CN109570489B - Device and method for increasing oxygen content of metal powder by ozone oxidation - Google Patents
Device and method for increasing oxygen content of metal powder by ozone oxidation Download PDFInfo
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- CN109570489B CN109570489B CN201811609173.8A CN201811609173A CN109570489B CN 109570489 B CN109570489 B CN 109570489B CN 201811609173 A CN201811609173 A CN 201811609173A CN 109570489 B CN109570489 B CN 109570489B
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- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 title claims abstract description 218
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 83
- 239000002184 metal Substances 0.000 title claims abstract description 83
- 239000000843 powder Substances 0.000 title claims abstract description 82
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000001301 oxygen Substances 0.000 title claims abstract description 67
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 67
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 48
- 230000001965 increasing effect Effects 0.000 title claims abstract description 46
- 230000003647 oxidation Effects 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims description 30
- 238000006213 oxygenation reaction Methods 0.000 claims abstract description 70
- 230000035484 reaction time Effects 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 29
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 26
- 239000000498 cooling water Substances 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 16
- 239000010935 stainless steel Substances 0.000 claims description 16
- 229910001220 stainless steel Inorganic materials 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000009703 powder rolling Methods 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 230000000694 effects Effects 0.000 description 36
- 238000007790 scraping Methods 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 230000008569 process Effects 0.000 description 8
- 238000010586 diagram Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000000269 nucleophilic effect Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000006385 ozonation reaction Methods 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- -1 and actually Chemical compound 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
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- 239000002912 waste gas Substances 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
Abstract
An ozone oxidation catalystThe device comprises an ozone generator, an ozone adding distributor and an oxygenation reactor; the ozone generator conveys ozone into the ozone adding distributor through a pipeline, the ozone adding distributor is arranged in the oxygenation reactor, and the conveyed ozone is contacted with metal to be oxygenated arranged in the oxygenation reactor; the oxygenation reactor can rotate in the circumferential direction and can heat; the reaction temperature in the oxygenation reactor is 10-120 ℃, the rotation speed of the oxygenation reactor is 1-60 rpm, and the conveying amount of ozone is controlled to be 0.1m3/h‑3.0m3The reaction time is 0.5-5 h. The metal powder with the required increased oxygen content can be obtained by reasonably controlling the concentration of the generated ozone and the continuous reaction time.
Description
Technical Field
The invention relates to a technology for increasing the oxygen content of metal powder by using ozone oxidation, belongs to the field of powder oxidation treatment, and particularly relates to a device and a method for increasing the oxygen content of metal powder by using ozone oxidation.
Background
The metal powder needs to have an increased oxygen content in several cases:
1) when the average particle size of the metal powder is smaller and smaller, the activity of the metal powder is too high due to the large specific surface area, and an oxidation protection film needs to be added on the surface of the metal powder for passivation, so that the metal powder is beneficial to transportation and storage.
2) When the metal powder is used for sintering, in order to increase the sintering temperature and match the metal powder with other sintering materials and avoid faults and cracks on a sintering surface, an oxide layer needs to be added on the surface of the powder.
Generally, the method for increasing the oxygen content of the metal powder is to heat the metal powder to over 220 ℃ to reach the temperature required by the metal oxidation reaction; the reaction is more violent and the oxygen content is increased more rapidly at higher temperature, but the oxygen increasing condition has larger influence on the powder, so the powder is inflammable and explosive and generates sintering and agglomeration, the dispersibility of the powder is rapidly deteriorated, and the using effect of the powder is poor.
