CN116199218B - Surface cerium oxide coating method of micron diamond particles - Google Patents
Surface cerium oxide coating method of micron diamond particles Download PDFInfo
- Publication number
- CN116199218B CN116199218B CN202310213929.1A CN202310213929A CN116199218B CN 116199218 B CN116199218 B CN 116199218B CN 202310213929 A CN202310213929 A CN 202310213929A CN 116199218 B CN116199218 B CN 116199218B
- Authority
- CN
- China
- Prior art keywords
- diamond particles
- cecl
- thermal decomposition
- ethanol
- coated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000010432 diamond Substances 0.000 title claims abstract description 148
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 148
- 239000002245 particle Substances 0.000 title claims abstract description 147
- 238000000576 coating method Methods 0.000 title claims abstract description 33
- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 19
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 144
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000012047 saturated solution Substances 0.000 claims abstract description 11
- 238000009423 ventilation Methods 0.000 claims abstract description 9
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 239000011248 coating agent Substances 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000007747 plating Methods 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000012466 permeate Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002905 metal composite material Substances 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/008—Pyrolysis reactions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/035—Preparation of hydrogen chloride from chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a surface cerium oxide coating method of micron diamond particles, and belongs to the field of diamond particle surface treatment. The method of the invention comprises the following steps: ceCl is added 3 And placing the pretreated diamond into ethanol for magnetic stirring to obtain CeCl containing diamond particles 3 Ethanol saturated solution; placing the mixture into a low-temperature incubator, reducing the temperature to-50 to-100 ℃ and magnetically stirring the mixture, and CeCl 3 The solubility in ultra-low temperature ethanol is greatly reduced and the diamond particles are crystallized and separated out on the surface, and then the ultra-low temperature ethanol is filtered and separated to obtain the CeCl coated on the surface 3 Diamond particles of the film, ceCl obtained 3 The film-coated diamond particles undergo thermal decomposition. The invention uses CeCl 3 The diamond particles coated by the film are loosely arranged in a ventilation vessel and fully contacted with flowing water vapor and oxygen, so that the thermal decomposition reaction is more efficient; the invention has the characteristics of simple process, low cost, high efficiency and environmental protection, and can realize industrialized application.
Description
Technical Field
The invention discloses a surface cerium oxide coating method of micron diamond particles, and belongs to the field of diamond particle surface treatment.
Background
Diamond particles are of great interest because of their high hardness, modulus of elasticity, low coefficient of thermal expansion, good thermal conductivity, etc. At present, the diamond/metal composite material is widely applied to the fields of high-rigidity structural materials, thermal management and the like. However, during the preparation and use of the composite, diamond may chemically react with the matrix metal, thereby degrading the performance and stability of the composite. Cerium oxide is a preferred plating material for diamond surface passivation treatment because of its low free energy of formation and its stable structure under different environments. By plating cerium oxide on the surfaces of the diamond particles, the surfaces of the diamond particles are passivated, so that the stability, the performance and the service life of the diamond/metal composite material are effectively improved.
Currently, the surface passivation treatment of diamond particles is an alternative chemical vapor deposition method and a pulse laser deposition method. The chemical vapor deposition method is a chemical process that gaseous substances generate solid substances through chemical reaction and deposit on the surface of a substrate, and has the advantages that the uniformity degree of a film is high, but the operation temperature of the method is too high, and the method is generally carried out at 850-1100 ℃, so that the diamond is easy to change phase (the temperature of the diamond for starting phase change in air is 850 ℃, and the temperature for starting phase change in vacuum or inert atmosphere is 1500 ℃); the pulse laser deposition method is to make the material in the irradiated area ablate by laser projected onto the target, the ablated material is preferentially transmitted along the normal direction of the target, and finally deposited on the surface of the matrix.
