CN102259100B - Method for cleaning electronic-grade polycrystalline silicon production device and process pipe - Google Patents
Method for cleaning electronic-grade polycrystalline silicon production device and process pipe Download PDFInfo
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- CN102259100B CN102259100B CN201110122833A CN201110122833A CN102259100B CN 102259100 B CN102259100 B CN 102259100B CN 201110122833 A CN201110122833 A CN 201110122833A CN 201110122833 A CN201110122833 A CN 201110122833A CN 102259100 B CN102259100 B CN 102259100B
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Abstract
The invention discloses a method for cleaning an electronic-grade polycrystalline silicon production device and process pipe, comprising the steps of: 1, decreasing and cleaning; 2, water washing; 3, complexation rust cleaning: carrying out rust cleaning by utilizing a complexation cleaning agent; 4, rinsing; 5, ammonia water washing: washing at a temperature of 55-60 DEG C by utilizing an ammonia solution; 6, passivation: carrying out the passivation at a temperature of 80-90DEG C by utilizing a hydrogen peroxide solution; 7, ultrapure water washing: washing by utilizing ultrapure water withresistivity not more than 12megohm.cm; 8, drying treatment: drying by utilizing compressed-air drying equipment; and 9, encapsulating. The cleaning method disclosed by the invention has the advantages of reasonable design, simple steps, simpleness and convenience for operation and realization, good cleaning effect and no over etching and hydrogen embrittlement forming and can solve the problems of the over etching, easiness in having residual Na and P ions on the surface of a passivation film and the like in a conventional cleaning method.
Description
Technical field
The invention belongs to industrial equipment and pipeline cleaning technique field, especially relate to the cleaning method of a kind of electronic-grade polycrystalline silicon production equipment and process pipe.
Background technology
Along with the progress of society, human increasingly high to the attention rate of the energy, as the foundation stone material of new forms of energy, the demand of the polysilicon particularly demand of electronic-grade polycrystalline silicon also increases day by day.Polysilicon is a primary raw material of making silicon polished, solar cell and HIGH-PURITY SILICON goods, is information industry and the most basic raw material of new forms of energy industry.Being merely limited in the world several developed countries as the production technology of the highest electronic-grade polycrystalline silicon of polysilicon product moderate purity (purity is 11 9, and promptly its purity is 99.999999999%) is grasped.The manufacturing technique requirent raw material of electronic-grade polycrystalline silicon will move under the environment of " not having oily, anhydrous, dustless ".At present, domestic still do not have professional, targetedly standard, standard can be for reference.
At present, pickling, passivation mode are adopted in the cleaning of domestic industry equipment and pipeline mostly, and medicament is selected inorganic acid for use, and through inorganic acid with the oxide reaction that is cleaned the metal surface and generate water-soluble salt; Utilize NaOH, Na again
3PO
3Deng basic salt be cleaned metal reaction, to produce fine and close passivation layer in the metal surface.The characteristics of above-mentioned conventional cleaning method are that reaction speed is fast, condition is simple, but existing shortcoming is to cause excessive erosion easily, make the effective thickness attenuate of mother metal, and the passivating film surface is prone to residual Na ion, P ion etc. simultaneously.
Summary of the invention
Technical problem to be solved by this invention is to above-mentioned deficiency of the prior art; The cleaning method of a kind of electronic-grade polycrystalline silicon production equipment and process pipe is provided; It is reasonable in design, the cleaning method step is simple, easy and simple to handle and it is convenient to realize, cleaning performance is good; Can not form excessive erosion and hydrogen embrittlement, can effectively solve being prone to that existing cleaning method exists and cause excessive erosion, passivating film surface to be prone to problems such as residual Na ion, P ion.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: the cleaning method of a kind of electronic-grade polycrystalline silicon production equipment and process pipe is characterized in that this method may further comprise the steps:
Step 1, cleaning by degreasing: the conventional cleaning by degreasing method that adopts the degreasing metal cleaning agent and press metal equipment and metallic conduit, carry out cleaning by degreasing to being cleaned metal objects; The said metal objects that is cleaned is production of polysilicon equipment or polysilicon process pipeline;
Water flushing after step 2, the degreasing: adopt running water to wash to being cleaned metal objects;
Step 3, complexing rust cleaning: adopt the complexing cleaning agent to being cleaned the metal objects cleaning that eliminates rust;
Step 4, rinsing: adopt purificant to carry out rinsing to being cleaned metal objects;
Step 5, ammonia plug flushing: adopt ammonia spirit and under 55 ℃～60 ℃ temperature conditions, wash to being cleaned metal objects;
Step 6, Passivation Treatment: adopt hydrogen peroxide solution and under 80 ℃～90 ℃ temperature conditions, carry out Passivation Treatment to being cleaned metal objects;
Step 7, ultra-pure water flushing: be not more than the ultra-pure water of 12M Ω cm with resistivity, wash to being cleaned metal objects;
Step 8, dried: adopt compressed air drying equipment and, carry out dried to being cleaned metal objects by conventional compressed air drying processing method;
Step 9, seal: the metal objects that is cleaned to after dried and quality examination are qualified, seal protection.