Ozone has strong oxidizing property (E0 is + 2.07V), the oxidation-reduction potential of the ozone is second to that of fluorine, the ozone directly participates in the reaction through nucleophilic or electrophilic action, under ideal reaction conditions, most simple substances and compounds in the environment can be oxidized to the highest oxidation state of the simple substances and the compounds, and the ozone has strong oxidative degradation effect on organic matters through active free radicals under the action of factors such as alkali, so that the ozone oxidation technology has good treatment effect and no secondary pollution when being applied to environmental management engineering. Therefore, the development field of ozone oxidation application technology mainly in the aspect of treating waste water and waste gas has not found research on the oxidation of metal surfaces, particularly metal powder, by ozone, and actually, ozone has a strong oxidation effect on metal materials, and the chemical reaction formula is as follows:
O3+Me＝MeO+O2；
one of the characteristics of the ozone oxidation reaction is that the ozone oxidation reaction can play a role in oxidation under the condition of low temperature, so that the technology for increasing oxygen by using ozone is provided, and the technology has very important significance for metal, particularly metal powder.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a device for increasing the oxygen content of metal powder by utilizing the ozone oxidation effect, which can realize the oxygen increase of the metal under the low-temperature environment, thereby solving the problems of the dispersion deterioration and the like caused by high oxidation temperature when the oxygen content of the metal powder is increased, and can maintain the dispersion and the using effect of the metal powder.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a device for increasing the oxygen content of metal powder by using the ozone oxidation effect comprises an ozone generator, an ozone adding distributor and an oxygenation reactor; the ozone generator conveys ozone into the ozone adding distributor through a pipeline, the ozone adding distributor is arranged in the oxygenation reactor, and the conveyed ozone is contacted with metal to be oxygenated arranged in the oxygenation reactor; the oxygenation reactor can rotate in the circumferential direction and can heat.
By adopting the structure, the oxygen increasing effect of ozone on metal can be realized, and the temperature of the ozone oxygen increasing process can be increased according to the requirement, so that the oxygen increasing efficiency is improved; in addition, the oxygenation reactor can rotate in the circumferential direction, so that the metal powder in the oxygenation reactor can be driven to move and turn over continuously, the contact surface between the oxygenation reactor and ozone can be increased, and the oxygenation efficiency can be improved.
Preferably, the device for increasing the oxygen content of the metal powder by using the ozone oxidation effect further comprises a cooling circulation system, wherein the cooling circulation system comprises a circulating cooling water pump and a circulating cooling water holding container, and the circulating cooling water pump and the circulating cooling water holding container are sequentially connected through a pipeline and are mutually connected with two ends of an ozone generator; by adopting the structure, the temperature of the ozone generator can be effectively cooled, so that the ozone generator can obtain a more stable ozone source.
Preferably, a gas flowmeter is arranged on a pipeline which is connected with the ozone generator and the ozone adding distributor; through the setting, the ozone introducing amount can be effectively controlled, and the ozone oxygenation efficiency is improved to the greatest extent. The gas flowmeter can be one of a glass rotor flowmeter and a digital display flowmeter.
Preferably, one end of the ozone generator is connected with an air source, and the other end of the ozone generator is connected with an ozone adding distributor.
Preferably, the oxygenation reactor is also provided with a porous filter pipe for discharging gas, and the outlet end of the porous filter pipe is provided with a booster pump; adopt the device can discharge the ozone after the reaction, can also filter the metal powder in the ozone simultaneously, not taken out.
Preferably, the ozone generator is provided with an air source air inlet, and the air source air inlet is provided with an air filter for filtering impurities, dust and the like in air and preventing the metal powder from being influenced; the gas source may be air or oxygen.
The ozone adding distributor is a straight pipe, one end of the pipe is closed, the other end of the pipe is connected with an ozone inlet pipeline, a row of branch pipes are arranged on the straight pipe, and the aperture of each branch pipe is arranged from the end connected with the ozone inlet pipeline to the closed end from small to large (from the end close to the air inlet end to the other end); this setting can guarantee that ozone from each branch pipe is even be full of whole ozone reactor in, realize the more even contact to metal powder, guarantee that the oxidation effect of ozone is better.
The invention also provides a method for increasing the oxygen content of metal powder by using the device for increasing the oxygen content of metal powder by ozone oxidation, which comprises the following steps:
(1) the metal powder is put into an oxygenation reactor and sealed by a sealing cover (the sealing is that the other parts except ozone inlet and outlet are sealed to prevent the powder from contacting with the outside air); an ozone adding distributor and a porous filter pipe are arranged in the oxygenation reactor;
(2) the gas source enters an ozone generator to obtain ozone, and then enters an ozone adding distributor through a pipeline;
(3) conveying ozone by an ozone adding distributor, mixing and contacting with metal powder rolling in a rotary closed oxygenation reactor to generate oxidation reaction, and generating oxide on the surface of metal;
(4) the reacted gas is filtered by a porous filter tube in the oxygenation reactor and then is discharged by a booster pump; and after the reaction time is up, opening a sealing cover of the oxygenation reactor to take out the metal powder after oxygenation.
The metal powder in the step (1) of the invention can be copper, iron, nickel, aluminum, tin, stainless steel and other metal powder or alloy powder thereof, the average particle size of the powder is 0.005 um-100 um (micrometer), and the metal powder can be prepared by a PVD method.
