Indium cerium tantalum titanium holmium oxide target material and method for manufacturing the same
By preparing indium cerium tantalum titanium holmium target materials and using a specific ratio of indium and multivalent metal doping, the shortcomings of ITO thin films in terms of hardness, mobility and carrier concentration were solved, and the sputtering coating effect of high-performance thin films was achieved.
Patent Information
- Application Number
- CN202311193722.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-15
- Publication Date
- 2026-01-09
- Estimated Expiration
- 2043-09-15
AI Technical Summary
Existing ITO thin films have shortcomings in terms of hardness, mobility, and carrier concentration, making it difficult to meet the requirements of modern optoelectronic devices.
Indium oxide cerium tantalum titanium holmium target material was prepared by using indium as the main material and combining it with trivalent, tetravalent and pentavalent metals for doping. The specific steps include dispersion, grinding, spray drying and sintering of mixed powders, and controlling the molar ratio to be 66.3~71.8:0.058~1.163:0.045~0.905:0.125~2.5:0.053~1.058.
The prepared target material has high hardness, high electron mobility and carrier concentration, making it suitable for sputtering deposition and improving the performance of the thin film.
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Figure BDA0004451527680000201 
Figure BDA0004451527680000211
Abstract
Description
TECHNICAL FIELD
[0001] The application relates to the technical field of target materials, in particular to an indium cerium tantalum titanium holmium oxide target material and a preparation method thereof. BACKGROUND
[0002] ITO thin films still have some defects to be solved, such as the scarcity of In elements leading to high cost of ITO thin films, poor light transmittance of the thin films in the near-infrared region, and large brittleness which is difficult to meet the requirements of modern optoelectronic devices on flexibility. With the development of science and technology and the updating of various electronic components, the performances of ITO thin films can no longer meet the application requirements. In order to prepare high-performance oxide thin films, in addition to sputtering parameters, there are also requirements for the target materials themselves, such as film hardness, mobility, carrier concentration and the like.
[0003] CN102160182A discloses a thin film transistor having a crystalline indium oxide semiconductor film, which has a crystalline indium oxide semiconductor film taking indium oxide as a main component and containing a trivalent metal oxide; the trivalent metal oxide is one or two or more oxides selected from boron oxide, aluminum oxide, gallium oxide, scandium oxide, yttrium oxide, lanthanum oxide, praseodymium oxide, neodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide and lutetium oxide;
[0004] The specification records that the electric field effect mobility of the thin film transistor is 10.8 cm 2 / V·sec, and the On-Off ratio is 10 8 , and the thin film transistor has a normally-off characteristic; the semiconductor film is crystalline. In addition, the carrier concentration obtained by hole measurement is 6*10 +16 / cm 3 ;
[0005] It only selects to use trivalent metal doping, but in actual research, we find that only using trivalent metal doping may not be optimal in some aspects, such as hardness, mobility and the like.
[0006] The problem to be solved by the present application is how to develop a target material with high hardness, large electron mobility and carrier concentration. SUMMARY
[0007] The purpose of the present application is to provide an improved indium cerium tantalum titanium holmium oxide target material, which uses indium as a main material and is doped with trivalent, tetravalent and pentavalent metals, so that the obtained target material has the characteristics of high hardness, large electron mobility and carrier concentration.
[0008] As above, the application also discloses a preparation method of the target material.
[0009] To achieve the above object, the application discloses an indium cerium tantalum titanium holmium oxide target material, and the molar ratio of indium, cerium, tantalum, titanium and holmium in the target material is 66.3-71.8:0.058-1.163:0.045-0.905:0.125-2.5:0.053-1.058.
[0010] In the above-mentioned indium cerium tantalum titanium holmium oxide target material, the molar ratio of indium, cerium, tantalum, titanium and holmium in the target material is 66.3-71.1:0.232-1.163:0.136-0.905:0.625-2.5:0.053-1.058.
[0011] Meanwhile, the application also discloses a preparation method of the above-mentioned indium cerium tantalum titanium holmium oxide target material, and the method specifically comprises the following steps: dispersing, grinding and drying indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder and holmium oxide powder in water to obtain mixed powder; and performing mold pressing and cold isostatic pressing on the mixed powder, and then performing heating, degreasing and sintering.
[0012] In the above-mentioned preparation method of the indium cerium tantalum titanium holmium oxide target material, the preparation method of the mixed powder specifically comprises the following steps:
[0013] Step 1: adding cerium oxide powder, tantalum oxide powder, titanium oxide powder and holmium oxide powder into pure water containing a first dispersant to obtain slurry one;
[0014] Step 2: grinding slurry one in a sand mill by using a pneumatic diaphragm pump to obtain slurry two;
[0015] Step 3: adding indium oxide powder and a second dispersant into slurry two to obtain slurry three;
[0016] Step 4: grinding slurry three in a sand mill by using a pneumatic diaphragm pump to obtain slurry four;
[0017] Step 5: adding a binder into slurry four, mixing, and then grinding the mixture in a sand mill by using a pneumatic diaphragm pump to obtain slurry five;
[0018] Step 6: spraying slurry five into a co-current spray drying tower, performing spray granulation, mixing and screening to obtain the mixed powder.
[0019] In the above-mentioned preparation method of the indium cerium tantalum titanium holmium oxide target material, the first dispersant and the second dispersant are each independently selected from one or more of polyvinylpyrrolidone, sodium dodecylbenzenesulfonate, a polycarboxylic acid compound, polyvinyl acetate or sodium cetylbenzenesulfonate.
[0020] In the preparation method of the indium cerium tantalum titanium holmium oxide target material, the binder accounts for 5-20% of the total mass of the added indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder and holmium oxide powder and binder; the binder is one or both of a mixture of polyvinyl alcohol and polyethylene glycol, polyvinyl alcohol or polyvinyl butyral.
[0021] In the preparation method of the indium cerium tantalum titanium holmium oxide target material, the sintering temperature is 1100-1500℃, the heating rate is 0.1-0.5 / min, and the holding time is 8-12h.