The cleaning method of above-mentioned a kind of electronic-grade polycrystalline silicon production equipment and process pipe is characterized in that: described in the step 1 when being cleaned metal objects and carrying out cleaning by degreasing, its cleaning by degreasing process is following:
101, thick cleaning by degreasing: under the normal temperature state, adopt the trichloro-ethylene cleaning agent to clean, and scavenging period is 2 hours～3 hours to being cleaned metal objects;
102, heated-air drying: after thick cleaning by degreasing finishes, adopt hot-air seasoning equipment, will be cleaned metal objects and dry up;
103, smart cleaning by degreasing: adopt AEO solution and under 40 ℃～50 ℃ temperature conditions, the metal objects that is cleaned after cleaning by degreasing is slightly cleaned, scavenging period is 3 hours～5 hours.
The cleaning method of above-mentioned a kind of electronic-grade polycrystalline silicon production equipment and process pipe is characterized in that: the temperature of the hot blast that equipment provides of hot-air seasoning described in the step 102 is 40 ℃～50 ℃; After will be cleaned metal objects and dry up described in the step 102, also need adopt oil suction filter paper whether to exist greasy dirt to detect: when detection draws the inner surface that is cleaned metal objects and do not have greasy dirt, then to get into step 103 to being cleaned the metal objects inner surface; Otherwise, change step 101 over to, repeat thick cleaning by degreasing to being cleaned metal objects.
The cleaning method of above-mentioned a kind of electronic-grade polycrystalline silicon production equipment and process pipe; It is characterized in that: the metal objects that is cleaned to after thick cleaning by degreasing described in the step 103 carries out in the cleaning process, and the pH value of said AEO solution is controlled between 9～11.
The cleaning method of above-mentioned a kind of electronic-grade polycrystalline silicon production equipment and process pipe; It is characterized in that: when the employing running water described in the step 2 washes being cleaned metal objects; Carry out cleaning down with running water to being cleaned metal objects inside; And after flushing finishes, be cleaned the inner surface of metal objects with ultra violet lamp: when the inner surface that is cleaned metal objects presents purple light, then get into step 3; Otherwise, proceed flushing to being cleaned metal objects inside with running water.
The cleaning method of above-mentioned a kind of electronic-grade polycrystalline silicon production equipment and process pipe; It is characterized in that: the complexing cleaning agent described in the step 3 is a sodium ethylene diamine tetracetate solution; And the cleaning that under 40 ℃～50 ℃ temperature conditions, eliminates rust, the rust cleaning scavenging period is 8 hours～10 hours; In the rust cleaning cleaning process, the pH value that rust cleaning is cleaned with sodium ethylene diamine tetracetate solution is controlled between 1～4.
The cleaning method of above-mentioned a kind of electronic-grade polycrystalline silicon production equipment and process pipe is characterized in that: the purificant described in the step 4 is a citric acid solution, and under 70 ℃～75 ℃ temperature conditions, carries out rinsing, and the rinsing time is 3 hours～4 hours; In the rinse cycle, the pH value of rinsing with citric acid solution is controlled between 3.5～4.
The cleaning method of above-mentioned a kind of electronic-grade polycrystalline silicon production equipment and process pipe; It is characterized in that: carrying out in the flushing process described in the step 5 being cleaned metal objects; The pH value of flushing with ammonia spirit is controlled between 8～9, and washing time is 2 hours～3 hours.
The cleaning method of above-mentioned a kind of electronic-grade polycrystalline silicon production equipment and process pipe; It is characterized in that: carrying out in the Passivation Treatment process described in the step 6 being cleaned metal objects; The pH value of Passivation Treatment with hydrogen peroxide solution is controlled between 9～10, and the Passivation Treatment time is 6 hours～8 hours.
The cleaning method of above-mentioned a kind of electronic-grade polycrystalline silicon production equipment and process pipe; It is characterized in that: the compressed air drying equipment described in the step 8 is for providing the drying equipment of oil-free compressed air; And carry out before the dried being cleaned metal objects, need said oil-free compressed air is heated to 70 ℃～90 ℃.
The present invention compared with prior art has the following advantages:
1, simple, the easy and simple to handle and realization convenience of cleaning method step.
2, clean range is unrestricted; Can clean production of polysilicon equipment and supporting process pipe (comprising valve, flange, pipe fitting accessory etc.) thereof etc.; Simultaneously can remove the inner iron rust of production of polysilicon equipment and process pipe, greasy dirt etc., and clean back production of polysilicon equipment and the inner cleanliness factor of process pipe is high through Chemical cleaning.
3, whole cleaning process design, each cleaning step tight association and cleaning performance are good; Specifically be to adopt chemical cleaning method; Utilize organic compound under certain concentration and temperature with reactions such as the grease of metal surface, iron filings, oxide, chemical residue, generate the compound of solubility; After rinsing well, utilize hydrogen peroxide solution and metal reaction again, form the fine and close passivating film of one deck in the metal surface; Afterwards, rinse well less than the ultra-pure water of 12M Ω cm with electrical conductivity, and utilize dry nothing oil hot-air will be cleaned production of polysilicon equipment and the oven dry of process pipe inside, thereby make it inner clean, reaching does not have oily, anhydrous, dustless, the assorted pest effect of nothing.