Disclosure of Invention
The invention aims to provide a method for coating surface cerium oxide of micron diamond particles, which comprises the steps of coating CeCl containing diamond particles 3 The temperature of the ethanol saturated solution is reduced to the ultralow temperature of minus 50 ℃ to minus 100 ℃ to lead CeCl 3 The solubility in ethanol is greatly reduced and the diamond particles are crystallized and separated out on the surface, then the mixture is filtered and separated at ultralow temperature, and then the CeCl obtained after separation 3 The diamond particles coated by the film are put into a thermal decomposition cavity (figure 3) in a thermal decomposition device to carry out thermal decomposition reaction, and finally CeO is obtained 2 Coated diamond particles. First, ceCl 3 The coating process of the diamond particles fully utilizes the physical property of low solidifying point (-114.1 ℃) of the ethanol, and CeCl in the ethanol is reduced to ultralow temperature (-50 ℃ to minus 100 ℃) 3 High-proportion precipitation on the surface of diamond particles to make CeCl 3 Fully utilizes and saves raw materials; next, in the course of carrying out the thermal decomposition reaction in the thermal decomposition device, ceCl of the present invention 3 Film coated diamond particle pineThe catalyst is arranged in a ventilation vessel and fully contacted with flowing water vapor and oxygen, so that the thermal decomposition reaction is more efficient; finally, HCl gas generated by the thermal decomposition reaction can be recovered in a water tank. Therefore, the invention has the characteristics of simple process, low cost, high efficiency and environmental protection, and can realize industrialized application.
The aim of the invention is achieved by the following technical scheme:
the surface cerium oxide coating method of the micron diamond particles specifically comprises the following steps:
(1) According to the mass of diamond particles: cerium chloride mass: ethanol mass= (20-26): (90-96): 100 ratio stock, ceCl 3 And adding the pretreated diamond particles into ethanol, and magnetically stirring (preferably for 15 minutes) to obtain CeCl containing diamond particles 3 Saturated solution of ethanol.
(2) Placing the mixture in a low-temperature incubator, reducing the temperature to-50 to-100 ℃ and magnetically stirring (preferably 20-40 min), ceCl 3 The solubility in ultra-low temperature ethanol is greatly reduced and the diamond particles are crystallized and separated out on the surface, and then the ultra-low temperature ethanol is filtered and separated to obtain the CeCl coated on the surface 3 Diamond particles of the film, ceCl obtained 3 The diamond particles coated by the film are thermally decomposed to obtain CeO 2 Film coated diamond particles.
The pretreatment process of the diamond particles comprises the following steps: the diamond particles are respectively immersed into 2mol/L hydrochloric acid and 1mol/L sodium hydroxide solution for magnetic stirring, repeatedly washed to be neutral by deionized water, and then placed into a drying oven for drying for standby.
Preferably, the micron diamond particles of the present invention have a particle size of 1-100 μm.
Preferably, the device for thermal decomposition comprises a dropper 1, a drip 2, a thermal decomposition cavity 3, a gas-permeable dish 5, a water tank 6, a thermocouple 7 and a resistance furnace 8, wherein the thermal decomposition cavity 3 is arranged in the resistance furnace 8, the gas-permeable dish 5 is fixed in the middle of the thermal decomposition cavity 3, the top of the thermal decomposition cavity 3 is communicated with the water tank 6 through a pipeline, the bottom of the thermal decomposition cavity 3 is communicated with the drip 2 above the thermal decomposition cavity 3 through a pipeline, the dropper 1 is arranged above the drip 2, and the thermocouple is arranged at the bottom of the resistance furnace 8.
Preferably, the CeCl of the invention 3 The specific process of thermally decomposing the film-coated diamond particles is as follows: ceCl is added 3 The coated diamond particles are placed into a thermal decomposition chamber 3 in a thermal decomposition device to be heated to 700-800 ℃, then dripped into a drip tank 2 by a dropper 1, heated by a resistance furnace 8, the dripped water is converted into water vapor, and the flowing water vapor and oxygen penetrate a ventilation dish 5 and CeCl 3 The coated diamond particles are fully contacted to enable CeCl 3 High-efficiency thermal decomposition is carried out for 30-60min to obtain CeO 2 The membrane-coated diamond particles are simultaneously recycled by passing the HCl gas produced into a water tank 6.