[0022] The beneficial effects of the present application are:
[0023] In the present application, the target material is prepared by using indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder and holmium oxide powder as raw materials in a mass ratio of 92-99.6:0.1-2:0.1-2:0.1-2:0.1-2 (molar ratio of each metal element is 66.3-71.8:0.058-1.163:0.045-0.905:0.125-2.5:0.053-1.058), and the target material has the characteristics of high hardness, high mobility and high carrier concentration, and is an excellent target material. DETAILED DESCRIPTION
[0024] In the description of the present application, it should be noted that, in the examples, the specific conditions not specified are carried out according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not specified by the manufacturer, and are all conventional products that can be purchased on the market.
[0025] The present application will be described clearly and completely below with reference to the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.
[0026] Example 1
[0027] Step 1: weigh 9200g of indium oxide powder, 200g of cerium oxide powder, 200g of tantalum oxide powder, 200g of titanium oxide powder and 200g of holmium oxide powder for standby;
[0028] Step 2: add 1500g of pure water and polyvinylpyrrolidone dispersant to the slurry barrel. The polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder.
[0029] Step 3: The cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder weighed in step (1) are added to the solution of step (2) to obtain slurry one by pre-dispersing, wherein the pre-dispersing time is 30 min, the pre-dispersing rotation speed is 100 rpm, and the solid content in the slurry is 60%.
[0030] Step 4: The slurry one obtained in step (3) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry two, wherein the grinding rotation speed is 1200 rpm, and the grinding time is 6 h;
[0031] Step 5: The indium oxide powder weighed in step (1) and 500 g of polyvinylpyrrolidone dispersant and 3500 g of pure water are added to the slurry two for stirring and pre-dispersing to obtain slurry three, wherein the mass of the polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the indium oxide, cerium oxide, tantalum oxide, titanium oxide powder and holmium oxide powder. The dispersing rotation speed is 100 rpm, the dispersing time is 40 min, and the solid content in the slurry is 65%.
[0032] Step 6: The slurry three obtained in step (5) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry four, wherein the grinding rotation speed is 1200 rpm, and the grinding time is 10 h;
[0033] Step 7: The binder is added to the slurry four obtained in step (6) for pre-dispersing, the pre-dispersing time is 30 min, and the dispersing rotation speed is 100 rpm; the obtained slurry is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry five, wherein the grinding time is 2 h, the grinding rotation speed is 1200 rpm, and the binder accounts for 10% of the total mass of the added powder and the binder.
[0034] Step 8: The slurry five obtained in step (7) is pumped into a co-current spray drying tower for spray granulation, then mixed and sieved to obtain the required precursor powder. The air outlet temperature is 70°C, and the atomizer frequency is 120 Hz.
[0035] Step 9: The powder prepared in step (8) is sequentially subjected to die pressing and cold isostatic pressing to obtain a green compact of the target material, wherein the die pressing pressure of the target material is 90 Mpa, and the pressure holding time is 120 s; the cold isostatic pressing pressure is 350 Mpa, and the pressure holding time is 120 s.
[0036] Step 10: The indium cerium tantalum titanium holmium oxide target blank obtained in step (9) is subjected to heat treatment, the temperature is controlled at 550°C for degreasing treatment (the holding time is 2.5 hours, and the heating rate is 0.15°C / min), then cooled to room temperature, oxygen is introduced, the sintering temperature is increased to obtain a sintered indium cerium tantalum titanium holmium oxide target material (the sintering temperature is 1380°C, the heating rate is 0.1°C / min, and the holding time is 12 h);
[0037] Step 11: The relative density of the target material is 99.12% by measurement, and the conductivity of the target material is 987 s / cm;
[0038] Sputtering experiment
[0039] (1) Put the target into a culture dish containing acetone, anhydrous ethanol and deionized water, and ultrasonically clean for 15 min to remove grease and particles and other contaminants on the surface of the substrate, and then dry with a ear ball; (2) Put the target on the workpiece table in the coating chamber; (3) First use a mechanical pump to pump the chamber pressure to a limit pressure of 10 Pa, then use a molecular pump to pump the chamber pressure to 2.66*10 -6 Pa or lower, (4) Set the target base distance to 15 mm, the base pressure to 2.6*10 -6 Pa, the sputtering pressure to 1.6 Pa, Ar:O2=1:1, the deposition temperature to 500℃, the sputtering power to 100 W, and the sputtering time to 50 min.
[0040] The sputtered film has a mobility of 77.31 cm 2 / (v.s), a carrier concentration of 1.41 cm -3 , and a film hardness of 10.35 Mpa.
[0041] Example 2
[0042] Step 1: Weigh 9250g of indium oxide powder, 200g of cerium oxide powder, 200g of tantalum oxide powder, 200g of titanium oxide and 150g of holmium oxide powder for standby;
[0043] Step 2: Add 1500g of pure water and polyvinylpyrrolidone dispersant to the slurry barrel. The polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the cerium oxide, tantalum oxide powder, titanium oxide and holmium oxide powder.
[0044] Step 3: Add the weighed cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder in step (1) to the solution in step (2) to obtain a slurry one by pre-dispersing. The pre-dispersing time is 30 min, the pre-dispersing speed is 100 rpm, and the solid content in the slurry is 62%.
[0045] Step 4: Pump the slurry one obtained in step (3) into a sand mill with a pneumatic diaphragm pump for grinding to obtain a slurry two. The grinding speed is 1200 rpm, and the grinding time is 6h;
[0046] Step 5: Put the weighed indium oxide powder in step (1) and polyvinylpyrrolidone dispersant 500g and pure water 3500g into slurry two for pre-dispersion, to obtain slurry three. The mass of polyvinylpyrrolidone dispersant accounts for 5% of the total mass of indium oxide, cerium oxide, tantalum oxide, titanium oxide powder and holmium oxide powder; the dispersion rotation speed is 100 rpm, the dispersion time is 40 min, and the solid content in the slurry is 65%.
