Preparation method and device of nickel oxide doped oxide target material for perovskite

Abstract

The invention discloses a preparation method and device of a nickel oxide doped oxide target material for perovskite, and the method comprises the steps: carrying out spray granulation on obtained defoamed mixed slurry by using a sprayer, then uniformly stirring the mixed slurry subjected to spray granulation, screening the uniformly stirred mixed slurry to obtain mixed powder of nickel oxide and an additive, and carrying out spray granulation on the mixed powder to obtain the nickel oxide doped oxide target material for perovskite. The method has low requirements on powder granularity, and the powder utilization rate can reach 90%; the obtained nickel oxide and additive mixed powder is subjected to pressure forming through a hydraulic machine to obtain a nickel oxide doped oxide target blank, the pressure of a pressed product is reduced to 120-160 Mpa through the method, the pressing pressure is greatly reduced compared with the conventional pressure of 250-300 Mpa of the pressed product, and the service life of cold isostatic pressing is greatly prolonged; the refractive index of the finally obtained nickel oxide doped oxide target material is high, and the refractive index of the nickel oxide doped oxide target material is generally 1.6 or above under the wave band of 550-650 nm.

Description

Technical Field

[0001] The present invention belongs to the technical field of preparation of nickel oxide-doped oxide target materials for perovskite, and specifically relates to a preparation method and device for nickel oxide-doped oxide target materials for perovskite. Background Art

[0002] Perovskite solar cells are solar cells that use perovskite-type organic metal halide semiconductors as light-absorbing materials. They belong to the third generation of solar cells and are also called new concept solar cells. The application of NiO targets in the field of solar cells, especially in perovskite solar cells, shows its irreplaceable advantages. NiO targets can be used as electron transport layers or hole transport layers to effectively improve the conversion efficiency and stability of the battery.

[0003] There are various methods for preparing nickel oxide targets for perovskite. For example, the prior art solution with patent publication number "CN117026179A" is one of the methods for preparing nickel oxide targets for perovskite. Various methods for preparing nickel oxide targets for perovskite generally dope some additives to improve the performance of the target. However, these methods for preparing nickel oxide targets for perovskite doped with some additives still have the following defects: In the prior art, the preparation method of the nickel oxide target material for perovskite doped with some additives often uses a pressing product pressure in the range of 250~300Mpa, which makes the service life of the cold isostatic pressing not long; the powder utilization rate in the preparation method of the nickel oxide target material for perovskite doped with some additives is not high, which is below 80%; the refractive index of the nickel oxide doped oxide target material finally obtained by the preparation method of the nickel oxide target material for perovskite doped with some additives is not high, and the refractive index of the nickel oxide doped oxide target material is generally below 1.3 in the 550~650nm band. Summary of the invention

[0004] In order to solve the shortcomings of the prior art, the present invention proposes a method and device for preparing a nickel oxide doped oxide target for perovskite, wherein the obtained defoamed mixed slurry is spray granulated by a sprayer, and then the spray granulated mixed slurry is evenly mixed, and then the evenly mixed mixed slurry is sieved to obtain a mixed powder of nickel oxide and additives. This method has low requirements on powder particle size, and the powder utilization rate can reach 90%; the obtained mixed powder of nickel oxide and additives is pressure-formed by a hydraulic press to obtain a nickel oxide doped oxide target blank, and the pressing pressure of the product is reduced to 120-160Mpa by this method, which greatly reduces the pressing pressure compared with the conventional pressing product pressure of 250-300Mpa, and greatly prolongs the service life of cold isostatic pressing; the nickel oxide doped oxide target finally obtained by the present invention has a high refractive index, and the refractive index of the nickel oxide doped oxide target is generally above 1.6 in the 550-650nm band.

[0005] The present invention utilizes the following technical solutions.

[0006] A method for preparing a nickel oxide-doped oxide target for perovskite, comprising the following steps: Step 1: preparing nickel oxide, additives, dispersants, binders and water into a mixed slurry using a sand mill and defoaming the mixed slurry using a defoaming agent; Preferably, the average particle size of the nickel oxide in the mixed slurry is 250-500 nm; the average particle size of the additive in the mixed slurry is 250-500 nm; the weight of the dispersant accounts for 0.4%-1% of the total weight of the nickel oxide and the additive, the additive accounts for 1%-15% of the total weight of the nickel oxide and the additive, the weight of the binder accounts for 2%-5% of the total weight of the nickel oxide and the additive, and the water accounts for 40%-50% of the total weight of the nickel oxide and the additive.

[0007] Preferably, the additive is a mixture of one or more of lithium oxide, magnesium oxide, copper oxide, potassium oxide and sodium oxide, and the weight of each component of the additive is the same.

[0008] Preferably, the dispersant is ammonium polyacrylate.

[0009] Preferably, the binder is a mixture of one or more components selected from the group consisting of polyvinyl alcohol, carboxymethyl cellulose, polyacrylamide, polyacrylic acid salt, and polyethylene glycol, and the weights of the components of the binder are the same.

[0010] Preferably, the defoaming agent is a mixture of one or more components selected from the group consisting of polydimethylsiloxane, polyoxypropylene oxyethylene glycerol ether, and n-butanol, and the weights of the components of the defoaming agent are the same.

[0011] Preferably, the defoaming agent accounts for 2% to 4% of the total weight of the nickel oxide and the additive, and the defoaming time of the defoaming agent is 6 to 28 minutes.

[0012] Step 2: The defoamed mixed slurry obtained in step 1 is sprayed and granulated using a sprayer, and then the spray-granulated mixed slurry is mixed evenly, and then the mixed mixed slurry is sieved to obtain a mixed powder of nickel oxide and additives; Preferably, the average particle size of the mixed powder of nickel oxide and additives is 40 to 100 microns.