The volume of the oxygenation reactor is 0.005m3～1.0m3The reactor may be heated or not, and the reaction temperature in the reactor is 10-120 deg.c and the metal powder amount is 100-100000 g.
The air source in the step (2) of the invention is air or oxygen, the concentration of the oxygen is 50-99.9% (volume concentration), and the concentration of the ozone generated by the ozone generator by taking the air as the air source is 0.5g/m3～50g/m3The concentration of ozone generated by oxygen as a gas source is 20g/m3～120g/m3。
The rotation speed of the oxygenation reactor in the step (3) is 1-60 rpm (revolutions per minute), the rotation is for rolling and overturning powder, so that the powder is uniformly contacted with ozone in the oxidation process, and the delivery quantity of the ozone is controlled to be 0.1m3/h-3.0m3H; the reaction time in the step (3) is 0.5-5 h. The metal powder with the required increased oxygen content can be obtained by reasonably controlling the concentration of the generated ozone and the continuous reaction time.
The size of the porous filter pipe in the step (4) of the invention is determined according to the volume of the oxygenation reactor, the size of the booster pump can be selected according to the volume of the discharged gas, and the amount of the discharged gas is equal to the flow of the inlet gas, so as to ensure the balance of the internal pressure of the oxygenation reactor.
Advantages and advantageous effects of the invention
1. According to the ozone oxygenation method, special gas is not needed in the metal powder oxygenation process, and air or oxygen is used for producing ozone; the reaction of the invention is an oxidation reaction, has no pollution to air and water environment, and has no generation of other harmful gases; the oxygen increasing can be realized under the condition of normal temperature or heating (the temperature is 10-120 ℃, which is far lower than the oxidation temperature of the traditional metal powder by more than 220 ℃), the process has low energy consumption, more importantly, agglomeration caused by sintering due to high temperature is not easy to generate to the metal powder, the dispersion performance of the powder is good, and the using effect is not influenced.
2. Compared with the traditional methods such as high-temperature oxygenation and the like, the equipment and the ozone oxygenation method have the advantages of simple process, low production cost, easiness in control, low requirement on equipment and strong operability.
3. By controlling the appropriate reaction time and ozone concentration, the invention can effectively control the oxygen content of the metal powder which needs to be increased, and the obtained metal powder can meet the requirements of oxygen content and the use requirement of the metal powder.
Drawings
FIG. 1 is an apparatus for increasing the oxygen content of metal powder by ozone oxidation.
Figure 2 is a schematic structural view of an ozone dosing distributor.
FIG. 3 is a diagram showing the effect of nickel powder with an average particle size of about 0.4um on oxygen enrichment before scraping.
FIG. 4 is a graph showing the effect of scraping the nickel powder with an average particle size of about 0.4um after oxygenation for 1 hour at 210 ℃.
FIG. 5 is a diagram showing the effect of scraping the nickel powder with an average particle size of about 0.4um after oxygenation at 230 ℃ for 1 hour.
FIG. 6 is a diagram showing the effect of scraping the nickel powder with an average particle size of about 0.4um after oxygenation for 1 hour at 260 ℃.
FIG. 7 is a diagram showing the effect of scraping nickel powder with an average particle size of about 0.3um before oxygenation.
FIG. 8 is a diagram of the effect of oxygen enrichment for 3 hours at 23 ℃ of nickel powder with an average particle size of about 0.3 um.
FIG. 9 is a graph of the effect of oxygen enrichment for 3 hours at 50 ℃ of nickel powder with an average particle size of about 0.3 um.
FIG. 10 is a diagram showing the effect of scraping nickel powder with an average particle size of about 0.3um by increasing oxygen at 110 ℃ for 3 hours.
The specific implementation mode is as follows:
the present invention will be described in further detail below by way of examples, but the present invention is not limited to the following examples.