[0047] Step 6: The slurry three obtained in step (5) is pumped into a sand mill with a pneumatic diaphragm pump for grinding to obtain slurry four. The grinding speed is 1200 rpm, and the grinding time is 10 h;
[0048] Step 7: Add a binder to the slurry four obtained in step (6) for pre-dispersion, and the pre-dispersion time is 30 min and the dispersion rotation speed is 100 rpm; the obtained slurry is pumped into a sand mill for grinding with a pneumatic diaphragm pump to obtain slurry five. The grinding time is 2 h, and the grinding speed is 1200 rpm. The binder accounts for 10% of the total mass of the added powder and the binder.
[0049] Step 8: Pump the slurry five obtained in step (7) into a co-current spray drying tower for spray granulation, then mix and sieve to obtain the precursor of the indium cerium tantalum titanium holmium oxide target material. The outlet air temperature is 70℃, and the atomizer frequency is 120 Hz.
[0050] Step 9: The precursor prepared in step (8) is sequentially subjected to die pressing and cold isostatic pressing to obtain a green compact of the target material. The die pressing pressure of the target material is 90 Mpa, and the pressure holding time is 120 s; the cold isostatic pressing pressure is 350 Mpa, and the pressure holding time is 120 s.
[0051] Step 10: Heat treat the indium cerium tantalum titanium holmium oxide target blank obtained in step (9) at a temperature of 550℃ for degreasing treatment (heat preservation time 2.5 hours, heating rate 0.15℃ / min), then cool to room temperature, introduce oxygen, and increase the sintering temperature for sintering to obtain the indium cerium tantalum titanium holmium oxide target material (sintering temperature is 1380℃, heating rate is 0.1℃ / min, and heat preservation time is 12h)
[0052] The relative density of the target material is 99.09%, and the conductivity of the target material is 805 s / cm.
[0053] Sputtering film experiment
[0054] (1) Put the target material into a culture dish containing acetone, anhydrous ethanol and deionized water, and ultrasonically clean for 15 min to remove grease and particles and other contaminants on the surface of the substrate, and then dry with a suction ball; (2) Put the target material on the workpiece table in the coating chamber; (3) First, use a mechanical pump to pump the chamber to a limit pressure of 10 Pa, then use a molecular pump to pump the chamber to a pressure of 2.66*10 -6 Pa or lower, (4) Set the target base distance to 15 mm, the base pressure to 2.6*10 -6 Pa, the sputtering pressure to 1.6 Pa, Ar:O2=1:1, the deposition temperature to 500℃, the sputtering power to 100 W, and the sputtering time to 50 min.
[0055] The measured sputtering film has a mobility of 77.29 cm 2 / (v.s), a carrier concentration of 1.47 cm -3 , and a film hardness of 11.23 Mpa.
[0056] Example 3
[0057] Step 1: Weigh 9280g of indium oxide powder, 180g of cerium oxide powder, 190g of tantalum oxide powder, 180g of titanium oxide powder and 170g of holmium oxide powder for use;
[0058] Step 2: Add 1500g of pure water and polyvinylpyrrolidone dispersant to the slurry barrel. The polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder.
[0059] Step 3: Add the weighed cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder in step (1) to the solution in step (2) to obtain slurry one by pre-dispersing. The pre-dispersing time is 30 min, the pre-dispersing speed is 100 rpm, and the solid content in the slurry is 60%.
[0060] Step 4: The slurry one obtained in step (3) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry two. The grinding speed is 1200 rpm, and the grinding time is 6h;
[0061] Step 5: Add the weighed indium oxide powder in step (1), 500g of polyvinylpyrrolidone dispersant and 3500g of pure water to the slurry two and stir to pre-disperse to obtain slurry three. The mass of the polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the indium oxide, cerium oxide, tantalum oxide, titanium oxide powder and holmium oxide powder; the dispersing speed is 100 rpm, the dispersing time is 40 min, and the solid content in the slurry is 65%.
[0062] Step 6: The slurry obtained in step (5) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry four, wherein the grinding speed is 1200 rpm and the grinding time is 10 h;
[0063] Step 7: A binder is added to the slurry four obtained in step (6) for pre-dispersion, the pre-dispersion time is 30 min, and the dispersion speed is 100 rpm; the obtained slurry is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry five, wherein the grinding time is 2 h and the grinding speed is 1200 rpm, and the binder accounts for 10% of the total mass of the added powder and binder.
[0064] Step 8: The slurry five obtained in step (7) is pumped into a co-current spray drying tower for spray granulation, and then mixed and sieved to obtain the precursor of the indium cerium tantalum titanium holmium oxide target material. The outlet air temperature is 70°C, and the atomizer frequency is 120 Hz.
[0065] Step 9: The precursor prepared in step (8) is sequentially subjected to die pressing and cold isostatic pressing to obtain a green compact of the target material, wherein the pressure during die pressing of the target material is 90 Mpa, and the pressure holding time is 120 s; the pressure during cold isostatic pressing is 350 Mpa, and the pressure holding time is 120 s.
[0066] Step 10: The indium cerium tantalum titanium holmium oxide target blank obtained in step (9) is subjected to heat treatment, the temperature is controlled at 550°C for degreasing treatment (the holding time is 2.5 hours, and the heating rate is 0.15°C / min), then cooled to room temperature, oxygen is introduced, and the sintering temperature is increased to perform sintering to obtain the indium cerium tantalum titanium holmium oxide target material (the sintering temperature is 1380°C, the heating rate is 0.1°C / min, and the holding time is 12 h).
[0067] The relative density of the target material is 99.15%, and the conductivity of the target material is 815 s / cm.
[0068] Sputtering film experiment
[0069] (1) The target material is placed in a culture dish containing acetone, anhydrous ethanol and deionized water and ultrasonically cleaned for 15 min to remove grease and particles and other contaminants on the surface of the substrate, and then dried with a ear sucker; (2) The target material is placed on the workpiece table in the coating chamber; (3) First, use a mechanical pump to pump the chamber to a limit pressure of 10 Pa, then use a molecular pump to pump the chamber to a pressure of 2.66*10 -6 Pa, (4) Set the target base distance to 15 mm, the substrate pressure to 2.6*10 -6 Pa, the sputtering pressure to 1.6 Pa, Ar:O2 to 1:1, the deposition temperature to 500°C, the sputtering power to 100 W, and the sputtering time to 50 min.