4, adopt the complexing cleaning method, the main cleaning agent that is adopted in the cleaning process is an organic compound, does not wherein contain Na, P ion, and reaction speed is slow and need under certain temperature condition, carry out; Simultaneously, the cleaning agent that is adopted in the cleaning process only reacts with the oxidation on metal surface thing, can not form excessive erosion and hydrogen embrittlement.In addition; Because the cleaning agent that is adopted in the cleaning process is not for containing the organic compound of P, Na ion; Thereby can guarantee to be cleaned the purity of object; And can effectively avoid the medium reaction in residual chemical ion and production of polysilicon equipment and the process pipe, thereby make and do not have P, Na plasma in production of polysilicon equipment and the process pipe, effectively guarantee the cleanliness factor that production of polysilicon equipment and process pipe thereof are inner.
5, economical and practical, shortened the scavenging period of electronic-grade polycrystalline silicon production equipment and process pipe greatly, reduced the cleaning cost, and labour intensity is less.
6, applied widely, the present invention can effectively promote and be suitable for to the demanding industrial system cleaning process of other cleanliness factor.
7, have good economic benefit and social benefit,, shortened the driving time of production of polysilicon system greatly, for good condition has been created in production in that production of polysilicon equipment and the inner cleanliness factor of process pipe are control effectively.
In sum; The present invention is reasonable in design, the cleaning method step is simple, easy and simple to handle and it is convenient to realize, cleaning performance is good; Can not form excessive erosion and hydrogen embrittlement, can effectively solve being prone to that existing cleaning method exists and cause excessive erosion, passivating film surface to be prone to practical problems such as residual Na ion, P ion.
Through accompanying drawing and embodiment, technical scheme of the present invention is done further detailed description below.
Description of drawings
Fig. 1 is a cleaning method FB(flow block) of the present invention.
The specific embodiment
A kind of electronic-grade polycrystalline silicon production equipment as shown in Figure 1 and the cleaning method of process pipe may further comprise the steps:
Step 1, cleaning by degreasing: the conventional cleaning by degreasing method that adopts the degreasing metal cleaning agent and press metal equipment and metallic conduit, carry out cleaning by degreasing to being cleaned metal objects; The said metal objects that is cleaned is production of polysilicon equipment or polysilicon process pipeline.
When reality was carried out cleaning by degreasing to being cleaned metal objects, its cleaning by degreasing process was following:
101, thick cleaning by degreasing: under the normal temperature state, adopt the trichloro-ethylene cleaning agent to clean, and scavenging period is 2 hours～3 hours to being cleaned metal objects.
In the actual mechanical process, can also adjust accordingly scavenging period according to actual needs.
102, heated-air drying: after thick cleaning by degreasing finishes, adopt hot-air seasoning equipment, will be cleaned metal objects and dry up.
103, smart cleaning by degreasing: adopt AEO solution and under 40 ℃～50 ℃ temperature conditions, the metal objects that is cleaned after cleaning by degreasing is slightly cleaned, scavenging period is 3 hours～5 hours.Simultaneously, the metal objects that is cleaned after thick cleaning by degreasing is carried out in the cleaning process, the pH value of said AEO solution is controlled between 9～11.In the actual mechanical process, can also be according to actual needs in the cleaning process, the pH value of AEO solution, cleaning temperature, scavenging period etc. adjust accordingly.
The temperature of the hot blast that equipment provides of hot-air seasoning described in the step 102 is 40 ℃～50 ℃.After will be cleaned metal objects and dry up described in the step 102, also need adopt oil suction filter paper whether to exist greasy dirt to detect: when detection draws the inner surface that is cleaned metal objects and do not have greasy dirt, then to get into step 103 to being cleaned the metal objects inner surface; Otherwise, change step 101 over to, repeat thick cleaning by degreasing to being cleaned metal objects.
Water flushing after step 2, the degreasing: adopt running water to wash to being cleaned metal objects.
When actual employing running water washes being cleaned metal objects; Carry out cleaning down with running water to being cleaned metal objects inside; And after flushing finishes; Be cleaned the inner surface of metal objects with ultra violet lamp: when the inner surface that is cleaned metal objects presents purple light, then get into step 3; Otherwise, proceed flushing to being cleaned metal objects inside with running water.
Step 3, complexing rust cleaning: adopt the complexing cleaning agent to being cleaned the metal objects cleaning that eliminates rust.
The actual rust cleaning when cleaning, used complexing cleaning agent is a sodium ethylene diamine tetracetate solution, and the cleaning that under 40 ℃～50 ℃ temperature conditions, eliminates rust, the rust cleaning scavenging period is 8 hours～10 hours.In the rust cleaning cleaning process, the pH value that rust cleaning is cleaned with sodium ethylene diamine tetracetate solution is controlled between 1～4.