[0013] Step 3: The nickel oxide and additive mixed powder obtained in step 2 is pressure-molded by a hydraulic press to obtain a nickel oxide-doped oxide target blank; Preferably, the pressure forming using a hydraulic press includes a first hydraulic forming stage and a second hydraulic forming stage which are performed sequentially. The first hydraulic forming stage is to use a hydraulic press to pressure-form the nickel oxide and additive mixed powder, the pressure of the pressure forming is 60-100MPa, and the pressure forming time is 20-30 seconds; the second hydraulic forming stage is to use a hydraulic press to pressure-form the nickel oxide and additive mixed powder again, the pressure of the pressure forming is 120-160MPa, and the pressure forming time is 30-50 seconds.

[0014] Step 4: Evenly lay a layer of metal additive powder on the bottom of the nickel oxide-doped oxide target blank obtained in step 3, and then sinter it in a sintering furnace at a sintering temperature of 1300-1500° C. to obtain the nickel oxide-doped oxide target.

[0015] Preferably, the metal additive powder is a mixture of zinc oxide, aluminum oxide and zirconium oxide components, the average particle size of the metal additive powder is 40 to 100 microns, the weight of each component of the metal additive powder is the same, the weight of the metal additive powder is 4% to 8% of the weight of the nickel oxide-doped oxide target blank obtained in step 3, the sintering time for sintering the nickel oxide-doped oxide target is 9 to 12 hours, and after sintering is completed and the nickel oxide-doped oxide target is cooled to room temperature, the nickel oxide-doped oxide target is taken out from the sintering furnace.

[0016] A device used in a method for preparing a nickel oxide-doped oxide target material for perovskite, comprising: The sprayer for performing spray granulation comprises: a hollow shell, the bottom of the hollow shell is fixedly connected to a pair of traction motors distributed in a mirror image via a fixed plate, the rotating rods of the pair of traction motors are separated from each other and fixedly connected to wheels via rollers, the end of the wheel away from the traction motor is fixedly connected to a ratchet block, the lower wall inside the hollow shell is fixedly connected to a slewing support, the slewing support is connected to a rotating bar, the upper part of the rotating bar is penetrated through the upper wall of the hollow shell and fixedly connected to a handle, the outer wall of the rotating bar is fixedly connected to a ratchet disk in the hollow shell, the upper part of the hollow shell is provided with a strip-shaped running port on both sides of the rotating bar, the inner wall surface of the running port is movably connected to a pair of connecting pieces at the front and rear of the ratchet disk via the running bar, and the connecting piece is close to the ratchet disk One side is connected to the ratchet plate one through ratchet block two, and a cylindrical connecting rotating piece is installed on the sides of a pair of wheels facing away from each other. The side of the connecting rotating piece close to the wheel is connected to the ratchet block one through a ratchet bar. A pair of through-holes located on both sides of the slewing support one and distributed in a mirror image are opened on the lower wall of the hollow shell body. The outer wall of the connecting rotating piece is movably connected to the connecting strip through the circular opening opened thereon. The upper part of the connecting strip is provided with a through-hole and is fixedly connected to the lower part of the connecting piece. The lower part of the hollow shell body is fixedly connected to a pair of slewing supports two on the side facing away from each other and distributed in a mirror image on the pair of through-holes. The side of the connecting rotating piece facing away from the wheel is provided with a rotating column through the inner wall surface of the slewing support two and is fixedly connected to the ratchet plate two.

[0017] Preferably, both sides of the hollow shell are provided with exploration ports that communicate with the hollow shell, and both sides of the hollow shell are movably connected to the linkage bar below the exploration port via slewing bearing three, and the outer wall of the linkage bar is engaged with ratchet disc three and ratchet disc two, and the inner wall surface of the lower part of the hollow shell is fixedly connected to a slurry storage container that stores the defoamed mixed slurry to be spray granulated at the rear of slewing bearing one, and the inner wall surface of the rear part of the hollow shell is fixedly connected to a pumping motor located above the slurry storage container, and the liquid inlet end of the pumping motor is fixedly connected to the output end of the upper part of the slurry storage container via a connecting pipe.

[0018] Preferably, a pair of cross beams located on both sides of the liquid pumping motor and distributed in a mirror image are fixedly connected to the inner wall surface of the rear part of the hollow shell, and the liquid outlet ends on both sides of the liquid pumping motor are connected to annular columnar plastic channels for slurry discharge. One end of a pair of plastic channels for slurry discharge is away from the liquid pumping motor and is coiled around the outer wall of the cross beam and extends to both sides of the hollow shell through the exploration port, and the lower part of the plastic channel for slurry discharge is fixedly connected to the nozzle for spray granulation.

[0019] Preferably, the slurry delivery ports on both sides of the slurry storage container are connected to a cylindrical slurry delivery channel, and the end of the slurry delivery channel facing away from the slurry storage container is fixedly connected to the inner wall surface of the probe port. The slurry delivery channel is located below the spray granulation nozzle, and a storage groove communicating with the inside of the slurry delivery channel is opened on the upper part of the slurry delivery channel.

[0020] Preferably, both sides of the hollow shell are movably connected to the lead screw located above the exploration port via the slewing bearing three, the outer wall of the lead screw is linked via a chain plate and a linkage bar, the outer thread of the lead screw is threadedly connected to a through inner thread opened on the moving piece on the side of the chain plate away from the slewing bearing three, both sides of the hollow shell are fixedly connected to the running column located on the slewing bearing three, one end of the running column is provided with a moving piece and extends to the side of the moving piece away from the hollow shell, the lower part of the moving piece is fixedly connected to the upper part of the plastic channel for slurry discharge, the upper wall of the slurry delivery channel is an inclined wall, and the angle between the upper wall of the slurry delivery channel and the ground surface is between π / 6 and π / 4.