[0070] The measured migration rate of the sputtered film is 75.91 cm2 (v.s), carrier concentration of 1.58 cm -3 , film hardness of 11.81 Mpa.
[0071] Example 4
[0072] Step 1: weigh 9350g of indium oxide powder, 150g of cerium oxide powder, 170g of tantalum oxide powder, and 200g of titanium oxide and 130g of holmium oxide powder;
[0073] Step 2: add 1500g of pure water and polyvinylpyrrolidone dispersant to the slurry barrel. The polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder.
[0074] Step 3: add the weighed cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder in step (1) to the solution in step (2) to perform pre-dispersion to obtain slurry one. The pre-dispersion time is 30 min, the pre-dispersion speed is 100 rpm, and the solid content in the slurry is 60%.
[0075] Step 4: the slurry one obtained in step (3) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry two. The grinding speed is 1200 rpm, and the grinding time is 6h;
[0076] Step 5: add the weighed indium oxide powder in step (1) and 500g of polyvinylpyrrolidone dispersant and 3500g of pure water to the slurry two for stirring and pre-dispersion to obtain slurry three. The mass of the polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the indium oxide, cerium oxide, tantalum oxide, titanium oxide powder and holmium oxide powder; the dispersion speed is 100 rpm, the dispersion time is 40 min, and the solid content in the slurry is 65%.
[0077] Step 6: the slurry three obtained in step (5) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry four. The grinding speed is 1200 rpm, and the grinding time is 10h;
[0078] Step 7: add a binder to the slurry four obtained in step (6) for pre-dispersion, the pre-dispersion time is 30 min, and the dispersion speed is 100 rpm; the obtained slurry is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry five. The grinding time is 2h, the grinding speed is 1200 rpm, and the binder accounts for 10% of the total mass of the added powder and the binder.
[0079] Step 8: the slurry five obtained in step (7) is pumped into a co-current spray drying tower for spray granulation, mixing and screening to obtain the precursor of the indium cerium tantalum titanium holmium target material. The air outlet temperature is 70℃, and the atomizer frequency is 120Hz.
[0080] Step 9: The precursor prepared in step (8) is subjected to die pressing and cold isostatic pressing in sequence to obtain a green compact of the target material, wherein the pressure during die pressing of the target material is 90 MPa, and the pressure during cold isostatic pressing is 350 MPa, and the holding time is 120 s.
[0081] Step 10: The indium cerium tantalum titanium holmium oxide target blank obtained in step (9) is subjected to heat treatment, and the temperature is controlled at 550 ℃ for debinding treatment (the holding time is 2.5 h, and the heating rate is 0.15 ℃ / min). Then, the target blank is cooled to room temperature, oxygen is introduced, and the sintering temperature is increased to obtain the indium cerium tantalum titanium holmium oxide target material (the sintering temperature is 1380 ℃, the heating rate is 0.1 ℃ / min, and the holding time is 12 h).
[0082] The relative density of the target material is 99.18%, and the conductivity of the target material is 871 s / cm.
[0083] Sputtering film experiment
[0084] (1) The target material is placed in a culture dish containing acetone, anhydrous ethanol and deionized water, and is ultrasonically cleaned for 15 min to remove grease and particles and other contaminants on the surface of the substrate, and is then dried with an ear ball; (2) The target material is placed on the workpiece table in the film coating chamber; (3) The chamber is first pumped to a limit pressure of 10 Pa by a mechanical pump, and then pumped to a pressure of 2.66*10 -6 Pa or lower by a molecular pump, (4) The target material is set to a distance of 15 mm, the substrate pressure is 2.6*10 -6 Pa, the sputtering pressure is 1.6 Pa, Ar:O2 is 1:1, the deposition temperature is 500 ℃, the sputtering power is 100 W, and the sputtering time is 50 min.
[0085] The measured sputtering film has a mobility of 80.72 cm 2 / (v.s), a carrier concentration of 1.32 cm -3 , and a film hardness of 12.08 MPa.
[0086] Example 5
[0087] Step 1: 9450 g of indium oxide powder, 120 g of cerium oxide powder, 150 g of tantalum oxide powder, 190 g of titanium oxide powder and 90 g of holmium oxide powder are weighed for use.
[0088] Step 2: 1500 g of pure water and polyvinylpyrrolidone dispersant are added to the slurry barrel. The polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder.
[0089] Step 3: The cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder weighed in step (1) are added to the solution of step (2) to obtain slurry one by pre-dispersing, wherein the pre-dispersing time is 30 min, the pre-dispersing rotation speed is 100 rpm, and the solid content in the slurry is 60%.
[0090] Step 4: The slurry one obtained in step (3) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry two, wherein the grinding rotation speed is 1200 rpm, and the grinding time is 6 h.
[0091] Step 5: The indium oxide powder weighed in step (1) and 500 g of polyvinylpyrrolidone dispersant and 3500 g of pure water are added to the slurry two for stirring and pre-dispersing to obtain slurry three, wherein the mass of the polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the indium oxide, cerium oxide, tantalum oxide, titanium oxide powder and holmium oxide powder; the dispersing rotation speed is 100 rpm, the dispersing time is 40 min, and the solid content in the slurry is 65%.
[0092] Step 6: The slurry three obtained in step (5) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry four, wherein the grinding rotation speed is 1200 rpm, and the grinding time is 10 h.
[0093] Step 7: The binder is added to the slurry four obtained in step (6) for pre-dispersing, the pre-dispersing time is 30 min, and the dispersing rotation speed is 100 rpm; the obtained slurry is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry five, wherein the grinding time is 2 h, the grinding rotation speed is 1200 rpm, and the binder accounts for 10% of the total mass of the added powder and the binder.
[0094] Step 8: The slurry five obtained in step (7) is pumped into a co-current spray drying tower for spray granulation, then mixed and sieved to obtain the precursor of the indium cerium tantalum titanium holmium oxide target material. The air outlet temperature is 70°C, and the atomizer frequency is 120 Hz.