In the actual mechanical process, can also select the complexing cleaning agent of other type for use; Simultaneously, can also adjust accordingly the pH value of sodium ethylene diamine tetracetate solution in the rust cleaning cleaning process, the cleaning temperature that eliminates rust, rust cleaning scavenging period etc. according to actual needs.
Step 4, rinsing: adopt purificant to carry out rinsing to being cleaned metal objects.
Actual when carrying out rinsing, used purificant is a citric acid solution, and under 70 ℃～75 ℃ temperature conditions, carries out rinsing, and the rinsing time is 3 hours～4 hours; In the rinse cycle, the pH value of rinsing with citric acid solution is controlled between 3.5～4.
In the actual mechanical process, can also select the purificant of other type for use; Simultaneously, can also be according to actual needs the pH value of citric acid solution in the rinse cycle, rinsing temperature, rinsing time etc. be adjusted accordingly.
Step 5, ammonia plug flushing: adopt ammonia spirit and under 55 ℃～60 ℃ temperature conditions, wash to being cleaned metal objects.
During actual the cleaning; Adopt pH lower and be acid purificant rinsing and finish after; Need adopt the higher and solution that be alkalescence of pH to wash immediately, and with the pH of solution being brought up to more than 9.5 very soon after the demineralized water ammonification, thereby form " ammonia plug "; With rapid replacement " acid plug ", interface has a transition pH state of value.
Reality is carried out in the flushing process being cleaned metal objects, the pH value of flushing with ammonia spirit is controlled between 8～9, and washing time is 2 hours～3 hours.
In the actual mechanical process, can also be according to actual needs the pH value of ammonia spirit in the flushing process, washing time etc. be adjusted accordingly.
Step 6, Passivation Treatment: adopt hydrogen peroxide solution and under 80 ℃～90 ℃ temperature conditions, carry out Passivation Treatment to being cleaned metal objects.
Reality is carried out in the Passivation Treatment process being cleaned metal objects, the pH value of Passivation Treatment with hydrogen peroxide solution is controlled between 9～10, and the Passivation Treatment time is 6 hours～8 hours.
In the actual mechanical process, can also be according to actual needs the pH value of hydrogen peroxide solution in the Passivation Treatment process, Passivation Treatment temperature, Passivation Treatment time etc. be adjusted accordingly.
Step 7, ultra-pure water flushing: be not more than the ultra-pure water of 12M Ω cm with resistivity, wash to being cleaned metal objects.
Step 8, dried: adopt compressed air drying equipment and, carry out dried to being cleaned metal objects by conventional compressed air drying processing method.
Actual when carrying out dried, used compressed air drying equipment be for providing the drying equipment of oil-free compressed air, and carries out needing said oil-free compressed air is heated to 70 ℃～90 ℃ before the dried to being cleaned metal objects.
Simultaneously, in the actual mechanical process, also can select the compressed air drying equipment of other type for use.
Step 9, seal: the metal objects that is cleaned to after dried and quality examination are qualified, seal protection.
When reality was specifically cleaned production of polysilicon equipment and process pipe, the cleaning way that is adopted was identical with conventional cleaning way.Specifically, (specifically be greatly for volume greater than 10m
3) production of polysilicon equipment, in the manual work polishing, clean earlier with cleaning agent, the back adopts the cleaning way of cleaning agent spray to clean; For volume less than 10m
3Production of polysilicon equipment, adopt the wash cycles mode, clean and make the processing processing line in the construction voluntarily, the rinse bath on the Cleaning Line, service sink etc. must the periodic cleaning precipitated impurities; Adopt drill traverse or wash cycles mode for polysilicon process pipeline, valve, flange, pipe fitting etc., annex adopts the artificial cleaning way of cleaning in the production of polysilicon equipment.
Embodiment 1
In the present embodiment, as shown in Figure 1, be that 1250 tons production of polysilicon equipment cleans to annual production, and its cleaning process is following:
Step 1, cleaning by degreasing, its cleaning by degreasing process is following:
101, thick cleaning by degreasing: under the normal temperature state, adopt the trichloro-ethylene cleaning agent to clean, and scavenging period is 2 hours to being cleaned metal objects.
102, heated-air drying: after thick cleaning by degreasing finished, adopting hot-air seasoning equipment was that 40 ℃ hot blast will be cleaned production of polysilicon equipment and dry up with temperature.
And after the production of polysilicon equipment that is cleaned dried up, also need adopt oil suction filter paper whether to exist greasy dirt to detect: when detection draws inner surface and do not have greasy dirt, then to get into step 103 to the inner surface that is cleaned production of polysilicon equipment; Otherwise, change step 101 over to, the production of polysilicon equipment that is cleaned is repeated thick cleaning by degreasing.
103, smart cleaning by degreasing: adopt AEO solution and under 40 ℃ of temperature conditions, the production of polysilicon equipment that is cleaned is cleaned, scavenging period is 5 hours.Simultaneously, in the cleaning process, the pH value of AEO solution is controlled between 9～11.
