; 1780 ℃-2000 ℃ of temperature; intensification rises to heavy wall silica tube 21 lower port and begins fusion; diameter diminishes and is taper and flows out fire door vertically downward, and switch to nitrogen and feed in the burner hearth this moment.When drawing of taper expects that partly its profile is symmetrically, open the exhaust system of heavy wall silica tube upper port, make heavy wall silica tube centre hole form negative pressure, heavy wall silica tube 21 limits of the following contraction on melting formation of condition of high temperature negative pressure draw and produce quartz pushrod 24.Laser diameter measuring instrument 23 carries out diameter measurement in contactless mode to quartz pushrod, simultaneously by the closed-loop control of on-line measurement, guarantees the precision of quartz pushrod size.The quartz pushrod quality index contrast that method of the present invention and existing continuous smelting single stage method and oxyhydrogen flame two step method are produced is as shown in the table:
The quartz pushrod quality index contrast that table 1. the inventive method and prior art are produced
| The continuous smelting single stage method | The oxyhydrogen flame two step method | The present invention | |
| Foreign matter content (ppm) | 50 | 50 | 25 |
| Hydroxy radical content (ppm) | 150 | 240 | ≤ 20 |
| External diameter tolerance (mm) (external diameter scope 12mm-20mm) | ± 0.3 | ± 0.5 | ± 0.2 |
| Visual appearance | Defectives such as bubble, colo(u)r streak are arranged. | Defectives such as bubble, gas line, ditch rib are arranged. | Bubble, gas line are few. |
Although disclose embodiments of the invention and accompanying drawing for the purpose of illustration, but it will be appreciated by those skilled in the art that: without departing from the spirit and scope of the invention and the appended claims, various replacements, variation and modification all are possible, therefore, scope of the present invention is not limited to embodiment and the disclosed content of accompanying drawing.
Claims (8)
1. the production method of a quartz pushrod comprises the steps:
(1) using plasma flame heating, quartz sand founded to be become hollow quartz wool and sticks together;
(2) hollow quartz wool is sticked together be cold worked into the heavy wall silica tube by machinery;
(3) adopt Frequency Induction Heating, contactless trombone slide mode that the heavy wall silica tube is drawn into quartz pushrod, concrete steps are:
3-1. in the intermediate frequency furnace burner hearth, port feeds nitrogen or rare gas element from it with heavy wall silica tube vertical lifting;
3-2. earlier with heavy wall silica tube pre-heating temperature elevation to 1100 ℃-1500 ℃, keep behind the 40-60min again secondary temperature elevation to 1780 ℃-2000 ℃ to make heavy wall silica tube lower end begin fusion, treat after the closure of lower end nitrogen or rare gas element to be switched in the outer burner hearth of access tube;
3-3. take out from heavy wall silica tube upper port and to manage interior gas, make the air pressure in the heavy wall silica tube be lower than the outer air pressure of pipe;
3-4. the heavy wall silica tube of lower end contraction on melting is drawn into quartz pushrod.
2. the production method of quartz pushrod as claimed in claim 1 is characterized in that, the temperature of described step (1) ionic medium body flame is 2000～3000 ℃.
3. the production method of quartz pushrod as claimed in claim 2 is characterized in that, the temperature of described plasma flame is 2500 ℃.
4. as the method for claim 1 or 2 or 3 described production quartz pushrods, it is characterized in that, described step (1) adopts the horizontal lump maker of plasma to prepare quartz wool and sticks together, utilize the higher frequency electromagnetic field to make working gas ionization produce plasma flame, quartz sand sticks together being injected in the quartz wool of making hollow on the basic pipe under the heating of plasma flame simultaneously.
5. the production method of quartz pushrod as claimed in claim 4 is characterized in that, described working gas is pressurized air, oxygen, nitrogen or argon gas.
6. the production method of quartz pushrod as claimed in claim 1 is characterized in that, the rare gas element described in the step 3-1 is an argon gas.