[0095] Step 9: The precursor prepared in step (8) is sequentially subjected to die pressing and cold isostatic pressing to obtain a green compact of the target material, wherein the pressure during die pressing of the target material is 90 Mpa, and the pressure holding time is 120 s; the pressure during cold isostatic pressing is 350 Mpa, and the pressure holding time is 120 s.
[0096] Step 10: The indium cerium tantalum titanium holmium oxide target blank obtained in step (9) is subjected to heat treatment, the temperature is controlled at 550°C for degreasing treatment (the holding time is 2.5 hours, and the heating rate is 0.15°C / min), then cooled to room temperature, oxygen is introduced, the sintering temperature is increased to obtain a sintered indium cerium tantalum titanium holmium oxide target material (the sintering temperature is 1380°C, the heating rate is 0.1°C / min, and the holding time is 12 h).
[0097] The relative density of the target material is 99.02% and the conductivity of the target material is 825 s / cm.
[0098] Sputtering film experiment
[0099] (1) Put the target material into a culture dish containing acetone, anhydrous ethanol and deionized water, and ultrasonically clean for 15 min to remove grease and particles and other contaminants on the surface of the substrate, and then dry with a ear ball; (2) Put the target material on the workpiece table in the film coating chamber; (3) First use a mechanical pump to pump the pressure in the chamber to a limit pressure of 10 Pa, then use a molecular pump to pump the pressure in the chamber to 2.66*10 -6 Pa or lower; (4) Set the target standoff distance to 15 mm, the substrate pressure to 2.6*10 -6 Pa, the sputtering pressure to 1.6 Pa, Ar:O2=1:1, the deposition temperature to 500℃, the sputtering power to 100 W, and the sputtering time to 50 min.
[0100] The measured sputtering film has a mobility of 72.07 cm 2 / (v.s), a carrier concentration of 2.37 cm -3 , and a film hardness of 11.93 Mpa.
[0101] Example 6
[0102] Step 1: Weigh 9570g of indium oxide powder, 90g of cerium oxide powder, 110g of tantalum oxide powder, 160g of titanium oxide and 70g of holmium oxide powder for standby;
[0103] Step 2: Add 1500g of pure water and polyvinylpyrrolidone dispersant to the slurry barrel. The polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder.
[0104] Step 3: Add the weighed cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder in step (1) to the solution in step (2) to obtain slurry one by pre-dispersing. The pre-dispersing time is 30 min, the pre-dispersing speed is 100 rpm, and the solid content in the slurry is 60%.
[0105] Step 4: Pump the slurry one obtained in step (3) into a sand mill with a pneumatic diaphragm pump for grinding to obtain slurry two. The grinding speed is 1200 rpm and the grinding time is 6h;
[0106] Step 5: Put the weighed indium oxide powder in step (1) and polyvinylpyrrolidone dispersant 500 g and pure water 3500 g into slurry two for pre-dispersion, to obtain slurry three. The mass of polyvinylpyrrolidone dispersant accounts for 5% of the total mass of indium oxide, cerium oxide, tantalum oxide, titanium oxide powder and holmium oxide powder; the dispersion rotation speed is 100 rpm, the dispersion time is 40 min, and the solid content in the slurry is 65%.
[0107] Step 6: The slurry three obtained in step (5) is pumped into a sand mill with a pneumatic diaphragm pump for grinding to obtain slurry four. The grinding rotation speed is 1200 rpm, and the grinding time is 10 h;
[0108] Step 7: Add a binder to the slurry four obtained in step (6) for pre-dispersion, the pre-dispersion time is 30 min, and the dispersion rotation speed is 100 rpm; the obtained slurry is pumped into a sand mill for grinding with a pneumatic diaphragm pump to obtain slurry five. The grinding time is 2 h, and the grinding rotation speed is 1200 rpm. The binder accounts for 10% of the total mass of the added powder and the binder.
[0109] Step 8: Pump the slurry five obtained in step (7) into a co-current spray drying tower for spray granulation, then mix and sieve to obtain the precursor of the indium cerium tantalum titanium holmium oxide target material. The outlet air temperature is 70℃, and the atomizer frequency is 120 Hz.
[0110] Step 9: The precursor prepared in step (8) is sequentially subjected to die pressing and cold isostatic pressing to obtain a green compact of the target material. The die pressing pressure of the target material is 90 Mpa, and the pressure holding time is 120 s; the cold isostatic pressing pressure is 350 Mpa, and the pressure holding time is 120 s.
[0111] Step 10: Heat treat the indium cerium tantalum titanium holmium oxide target blank obtained in step (9) at a temperature of 550℃ for degreasing treatment (heat preservation time 2.5 hours, heating rate 0.15℃ / min), then cool to room temperature, introduce oxygen, and increase the sintering temperature for sintering to obtain the indium cerium tantalum titanium holmium oxide target material (sintering temperature is 1380℃, heating rate is 0.1℃ / min, and heat preservation time is 12 h).
[0112] The relative density of the target material is 98.91%, and the conductivity of the target material is 798 s / cm.
[0113] Sputtering film experiment
[0114] (1) Put the target material into a culture dish containing acetone, anhydrous ethanol and deionized water, and ultrasonically clean for 15 min to remove grease and particles and other contaminants on the surface of the substrate, and then dry with a suction ball; (2) Put the target material on the workpiece table in the coating chamber; (3) First, use a mechanical pump to pump the chamber to a limit pressure of 10 Pa, then use a molecular pump to pump the chamber to a pressure below 2.66*10 -6 Pa, (4) set the target base distance to 15 mm, the base pressure to 2.6*10 -6 Pa, the sputtering pressure to 1.6 Pa, Ar:O2=1:1, the deposition temperature to 500℃, the sputtering power to 100 W, and the sputtering time to 50 min.
[0115] The measured sputtering film mobility is 73.58 cm 2 / (v.s), the carrier concentration is 2.25 cm -3 , and the film hardness is 12.18 Mpa.