Water flushing after step 2, the degreasing: adopt running water to wash; And after flushing finishes, be cleaned the inner surface of production of polysilicon equipment with ultra violet lamp: when being cleaned production of polysilicon equipment inner surface and presenting purple light, then get into step 3; Otherwise, the production of polysilicon device interior that is cleaned is proceeded flushing with running water.
Step 3, complexing rust cleaning: adopt the sodium ethylene diamine tetracetate solution and the cleaning that under 40 ℃ of temperature conditions, eliminates rust, the rust cleaning scavenging period is 10 hours.In the rust cleaning cleaning process, the pH value of sodium ethylene diamine tetracetate solution is controlled between 1～4.
In the present embodiment, in the actual cleaning process that eliminates rust, whenever detected once rust cleaning and clean, and each time testing result is carried out record synchronously with the iron concentration in the sodium ethylene diamine tetracetate solution at a distance from 20 minutes minutes; Simultaneously, adjacent twice testing result in front and back made difference relatively and when differ above 2mg/l between the two, the sodium ethylene diamine tetracetate solution of rust cleaning cleaning usefulness is changed.Simultaneously, rust cleaning is cleaned when detecting with the iron concentration in the sodium ethylene diamine tetracetate solution, the detection of taking a sample of employing spectrophotometer, and check the spectrophotometer examining report synchronously.In addition, also can adopt the iron concentration detector to detect.
Step 4, rinsing: adopt citric acid solution and under 70 ℃ of temperature conditions, the production of polysilicon equipment that is cleaned is carried out rinsing, the rinsing time is 4 hours; In the rinse cycle, the pH value of rinsing with citric acid solution is controlled between 3.5～4.
Step 5, ammonia plug flushing: adopt ammonia spirit and under 55 ℃ of temperature conditions, the production of polysilicon equipment that is cleaned is washed; In the actual flushing process, the pH value of flushing with ammonia spirit is controlled between 8～9, and washing time is 3 hours.
Step 6, Passivation Treatment: adopt hydrogen peroxide solution and under 80 ℃ of temperature conditions, the production of polysilicon equipment that is cleaned is carried out Passivation Treatment, and the Passivation Treatment time is 8 hours.In the Passivation Treatment process, the pH value of Passivation Treatment with hydrogen peroxide solution is controlled between 9～10.
In the present embodiment, in the Passivation Treatment process, estimate, and stop Passivation Treatment when treating formed passivation layer compact and complete being cleaned the passivation layer that the production of polysilicon device interior forms.
Step 7, ultra-pure water flushing: be not more than the ultra-pure water of 12M Ω cm with resistivity, the production of polysilicon equipment that is cleaned is washed.
In the present embodiment, actual carrying out in the flushing process dashes to the current that are cleaned the production of polysilicon device interior and is evenly distributed, and needs carry out cleaning down to the production of polysilicon device interior that is cleaned.
Step 8, dried: adopt compressed air drying equipment and, the production of polysilicon equipment that is cleaned is carried out dried by conventional compressed air drying processing method.
In the present embodiment, used compressed air drying equipment be for can provide the drying equipment of oil-free compressed air, and carries out before the dried, needs said oil-free compressed air is heated to 70 ℃.
In the present embodiment, actual carrying out in the dried process, wait to estimate to the inner surface that is cleaned production of polysilicon equipment anhydrous after, stop dried.
Step 9, seal: the production of polysilicon equipment to after dried and quality examination are qualified, seal protection.
In the present embodiment, when the production of polysilicon equipment after cleaning is sealed protection,, carry out shutoff in the outside with plastic closure more earlier at its interface outsourcing gas phase membrane paper.
Embodiment 2
In the present embodiment, be that 3000 tons production of polysilicon equipment cleans to annual production, what its cleaning process and embodiment 1 were different is: when carrying out thick cleaning by degreasing in the step 101, scavenging period is 3 hours; Adopting hot-air seasoning equipment in the step 102 is that 50 ℃ hot blast will be cleaned production of polysilicon equipment and dry up with temperature; Adopt AEO solution in the step 103 and under 50 ℃ of temperature conditions, clean, scavenging period is 3 hours; Adopt the sodium ethylene diamine tetracetate solution and the cleaning that under 50 ℃ of temperature conditions, eliminates rust in the step 3, the rust cleaning scavenging period is 8 hours; And in the actual cleaning process that eliminates rust, whenever detected once rust cleaning and clean, and each time testing result is carried out record synchronously with the iron concentration in the sodium ethylene diamine tetracetate solution at a distance from 30 minutes minutes; Adopt citric acid solution in the step 4 and under 75 ℃ of temperature conditions, the production of polysilicon equipment that is cleaned is carried out rinsing, the rinsing time is 3 hours; Adopt ammonia spirit in the step 5 and under 60 ℃ of temperature conditions, the production of polysilicon equipment that is cleaned is washed, washing time is 2 hours; Adopt hydrogen peroxide solution in the step 6 and under 90 ℃ of temperature conditions, carry out Passivation Treatment, and the Passivation Treatment time is 6 hours; Carry out in the step 8 before the dried, need said oil-free compressed air is heated to 70 ℃.
In the present embodiment, all the other cleaning steps, technological parameter and cleaning principle are all identical with embodiment 1.