[0021] Preferably, the outer wall of the handle is provided with a gripping opening for preventing separation, and the front portion of the gripping opening for preventing separation on the outer wall of the handle is fan-shaped and the angle of the fan-shaped ring is not less than π / 2.

[0022] Preferably, a smooth sheet is fixedly connected to the inner wall surface of the running port, a frosted sheet is fixedly connected to the outer wall of the running bar, and the running port and the front part of the running bar are both rectangular in shape.

[0023] Preferably, the number of ratchet teeth evenly distributed on the ratchet tooth block 2 on one side of the connecting piece is more than eight, and the shape of the ratchet teeth on the ratchet tooth block 2 is terraced.

[0024] Preferably, the number of the spray granulation nozzles at the lower part of the plastic channel for pulp discharge is twelve, and the spray granulation nozzles are linearly distributed.

[0025] The beneficial effect of the present invention lies in that, compared with the prior art, the purpose of the present invention is to use a sprayer to spray granulate the obtained mixed slurry after defoaming, then mix the mixed slurry after spray granulation, and then sieve the mixed slurry after mixing to obtain a mixed powder of nickel oxide and additives. This method has low requirements on powder particle size and the powder utilization rate can reach 90%; the obtained mixed powder of nickel oxide and additives is pressure-formed by a hydraulic press to obtain a nickel oxide-doped oxide target blank. This method reduces the pressing pressure of the product to 120-160Mpa, which greatly reduces the pressing pressure compared with the conventional pressing product pressure of 250-300Mpa, and greatly prolongs the service life of cold isostatic pressing; the nickel oxide-doped oxide target material finally obtained by the present invention has a high refractive index, and the refractive index of the nickel oxide-doped oxide target material is generally above 1.6 in the 550-650nm band. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 It is an overall flow chart of the method for preparing the nickel oxide-doped oxide target for perovskite described in the present invention; Figure 2 is a side view schematic diagram of a sprayer for performing spray granulation according to the present invention; Figure 3It is a partial connection schematic diagram of the ratchet disc 1 of the sprayer for performing spray granulation in the present invention; Figure 4 yes Figure 2 The local schematic diagram of point B in the middle; Figure 5 yes Figure 2 The local schematic diagram of the C in the middle; Figure 6 yes Figure 2 Partial schematic diagram at point D in the middle. DETAILED DESCRIPTION

[0027] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be clearly and completely expressed in combination with the drawings in the embodiments of the present invention. The embodiments expressed in this application are only part of the embodiments of the present invention, not all of them. Based on the spirit of the present invention, other embodiments obtained by ordinary technicians in this field without creative work are all within the scope of protection of the present invention.

[0028] like Figure 1 As shown, the method for preparing a nickel oxide-doped oxide target for perovskite according to the present invention comprises: Step 1: preparing nickel oxide, additives, dispersants, binders and water into a mixed slurry using a sand mill and defoaming the mixed slurry using a defoaming agent; In a preferred but non-limiting embodiment of the present invention, the average particle size of the nickel oxide in the mixed slurry is 250-500 nm; the average particle size of the additive in the mixed slurry is 250-500 nm; the weight of the dispersant accounts for 0.4%-1% of the total weight of the nickel oxide and the additive, the additive accounts for 1%-15% of the total weight of the nickel oxide and the additive, the weight of the binder accounts for 2%-5% of the total weight of the nickel oxide and the additive, and the water accounts for 40%-50% of the total weight of the nickel oxide and the additive.

[0029] In a preferred but non-limiting embodiment of the present invention, the component of the additive is a mixture of one or more components of lithium oxide, magnesium oxide, copper oxide, potassium oxide and sodium oxide, and the weight of each component of the additive is the same.

[0030] In a preferred but non-limiting embodiment of the present invention, the dispersant is ammonium polyacrylate.

[0031] In a preferred but non-limiting embodiment of the present invention, the binder is a mixture of one or more components selected from the group consisting of polyvinyl alcohol, carboxymethyl cellulose, polyacrylamide, polyacrylate, and polyethylene glycol, and the weights of the various components of the binder are the same.

[0032] In a preferred but non-limiting embodiment of the present invention, the defoaming agent is a mixture of one or more components of polydimethylsiloxane, polyoxypropylene oxyethylene glycerol ether, and n-butanol, and the weights of the various components of the defoaming agent are the same.

[0033] In a preferred but non-limiting embodiment of the present invention, the defoaming agent accounts for 2% to 4% of the total weight of the nickel oxide and the additive, and the defoaming time of the defoaming agent is 6 to 28 minutes.

[0034] Step 2: The defoamed mixed slurry obtained in step 1 is sprayed and granulated using a sprayer, and then the sprayed and granulated mixed slurry is mixed evenly, and then the mixed mixed slurry is sieved to obtain a mixed powder of nickel oxide and additives. This method has a low requirement on the powder particle size, and the powder utilization rate can reach 90%; In a preferred but non-limiting embodiment of the present invention, the average particle size of the mixed powder of nickel oxide and additives is 40 to 100 microns.

[0035] Step 3: The nickel oxide and additive mixed powder obtained in step 2 is pressed by a hydraulic press to obtain a nickel oxide doped oxide target blank. This method reduces the pressing pressure of the product to 120-160 MPa, which is greatly reduced compared with the conventional pressing pressure of 250-300 MPa, and greatly extends the service life of the cold isostatic pressing; In a preferred but non-limiting embodiment of the present invention, pressure molding using a hydraulic press includes a first hydraulic molding stage and a second hydraulic molding stage performed sequentially. The first hydraulic molding stage is to use a hydraulic press to pressure mold the nickel oxide and additive mixed powder, the pressure of the pressure molding is 60~100MPa, and the molding time of the pressure molding is 20~30 seconds; the second hydraulic molding stage is to use a hydraulic press to pressure mold the nickel oxide and additive mixed powder again, the pressure of the pressure molding is 120~160MPa, and the molding time of the pressure molding is 30~50 seconds.