[0116] Example 7
[0117] Step 1: weigh 9720g of indium oxide powder, 80g of cerium oxide powder, 90g of tantalum oxide powder, 90g of titanium oxide and 20g of holmium oxide powder;
[0118] Step 2: Add 1500g of pure water and polyvinylpyrrolidone dispersant to the slurry barrel. The polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder.
[0119] Step 3: Add the weighed cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder in step (1) to the solution in step (2) and pre-disperse to obtain slurry one. The pre-dispersion time is 30 min, the pre-dispersion speed is 100 rpm, and the solid content in the slurry is 60%.
[0120] Step 4: Pump the slurry one obtained in step (3) into a sand mill with a pneumatic diaphragm pump for grinding to obtain slurry two. The grinding speed is 1200 rpm and the grinding time is 6h;
[0121] Step 5: Add the weighed indium oxide powder in step (1), 500g of polyvinylpyrrolidone dispersant and 3500g of pure water to the slurry two and stir to pre-disperse to obtain slurry three. The mass of the polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the indium oxide, cerium oxide, tantalum oxide, titanium oxide powder and holmium oxide powder; the dispersion speed is 100 rpm, the dispersion time is 40 min, and the solid content in the slurry is 65%.
[0122] Step 6: The slurry obtained in step (5) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry four, wherein the grinding speed is 1200 rpm and the grinding time is 10 h;
[0123] Step 7: A binder is added to the slurry four obtained in step (6) for pre-dispersion, the pre-dispersion time is 30 min, and the dispersion speed is 100 rpm; the obtained slurry is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry five, wherein the grinding time is 2 h and the grinding speed is 1200 rpm, and the binder accounts for 10% of the total mass of the added powder and binder.
[0124] Step 8: The slurry five obtained in step (7) is pumped into a co-current spray drying tower for spray granulation, and then mixed and sieved to obtain the precursor of the indium cerium tantalum titanium holmium oxide target material. The outlet air temperature is 70°C, and the atomizer frequency is 120 Hz.
[0125] Step 9: The precursor prepared in step (8) is sequentially subjected to die pressing and cold isostatic pressing to obtain a green compact of the target material, wherein the pressure during die pressing of the target material is 90 Mpa, and the pressure holding time is 120 s; the pressure during cold isostatic pressing is 350 Mpa, and the pressure holding time is 120 s.
[0126] Step 10: The indium cerium tantalum titanium holmium oxide target blank obtained in step (9) is subjected to heat treatment, the temperature is controlled at 550°C for degreasing treatment (the holding time is 2.5 hours, and the heating rate is 0.15°C / min), then cooled to room temperature, oxygen is introduced, and the sintering temperature is increased for sintering to obtain the indium cerium tantalum titanium holmium oxide target material (the sintering temperature is 1380°C, the heating rate is 0.1°C / min, and the holding time is 12 h).
[0127] The relative density of the target material is 98.89%, and the conductivity of the target material is 838 s / cm.
[0128] Sputtering film experiment
[0129] (1) Put the target into a culture dish containing acetone, anhydrous ethanol and deionized water, and ultrasonic clean for 15 min to remove grease and particles and other pollutants on the surface of the substrate, and then dry with a ear ball; (2) Put the target on the workpiece table in the coating chamber; (3) First, use a mechanical pump to pump the chamber pressure to a limit pressure of 10 Pa, then use a molecular pump to pump the chamber pressure to below 2.66*10 -6 Pa, (4) Set the target base distance to 15 mm, the substrate pressure to 2.6*10 -6 Pa, the sputtering pressure to 1.6 Pa, Ar:O2 to 1:1, the deposition temperature to 500°C, the sputtering power to 100 W, and the sputtering time to 50 min.
[0130] The measured migration rate of the sputtered film is 71.89 cm2 (v.s), carrier concentration of 2.42 cm -3 , film hardness of 11.47 Mpa.
[0131] Example 8
[0132] Step 1: weigh 9870 g of indium oxide powder, 40 g of cerium oxide powder, 30 g of tantalum oxide powder, 50 g of titanium oxide and 10 g of holmium oxide powder;
[0133] Step 2: add 1500 g of pure water and polyvinylpyrrolidone dispersant to the slurry barrel. The polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder.
[0134] Step 3: add the weighed cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder in step (1) to the solution in step (2) to perform pre-dispersion to obtain slurry one. The pre-dispersion time is 30 min, the pre-dispersion speed is 100 rpm, and the solid content in the slurry is 60%.
[0135] Step 4: the slurry one obtained in step (3) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry two. The grinding speed is 1200 rpm, and the grinding time is 6h;
[0136] Step 5: add the weighed indium oxide powder in step (1) and 500 g of polyvinylpyrrolidone dispersant and 3500 g of pure water to the slurry two for stirring and pre-dispersion to obtain slurry three. The mass of the polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the indium oxide, cerium oxide, tantalum oxide, titanium oxide powder and holmium oxide powder; the dispersion speed is 100 rpm, the dispersion time is 40 min, and the solid content in the slurry is 65%.
[0137] Step 6: the slurry three obtained in step (5) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry four. The grinding speed is 1200 rpm, and the grinding time is 10h;
[0138] Step 7: add a binder to the slurry four obtained in step (6) for pre-dispersion, the pre-dispersion time is 30 min, and the dispersion speed is 100 rpm; the obtained slurry is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry five. The grinding time is 2h, the grinding speed is 1200 rpm, and the binder accounts for 10% of the total mass of the added powder and the binder.
[0139] Step 8: the slurry five obtained in step (7) is pumped into a co-current spray drying tower for spray granulation, then mixed and sieved to obtain the precursor of the indium cerium tantalum titanium holmium target material. The air outlet temperature is 70℃, and the atomizer frequency is 120 Hz.
[0140] Step 9: The precursor prepared in step (8) is subjected to die pressing and cold isostatic pressing in sequence to obtain a green body of the target material, wherein the pressure during die pressing of the target material is 90 MPa, and the pressure during cold isostatic pressing is 350 MPa, and the pressure is maintained for 120 s.
