CN102864435A - Method for preparing composite type millipore filtration membrane for filtering organic waste water - Google Patents
Method for preparing composite type millipore filtration membrane for filtering organic waste water Download PDFInfo
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- CN102864435A CN102864435A CN2012104120342A CN201210412034A CN102864435A CN 102864435 A CN102864435 A CN 102864435A CN 2012104120342 A CN2012104120342 A CN 2012104120342A CN 201210412034 A CN201210412034 A CN 201210412034A CN 102864435 A CN102864435 A CN 102864435A
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Abstract
Provided is a method for preparing a composite type millipore filtration membrane for filtering organic waste water. The BDD-Ta-Ti composite type millipore filtration membrane having a good electric-conducting characteristic is prepared by depositing a tantalum membrane and a thin diamond-doped membrane on a Millipore material. The method comprises the steps of (1) pre-treating a substrate; (2) sputtering the tantalum membrane; and (3) preparing the thin diamond-doped membrane. Before the thin diamond-doped membrane deposits, the surface of a hot filament of a hot filament chemical vapor deposition method (HFCVD) device is carbonized to prevent hot filament from performing carbonization reaction, using a large amount of carbon sources and accordingly influencing diamond nucleation and growing in the diamond nucleation and growing process, and then utilizing an HFCVD process to deposit a layer of thin diamond membrane. The method has the advantages that the prepared thin membrane is excellent in quality, has strong anti-pollution capacity and is especially suitable for filtering of the organic waste water produced by the industries of petroleum, dyestuff processing, machinery manufacturing and the like. The thin membrane is simple in preparation process condition, easy to operate, low in cost and easy to popularize.
Description
Technical field
The invention belongs to the membrane sepn technology of preparing, particularly a kind of compound millipore filtration preparation method who filters organic pollutant wastewater.
Background technology
Fast development along with industry, the organic pollutant value volume and range of product of producing discharging increases gradually, a large amount of organic pollutants enter in the water body, cause the organic content sharp increase in the trade effluent, toxicity is increasing, these objectionable impurities complicated components, and difficulty is carried out biological degradation, bring grievous injury to environment, have influence on the Sustainable development of daily life and society.Sewage disposal technology mainly contains physical treatment process, method of chemical treatment and three directions of biological treatment at present, and the means of employing mainly are membrane filtration and biochemical degradation.These technology and method come with some shortcomings, poisonous and to be difficult to carry out biodegradable organic pollutant not too applicable for those, the easy contaminated species restriction of biological degradation, and membrane separation process is disposed of sewage in the process, it is to restrict membrane separation technique at the obstacle that has breakthrough aspect the organic contamination processing all the time that film pollutes, and final treatment effect is all not ideal enough.How effectively to dispose difficult degradation toxic organic compound in the sewage and become the focus that environment and industry member are paid close attention to.Developing a kind of novel pollution-resistant membrane material is current membrane separation technique field key issue in the urgent need to address.
As everyone knows, diamond has the physics and chemistry character of many excellences, is widely used in gradually the fields such as mechanical workout, wireless communication, semi-conductor manufacturing, chemical industry measurement.Utilize the diamond thin of CVD technology preparation to have good chemical stability, the surface has again the absorption inertia, and good electroconductibility is arranged after the doping, and very wide TV window, low background current are arranged itself, and contamination resistance is strong, is desirable electrode materials.Utilize the titanium plate of powder metallurgy technology preparation, have good infiltration function, but have the existence of transition layer titanium carbide owing to preparing diamond on the titanium, affect the attachment characteristic of the two.Tantalum metal and diamond thin do not exist transition layer to affect the problem of attachment characteristic and good corrosion resistance.With triplicity, tantalum is as the middle layer, prepare novel compound millipore filtration, it is a kind of millipore filtration with self-cleaning function, can well filter organic pollutant wastewater, utilize electrochemical method that composite membrane is used as anode, when filtering organic pollutant wastewater, the organism on film surface can be carried out mineralising, prevent that the membrane flux that cause because of pollution on the film surface from descending and the film inefficacy.