[0036] Step 4: Evenly lay a layer of metal additive powder on the bottom of the nickel oxide-doped oxide target blank obtained in step 3, and then sinter it in a sintering furnace at a sintering temperature of 1300-1500° C. to obtain the nickel oxide-doped oxide target.

[0037] In a preferred but non-limiting embodiment of the present invention, the metal additive powder is a mixture of zinc oxide, aluminum oxide and zirconium oxide components, the average particle size of the metal additive powder is 40 to 100 microns, the weight of each component of the metal additive powder is the same, the weight of the metal additive powder is 4% to 8% of the weight of the nickel oxide-doped oxide target blank obtained in step 3, the sintering time for sintering the nickel oxide-doped oxide target is 9 to 12 hours, and after sintering is completed and the nickel oxide-doped oxide target is cooled to room temperature, the nickel oxide-doped oxide target is taken out from the sintering furnace.

[0038] The purpose of the present invention is to use a sprayer to spray granulate the obtained mixed slurry after defoaming, then mix the mixed slurry after spray granulation, and then screen the mixed slurry after mixing to obtain a mixed powder of nickel oxide and additives. This method has low requirements on powder particle size and the powder utilization rate can reach 90%; the obtained mixed powder of nickel oxide and additives is pressure-formed by a hydraulic press to obtain a nickel oxide-doped oxide target blank. This method reduces the pressing pressure of the product to 120-160Mpa, which greatly reduces the pressing pressure compared with the conventional pressing product pressure of 250-300Mpa, and greatly prolongs the service life of cold isostatic pressing; the nickel oxide-doped oxide target material finally obtained by the present invention has a high refractive index, and the refractive index of the nickel oxide-doped oxide target material is generally above 1.6 in the 550-650nm band.

[0039] The embodiments of the preparation method of the present invention are as follows: Example 1

[0040] A method for preparing a nickel oxide-doped oxide target material for perovskite, comprising: Step 1: preparing nickel oxide, additives, dispersants, binders and water into a mixed slurry using a sand mill and defoaming the mixed slurry using a defoaming agent; The average particle size of the nickel oxide in the mixed slurry is 250nm; the average particle size of the additive in the mixed slurry is 250nm; the weight of the dispersant accounts for 0.4% of the total weight of the nickel oxide and the additive, the additive accounts for 1% of the total weight of the nickel oxide and the additive, the weight of the binder accounts for 2% of the total weight of the nickel oxide and the additive, and the water accounts for 40% of the total weight of the nickel oxide and the additive.

[0041] The additive is a mixture of lithium oxide, magnesium oxide and copper oxide, and the weights of the various components of the additive are the same.

[0042] The dispersant is ammonium polyacrylate.

[0043] The binder is a mixture of polyvinyl alcohol, carboxymethyl cellulose and polyacrylamide, and the weights of the various components of the binder are the same.

[0044] The defoaming agent is polydimethylsiloxane.

[0045] The defoaming agent accounts for 2% of the total weight of the nickel oxide and the additives, and the defoaming time of the defoaming agent is 6 minutes.

[0046] Step 2: The defoamed mixed slurry obtained in step 1 is sprayed and granulated using a sprayer, and then the spray-granulated mixed slurry is mixed evenly, and then the mixed mixed slurry is sieved to obtain a mixed powder of nickel oxide and additives; The average particle size of the mixed powder of nickel oxide and additives is 40 microns.

[0047] Step 3: The nickel oxide and additive mixed powder obtained in step 2 is pressure-molded by a hydraulic press to obtain a nickel oxide-doped oxide target blank; The pressure forming using a hydraulic press includes a first hydraulic forming stage and a second hydraulic forming stage which are performed sequentially. The first hydraulic forming stage is to use a hydraulic press to pressure-form the nickel oxide and the additive mixed powder. The pressure of the pressure forming is 60MPa, and the pressure forming time is 20 seconds. The second hydraulic forming stage is to use a hydraulic press to pressure-form the nickel oxide and the additive mixed powder again. The pressure of the pressure forming is 120MPa, and the pressure forming time is 30 seconds.

[0048] Step 4: Evenly lay a layer of metal additive powder on the bottom of the nickel oxide-doped oxide target blank obtained in step 3, and then sinter it in a sintering furnace at a sintering temperature of 1300° C. to obtain the nickel oxide-doped oxide target.

[0049] The metal additive powder is a mixture of zinc oxide, aluminum oxide and zirconium oxide components. The average particle size of the metal additive powder is 40 microns. The weight of each component of the metal additive powder is the same. The weight of the metal additive powder is 4% of the weight of the nickel oxide-doped oxide target blank obtained in step 3. The sintering time for sintering the nickel oxide-doped oxide target is 9 hours. After the sintering is completed and the nickel oxide-doped oxide target is cooled to room temperature, the nickel oxide-doped oxide target is taken out from the sintering furnace.

[0050] Example 2

[0051] A method for preparing a nickel oxide-doped oxide target material for perovskite, comprising: Step 1: preparing nickel oxide, additives, dispersants, binders and water into a mixed slurry using a sand mill and defoaming the mixed slurry using a defoaming agent; The average particle size of nickel oxide in the mixed slurry is 376nm; the average particle size of the additive in the mixed slurry is 376nm; the weight of the dispersant accounts for 0.7% of the total weight of the nickel oxide and the additive, the additive accounts for 8% of the total weight of the nickel oxide and the additive, the weight of the binder accounts for 4% of the total weight of the nickel oxide and the additive, and the water accounts for 45% of the total weight of the nickel oxide and the additive.