[0141] Step 10: The indium cerium tantalum titanium holmium oxide target blank obtained in step (9) is subjected to heat treatment, and the temperature is controlled at 550 ℃ for debinding treatment (the holding time is 2.5 h, and the heating rate is 0.15 ℃ / min). Then, the target blank is cooled to room temperature, oxygen is introduced, and the sintering temperature is increased to obtain the indium cerium tantalum titanium holmium oxide target material (the sintering temperature is 1380 ℃, the heating rate is 0.1 ℃ / min, and the holding time is 12 h).
[0142] The relative density of the target material is 98.97%, and the conductivity of the target material is 824 s / cm.
[0143] Sputtering film experiment
[0144] (1) The target material is placed in a culture dish containing acetone, anhydrous ethanol and deionized water, and is ultrasonically cleaned for 15 min to remove grease and particles and other contaminants on the surface of the substrate, and is then dried with an ear ball; (2) The target material is placed on the workpiece table in the film coating chamber; (3) The chamber is first pumped to a limit pressure of 10 Pa by a mechanical pump, and then pumped to a pressure of 2.66*10 -6 Pa or lower by a molecular pump, (4) The target material is set to a distance of 15 mm, the substrate pressure is 2.6*10 -6 Pa, the sputtering pressure is 1.6 Pa, Ar:O2 is 1:1, the deposition temperature is 500 ℃, the sputtering power is 100 W, and the sputtering time is 50 min.
[0145] The measured sputtering film has a mobility of 70.11 cm 2 / (v.s), a carrier concentration of 2.64 cm -3 , and a film hardness of 12.72 MPa.
[0146] Comparative Example 1
[0147] Step 1: 8990 g of indium oxide powder, 250 g of cerium oxide powder, 230 g of tantalum oxide powder, 250 g of titanium oxide and 280 g of holmium oxide are weighed for use.
[0148] Step 2: 1500 g of pure water and polyvinylpyrrolidone dispersant are added to the slurry barrel. The polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the cerium oxide, tantalum oxide powder, titanium oxide powder and holmium oxide powder.
[0149] Step 3: The cerium oxide, tantalum oxide powder and titanium oxide powder weighed in step (1) are added to the solution of step (2) to pre-disperse to obtain slurry one. The pre-dispersing time is 30 min, the pre-dispersing rotation speed is 100 rpm, and the solid content in the slurry is 50%.
[0150] Step 4: The slurry one obtained in step (3) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry two. The grinding rotation speed is 1200 rpm, and the grinding time is 6 h.
[0151] Step 5: The indium oxide powder weighed in step (1) and 500 g of polyvinylpyrrolidone dispersant and 3500 g of pure water are added to the slurry two for stirring and pre-dispersing to obtain slurry three. The mass of the polyvinylpyrrolidone dispersant accounts for 5% of the total mass of the indium oxide, cerium oxide, tantalum oxide and titanium oxide powders. The dispersing rotation speed is 100 rpm, the dispersing time is 40 min, and the solid content in the slurry is 65%.
[0152] Step 6: The slurry three obtained in step (5) is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry four. The grinding rotation speed is 1200 rpm, and the grinding time is 10 h.
[0153] Step 7: The binder is added to the slurry four obtained in step (6) for pre-dispersing. The pre-dispersing time is 30 min, and the dispersing rotation speed is 100 rpm. The obtained slurry is pumped into a sand mill by a pneumatic diaphragm pump for grinding to obtain slurry five. The grinding time is 2 h, and the grinding rotation speed is 1200 rpm. The binder accounts for 10% of the total mass of the added powders and the binder.
[0154] Step 8: The slurry five obtained in step (7) is pumped into a co-current spray drying tower for spray granulation, mixing and sieving to obtain the precursor of the indium cerium tantalum titanium holmium oxide target material.
[0155] Step 9: The indium cerium tantalum titanium holmium oxide target precursor obtained in step (8) is subjected to die pressing and cold isostatic pressing to obtain an indium cerium tantalum titanium holmium oxide target blank.
[0156] Step 10: The indium cerium tantalum titanium holmium oxide target blank obtained in step (9) is subjected to heat treatment. The temperature is controlled at 500℃ for degreasing treatment (the holding time is 2 hours, and the heating rate is 0.1℃ / min). Then, the temperature is cooled to room temperature, oxygen is introduced, and the sintering temperature is increased to obtain the sintered indium cerium tantalum titanium holmium oxide target material (the sintering temperature is 1400℃, the heating rate is 0.2℃ / min, and the holding time is 8 h). The sintered indium cerium tantalum titanium holmium oxide target material is obtained.
[0157] The relative density of the target material is 97.56%, and the conductivity of the target material is 324 s / cm.
[0158] Sputtering experiment
[0159] (1) Put the target into a culture dish containing acetone, anhydrous ethanol and deionized water, and ultrasonic clean for 15 min to remove grease and particles on the surface of the substrate, and then dry with a ear ball; (2) Put the target on the workpiece table in the coating chamber; (3) First, use a mechanical pump to pump the chamber pressure to the limit pressure 10 Pa, then use a molecular pump to pump the chamber pressure to 2.66*10 -6 Pa, (4) Set the target base distance to 15 mm, the base pressure to 2.6*10 -6 Pa, the sputtering pressure to 1.6 Pa, Ar:O2=1:1, the deposition temperature to 500℃, the sputtering power to 100 W, and the sputtering time to 50 min.
[0160] The measured sputtering film mobility is 52.08 cm 2 / (v.s), the carrier concentration is 4.28 cm -3 , and the film hardness is 6.68 Mpa.
[0161] Comparative example 2
[0162] The mass of the added indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder and holmium oxide powder in this comparative example is 8990 g, 250 g, 230 g, 250 g and 280 g respectively, and the other conditions are the same as those in example 2.
[0163] Comparative example 3
[0164] The mass of the added indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder and holmium oxide powder in this comparative example is 8920 g, 280 g, 260 g, 270 g and 270 g respectively, and the other conditions are the same as those in example 3.