Summary of the invention
The objective of the invention is for above-mentioned existing problems and technical Analysis, a kind of compound millipore filtration preparation method who filters organic pollutant wastewater is provided, the method is by depositing tantalum film, doped diamond thin films (BDD) at porous material, prepare the compound millipore filtration of the BDD-Ta-Ti with good conductive characteristic, the film quality of preparation is good, have stronger contamination resistance, preparation process condition is simple, easily operation, cost are lower, is easy to promote.
Technical scheme of the present invention:
A kind of compound millipore filtration preparation method who filters organic pollutant wastewater by deposit tantalum film, doped diamond thin films at porous material, prepares the compound millipore filtration of the BDD-Ta-Ti with good conductive characteristic, and step is as follows:
1) substrate pre-treatment: selecting thickness is that 2mm, aperture are that 1 μ m, porosity are 30% titanium plate, with dehydrated alcohol it is carried out ultrasonic cleaning, then on substrate, evenly sprinkle the bortz powder that one deck particle diameter is 0.2 μ m, it was slightly polished 5 minutes so that the diamond powder particle can be stayed substrate surface when substrate forms scratch defects with No.600 sand paper, use again the deionized water ultrasonic cleaning, dry for subsequent use;
2) tantalum film sputter: will put into the magnetron sputtering vapor deposition apparatus through pretreated POROUS TITANIUM substrate, and adopt d.c. sputtering, and pass under the argon gas condition, power 100-120W, flow 20sccm, chamber pressure 1Pa, temperature are room temperature, sputter 8-10 minute;
3) doped diamond thin films preparation: before depositing diamond film, to carry out surperficial carbonization to the heated filament of HFCVD equipment first, affect diamond nucleation and growth and guarantee heated filament surface carbonization to prevent that a large amount of carbon sources is fought in heated filament generation carburizing reagent in diamond nucleation and process of growth, method is: take acetone as carbon source, reaction chamber vacuum tightness is 5Pa, hydrogen flowing quantity is 200sccm, and carrier gas flux is 60sccm, and the time of filament carbonization was greater than one hour; Then utilize HFCVD technique at above-mentioned substrate deposition layer of gold diamond thin film, carbon source is acetone, hydrogen is as carrier gas, and doped element is boron, and the boron source is boron trioxide, during thin film deposition, the hydrogen flowing quantity in forming core stage is that 200sccm, carrier gas flux are 50-65sccm, and the hydrogen flowing quantity of growth phase is that 200sccm, carrier gas flux are 40sccm, and sinking to the bottom temperature is 800 ℃, depositing time is 5 hours, can make the compound millipore filtration of BDD-Ta-Ti.
Advantage of the present invention is: the film quality of preparation is good, has stronger contamination resistance, is specially adapted to the filtration that the industries such as petroleum industry, dyestuff processing, machinofacture produce organic pollutant wastewater; This thin film preparation process condition is simple, easily operation, cost are lower, is easy to promote.
Description of drawings
Accompanying drawing is boron-doped diamond/POROUS TITANIUM composite membrane SEM image, and wherein: Fig. 1 a is for amplifying 1000 times of SEM images, and Fig. 1 b is for amplifying 5000 times of images.