[0052] The additive is a mixture of magnesium oxide, copper oxide and potassium oxide, and the weights of the various components of the additive are the same.

[0053] The dispersant is ammonium polyacrylate.

[0054] The binder is a mixture of carboxymethyl cellulose, polyacrylamide and polyacrylic acid salt, and the weights of the various components of the binder are the same.

[0055] The defoamer is a mixture of polydimethylsiloxane, polyoxypropylene oxyethylene glycerol ether, and the weights of the various components of the defoamer are the same.

[0056] The defoaming agent accounts for 3% of the total weight of the nickel oxide and the additives, and the defoaming time of the defoaming agent is 18 minutes.

[0057] Step 2: The defoamed mixed slurry obtained in step 1 is sprayed and granulated using a sprayer, and then the spray-granulated mixed slurry is mixed evenly, and then the mixed mixed slurry is sieved to obtain a mixed powder of nickel oxide and additives; The average particle size of the mixed powder of nickel oxide and additives is 75 microns.

[0058] Step 3: The nickel oxide and additive mixed powder obtained in step 2 is pressure-molded by a hydraulic press to obtain a nickel oxide-doped oxide target blank; The pressure forming using a hydraulic press includes a first hydraulic forming stage and a second hydraulic forming stage which are performed sequentially. The first hydraulic forming stage is to use a hydraulic press to pressure-form the nickel oxide and additive mixed powder. The pressure of the pressure forming is 80MPa, and the pressure forming time is 25 seconds. The second hydraulic forming stage is to use a hydraulic press to pressure-form the nickel oxide and additive mixed powder again. The pressure of the pressure forming is 140MPa, and the pressure forming time is 42 seconds.

[0059] Step 4: Evenly lay a layer of metal additive powder on the bottom of the nickel oxide-doped oxide target blank obtained in step 3, and then sinter it in a sintering furnace at a sintering temperature of 1420° C. to obtain the nickel oxide-doped oxide target.

[0060] The metal additive powder is a mixture of zinc oxide, aluminum oxide and zirconium oxide components. The average particle size of the metal additive powder is 72 microns. The weight of each component of the metal additive powder is the same. The weight of the metal additive powder is 7% of the weight of the nickel oxide-doped oxide target blank obtained in step 3. The sintering time for sintering the nickel oxide-doped oxide target is 11 hours. After the sintering is completed and the nickel oxide-doped oxide target is cooled to room temperature, the nickel oxide-doped oxide target is taken out from the sintering furnace.

[0061] Example 3

[0062] A method for preparing a nickel oxide-doped oxide target material for perovskite, comprising: Step 1: preparing nickel oxide, additives, dispersants, binders and water into a mixed slurry using a sand mill and defoaming the mixed slurry using a defoaming agent; The average particle size of the nickel oxide in the mixed slurry is 500nm; the average particle size of the additive in the mixed slurry is 500nm; the weight of the dispersant accounts for 1% of the total weight of the nickel oxide and the additive, the additive accounts for 15% of the total weight of the nickel oxide and the additive, the weight of the binder accounts for 5% of the total weight of the nickel oxide and the additive, and the water accounts for 50% of the total weight of the nickel oxide and the additive.

[0063] The additive is a mixture of copper oxide, potassium oxide and sodium oxide, and the weights of the various components of the additive are the same.

[0064] The dispersant is ammonium polyacrylate.

[0065] The binder is a mixture of polyacrylate, polyethylene glycol and several other components, and the weights of the various components of the binder are the same.

[0066] The defoaming agent is n-butanol.

[0067] The defoaming agent accounts for 4% of the total weight of the nickel oxide and the additives, and the defoaming time of the defoaming agent is 28 minutes.

[0068] Step 2: The defoamed mixed slurry obtained in step 1 is sprayed and granulated using a sprayer, and then the spray-granulated mixed slurry is mixed evenly, and then the mixed mixed slurry is sieved to obtain a mixed powder of nickel oxide and additives; The average particle size of the mixed powder of nickel oxide and additives is 100 microns.

[0069] Step 3: The nickel oxide and additive mixed powder obtained in step 2 is pressure-molded by a hydraulic press to obtain a nickel oxide-doped oxide target blank; The pressure forming using a hydraulic press includes a first hydraulic forming stage and a second hydraulic forming stage which are performed sequentially. The first hydraulic forming stage is to use a hydraulic press to pressure-form the nickel oxide and the additive mixed powder. The pressure of the pressure forming is 100MPa, and the forming time of the pressure forming is 30 seconds. The second hydraulic forming stage is to use a hydraulic press to pressure-form the nickel oxide and the additive mixed powder again. The pressure of the pressure forming is 160MPa, and the forming time of the pressure forming is 50 seconds.

[0070] Step 4: Evenly lay a layer of metal additive powder on the bottom of the nickel oxide-doped oxide target blank obtained in step 3, and then sinter it in a sintering furnace at a sintering temperature of 1500° C. to obtain the nickel oxide-doped oxide target.

[0071] The metal additive powder is a mixture of zinc oxide, aluminum oxide and zirconium oxide components. The average particle size of the metal additive powder is 100 microns. The weight of each component of the metal additive powder is the same. The weight of the metal additive powder is 8% of the weight of the nickel oxide-doped oxide target blank obtained in step 3. The sintering time for sintering the nickel oxide-doped oxide target is 12 hours. After the sintering is completed and the nickel oxide-doped oxide target is cooled to room temperature, the nickel oxide-doped oxide target is taken out from the sintering furnace.

[0072] In addition, two control groups were used to perform the reference instructions: Control group 1 and control group 2 are two groups of nickel oxide-doped oxide targets prepared under different ratio conditions using the existing technical solution with patent publication number "CN117026179A".