[0165] Comparative example 4
[0166] The mass of the added indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder and holmium oxide powder in this comparative example is 8850 g, 310 g, 290 g, 290 g and 260 g respectively, and the other conditions are the same as those in example 4.
[0167] Comparative example 5
[0168] The mass of the added indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder and holmium oxide powder in this comparative example is 8810 g, 310 g, 310 g, 320 g and 250 g respectively, and the other conditions are the same as those in example 5.
[0169] Comparative example 6
[0170] Comparative Example 2 The comparative example is the same as Example 1 except that the mass of indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder, and holmium oxide powder added is 8750 g, 360 g, 280 g, 310 g, and 300 g, respectively.
[0171] Comparative Example 3
[0172] Comparative Example 3 The comparative example is the same as Example 2 except that the mass of indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder, and holmium oxide powder added is 8720 g, 370 g, 290 g, 240 g, and 380 g, respectively.
[0173] Comparative Example 4
[0174] Comparative Example 4 The comparative example is the same as Example 3 except that the mass of indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder, and holmium oxide powder added is 8200 g, 400 g, 350 g, 550 g, and 500 g, respectively.
[0175] Comparative Example 5
[0176] Comparative Example 5 The comparative example is the same as Example 6 except that hexavalent tungsten is used instead of pentavalent tantalum; the oxide powder composition is:
[0177] 9570 g of indium oxide powder, 90 g of cerium oxide powder, 110 g of tungsten oxide powder, 160 g of titanium oxide, and 70 g of holmium oxide.
[0178] Comparative Example 6
[0179] Comparative Example 6 The comparative example is the same as Example 6 except that tetravalent zirconium is used instead of tetravalent titanium; the oxide powder composition is:
[0180] 9570 g of indium oxide powder, 90 g of cerium oxide powder, 110 g of tantalum oxide powder, 160 g of zirconium oxide, and 70 g of holmium oxide.
[0181] Comparative Example 7
[0182] Comparative Example 7 The comparative example is the same as Example 6 except that tetravalent cerium is used instead of tetravalent titanium; the oxide powder composition is:
[0183] 9570 g of indium oxide powder, 250 g of cerium oxide powder, 110 g of tantalum oxide powder, and 70 g of holmium oxide.
[0184] Comparative Example 8
[0185] Comparative Example 8 The comparative example is the same as Example 6 except that trivalent gallium is used instead of trivalent holmium; the oxide powder composition is:
[0186] 9570 g of indium oxide powder, 90 g of cerium oxide powder, 110 g of tantalum oxide powder, 160 g of titanium oxide, and 70 g of gallium oxide.
[0187] All experimental data of the above examples and comparative examples are shown in Table 1 below:
[0188] Table 1 Test results
[0189]
[0190]
[0191] Result analysis:
[0192] 1. From the comparison results of Examples 1-8 and Comparative Examples 1-8 above, it can be seen that the composition ratio of the indium oxide doped titanium-tantalum-cerium-holmium target material of the present application has a more critical effect on the performance. In the case where the mass ratio of indium oxide is less than 90% and the remaining components are not within the corresponding range, the performance of the obtained target material is significantly reduced.
[0193] 2. From the comparison results of Examples 1-8 and Comparative Examples 9-12 above, it can be seen that the composition of the indium oxide doped titanium-tantalum-cerium-holmium target material of the present application has a more critical effect on the performance. After changing one of the oxide components, the performance of the obtained target material is significantly reduced.
[0194] 3. From the comparison results of Comparative Examples 1-8 and Comparative Examples 9-12 above, it can be seen that in the case of changing the oxide components and the ratio in the present application, the performance of the obtained target material is lower than that in the case of changing only one oxide component in the present application without changing the ratio.
[0195] The above examples are the preferred embodiments of the present application, but the embodiments of the present application are not limited by the above examples, and any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present application should be equivalent replacement methods, and are all included in the protection scope of the present application.
Claims
1. An indium cerium tantalum titanium holmium oxide target material, characterized by, The molar ratio of indium, cerium, tantalum, titanium, and holmium in the target material is 66.3-71.1:0.232-1.163:0.136-0.905:0.625-2.5:0.053-1.058; The preparation method of the indium cerium tantalum titanium holmium oxide target material specifically comprises: dispersing, grinding, and drying indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder, and holmium oxide powder in water to obtain a mixed powder; and performing cold isostatic pressing and heating, degreasing, and sintering after die pressing to obtain the target material. The preparation method of the mixed powder specifically comprises: Step 1: adding cerium oxide powder, tantalum oxide powder, titanium oxide powder, and holmium oxide powder into pure water containing a first dispersant to obtain slurry one; Step 2: grinding slurry one in a sand mill by using a pneumatic diaphragm pump to obtain slurry two; Step 3: adding indium oxide powder and a second dispersant into slurry two to obtain slurry three; Step 4: grinding slurry three in a sand mill by using a pneumatic diaphragm pump to obtain slurry four; Step 5: adding a binder into slurry four, mixing, and then grinding the slurry in a sand mill by using a pneumatic diaphragm pump to obtain slurry five; Step 6: spraying slurry five into a co-current spray drying tower, performing spray granulation, mixing, and sieving to obtain the mixed powder.
2. The indium cerium tantalum titanium holmium oxide target according to claim 1, wherein The first dispersant and the second dispersant are each independently selected from one or more of polyvinylpyrrolidone, sodium dodecylbenzenesulfonate, a polycarboxylic acid compound, a polyvinyl acetate salt, or sodium cetylbenzenesulfonate.
3. The indium cerium tantalum titanium holmium oxide target of claim 1, wherein The binder accounts for 5-20% of the total mass of the added indium oxide powder, cerium oxide powder, tantalum oxide powder, titanium oxide powder, and holmium oxide powder and the binder; and the binder is one or both of a mixture of polyvinyl alcohol and polyethylene glycol, polyvinyl alcohol, or polyvinyl butyral.
4. The indium cerium tantalum titanium holmium oxide target of claim 1, wherein The sintering temperature is 1100-1500°C, the heating rate is 0.1-0.5 / min, and the holding time is 8-12 h.
Citation Information
Patent Citations
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