Principles of the invention
1. Ultralow temperature crystallization cerium chloride plating principle
By reacting CeCl at room temperature 3 And adding the pretreated diamond particles into ethanol (freezing point-114.1 ℃) to obtain CeCl containing diamond particles 3 Saturated solution of ethanol. FIG. 1 shows the measured CeCl 3 As can be seen from FIG. 1, ceCl has a temperature dependence of solubility in ethanol 3 There was a large difference in solubility in ethanol at room temperature (20 ℃ -30 ℃) and-100 ℃, so CeCl was selected at room temperature (20 ℃ -30 ℃) 3 Dissolving in ethanol, wherein the preferable cooling range is-50 ℃ to-100 ℃; ceCl 3 The solubility in ultra-low temperature ethanol is greatly reduced and the diamond particles are crystallized and separated out, and then the CeCl is obtained by filtering and separating at ultra-low temperature 3 Film coated diamond particles.
2、CeCl 3 Working principle of thermal decomposition device and selection of thermal decomposition temperature and time
(1)CeCl 3 The working principle of the thermal decomposition device is as follows: the CeCl obtained 3 The diamond particles 4 coated by the film are put into a thermal decomposition cavity 3 in a thermal decomposition device, then drip water in a drip tank 2 by a dropper 1, heat the water through a resistance furnace 8, convert the water drop into water vapor, and CeCl under the action of the water vapor and oxygen 3 Thermal decomposition is carried out to obtain CeO 2 Film-coated diamond particles, while being producedHCl gas is introduced into the water tank 6 for recovery; in the process of carrying out thermal decomposition reaction in the thermal decomposition device, the CeCl of the invention 3 The diamond particles coated by the film are loosely arranged in a ventilation vessel and fully contacted with flowing water vapor and oxygen, so that the thermal decomposition reaction is more efficient; HCl gas generated by the thermal decomposition reaction can be recycled in a water tank, so that the method has the characteristics of simple process, low cost, high efficiency and environmental protection, and can realize industrial application.
(2)CeCl 3 Selection of thermal decomposition temperature and time
CeCl at 445 degree C 3 The CeO is generated after the CeO is fully contacted with flowing water vapor and oxygen 2 And HCl gas to 700℃ CeCl 3 The decomposition is complete; ceCl for coating diamond particle surface 3 Completely decompose into CeO 2 The invention uses high-efficiency thermal decomposition device (figure 3), the selected decomposition temperature range is 700-800 deg.C, and the decomposition time is 30-60min.
3. Cerium oxide coating layer thickness control principle
According to the mass of diamond particles: cerium chloride mass: ethanol mass= (20-26): (90-96): 100 ratio diamond particles and CeCl 3 Adding into ethanol, and controlling CeCl containing diamond particles 3 The temperature of the ethanol saturated solution is reduced to enable CeCl 3 The solubility in the ultra-low temperature ethanol is reduced, and then the diamond particles are crystallized and separated out on the surface; according to CeCl in FIG. 1 3 The CeCl can be calculated by fitting the curve of the solubility in ethanol along with the temperature change and the fitting formula (1) 3 Solubility R in ethanol at normal and ultra-low temperatures T ：
(1) Wherein, T is the temperature, DEG C; r is R T —CeCl 3 Solubility in ethanol at T ℃, g/100g ethanol.
CeCl according to formula (1) 3 The difference between the solubility in ethanol at normal temperature and ultra-low temperature can obtain CeCl 3 Mass M of precipitation on diamond particle surface 1 ：
M 1 ＝R T1 -R T2 (2)
In the formula (2), M 1 —CeCl 3 The mass of precipitation on the surface of diamond particles is g/100g ethanol; r is R T1 —CeCl 3 At normal temperature T 1 Solubility in ethanol, g/100g ethanol; r is R T2 —CeCl 3 At ultra-low temperature T 2 Solubility in ethanol, g/100g ethanol.