As shown in figure 1: the device for increasing the oxygen content of metal powder by using the ozone oxidation effect comprises an ozone generator 2, an ozone adding distributor 6 and an oxygenation reactor 7; the ozone generator 2 conveys ozone into the ozone adding distributor through a pipeline, the ozone adding distributor is arranged in the oxygenation reactor, and the conveyed ozone is contacted with metal to be oxygenated arranged in the oxygenation reactor; the oxygenation reactor can rotate in the circumferential direction and can heat. The oxygenation reactor described in this embodiment is further provided with a porous filter pipe 8 (a stainless steel porous filter pipe, which can pass gas but cannot pass metal powder) for gas discharge, and the outlet end of the porous filter pipe is provided with a booster pump 9, the gas outlet end of the booster pump 9 is connected with a pipeline to discharge ozone in the oxygenation reactor, so as to realize the balance of ozone in the oxygenation reactor; meanwhile, the metal powder in the ozone can be filtered out and is not taken out.
In addition, the device for increasing the oxygen content of the metal powder by using the ozone oxidation effect further comprises a cooling circulation system, wherein the cooling circulation system comprises a circulating cooling water pump 3 and a circulating cooling water containing container 4 (a circulating cooling water pool is arranged in the embodiment, water is filled in the circulating cooling water pool), the circulating cooling water pump and the circulating cooling water containing container are sequentially connected through pipelines and are mutually connected with two ends of an ozone generator, a water outlet pipe orifice of the specific ozone generator is connected with the cooling water pool, the cooling water pool is connected with an inlet of a cooling water circulation pump, and an outlet of the cooling water circulation pump is connected with a water inlet pipe orifice of the ozone generator; by adopting the structure, the temperature of the ozone generator can be effectively cooled, the generated ozone is prevented from being decomposed, and meanwhile, a more stable ozone source is obtained; the cooling circulation system is characterized in that an interlayer is arranged on the outer wall of the ozone generator, a water inlet and a water outlet are arranged, cooling water enters the interlayer from the water inlet to cool the ozone generator, and is discharged from the water outlet after heat exchange, so that cooling is realized.
In addition, a gas flowmeter 5 is arranged on a pipeline which is connected with the ozone generator and the ozone adding distributor; through the setting, the ozone introducing amount can be effectively controlled, and the ozone oxygenation efficiency is improved to the greatest extent. The gas flowmeter can be one of a glass rotor flowmeter and a digital display flowmeter, and is a flowmeter conventionally used in the industry.
In the embodiment, one end of the ozone generator 2 is connected with an air source, and the other end of the ozone generator is connected with an ozone adding distributor.
The ozone generator is provided with an air source air inlet, the air source air inlet is provided with an air filter 1, impurities, dust and the like in air are filtered, and the influence on metal powder is prevented; the gas source may be air or oxygen.
The ozone adding distributor is a straight pipe, one end of the pipe is closed, the other end of the pipe is connected with an ozone inlet pipeline, a row of branch pipes are arranged on the straight pipe, and the aperture of each branch pipe is arranged from the end connected with the ozone inlet pipeline to the closed end from small to large (from the end close to the air inlet end to the other end); the arrangement can ensure that ozone is uniformly filled in the whole ozone reactor from each branch pipe, and if the branch pipes with the same aperture are arranged, the ozone directly flows out from the branch pipe closest to the inlet channel, so that the ozone is not uniformly distributed, and the oxidation effect of the metal powder is influenced; the gradually increased aperture can effectively balance the outflow of ozone, so that the flow of each branch pipe is basically balanced, the metal powder is more uniformly contacted, and the better oxidation effect of ozone is ensured; the specific figure is as shown in figure 2: comprises a straight pipe, the straight pipe extends from one end of the oxygenation reactor 7 to the other end, but a certain clearance is formed between the straight pipe and the other end, so that the straight pipe is prevented from rubbing the inner wall of the oxygenation reactor 7 in the rotation process; the oxygenation reactor can rotate in the circumferential direction, the ozone adding distributor does not need to rotate, and the porous filter does not need to rotate; the powder continuously rolls through the rotation of the oxygenation reactor, so that the powder is fully contacted with ozone coming from a straight pipe on the ozone adding distributor; in addition, the branch pipes on the ozone adding distributor can be linearly arranged in a row along the extension direction of the straight pipe, and also can be arranged on the pipe body in a staggered and irregular manner; in addition, the ozone adding distributor can extend along the direction which is mutually overlapped with the axial direction of the oxygenation reactor, thereby ensuring the uniform dispersion of gas.
The heating mode of the oxygenation reactor can be one of an oven and an electric heating furnace.