[0073] In this way, the refractive index of the target materials obtained in Examples 1 to 3 and Control Groups 1 to 2 in the 550-650 nm band was tested, and the test results in Table 1 were obtained: Table 1

[0074] It can be seen from Table 1 that the refractive index of the target material obtained by the embodiment of the present invention in the 550-650nm band is significantly higher than the refractive index of the control group 1 and the control group 2 using the prior art solution, that is, the refractive index of the target material in the embodiment of the present invention is significantly higher than 1.6, which is much higher than the refractive index of the target material obtained by the control group 1 and the control group 2 obtained by the prior art, which is no more than 1.3.

[0075] In addition, the current spray granulation sprayer needs additional energy-consuming parts to perform traction when changing the spraying interval. Increasing the additional energy-consuming parts to perform traction to change the spraying interval of the sprayer consumes a lot of energy, so it has the defect of high energy consumption.

[0076] After improvement, such as Figures 2 to 6 As shown, the device used in the method for preparing a nickel oxide-doped oxide target material for perovskite according to the present invention comprises: A sprayer for performing spray granulation comprises: a hollow shell 2, the bottom of the hollow shell 2 is fixedly connected to a pair of traction motors 3 distributed in a mirror image via a fixed plate, the rotating rods of the pair of traction motors 3 are separated from each other and fixedly connected to a wheel 4 via a roller, the end of the wheel 4 away from the traction motor 3 is fixedly connected to a ratchet block 5, a slewing bearing 6 is fixedly connected to the lower wall inside the hollow shell 2, the slewing bearing 6 is hooped with a rotating bar 7, the upper part of the rotating bar 7 is penetrated through the upper wall of the hollow shell 2 and is fixedly connected to a handle 8, the outer wall of the rotating bar 7 is fixedly connected to a ratchet disk 9 in the hollow shell 2, the upper part of the hollow shell 2 is provided with a strip-shaped running port 10 on both sides of the rotating bar 7, the inner wall surface of the running port 10 is movably connected to a pair of connecting pieces 22 at the front and rear of the ratchet disk 9 via a running strip 21, and the connecting piece 22 is close to the ratchet disk 9. The side is meshed with the ratchet plate 9 via a ratchet block 23, and a cylindrical connecting rotating piece 24 is installed on the side of a pair of wheels 4 that are away from each other. The side of the connecting rotating piece 24 close to the wheel 4 is meshed with the ratchet block 5 via a ratchet bar. A pair of through-holes 26 located on both sides of the slewing support 6 and distributed in a mirror image are opened on the lower wall of the hollow shell 2. The outer wall of the connecting rotating piece 24 is movably connected to the connecting strip 25 via the circular opening opened thereon. The upper part of the connecting strip 25 is through the through-hole 26 and is fixedly connected to the lower part of the connecting piece 22. The lower part of the hollow shell 2 is fixedly connected to a pair of slewing supports 42 that are located on the side of the pair of through-holes 26 that are away from each other and distributed in a mirror image. The side of the connecting rotating piece 24 away from the wheel 4 is through the rotating column and penetrates through the inner wall of the slewing support 42 and is fixedly connected to the ratchet plate 27.

[0077] In a preferred but non-restrictive embodiment of the present invention, both sides of the hollow shell 2 are provided with an exploration port 35 which is communicated with the hollow shell 2. Both sides of the hollow shell 2 are movably connected to the linkage bar 28 located below the exploration port 35 via a slewing bearing three. The outer wall of the linkage bar 28 is engaged with the ratchet disc three 29 and the ratchet disc two 27. A slurry storage container 36 which is located behind the slewing bearing one 6 and stores the defoamed mixed slurry to be spray granulated is fixedly connected to the inner wall surface of the lower part of the hollow shell 2. A pumping motor 37 which is located above the slurry storage container 36 is fixedly connected to the inner wall surface of the rear part of the hollow shell 2. The liquid inlet end of the pumping motor 37 is fixedly connected to the output end of the upper part of the slurry storage container 36 via a connecting pipe.

[0078] In a preferred but non-restrictive embodiment of the present invention, a pair of cross beams 38 located on both sides of the liquid pumping motor 37 and distributed in a mirror image are fixedly connected to the inner wall surface of the rear part of the hollow shell 2, and the liquid outlet ends on both sides of the liquid pumping motor 37 are connected to the annular columnar plastic channel 39 for slurry discharge. The end of a pair of plastic channels 39 for slurry discharge facing away from the liquid pumping motor 37 is coiled around the outer wall of the cross beam 38 and extends to both sides of the hollow shell 2 through the probe port 35. The lower part of the plastic channel 39 for slurry discharge is fixedly connected to the spray granulation nozzle 40. By having some spray granulation nozzles 40 in the hollow shell 2, the function of changing the spray granulation amount during the change of the spray range of the plastic channel 39 for slurry discharge is achieved.

[0079] In a preferred but non-restrictive embodiment of the present invention, the slurry delivery ports on both sides of the slurry storage container 36 are connected to a cylindrical slurry delivery channel 41, and the end of the slurry delivery channel 41 facing away from the slurry storage container 36 is fixedly connected to the inner wall surface of the probe port 35, and the slurry delivery channel 41 is located below the spray granulation nozzle 40. A storage groove communicating with the inside of the slurry delivery channel 41 is opened on the upper part of the slurry delivery channel 41. The slurry delivery channel 41 is located below the spray granulation nozzle 40, so that the fluid material ejected by the spray granulation nozzle 40 in the hollow shell body 2 can be collected into the slurry storage container 36, thereby achieving the effect of repeated spray granulation of the fluid material.