CeCl 3 The chemical equation for the thermal decomposition reaction is as follows:
CeCl according to formula (2) and (3) 3 With CeO 2 The ratio of the relative molecular masses of (C) to obtain CeCl 3 CeO obtained by thermal decomposition 2 Mass M 2 ：
M 2 ＝0.70(R T1 -R T2 ) (4)
In the formula (4), M 2 —CeCl 3 CeO obtained after thermal decomposition reaction 2 Mass, g/100g ethanol; r is R T1 —CeCl 3 At normal temperature T 1 Solubility in ethanol, g/100g ethanol; r is R T2 —CeCl 3 At ultra-low temperature T 2 Solubility in ethanol, g/100g ethanol.
The calculation formula of the surface area of the diamond particles can be obtained according to the density formula, the particle size and the mass of the diamond particles:
in the formula (5), the surface area of the S-diamond particles is cm 2 ；ρ 1 -goldDensity of diamond particles, g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the m-mass of diamond particles, g/100g ethanol; r-particle diameter of diamond particles, μm.
According to the mass of diamond particles: cerium chloride mass: ethanol mass= (20-26): (90-96): 100 in combination with formulae (1), (2), (4) and (5), ceCl can be deduced 3 Thickness calculation formula (6) and CeO 2 Thickness calculation formula (7):
in the formula (6) and (7),—CeCl 3 average thickness of the plating layer, μm; />—CeO 2 Average thickness of the plating layer, μm; s-surface area of diamond particles, cm 2 ；M 2 —CeO 2 The mass of the coating is g/100g ethanol; ρ 1 Density of diamond particles, g/cm 3 ；ρ 2 —CeCl 3 Density (3.97 g/cm) 3 )；ρ 3 —CeO 2 Density (7.13 g/cm) 3 ) The method comprises the steps of carrying out a first treatment on the surface of the m-mass of diamond particles, g/100g ethanol; r-particle diameter of diamond particles, μm; r is R T1 —CeCl 3 At normal temperature T 1 Solubility in ethanol, g/100g ethanol; r is R T2 —CeCl 3 At ultra-low temperature T 2 Solubility in ethanol, g/100g ethanol.
The invention aims to provide a method for coating surface cerium oxide of micron diamond particles, which comprises the steps of coating CeCl containing diamond particles 3 The temperature of the ethanol saturated solution is reduced to the ultralow temperature of minus 50 ℃ to minus 100 ℃ to lead CeCl 3 High solubility in ethanolThe amplitude is reduced, crystallization is separated out on the surface of diamond particles, then filtration and separation are carried out at ultralow temperature, and then CeCl obtained after separation is carried out 3 The diamond particles coated by the film are put into a thermal decomposition cavity (figure 3) in a thermal decomposition device to carry out thermal decomposition reaction, and finally CeO is obtained 2 Coated diamond particles. First, ceCl 3 The coating process of the diamond particles fully utilizes the physical property of low solidifying point (-114.1 ℃) of the ethanol, and CeCl in the ethanol is reduced to ultralow temperature (-50 ℃ to minus 100 ℃) 3 High-proportion precipitation on the surface of diamond particles to make CeCl 3 Fully utilizes and saves raw materials; next, in the course of carrying out the thermal decomposition reaction in the thermal decomposition device, ceCl of the present invention 3 The diamond particles coated by the film are loosely arranged in a ventilation vessel and fully contacted with flowing water vapor and oxygen, so that the thermal decomposition reaction is more efficient; finally, HCl gas generated by the thermal decomposition reaction can be recovered in a water tank; therefore, the invention has the characteristics of simple process, low cost, high efficiency and environmental protection, and can realize industrialized application.
Drawings
FIG. 1CeCl 3 Solubility in ethanol versus temperature.
Fig. 2 is a process flow diagram of the coating of cerium oxide on the surface of diamond particles.
FIG. 3CeCl 3 Thermal exploded device view, fig. 3: 1-a dropper; 2-a drip; 3-a thermal decomposition chamber; 4-CeC1 3 Coated diamond particles; 5-breathable dishes; 6-a water tank; 7-thermocouple; 8-resistance furnace.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific embodiments, but the scope of the invention is not limited to the description.