7. the production method of quartz pushrod as claimed in claim 1 is characterized in that, treats among the described step 3-3 that taper that heavy wall silica tube lower end is melt into draws partly profile symmetrically time of material, begins to take out from heavy wall silica tube upper port to manage interior gas.
8. the production method of quartz pushrod as claimed in claim 1 is characterized in that, utilizes the non-contact type laser measuring apparatus that quartz pushrod is carried out diameter measurement in the process of step 3-4 drawing quartz pushrod, adjusts pulling rate by the closed-loop control of on-line measurement simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610144810A CN100590084C (en) | 2006-11-21 | 2006-11-21 | Quartz rod production method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610144810A CN100590084C (en) | 2006-11-21 | 2006-11-21 | Quartz rod production method |
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| CN1966437A CN1966437A (en) | 2007-05-23 |
| CN100590084C true CN100590084C (en) | 2010-02-17 |
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| CN200610144810A Active CN100590084C (en) | 2006-11-21 | 2006-11-21 | Quartz rod production method |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103121788A (en) * | 2011-11-21 | 2013-05-29 | 袁晶 | Joint-melting quartz block hitting furnace |
| CN108218195B (en) * | 2018-03-27 | 2023-04-25 | 中建材衢州金格兰石英有限公司 | Diameter reducing device and diameter reducing method for quartz glass rod |
| CN114406218B (en) * | 2022-01-23 | 2023-10-03 | 宁波磁性材料应用技术创新中心有限公司 | Quartz nozzle and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3227785A1 (en) * | 1982-07-24 | 1984-01-26 | Heraeus Quarzschmelze Gmbh, 6450 Hanau | Process for the production of a quartz glass rod or bar |
| US5180410A (en) * | 1990-07-30 | 1993-01-19 | Corning Incorporated | Method of making polarization retaining fiber |
| EP0905098A1 (en) * | 1997-09-29 | 1999-03-31 | Lucent Technologies Inc. | Method for thermal treatment of a refractory dielectric body, such as glass, using plasma |
| CN1354730A (en) * | 1999-06-08 | 2002-06-19 | 阿尔卡诺尔公司 | Process and apparatus for producing optical fiber preform by plasma deposition |
| CN1356278A (en) * | 2000-11-08 | 2002-07-03 | 赫罗伊斯石英玻璃股份有限两合公司 | Process for preparing SiO2 blank and apparatus for implementing said process |
| CN1364147A (en) * | 2000-03-14 | 2002-08-14 | 赫罗伊斯石英玻璃股份有限两合公司 | Method for producing quartz glass body |
| CN1718553A (en) * | 2004-07-07 | 2006-01-11 | 纪高仁 | Production method of quartz stick |
-
2006
- 2006-11-21 CN CN200610144810A patent/CN100590084C/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3227785A1 (en) * | 1982-07-24 | 1984-01-26 | Heraeus Quarzschmelze Gmbh, 6450 Hanau | Process for the production of a quartz glass rod or bar |
| US5180410A (en) * | 1990-07-30 | 1993-01-19 | Corning Incorporated | Method of making polarization retaining fiber |
| EP0905098A1 (en) * | 1997-09-29 | 1999-03-31 | Lucent Technologies Inc. | Method for thermal treatment of a refractory dielectric body, such as glass, using plasma |
| CN1354730A (en) * | 1999-06-08 | 2002-06-19 | 阿尔卡诺尔公司 | Process and apparatus for producing optical fiber preform by plasma deposition |
| CN1364147A (en) * | 2000-03-14 | 2002-08-14 | 赫罗伊斯石英玻璃股份有限两合公司 | Method for producing quartz glass body |
| CN1356278A (en) * | 2000-11-08 | 2002-07-03 | 赫罗伊斯石英玻璃股份有限两合公司 | Process for preparing SiO2 blank and apparatus for implementing said process |
| CN1718553A (en) * | 2004-07-07 | 2006-01-11 | 纪高仁 | Production method of quartz stick |
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| CN1966437A (en) | 2007-05-23 |
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