The oxygenation reactor can adopt a cylindrical stainless steel cylindrical barrel and is transversely arranged, and the ozone adding distributor is axially arranged in the stainless steel cylindrical barrel and positioned on the central shaft of the stainless steel cylindrical barrel; the ozone adding distributor is a stainless steel straight pipe, one end of the stainless steel straight pipe is fixed on one transverse end face of the stainless steel cylindrical barrel and is communicated with a pipeline for entering ozone, the other end of the stainless steel straight pipe is closed, a row of branch pipes with different apertures are arranged on the straight pipe, the ozone can conveniently enter, and the apertures of the branch pipes are gradually increased from the fixed end to the closed section; the circumferential rotation of the oxygenation reactor can adopt an industry conventional rotating structure, such as the driving of a motor output shaft through gear transmission or the driving of a belt pulley and the like; the end face of one end of the oxygenation reactor, which is provided with the ozone adding distributor and the porous filter pipe, is not rotated, and only the cylinder rotates.
Ozone generator(O3) Is oxygen (O)2) Is a light blue gas with a particular odor. The molecular structure is triangular, the bond angle is 116 degrees, the density is 1.5 times of oxygen, and the solubility in water is 10 times of oxygen. Ozone is a strong oxidant, second only to fluorine in its redox potential. The reaction path is two: firstly, ozone directly participates in the reaction through nucleophilic or electrophilic action; secondly, ozone reacts with pollutants through active free radicals, mainly OH, under the action of factors such as alkali and the like.
The ozone generator is used for producing ozone gas (O)3) The apparatus of (1). Ozone is easy to decompose and cannot be stored, and the ozone needs to be prepared on site for use (the ozone can be stored for a short time under special conditions), so that an ozone generator is needed to be used in all places where the ozone can be used. The high-pressure ionization (or chemical and photochemical reaction) is utilized to decompose and polymerize partial oxygen in the air into ozone, which is the allotropic transformation process of oxygen; can also be obtained by water electrolysis. The classification of ozone generators is divided according to the mode of ozone generation, and the ozone generators mainly have three types: the first is a high-voltage discharge type, the second is an ultraviolet irradiation type, and the third is an electrolysis type. The ozone concentration is an important index for measuring the technical content and the performance of the ozone generator, and the concentration of the ozone is mixed gas and is usually expressed by mass ratio and volume ratio. The mass ratio is the mass of ozone contained in the mixed gas in unit volume, and the unit of ozone is commonly mg/L, mg/m3Or g/m3Etc. The volume ratio refers to the volume content or percentage content of ozone in a unit volume, and the percentage is expressed as 2%, 5%, 12% and the like. The ozone generator equipment manufacturers used in this test are: ozone generators sold by Qingdao Zhongkuan ozone purification plant Co.
The usage models correspond to the following:
(1) the ozone concentration is 15-30 g/h, and the use types are as follows: OZ-20 g ozone tube, the specification is shown in Table 1:
TABLE 1
| Model number | Ozone concentration (mg/L) | Product size (Length diameter height mm) | Cooling method |
| OZ-20 | 15～30 | 310*60*140 | Free selection of air cooling and water cooling |
(2) The ozone concentration is 50g/h, and the use types are as follows: OZ-50 g ozone tube, the specification is shown in Table 2:
TABLE 2
| Model number | Ozone concentration (mg/L) | Product size (Length diameter height mm) | Cooling method |
| OZ-50 | 30～30 | 610*60*140 | Free selection of air cooling and water cooling |
(3) The ozone concentration is 80g/h, and the use types are as follows: OZ-100 g ozone tube, the specification is shown in Table 3:
TABLE 3
| Model number | Ozone concentration (mg/L) | Product size (Length diameter height mm) | Cooling method |
| OZ-100 | 15～30 | 810*60*140 | Free selection of air cooling and water cooling |
Example 1:
the nickel powder is treated by adopting the treatment method for increasing the oxygen content of the metal powder by ozone oxidation, and the specific operation steps are as follows:
(1) taking metal nickel powder with the average particle size of 0.3-0.4 um (micrometer) produced by a PVD method, placing the metal nickel powder in a rotatable and sealable stainless steel cylindrical barrel (an oxygenation reactor) with the diameter of 50kg, the length of 1500mm and the volume of 0.3m3An ozone adding distributor and a porous filter pipe are arranged in the barrel body.