[0080] In a preferred but non-restrictive embodiment of the present invention, both sides of the hollow shell 2 are movably connected to the lead screw located above the exploration port 35 via the slewing bearing three 30, and the outer wall of the lead screw is linked via the chain plate 32 and the linkage bar 28. The outer thread of the lead screw is threadedly connected to the through inner thread opened on the moving piece 33 on the side of the chain plate 32 away from the slewing bearing three 30. Both sides of the hollow shell 2 are fixedly connected to the running column 34 located on the slewing bearing three 30, and one end of the running column 34 is provided with the moving piece 33 and extends to the side of the moving piece 33 away from the hollow shell 2. The lower part of the moving piece 33 is fixedly connected to the upper part of the plastic channel 39 for slurry discharge, and the upper wall of the slurry delivery channel 41 is an inclined wall, and the angle between the upper wall of the slurry delivery channel 41 and the ground surface is between π / 6 and π / 4.

[0081] In a preferred but non-limiting embodiment of the present invention, the outer wall of the handle 8 is provided with a gripping opening for preventing separation, and the front portion of the gripping opening for preventing separation on the outer wall of the handle 8 is in the shape of a fan ring, and the angle of the fan ring is not less than π / 2. Therefore, the hand can increase the adhesion force in the gripping opening for preventing separation to prevent the hand from falling off the handle 8.

[0082] In a preferred but non-limiting embodiment of the present invention, a smooth sheet is fixedly connected to the inner wall surface of the running port 10, and a frosted sheet is fixedly connected to the outer wall of the running bar 21. The front portions of the running port 10 and the running bar 21 are both rectangular in shape.

[0083] In a preferred but non-limiting embodiment of the present invention, the number of ratchets evenly distributed on the second ratchets block 23 on one side of the connecting piece 22 is more than eight, and the shape of the ratchets on the second ratchets block 23 is terraced.

[0084] In a preferred but non-limiting embodiment of the present invention, the number of the spray granulation nozzles 40 at the lower part of the plastic channel 39 for pulp discharge is twelve, and the spray granulation nozzles 40 are linearly distributed.

[0085] The traction motor 3 is operated to rotate the wheel 4 to achieve the function of allowing the sprayer to move. When the spray range is to be changed, the handle 8 is manually rotated to allow the ratchet disc 1 9 to pull the connecting piece 22 to move, so that the connecting piece 22 controls the connecting rotating piece 24 to engage with the wheel 4, so that during the movement, the rotation of the wheel 4 causes the connecting rotating piece 24 to rotate, and the rotation of the connecting rotating piece 24 causes the ratchet disc 2 27 to pull the ratchet disc 3 29 to rotate, and the rotation of the ratchet disc 3 29 causes the linkage bar 28 to rotate. The rotation of the linkage bar 28 allows the chain plate 32 to pull the lead screw to rotate, and the rotation of the lead screw allows the moving piece 33 to pull the plastic channel 39 for slurry discharge and the nozzle 40 for spray granulation to move to both sides under the traction of the running column 34. The function of changing the spray range is achieved by using the parts of the traction equipment to perform linkage. By reducing the installation of energy-consuming parts in the changing spray range, it is also possible to achieve the function of energy saving by changing the spray range, thereby achieving the function of spray granulation that is more energy-saving.

[0086] By introducing the handle, ratchet plate 1 and ratchet block 2, the operator only needs to manually rotate the control handle to control the function of the connecting rotating piece and the wheel meshing connection, and then introduce the ratchet plate 2, ratchet plate 3 and chain plate to control the linkage bar to pull the lead screw to rotate. The rotation of the lead screw allows the moving piece to pull the plastic channel for pulp discharge and the spray granulation nozzle downward under the drive of the running column to execute the function of changing the spray range in both directions. The function of changing the spray range is achieved by using the parts of the traction equipment to perform linkage, and thus by reducing the installation of energy-consuming parts in the changing spray range, it is also convenient to implement the changing spray range and achieve the function of energy saving, thereby achieving the function of spray granulation that is more energy-saving.

[0087] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, ordinary technicians in the relevant field should understand that the specific implementation methods of the present invention can still be modified or replaced by equivalents, and any modifications or equivalent replacements that do not deviate from the spirit and scope of the present invention should be included in the protection scope of the claims of the present invention.