Embodiment 3
In the present embodiment, be that 500 tons production of polysilicon equipment cleans to annual production, what its cleaning process and embodiment 1 were different is: when carrying out thick cleaning by degreasing in the step 101, scavenging period is 2.5 hours; Adopting hot-air seasoning equipment in the step 102 is that 45 ℃ hot blast will be cleaned production of polysilicon equipment and dry up with temperature; Adopt AEO solution in the step 103 and under 45 ℃ of temperature conditions, clean, scavenging period is 4 hours; Adopt the sodium ethylene diamine tetracetate solution and the cleaning that under 45 ℃ of temperature conditions, eliminates rust in the step 3, the rust cleaning scavenging period is 9 hours; And in the actual cleaning process that eliminates rust, whenever detected once rust cleaning and clean, and each time testing result is carried out record synchronously with the iron concentration in the sodium ethylene diamine tetracetate solution at a distance from 40 minutes minutes; Adopt citric acid solution in the step 4 and under 72 ℃ of temperature conditions, the production of polysilicon equipment that is cleaned is carried out rinsing, the rinsing time is 3.5 hours; Adopt ammonia spirit in the step 5 and under 58 ℃ of temperature conditions, the production of polysilicon equipment that is cleaned is washed, washing time is 2.5 hours; Adopt hydrogen peroxide solution in the step 6 and under 85 ℃ of temperature conditions, carry out Passivation Treatment, and the Passivation Treatment time is 7 hours; Carry out in the step 8 before the dried, need said oil-free compressed air is heated to 75 ℃.
In the present embodiment, all the other cleaning steps, technological parameter and cleaning principle are all identical with embodiment 1.
Embodiment 4
In the present embodiment, as shown in Figure 1, to the polysilicon process pipeline clean and its cleaning process following:
Step 1, cleaning by degreasing, its cleaning by degreasing process is following:
101, thick cleaning by degreasing: under the normal temperature state, adopt the trichloro-ethylene cleaning agent to clean, and scavenging period is 2.2 hours to being cleaned metal objects.
102, heated-air drying: after thick cleaning by degreasing finished, adopting hot-air seasoning equipment was that 42 ℃ hot blast will be cleaned the polysilicon process pipeline and dry up with temperature.
And after the polysilicon process pipeline that is cleaned dried up, also need adopt oil suction filter paper whether to exist greasy dirt to detect: when detection draws inner surface and do not have greasy dirt, then to get into step 103 to being cleaned the polysilicon process side opposite; Otherwise, change step 101 over to, the polysilicon process pipeline that is cleaned is repeated thick cleaning by degreasing.
103, smart cleaning by degreasing: adopt AEO solution and under 42 ℃ of temperature conditions, the polysilicon process pipeline that is cleaned is cleaned, scavenging period is 4.5 hours.Simultaneously, in the cleaning process, the pH value of AEO solution is controlled between 9～11.
Water flushing after step 2, the degreasing: adopt running water to wash; And after flushing finishes, be cleaned the polysilicon process side opposite: when being cleaned the polysilicon process inner surface of pipeline and presenting purple light, then get into step 3 with ultra violet lamp; Otherwise, the polysilicon process pipe interior that is cleaned is proceeded flushing with running water.
Step 3, complexing rust cleaning: adopt the sodium ethylene diamine tetracetate solution and the cleaning that under 42 ℃ of temperature conditions, eliminates rust, the rust cleaning scavenging period is 9.5 hours.In the rust cleaning cleaning process, the pH value of sodium ethylene diamine tetracetate solution is controlled between 1～4.
In the present embodiment, in the actual cleaning process that eliminates rust, whenever detected once rust cleaning and clean, and each time testing result is carried out record synchronously with the iron concentration in the sodium ethylene diamine tetracetate solution at a distance from 25 minutes minutes; Simultaneously, adjacent twice testing result in front and back made difference relatively and when differ above 2mg/l between the two, the sodium ethylene diamine tetracetate solution of rust cleaning cleaning usefulness is changed.Simultaneously, rust cleaning is cleaned when detecting with the iron concentration in the sodium ethylene diamine tetracetate solution, the detection of taking a sample of employing spectrophotometer, and check the spectrophotometer examining report synchronously.In addition, also can adopt the iron concentration detector to detect.
Step 4, rinsing: adopt citric acid solution and under 72 ℃ of temperature conditions, the polysilicon process pipeline that is cleaned is carried out rinsing, the rinsing time is 3.2 hours; In the rinse cycle, the pH value of rinsing with citric acid solution is controlled between 3.5～4.
Step 5, ammonia plug flushing: adopt ammonia spirit and under 56 ℃ of temperature conditions, the polysilicon process pipeline that is cleaned is washed; In the actual flushing process, the pH value of flushing with ammonia spirit is controlled between 8～9, and washing time is 2.2 hours.
Step 6, Passivation Treatment: adopt hydrogen peroxide solution and under 82 ℃ of temperature conditions, the polysilicon process pipeline that is cleaned is carried out Passivation Treatment, and the Passivation Treatment time is 7.5 hours.In the Passivation Treatment process, the pH value of Passivation Treatment with hydrogen peroxide solution is controlled between 9～10.