(2) Starting the circumferential rotation of the stainless steel cylindrical barrel body, wherein the rotation speed is 10rpm (revolutions per minute);
(3) and starting an ozone generator (OZ-50 g ozone tube) to generate ozone with the concentration of 30g/m3The air source is air;
(4) starting a booster pump, and adjusting the air flow in the step (3) to be 2.2-2.5m3The continuous air inlet time is about 1-5 h;
(5) stopping the steps (2), (3) and (4), and sampling to measure the oxygen content.
Table 4 shows the ozone oxidation effect data at the same temperature and different time
Example 2
(1) Taking metal nickel powder with the average particle size of 0.3-0.4 um produced by a PVD method, and placing the metal nickel powder in a rotatable and sealable stainless steel cylindrical barrel with the diameter of 500mm, the length of about 1500mm and the volume of about 0.3m by 50kg3An ozone adding distributor and a perforated pipe are arranged in the barrel body.
(2) Starting a heating system in the step (1), and heating the stainless steel barrel to 50-110 ℃;
(3) starting the barrel body in the step (1) to rotate circumferentially at a speed of 10rpm (revolutions per minute);
(4) starting an ozone generator (OZ-50 g ozone tube) in the step (2) to generate ozone with the concentration of 30g/m3The air source is air;
(5) starting a booster pump, and adjusting the air flow in the step (3) to be 2.2-2.5m3H, the continuous air inlet time is about 3 h;
(6) stopping the steps (2), (3), (4) and (5), and sampling to measure the oxygen content.
Table 5 shows the ozone oxidation effect data at different temperatures and at the same time
Example 3
(1) Taking metal nickel powder with the average particle size of 0.3-0.4 um produced by a PVD method, placing the metal nickel powder in a rotatable and airtight stainless steel cylindrical barrel of 50kg, wherein the stainless steel barrel is straightDiameter of 500mm, length of 1500mm, and volume of 0.3m3An ozone adding distributor and a perforated pipe are arranged in the barrel body.
(2) Starting the barrel body in the step (1) to rotate circumferentially at a speed of 10rpm (revolutions per minute);
(3) starting an ozone generator (OZ-20 g of ozone tube OZ-50 g of ozone tube or OZ-100 g of ozone tube) in the step (2) to generate ozone with the concentration of 30g/m3The air source is air;
(4) starting a booster pump, and adjusting the air flow in the step (3) to be 0.8-6.0 m3H, the continuous air inlet time is about 3 h;
(5) stopping the steps (2), (3) and (4), and sampling to measure the oxygen content.
Table 6 shows the ozone oxidation effect data of different ozone concentrations at the same time and temperature
From tables 4, 5 and 6, it can be seen that the method of the present invention has a significant effect on the ozone oxidation of nickel powder produced by PVD method.
As can be seen from table 4, at the same temperature, the percentage of oxygen content increased with time, and the magnitude of the change in the percentage of increase in oxygen content decreased when the time reached a certain degree.
As can be seen from Table 5, when ozonation was carried out at the same time, the percentage increase in oxygen content was insignificant with increasing temperature, indicating that ozonation was less affected by temperature.
As can be seen from Table 6, the amount of ozone has a large influence on the oxidation of ozone in different unit times at the same temperature and the amount of oxygen increases more remarkably as the amount of ozone increases.
The method is characterized in that whether the dispersibility of the nickel powder after oxygenation is influenced or not is generally performed by scraping the sample before and after oxygenation, and the sample is checked by a method for comparing the scraping effect; the smoother the pulp scraping effect is, the less the surface powder agglomerates are, and the better the dispersity is; conversely, the poorer the dispersibility. By utilizing the high-temperature oxidation effect, the oxygen content of the nickel powder is increased by heating the nickel powder in the air, and the scraping effect of the sample is compared, as shown in the attached figures 3-6: is a comparison of the scraping effect of nickel powder with average particle size of about 0.4um after oxygenation for 1 hour at different temperatures, which is illustrated by the results shown in the attached figures 3-4: with the increase of the heating temperature, the sample scraping effect is poorer, namely the dispersity is poorer. As shown in the attached figures 7-10, the scraping effect of nickel powder with an average particle size of about 0.3um after different oxygen increasing time is compared, and can be seen from the attached figures: with the increase of the heating temperature, the change of the sample scraping effect is not obvious, namely the dispersion change is small and the dispersion is good.
The results from the samples of the above examples show: the method for increasing the oxygen content of the nickel powder by ozone oxidation is completely effective and easy to control, and the ozone oxidation process has the advantages of stable production, simple operation, no pollution, controllable oxygen content amplification and the like, and has feasibility.