Example 1
The surface cerium oxide coating method of the micron diamond particles is characterized by comprising the following steps of:
(1) Pretreatment of raw materials: the commercial artificial diamond particles with the particle size of 1 μm are respectively immersed into hydrochloric acid (2 mol/L) and sodium hydroxide (1 mol/L) solution for magnetic stirring, repeatedly washed to be neutral by deionized water, and then placed in a drying oven for drying for standby.
(2) A mixed solution was obtained: according to the mass of the diamond particles: the mass of cerium chloride: mass of ethanol = 26:90:100, diamond particles and CeCl at room temperature (20 ℃) 3 Adding into ethanol, magnetically stirring for 15 min to obtain CeCl containing diamond particles 3 Saturated solution of ethanol.
(3)CeCl 3 Coating diamond particles: ceCl containing diamond particles obtained in the step (2) 3 Placing the saturated ethanol solution into a low-temperature incubator, and magnetically stirring for 40min after the temperature is reduced to-50deg.C to obtain CeCl 3 The solubility in ultra-low temperature ethanol is greatly reduced, and the diamond particles are crystallized and separated out on the surface, and then the ultra-low temperature is filtered and separated to obtain the CeCl with the thickness of 0.2 mu m 3 Film coated diamond particles.
(4)CeO 2 Coating diamond particles: ceCl obtained in the step (3) 3 The diamond particles 4 coated with the film are put into a thermal decomposition chamber 3 of a thermal decomposition device to be heated to 700 ℃, then drip water in a drip tank 2 by a dropper 1, and are heated by a resistance furnace 8, the water drops are converted into water vapor, and the flowing water vapor and oxygen penetrate a ventilation dish 5 and CeCl 3 The coated diamond particles are fully contacted to enable CeCl 3 High-efficiency thermal decomposition is carried out for 60min to obtain CeO with thickness of 0.1 μm 2 The membrane-coated diamond particles are recycled by passing the HCl gas produced into a water tank 6.
Example 2
The surface cerium oxide coating method of the micron diamond particles is characterized by comprising the following steps of:
(1) Pretreatment of raw materials: diamond particles with the grain size of 40 mu m sold in the market are respectively immersed into hydrochloric acid (2 mol/L) and sodium hydroxide (1 mol/L) solution for magnetic stirring, repeatedly washed to be neutral by deionized water, and then placed in a drying oven for drying for standby.
(2) A mixed solution was obtained: according to the mass of the diamond particles: the mass of cerium chloride: mass of ethanol = 24:92:100 ratio ofPreparing materials, diamond particles and CeCl at room temperature (23 ℃), and 3 adding into ethanol, magnetically stirring for 15 min to obtain CeCl containing diamond particles 3 Saturated solution of ethanol.
(3)CeCl 3 Coating diamond particles: ceCl containing diamond particles obtained in the step (2) 3 Placing the saturated ethanol solution into a low-temperature incubator, and magnetically stirring for 34 min after the temperature is reduced to-65deg.C to obtain CeCl 3 The solubility in ultra-low temperature ethanol is greatly reduced, and the diamond particles are crystallized and separated out on the surface, and then the ultra-low temperature is filtered and separated to obtain the CeCl with the thickness of 11.9 mu m 3 Film coated diamond particles.
(4)CeO 2 Coating diamond particles: coating the CeCl obtained in the step (3) 3 The diamond particles 4 of the film are placed in a thermal decomposition chamber 3 of a thermal decomposition device and heated to 735 ℃, then dripped in a drip tank 2 by a dropper 1, heated by a resistance furnace 8, the dripped water is converted into water vapor, and the flowing water vapor and oxygen permeate through a gas permeation dish 5 and CeCl 3 The coated diamond particles are fully contacted to enable CeCl 3 High-efficiency thermal decomposition is carried out for 50min to obtain CeO with thickness of 4.6 μm 2 The membrane-coated diamond particles are simultaneously recycled by passing the HCl gas produced into the water tank 6.