Embodiment
The present invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment 1:
A kind of compound millipore filtration preparation method who filters organic pollutant wastewater, step is as follows:
1) substrate pre-treatment: selecting thickness is that 2mm, aperture are that 1 μ m, porosity are 30% titanium plate, with dehydrated alcohol it is carried out ultrasonic cleaning, then on substrate, evenly sprinkle the bortz powder that one deck particle diameter is 0.2 μ m, it was slightly polished 5 minutes so that the diamond powder particle can be stayed substrate surface when substrate forms scratch defects with No.600 sand paper, use again the deionized water ultrasonic cleaning, dry for subsequent use;
2) tantalum film sputter: will put into the magnetron sputtering vapor deposition apparatus through pretreated POROUS TITANIUM substrate, and adopt d.c. sputtering, and pass under the argon gas condition, power 100W, flow 20sccm, chamber pressure 1Pa, temperature are room temperature, sputter 10 minutes;
3) doped diamond thin films preparation: before depositing diamond film, to carry out surperficial carbonization to the heated filament of HFCVD equipment first, affect diamond nucleation and growth and guarantee heated filament surface carbonization to prevent that a large amount of carbon sources is fought in heated filament generation carburizing reagent in diamond nucleation and process of growth, method is: take acetone as carbon source, reaction chamber vacuum tightness is 5Pa, hydrogen flowing quantity is 200sccm, and carrier gas flux is 60sccm, and the time of filament carbonization is 1.5 hours; Then utilize HFCVD technique at above-mentioned substrate deposition layer of gold diamond thin film, carbon source is acetone, hydrogen is as carrier gas, and doped element is boron, and the boron source is boron trioxide, during thin film deposition, the hydrogen flowing quantity in forming core stage is that 200sccm, carrier gas flux are 50-65sccm, and the hydrogen flowing quantity of growth phase is that 200sccm, carrier gas flux are 40sccm, and sinking to the bottom temperature is 800 ℃, depositing time is 5 hours, can make the compound millipore filtration of BDD-Ta-Ti.
Accompanying drawing is boron-doped diamond/POROUS TITANIUM composite membrane SEM image, and wherein: Fig. 1 a is for amplifying 1000 times of SEM images, and Fig. 1 b is for amplifying 5000 times of images.Show among the figure: diamond crystals is of moderate size, and crystalline form is good, and the film growth quality meets the requirements.
Embodiment 2:
A kind of compound millipore filtration preparation method who filters organic pollutant wastewater, its processing condition and operation steps and embodiment 1 are identical, and difference is the carrier gas flux in diamond film growth stage is transferred to 50sccm.The compound millipore filtration detected result of preparation is identical with embodiment 1.
Embodiment 3:
A kind of compound millipore filtration preparation method who filters organic pollutant wastewater, its processing condition and operation steps and embodiment 1 are identical, and difference is the carrier gas flux in diamond film growth stage is transferred to 65sccm.The compound millipore filtration detected result of preparation is identical with embodiment 1.
Claims (1)
1. compound millipore filtration preparation method who filters organic pollutant wastewater, it is characterized in that: by deposit tantalum film, doped diamond thin films at porous material, prepare the compound millipore filtration of the BDD-Ta-Ti with good conductive characteristic, step is as follows:
1) substrate pre-treatment: selecting thickness is that 2mm, aperture are that 1 μ m, porosity are 30% titanium plate, with dehydrated alcohol it is carried out ultrasonic cleaning, then on substrate, evenly sprinkle the bortz powder that one deck particle diameter is 0.2 μ m, it was slightly polished 5 minutes so that the diamond powder particle can be stayed substrate surface when substrate forms scratch defects with No.600 sand paper, use again the deionized water ultrasonic cleaning, dry for subsequent use;
2) tantalum film sputter: will put into the magnetron sputtering vapor deposition apparatus through pretreated POROUS TITANIUM substrate, and adopt d.c. sputtering, and pass under the argon gas condition, power 100-120W, flow 20sccm, chamber pressure 1Pa, temperature are room temperature, sputter 8-10 minute;