Claims (9)
1. A device for increasing the oxygen content of metal powder by using ozone oxidation is characterized in that: the device comprises an ozone generator, an ozone adding distributor and an oxygenation reactor; the ozone generator conveys ozone into the ozone adding distributor through a pipeline, the ozone adding distributor is arranged in the oxygenation reactor, and the conveyed ozone is contacted with metal to be oxygenated arranged in the oxygenation reactor; the oxygenation reactor can rotate in the circumferential direction and can heat, the ozone adding distributor is a straight pipe, one end of the pipe is closed, the other end of the pipe is connected with an ozone inlet pipeline, a row of branch pipes are arranged on the straight pipe, and the aperture of each branch pipe is arranged from the end connected with the ozone inlet pipeline to the closed end in a gradually-increasing mode.
2. The apparatus for increasing oxygen content of metal powder using ozone oxidation as claimed in claim 1, wherein: the ozone generator is characterized by further comprising a cooling circulation system, wherein the cooling circulation system comprises a circulating cooling water pump and a circulating cooling water containing container, and the circulating cooling water pump and the circulating cooling water containing container are sequentially connected through a pipeline and are mutually connected with the two ends of the ozone generator.
3. The apparatus for increasing oxygen content of metal powder using ozone oxidation as claimed in claim 1, wherein: a gas flowmeter is arranged on a pipeline which is connected with the ozone generator and the ozone adding distributor; the gas flowmeter is one of a glass rotor flowmeter and a digital display flowmeter.
4. The apparatus for increasing oxygen content of metal powder using ozone oxidation as claimed in claim 1, wherein: one end of the ozone generator is connected with the air source, and the other end of the ozone generator is connected with the ozone adding distributor.
5. The apparatus for increasing oxygen content of metal powder using ozone oxidation as claimed in claim 1, wherein: the oxygenation reactor is also provided with a porous filter pipe for discharging gas, and the outlet end of the porous filter pipe is provided with a booster pump.
6. The apparatus for increasing oxygen content of metal powder using ozone oxidation as claimed in claim 1, wherein: the ozone generator is provided with an air source air inlet, and the air source air inlet is provided with an air filter.
7. A method of increasing the oxygen content of a metal powder, comprising: an apparatus for increasing the oxygen content of metal powder by ozone oxidation according to any one of claims 1 to 6 is applied, the method comprising the steps of:
(1) filling metal powder into the oxygenation reactor, and sealing by a sealing cover; an ozone adding distributor and a porous filter pipe are arranged in the oxygenation reactor;
(2) the gas source enters an ozone generator to obtain ozone, and then enters an ozone adding distributor through a pipeline;
(3) conveying ozone by an ozone adding distributor, mixing and contacting with metal powder rolling in a rotary closed oxygenation reactor to generate oxidation reaction, and generating oxide on the surface of metal;
(4) the reacted gas is filtered by a porous filter tube in the oxygenation reactor and then is discharged by a booster pump; and after the reaction time is up, opening a sealing cover of the oxygenation reactor to take out the metal powder after oxygenation.
8. The method of claim 7, wherein the oxygen content of the metal powder is increased by: the metal powder in the step (1) is copper, iron, nickel, aluminum, tin, stainless steel metal powder or alloy powder thereof, and the average particle size of the powder is 0.005-100 um; the air source in the step (2) is air or oxygen, the concentration of the oxygen is 50 to 99.9 percent, and the concentration of ozone generated by the ozone generator by taking the air as the air source is 0.5g/m3～50g/m3The concentration of ozone generated by oxygen as a gas source is 20g/m3～120g/m3(ii) a The rotating speed of the oxygenation reactor in the step (3) is 1-60 rpm, and the conveying amount of ozone is controlled to be 0.1m3/h-3.0m3And h, wherein the reaction time in the step (4) is 0.5-5 h.
9. The method of claim 7, wherein the oxygen content of the metal powder is increased by: the volume of the oxygenation reactor is 0.005m3～1.0m3The heating temperature of the oxygenation reactor is 10-120 ℃, and the powder adding amount of the metal powder in the oxygenation reactor is 100-100000 g.
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| CN113506648B (en) * | 2021-09-10 | 2021-12-21 | 西安宏星电子浆料科技股份有限公司 | Inner-layer gold conductor paste for Ca-B-Si system LTCC |
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