Example 3
The surface cerium oxide coating method of the micron diamond particles is characterized by comprising the following steps of:
(1) Pretreatment of raw materials: diamond particles with the grain size of 70 mu m sold in the market are respectively immersed into hydrochloric acid (2 mol/L) and sodium hydroxide (1 mol/L) solution for magnetic stirring, repeatedly washed to be neutral by deionized water, and then placed in a drying oven for drying for standby.
(2) A mixed solution was obtained: according to the mass of the diamond particles: the mass of cerium chloride: mass of ethanol = 22:94:100 ratio preparation diamond particles and CeCl at room temperature (26 ℃) 3 Adding into ethanol and magnetically stirring for 15 min to obtain CeCl containing diamond particles 3 Saturated solution of ethanol.
(3)CeCl 3 Coating diamond particles: placing the mixed solution obtained in the step (2) into a low-temperature constant-temperature box, and then magnetically stirring for 27 minutes after the temperature is reduced to the ultralow temperature of-85 ℃ to enable CeCl 3 The solubility in ultra-low temperature ethanol is greatly reduced, and the diamond particles are crystallized and separated out on the surface, and then the ultra-low temperature is filtered and separated to obtain the CeCl with the thickness of 31.3 mu m 3 Film coated diamond particles.
(4)CeO 2 Coating diamond particles: coating the CeCl obtained in the step (3) 3 The diamond particles 4 of the film are placed in a thermal decomposition chamber 3 of a thermal decomposition device and heated to 770 ℃, then dripped into a drip tank 2 by a dropper 1, heated by a resistance furnace 8, the dripped water is converted into water vapor, and the flowing water vapor and oxygen permeate through a gas permeation dish 5 and CeCl 3 The coated diamond particles are fully contacted to enable CeCl 3 High-efficiency thermal decomposition is carried out for 40min to obtain CeO with the thickness of 12.0 μm 2 The membrane-coated diamond particles are simultaneously recycled by passing the HCl gas produced into the water tank 6.
Example 4
The surface cerium oxide coating method of the micron diamond particles is characterized by comprising the following steps of:
(1) Pretreatment of raw materials: diamond particles with the grain size of 100 mu m sold in the market are respectively immersed into hydrochloric acid (2 mol/L) and sodium hydroxide (1 mol/L) solution for magnetic stirring, repeatedly washed to be neutral by deionized water, and then placed in a drying oven for drying for standby.
(2) A mixed solution was obtained: according to the mass of the diamond particles: the mass of cerium chloride: mass of ethanol = 20:96:100 ratio stock, diamond particles and CeCl were mixed at room temperature (30 ℃) 3 Adding into ethanol and magnetically stirring for 15 min to obtain CeCl containing diamond particles 3 Saturated solution of ethanol.
(3)CeCl 3 Coating diamond particles: placing the mixed solution obtained in the step (2) into a low-temperature constant-temperature box, and then magnetically stirring for 20 minutes after the temperature is reduced to the ultralow temperature of minus 100 ℃ to enable CeCl to be obtained 3 The solubility in ultra-low temperature ethanol is greatly reduced and the diamond particles are crystallized and separated out on the surfaceFiltering at ultralow temperature, separating to obtain CeCl with thickness of 60.8 μm 3 Film coated diamond particles.
(4)CeO 2 Coating diamond particles: coating the CeCl obtained in the step (3) 3 The diamond particles 4 of the film are placed in a thermal decomposition chamber 3 of a thermal decomposition device and heated to 800 ℃, then dripped into a drip tank 2 by a dropper 1, heated by a resistance furnace 8, and the flowing water vapor and oxygen permeate through a gas permeation dish 5 and CeCl 3 The coated diamond particles are fully contacted to enable CeCl 3 High-efficiency thermal decomposition is carried out for 30min to obtain CeO with thickness of 23.4 μm 2 The membrane-coated diamond particles are simultaneously recycled by passing the HCl gas produced into the water tank 6.