Claims

1. A method for preparing a nickel oxide-doped oxide target for perovskite, characterized in that: include: Step 1: preparing nickel oxide, additives, dispersants, binders and water into a mixed slurry using a sand mill and defoaming the mixed slurry using a defoaming agent; Step 2: The defoamed mixed slurry obtained in step 1 is sprayed and granulated using a sprayer, and then the spray-granulated mixed slurry is mixed evenly, and then the mixed mixed slurry is sieved to obtain a mixed powder of nickel oxide and additives; Step 3: The nickel oxide and additive mixed powder obtained in step 2 is pressure-molded by a hydraulic press to obtain a nickel oxide-doped oxide target blank; Step 4: evenly laying a layer of metal additive powder on the bottom of the nickel oxide-doped oxide target blank obtained in step 3, and sintering the target blank in a sintering furnace at a sintering temperature of 1300-1500° C. to obtain the nickel oxide-doped oxide target; A sprayer for performing spray granulation, comprising: a hollow shell, The bottom of the hollow shell is fixedly connected to a pair of traction motors distributed in a mirror image via a fixed plate, the rotating rods of the pair of traction motors are separated from each other and fixedly connected to the wheel via a roller, the end of the wheel away from the traction motor is fixedly connected to a ratchet block 1, the lower wall inside the hollow shell is fixedly connected to a slewing support 1, the slewing support 1 is connected to a rotating bar, the upper part of the rotating bar is penetrated through the upper wall of the hollow shell and fixedly connected to a handle, the outer wall of the rotating bar is fixedly connected to a ratchet disk 1 in the hollow shell, the upper part of the hollow shell is provided with a strip-shaped running opening on both sides of the rotating bar, the inner wall surface of the running opening is movably connected to a pair of connecting pieces at the front and rear of the ratchet disk 1 via the running bar, and the side of the connecting piece close to the ratchet disk 1 is connected to the ratchet block 2 at the same time The ratchet disc is engaged with each other, and a cylindrical connecting rotating piece is installed on the side of a pair of wheels that are away from each other. The side of the connecting rotating piece close to the wheel is engaged with each other through a ratchet bar and a ratchet block. A pair of through-holes located on both sides of the slewing support and distributed in a mirror image are opened on the lower wall of the hollow shell. The outer wall of the connecting rotating piece is movably connected to the connecting strip through the ring-shaped opening opened thereon. The upper part of the connecting strip is through the through-hole and is fixedly connected to the lower part of the connecting piece. The lower part of the hollow shell is fixedly connected to a pair of slewing supports 2 located on the side of the pair of through-holes that are away from each other and distributed in a mirror image. The side of the connecting rotating piece away from the wheel is through the inner wall of the slewing support 2 and is fixedly connected to the ratchet disc 2 via a rotating column. Both sides of the hollow shell are provided with exploration ports communicating with the hollow shell. Both sides of the hollow shell are movably connected to the linkage bar located below the exploration port via the slewing bearing 3. The outer wall of the linkage bar is engaged and connected via the ratchet disc 3 and the ratchet disc 2. The inner wall surface of the lower part of the hollow shell is fixedly connected to the slurry storage container located behind the slewing bearing 1 and storing the defoamed mixed slurry to be sprayed and granulated. The inner wall surface of the rear part of the hollow shell is fixedly connected to the pumping motor located above the slurry storage container. The liquid inlet end of the pumping motor is fixedly connected to the output end of the upper part of the slurry storage container via a connecting pipe. A pair of cross beams located on both sides of the pumping motor and distributed in mirror image are fixedly connected to the inner wall surface of the rear part of the hollow shell. The liquid outlet ends on both sides of the pumping motor are connected to annular columnar plastic channels for slurry discharge. One end of the pair of plastic channels for slurry discharge away from the pumping motor is coiled on the outer wall of the cross beam and extends to both sides of the hollow shell through the exploration port. The lower part of the plastic channel for slurry discharge is fixedly connected to the nozzle for spray granulation. The slurry delivery ports on both sides of the slurry storage container are connected to the annular columnar slurry delivery channel. The end of the slurry delivery channel away from the slurry storage container is fixedly connected to the inner wall surface of the probe port. The slurry delivery channel is located below the spray granulation nozzle. The upper part of the slurry delivery channel is provided with a receiving groove connected to the inside.

2. The method for preparing a nickel oxide-doped oxide target for perovskite according to claim 1, characterized in that: The average particle size of the nickel oxide in the mixed slurry is 250-500nm; the average particle size of the additive in the mixed slurry is 250-500nm; the weight of the dispersant accounts for 0.4%-1% of the total weight of the nickel oxide and the additive, the additive accounts for 1%-15% of the total weight of the nickel oxide and the additive, the weight of the binder accounts for 2%-5% of the total weight of the nickel oxide and the additive, and the water accounts for 40%-50% of the total weight of the nickel oxide and the additive.

3. The method for preparing a nickel oxide-doped oxide target for perovskite according to claim 2, characterized in that: The additive is a mixture of one or more of lithium oxide, magnesium oxide, copper oxide, potassium oxide and sodium oxide, and the weight of each component of the additive is the same.

4. The method for preparing a nickel oxide-doped oxide target for perovskite according to claim 3, characterized in that: The dispersant is ammonium polyacrylate.

5. The method for preparing a nickel oxide-doped oxide target for perovskite according to claim 4, characterized in that: The binder is a mixture of one or more components selected from polyvinyl alcohol, carboxymethyl cellulose, polyacrylamide, polyacrylic acid salt, and polyethylene glycol, and the weights of the components of the binder are the same.

6. The method for preparing a nickel oxide-doped oxide target for perovskite according to claim 5, characterized in that: The defoamer is a mixture of one or more components selected from the group consisting of polydimethylsiloxane, polyoxypropylene oxyethylene glycerol ether, and n-butanol, and the weights of the components of the defoamer are the same; The defoaming agent accounts for 2% to 4% of the total weight of the nickel oxide and the additives, and the defoaming time of the defoaming agent is 6 to 28 minutes.

7. The method for preparing a nickel oxide-doped oxide target for perovskite according to claim 6, characterized in that: The average particle size of the mixed powder of nickel oxide and additives is 40 to 100 microns.

8. The method for preparing a nickel oxide-doped oxide target for perovskite according to claim 7, characterized in that: The pressure forming using a hydraulic press includes a first hydraulic forming stage and a second hydraulic forming stage which are performed in sequence. The first hydraulic forming stage is to use a hydraulic press to pressure-form the nickel oxide and the additive mixed powder. The pressure of the pressure forming is 60-100MPa, and the forming time of the pressure forming is 20-30 seconds. The second hydraulic forming stage is to use a hydraulic press to pressure-form the nickel oxide and the additive mixed powder again. The pressure of the pressure forming is 120-160MPa, and the forming time of the pressure forming is 30-50 seconds.

9. The method for preparing a nickel oxide-doped oxide target for perovskite according to claim 8, characterized in that: The metal additive powder is a mixture of zinc oxide, aluminum oxide and zirconium oxide components, the average particle size of the metal additive powder is 40 to 100 microns, the weight of each component of the metal additive powder is the same, the weight of the metal additive powder is 4% to 8% of the weight of the nickel oxide doped oxide target blank obtained in step 3, the sintering time for sintering the nickel oxide doped oxide target is 9 to 12 hours, and after the sintering is completed and the nickel oxide doped oxide target is cooled to room temperature, the nickel oxide doped oxide target is taken out from the sintering furnace.

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