3) doped diamond thin films preparation: before depositing diamond film, to carry out surperficial carbonization to the heated filament of HFCVD equipment first, affect diamond nucleation and growth and guarantee heated filament surface carbonization to prevent that a large amount of carbon sources is fought in heated filament generation carburizing reagent in diamond nucleation and process of growth, method is: take acetone as carbon source, reaction chamber vacuum tightness is 5Pa, hydrogen flowing quantity is 200sccm, and carrier gas flux is 60sccm, and the time of filament carbonization was greater than one hour; Then utilize HFCVD technique at above-mentioned substrate deposition layer of gold diamond thin film, carbon source is acetone, hydrogen is as carrier gas, and doped element is boron, and the boron source is boron trioxide, during thin film deposition, the hydrogen flowing quantity in forming core stage is that 200sccm, carrier gas flux are 50-65sccm, and the hydrogen flowing quantity of growth phase is that 200sccm, carrier gas flux are 40sccm, and sinking to the bottom temperature is 800 ℃, depositing time is 5 hours, can make the compound millipore filtration of BDD-Ta-Ti.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104759272A (en) * | 2014-12-09 | 2015-07-08 | 上海维埃姆环保科技有限公司 | Membrane electrode of membrane electrode low-voltage electrolysis type ozone generator and manufacturing method for positive and negative electrodes of membrane electrode low-voltage electrolysis type ozone generator |
| CN108396307A (en) * | 2018-01-18 | 2018-08-14 | 昆明理工大学 | A kind of preparation method of the diamond thin with strong film base adhesion strength |
| CN111097297A (en) * | 2019-12-30 | 2020-05-05 | 江西师范大学 | Boron-doped microporous silicon dioxide membrane and preparation method and application thereof |
| CN113880316A (en) * | 2021-11-17 | 2022-01-04 | 青岛延晖环保科技有限公司 | Method for desalting seawater by using biological membrane |
| CN114751408A (en) * | 2022-03-25 | 2022-07-15 | 浙江工业大学 | Method for preparing diamond based on graphite under low pressure |
| CN115784763A (en) * | 2022-11-15 | 2023-03-14 | 华北水利水电大学 | Boron-doped diamond porous titanium composite membrane and preparation method thereof |
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| US5160544A (en) * | 1990-03-20 | 1992-11-03 | Diamonex Incorporated | Hot filament chemical vapor deposition reactor |
| CN102242374A (en) * | 2011-06-30 | 2011-11-16 | 南京航空航天大学 | Production method of titanium-based boron-doping diamond coating electrode |
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Patent Citations (2)
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| US5160544A (en) * | 1990-03-20 | 1992-11-03 | Diamonex Incorporated | Hot filament chemical vapor deposition reactor |
| CN102242374A (en) * | 2011-06-30 | 2011-11-16 | 南京航空航天大学 | Production method of titanium-based boron-doping diamond coating electrode |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104759272A (en) * | 2014-12-09 | 2015-07-08 | 上海维埃姆环保科技有限公司 | Membrane electrode of membrane electrode low-voltage electrolysis type ozone generator and manufacturing method for positive and negative electrodes of membrane electrode low-voltage electrolysis type ozone generator |
| CN104759272B (en) * | 2014-12-09 | 2018-09-11 | 上海维埃姆环保科技有限公司 | A kind of membrane electrode of membrane electrode low-voltage electrolysis formula ozone generator and its production method of anode and anode |
| CN108396307A (en) * | 2018-01-18 | 2018-08-14 | 昆明理工大学 | A kind of preparation method of the diamond thin with strong film base adhesion strength |
| CN111097297A (en) * | 2019-12-30 | 2020-05-05 | 江西师范大学 | Boron-doped microporous silicon dioxide membrane and preparation method and application thereof |
| CN113880316A (en) * | 2021-11-17 | 2022-01-04 | 青岛延晖环保科技有限公司 | Method for desalting seawater by using biological membrane |
| CN114751408A (en) * | 2022-03-25 | 2022-07-15 | 浙江工业大学 | Method for preparing diamond based on graphite under low pressure |
| CN114751408B (en) * | 2022-03-25 | 2023-09-05 | 浙江工业大学 | Method for preparing diamond based on graphite at low pressure |
| CN115784763A (en) * | 2022-11-15 | 2023-03-14 | 华北水利水电大学 | Boron-doped diamond porous titanium composite membrane and preparation method thereof |
| CN115784763B (en) * | 2022-11-15 | 2023-06-02 | 华北水利水电大学 | Boron-doped diamond porous titanium composite film and preparation method thereof |
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Application publication date: 20130109 |