Claims (4)
1. The surface cerium oxide coating method of the micron diamond particles is characterized by comprising the following steps of:
(1) According to the mass of diamond particles: cerium chloride mass: ethanol mass= (20-26): (90-96): 100 ratio stock, ceCl 3 And adding the pretreated diamond particles into ethanol for magnetic stirring to obtain CeCl containing the diamond particles 3 Ethanol saturated solution;
(2) Placing the mixture in a low-temperature incubator, reducing the temperature to-50 to-100 ℃ and magnetically stirring the mixture, and CeCl 3 The solubility in ultra-low temperature ethanol is greatly reduced and the diamond particles are crystallized and separated out on the surface, and then the ultra-low temperature ethanol is filtered and separated to obtain the CeCl coated on the surface 3 Diamond particles of the film, ceCl obtained 3 The diamond particles coated by the film are thermally decomposed to obtain CeO 2 Film coated diamond particles; the thermal decomposition temperature is 700-800 ℃;
CeCl 3 the specific process of thermally decomposing the film-coated diamond particles is as follows: ceCl is added 3 The coated diamond particles are put into a thermal decomposition cavity (3) in a thermal decomposition device to be heated to 700 ℃ to 800 ℃, then water is dripped into a drip groove (2) by a dropper (1), the water is heated by a resistance furnace (8), the water drops are converted into water vapor, and the flowing water vapor and oxygen penetrate through a ventilation dish (5) and CeCl 3 The coated diamond particles are fully contacted to enable CeCl 3 High-efficiency thermal decomposition is carried out for 30-60min to obtain CeO 2 And (3) introducing the HCl gas generated by the membrane-coated diamond particles into a water tank (6) for recycling.
2. The method for coating the surface of the micron diamond particles with cerium oxide according to claim 1, wherein: the device for thermal decomposition comprises a dropper (1), a drip groove (2), a thermal decomposition cavity (3), a ventilation dish (5), a water tank (6), a thermocouple (7) and a resistance furnace (8), wherein the thermal decomposition cavity (3) is arranged inside the resistance furnace (8), the ventilation dish (5) is fixed in the middle of the thermal decomposition cavity (3), the top of the thermal decomposition cavity (3) is communicated with the water tank (6) through a pipeline, the bottom of the thermal decomposition cavity (3) is communicated with the drip groove (2) above the thermal decomposition cavity (3) through a pipeline, the drip groove (2) is provided with the dropper (1), and the thermocouple is arranged at the bottom of the resistance furnace (8).
3. The method for coating the surface of the micron diamond particles with cerium oxide according to claim 1, wherein: the pretreatment process of the diamond particles comprises the following steps: the diamond particles are respectively immersed into 2mol/L hydrochloric acid and 1mol/L sodium hydroxide solution for magnetic stirring, repeatedly washed to be neutral by deionized water, and then placed into a drying oven for drying for standby.