In the present embodiment, in the Passivation Treatment process, estimate, and stop Passivation Treatment when treating formed passivation layer compact and complete being cleaned the passivation layer that the polysilicon process pipe interior forms.
Step 7, ultra-pure water flushing: be not more than the ultra-pure water of 12M Ω cm with resistivity, the polysilicon process pipeline that is cleaned is washed.
In the present embodiment, actual carrying out in the flushing process dashes to the current that are cleaned the polysilicon process pipe interior and is evenly distributed, and needs carry out cleaning down to the polysilicon process pipe interior that is cleaned.
Step 8, dried: adopt compressed air drying equipment and, the polysilicon process pipeline that is cleaned is carried out dried by conventional compressed air drying processing method.
In the present embodiment, used compressed air drying equipment be for can provide the drying equipment of oil-free compressed air, and carries out before the dried, needs said oil-free compressed air is heated to 72 ℃.
In the present embodiment, actual carrying out in the dried process, wait to estimate to be cleaned the polysilicon process side opposite anhydrous after, stop dried.
Step 9, seal: the polysilicon process pipeline to after dried and quality examination are qualified, seal protection.
In the present embodiment, the polysilicon process pipeline after cleaning is sealed before the protection, earlier when cleaning back polysilicon process pipeline and carry out the pressure testing test, and after the passed examination, seal protection again.Polysilicon process pipeline to after cleaning seals protection, earlier at its mouth of pipe outsourcing gas phase membrane paper, carries out shutoff in the outside with plastic closure again.
Embodiment 5
In the present embodiment, different with embodiment 4 is: when carrying out thick cleaning by degreasing in the step 101, scavenging period is 2.5 hours; Adopting hot-air seasoning equipment in the step 102 is that 48 ℃ hot blast will be cleaned the polysilicon process pipeline and dry up with temperature; Adopt AEO solution in the step 103 and under 48 ℃ of temperature conditions, clean, scavenging period is 3.5 hours; Adopt the sodium ethylene diamine tetracetate solution and the cleaning that under 48 ℃ of temperature conditions, eliminates rust in the step 3, the rust cleaning scavenging period is 8.5 hours; And in the actual cleaning process that eliminates rust, whenever detected once rust cleaning and clean, and each time testing result is carried out record synchronously with the iron concentration in the sodium ethylene diamine tetracetate solution at a distance from 30 minutes minutes; Adopt citric acid solution in the step 4 and under 74 ℃ of temperature conditions, the polysilicon process pipeline that is cleaned is carried out rinsing, the rinsing time is 3.5 hours; Adopt ammonia spirit in the step 5 and under 57 ℃ of temperature conditions, the polysilicon process pipeline that is cleaned is washed, washing time is 2.5 hours; Adopt hydrogen peroxide solution in the step 6 and under 88 ℃ of temperature conditions, carry out Passivation Treatment, and the Passivation Treatment time is 6.5 hours; Carry out in the step 8 before the dried, need said oil-free compressed air is heated to 78 ℃.
In the present embodiment, all the other cleaning steps, technological parameter and cleaning principle are all identical with embodiment 4.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any restriction, every technical spirit changes any simple modification, change and the equivalent structure that above embodiment did according to the present invention, all still belongs in the protection domain of technical scheme of the present invention.
Claims (10)
1. the cleaning method of electronic-grade polycrystalline silicon production equipment and process pipe is characterized in that this method may further comprise the steps:
Step 1, cleaning by degreasing: the conventional cleaning by degreasing method that adopts the degreasing metal cleaning agent and press metal equipment and metallic conduit, carry out cleaning by degreasing to being cleaned metal objects; The said metal objects that is cleaned is production of polysilicon equipment or polysilicon process pipeline;
Water flushing after step 2, the degreasing: adopt running water to wash to being cleaned metal objects;
Step 3, complexing rust cleaning: adopt the complexing cleaning agent to being cleaned the metal objects cleaning that eliminates rust;
Step 4, rinsing: adopt purificant to carry out rinsing to being cleaned metal objects;
Step 5, ammonia plug flushing: adopt ammonia spirit and under 55 ℃～60 ℃ temperature conditions, wash to being cleaned metal objects;
Step 6, Passivation Treatment: adopt hydrogen peroxide solution and under 80 ℃～90 ℃ temperature conditions, carry out Passivation Treatment to being cleaned metal objects;
Step 7, ultra-pure water flushing: be not more than the ultra-pure water of 12M Ω cm with resistivity, wash to being cleaned metal objects;
Step 8, dried: adopt compressed air drying equipment and, carry out dried to being cleaned metal objects by conventional compressed air drying processing method;
Step 9, seal: the metal objects that is cleaned to after dried and quality examination are qualified, seal protection.
2. according to the cleaning method of described a kind of electronic-grade polycrystalline silicon production equipment of claim 1 and process pipe, it is characterized in that: described in the step 1 when being cleaned metal objects and carrying out cleaning by degreasing, its cleaning by degreasing process is following:
101, thick cleaning by degreasing: under the normal temperature state, adopt the trichloro-ethylene cleaning agent to clean, and scavenging period is 2 hours～3 hours to being cleaned metal objects;
102, heated-air drying: after thick cleaning by degreasing finishes, adopt hot-air seasoning equipment, will be cleaned metal objects and dry up;
103, smart cleaning by degreasing: adopt AEO solution and under 40 ℃～50 ℃ temperature conditions, the metal objects that is cleaned after cleaning by degreasing is slightly cleaned, scavenging period is 3 hours～5 hours.
3. according to the cleaning method of described a kind of electronic-grade polycrystalline silicon production equipment of claim 2 and process pipe, it is characterized in that: the temperature of the hot blast that equipment provides of hot-air seasoning described in the step 102 is 40 ℃～50 ℃; After will be cleaned metal objects and dry up described in the step 102, also need adopt oil suction filter paper whether to exist greasy dirt to detect: when detection draws the inner surface that is cleaned metal objects and do not have greasy dirt, then to get into step 103 to being cleaned the metal objects inner surface; Otherwise, change step 101 over to, repeat thick cleaning by degreasing to being cleaned metal objects.
4. according to the cleaning method of claim 2 or 3 described a kind of electronic-grade polycrystalline silicon production equipments and process pipe; It is characterized in that: the metal objects that is cleaned to after thick cleaning by degreasing described in the step 103 carries out in the cleaning process, and the pH value of said AEO solution is controlled between 9～11.
5. according to the cleaning method of claim 1,2 or 3 described a kind of electronic-grade polycrystalline silicon production equipments and process pipe; It is characterized in that: when the employing running water described in the step 2 washes being cleaned metal objects; Carry out cleaning down with running water to being cleaned metal objects inside; And after flushing finishes, be cleaned the inner surface of metal objects with ultra violet lamp: when the inner surface that is cleaned metal objects presents purple light, then get into step 3; Otherwise, proceed flushing to being cleaned metal objects inside with running water.
6. according to the cleaning method of claim 1,2 or 3 described a kind of electronic-grade polycrystalline silicon production equipments and process pipe; It is characterized in that: the complexing cleaning agent described in the step 3 is a sodium ethylene diamine tetracetate solution; And the cleaning that under 40 ℃～50 ℃ temperature conditions, eliminates rust, the rust cleaning scavenging period is 8 hours～10 hours; In the rust cleaning cleaning process, the pH value that rust cleaning is cleaned with sodium ethylene diamine tetracetate solution is controlled between 1～4.
7. according to the cleaning method of claim 1,2 or 3 described a kind of electronic-grade polycrystalline silicon production equipments and process pipe; It is characterized in that: the purificant described in the step 4 is a citric acid solution; And under 70 ℃～75 ℃ temperature conditions, carry out rinsing, the rinsing time is 3 hours～4 hours; In the rinse cycle, the pH value of rinsing with citric acid solution is controlled between 3.5～4.
8. according to the cleaning method of claim 1,2 or 3 described a kind of electronic-grade polycrystalline silicon production equipments and process pipe; It is characterized in that: carrying out in the flushing process described in the step 5 being cleaned metal objects; The pH value of flushing with ammonia spirit is controlled between 8～9, and washing time is 2 hours～3 hours.
9. according to the cleaning method of claim 1,2 or 3 described a kind of electronic-grade polycrystalline silicon production equipments and process pipe; It is characterized in that: carrying out in the Passivation Treatment process described in the step 6 being cleaned metal objects; The pH value of Passivation Treatment with hydrogen peroxide solution is controlled between 9～10, and the Passivation Treatment time is 6 hours～8 hours.
10. according to the cleaning method of claim 1,2 or 3 described a kind of electronic-grade polycrystalline silicon production equipments and process pipe; It is characterized in that: the compressed air drying equipment described in the step 8 is for providing the drying equipment of oil-free compressed air; And carry out before the dried being cleaned metal objects, need said oil-free compressed air is heated to 70 ℃～90 ℃.
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| CN102489480B (en) * | 2011-12-16 | 2013-09-25 | 安徽康迪纳电力科技有限责任公司 | Chemical cleaning process of oil system of large equipment |
| CN105256320B (en) * | 2015-10-28 | 2018-04-27 | 陕西庄臣环保科技有限公司 | A kind of chemical complexing cleaning method of polysilicon equipment |
| CN106367815B (en) * | 2016-09-12 | 2018-10-19 | 英利能源（中国）有限公司 | The cleaning method of monocrystalline silicon etching device |
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| CN107460487B (en) * | 2017-08-11 | 2019-01-04 | 中国化学工程第六建设有限公司 | High pressure oxygen inner wall of the pipe cleaning by degreasing method |
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| CN109701962A (en) * | 2018-12-03 | 2019-05-03 | 巢湖鹏远金属焊管有限公司 | A kind of cleaning process of metallic conduit |
| CN114018086A (en) * | 2021-11-15 | 2022-02-08 | 上海亘满科技有限公司 | Method for cleaning magnesium ammonia heat pipe |
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