4. The method for coating the surface of the micron diamond particles with cerium oxide according to claim 1, wherein: the CeO 2 The particle size of the membrane-coated diamond particles is 1-100 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310213929.1A CN116199218B (en) | 2023-03-08 | 2023-03-08 | Surface cerium oxide coating method of micron diamond particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310213929.1A CN116199218B (en) | 2023-03-08 | 2023-03-08 | Surface cerium oxide coating method of micron diamond particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116199218A CN116199218A (en) | 2023-06-02 |
| CN116199218B true CN116199218B (en) | 2024-03-19 |
Family
ID=86510998
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310213929.1A Active CN116199218B (en) | 2023-03-08 | 2023-03-08 | Surface cerium oxide coating method of micron diamond particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116199218B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001198460A (en) * | 2000-01-18 | 2001-07-24 | Japan Science & Technology Corp | Dehydrogenation catalyst for hydrocarbon carried on diamond and method for preparing alkene using the catalyst |
| CN101139517A (en) * | 2007-07-24 | 2008-03-12 | 河南科技大学 | Bearing vibration-reducing chemical milling agent and method for using same |
| CN102974348A (en) * | 2011-09-07 | 2013-03-20 | 中国科学院金属研究所 | Oxide-supported nanodiamond catalyst and preparation method and applications thereof |
| CN109880533A (en) * | 2019-03-26 | 2019-06-14 | 中南大学 | A kind of composite abrasive grain polishing solution and preparation method thereof |
-
2023
- 2023-03-08 CN CN202310213929.1A patent/CN116199218B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001198460A (en) * | 2000-01-18 | 2001-07-24 | Japan Science & Technology Corp | Dehydrogenation catalyst for hydrocarbon carried on diamond and method for preparing alkene using the catalyst |
| CN101139517A (en) * | 2007-07-24 | 2008-03-12 | 河南科技大学 | Bearing vibration-reducing chemical milling agent and method for using same |
| CN102974348A (en) * | 2011-09-07 | 2013-03-20 | 中国科学院金属研究所 | Oxide-supported nanodiamond catalyst and preparation method and applications thereof |
| CN109880533A (en) * | 2019-03-26 | 2019-06-14 | 中南大学 | A kind of composite abrasive grain polishing solution and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王振廷等.《石墨深加工技术》.哈尔滨工业大学出版社,2017,第79页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116199218A (en) | 2023-06-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110510689B (en) | Photo-thermal seawater desalination material with multi-stage structure and preparation method and application thereof | |
| CN106848494B (en) | A kind of simple preparation method of carbon auto-dope nano carbon nitride film electrode | |
| WO2018120601A1 (en) | Preparation method for self-supporting thin film of graphene-enhanced three-dimensional porous carbon | |
| CN101003420B (en) | Technique for preparing Nano Sn02/Ti02 composite film in use for photovoltaic conversion | |
| CN101962770A (en) | Intermediate and high temperature solar energy selective absorbing coating and preparation method thereof | |
| CN112980399A (en) | Super-hydrophilic copper-based MOF (metal organic framework) photo-thermal material as well as preparation method and application thereof | |
| CN111841592A (en) | In-situ derivatization synthesis of TiO by using Ti-based MOF2-Ti3C2Tx composite photocatalyst and application thereof | |
| CN111020487A (en) | Method for preparing film of quasi-one-dimensional structure material with controllable orientation | |
| CN109351963A (en) | A kind of blacker-than-black material and its preparation method and application | |
| CN107161960B (en) | A kind of high pressure vapor prepares the method and apparatus of boron nitride spherical powder | |
| CN116199218B (en) | Surface cerium oxide coating method of micron diamond particles | |
| CN109052988A (en) | A kind of preparation method of zinc indium sulphur nano-chip arrays film | |
| CN106904943B (en) | Method for in-situ preparation of antimony oxide film | |
| CN105664900B (en) | The preparation method of composite photocatalyst coating and composite photocatalyst coating obtained | |
| CN107245689A (en) | A kind of large area prepares the chemical method of halogenation methylamine lead optoelectronic film | |
| CN114162809B (en) | Method for preparing graphene by two-step chemical vapor deposition method | |
| CN102557110B (en) | Preparation method of ZnO nanorod array in low-temperature steam | |
| CN108588713A (en) | A kind of preparation method of two dimension phosphatization molybdenum film | |
| CN112048746B (en) | Alternating current electroplating method for nickel-based metal organic framework film | |
| CN114920271A (en) | Method for preparing lithium hexafluorophosphate by dry method | |
| JP2003326637A (en) | Manganic acid nano-sheet ultrathin film and manufacturing method therefor | |
| US9017777B2 (en) | Inorganic films using a cascaded source for battery devices | |
| CN112663022A (en) | Bismuth oxyhalide nano-film and preparation method thereof | |
| CN109768113A (en) | A kind of AlN nanometers of film explorer and preparation method thereof | |
| TWI658002B (en) | Method of manufacturing silicon monoxide deposit and manufacturing equipment implementing such method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |