Alumina target material and preparation method thereof

Abstract

The present invention discloses a method for preparing an alumina target material, comprising the steps of ball-milling alumina and a ball-milling solution at a weight ratio of 5:2, pressing the alumina into a mold, and then sintering the alumina target material to obtain the alumina target material. The alumina target material of the present invention is obtained by subjecting alumina to a ball-milling solution, pressing the alumina into a mold, and then sintering the alumina target material to obtain the alumina target material. The density and transparency of the product are improved, and the product has significant acid corrosion resistance and stability.

Description

Technical Field

[0001] The present invention relates to the technical field of target materials, and in particular to an aluminum oxide target material and a preparation method thereof. Background Art

[0002] As an important coating material, targets are widely used in integrated circuits, flat-panel displays, and optical devices. Target preparation methods include smelting and powder metallurgy. Powder metallurgy can directly produce porous, semi-dense, or fully dense products with unique chemical compositions, mechanical, and physical properties. Therefore, powder metallurgy technology has become the primary method for preparing targets.

[0003] The existing alumina target material has poor density and poor transparency. It is difficult to coordinate and improve the density and transparency of the product. In addition, the product has poor acid corrosion resistance and stability, which limits the product's efficiency. Summary of the Invention

[0004] In view of the defects of the prior art, the purpose of the present invention is to provide an alumina target and a preparation method thereof to solve the problems raised in the above background technology.

[0005] The present invention solves the technical problem by adopting the following technical solutions:

[0006] The present invention provides a method for preparing an aluminum oxide target, comprising the following steps:

[0007] Alumina and ball milling liquid are ball milled in a weight ratio of 5:2. After the ball milling is completed, the target is pressed into a mold and then sintered to obtain an alumina target.

[0008] The ball milling solution includes silane coupling agent KH550, modified chitosan agent and sodium alginate solution; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate solution is 2:5:7.

[0009] Preferably, the ball milling speed of the ball milling treatment is 1000-1500 r / min, and the ball milling time is 2 hours.

[0010] Preferably, the pressing pressure is 35-40 MPa, and the pressing time is 2 h.

[0011] Preferably, the sintering temperature of the improved sintering is 1150-1200° C., and the sintering time is 1 hour.

[0012] Preferably, the preparation method of the modified chitosan agent is:

[0013] Immerse 4-7 parts of hydroxyapatite in 5-8 parts of yttrium nitrate solution, then add 1-3 parts of sodium carboxymethyl cellulose and 1-2 parts of stearic acid, and mix and ball-mill at a speed of 1500 r / min for 2 hours. After the ball milling is completed, filter and dry to obtain a hydroxyapatite agent;

[0014] Chitosan, water and citric acid are uniformly stirred in a weight ratio of 3:7:1, and then hydroxyapatite agent accounting for 4-7% of the total amount of chitosan is added thereto, and the mixture is further stirred thoroughly, and then filtered and dried to obtain a modified chitosan agent.

[0015] Preferably, the mass fraction of the yttrium nitrate solution is 2-5%.

[0016] Preferably, the preparation method of the sodium alginate solution is:

[0017] Preheat the nano-silica at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is 2-5 times the total amount of the nano-silica, and then add a sodium alginate solution that is 10-15% of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

[0018] Preferably, the mass fraction of the dopamine hydrochloride solution is 2-5%; the mass fraction of the sodium alginate solution is 4-7%.

[0019] The present invention also provides an aluminum oxide target material prepared by a method for preparing the aluminum oxide target material.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] The alumina target material of the present invention is prepared by treating alumina with a ball milling liquid, then putting the treated alumina into a mold, and sintering and improving the alumina target material. The density and transparency of the product are improved in a coordinated manner, and the acid corrosion resistance and stability of the product are significantly improved. The ball milling liquid is prepared by blending a silane coupling agent KH550, a modified chitosan agent and a sodium alginate liquid. At the same time, the hydroxyapatite in the modified chitosan agent is treated with a specific process and combined with chitosan, water and citric acid raw materials in a blending system. The sodium alginate liquid is further blended with nano-silicon dioxide, dopamine hydrochloride solution and sodium alginate to prepare the blending system. Through the improved coordination between the raw materials, the product performance is further improved. DETAILED DESCRIPTION

[0022] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0023] A method for preparing an aluminum oxide target material in this embodiment includes the following steps:

[0024] Alumina and ball milling liquid are ball milled in a weight ratio of 5:2. After the ball milling is completed, the target is pressed into a mold and then sintered to obtain an alumina target.

[0025] The ball milling solution includes silane coupling agent KH550, modified chitosan agent and sodium alginate solution; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate solution is 2:5:7.

[0026] The ball milling speed of the ball milling treatment in this embodiment is 1000-1500 r / min, and the ball milling is 2 h.

[0027] The pressing pressure of this embodiment is 35-40 MPa, and the pressing time is 2 hours.

[0028] The improved sintering temperature of this embodiment is 1150-1200° C., and the sintering time is 1 hour.

[0029] The preparation method of the modified chitosan agent of this embodiment is:

[0030] Immerse 4-7 parts of hydroxyapatite in 5-8 parts of yttrium nitrate solution, then add 1-3 parts of sodium carboxymethyl cellulose and 1-2 parts of stearic acid, and mix and ball-mill at a speed of 1500 r / min for 2 hours. After the ball milling is completed, filter and dry to obtain a hydroxyapatite agent;

[0031] Chitosan, water and citric acid are uniformly stirred in a weight ratio of 3:7:1, and then hydroxyapatite agent accounting for 4-7% of the total amount of chitosan is added thereto, and the mixture is further stirred thoroughly, and then filtered and dried to obtain a modified chitosan agent.

[0032] The mass fraction of the yttrium nitrate solution in this embodiment is 2-5%.

[0033] The preparation method of the sodium alginate solution of this embodiment is:

[0034] Preheat the nano-silica at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is 2-5 times the total amount of the nano-silica, and then add a sodium alginate solution that is 10-15% of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

[0035] The mass fraction of the dopamine hydrochloride solution in this embodiment is 2-5%; the mass fraction of the sodium alginate solution is 4-7%.

[0036] The aluminum oxide target material is prepared by a method for preparing an aluminum oxide target material in this embodiment.

[0037] Example 1.

[0038] A method for preparing an aluminum oxide target material in this embodiment includes the following steps:

[0039] Alumina and ball milling liquid are ball milled in a weight ratio of 5:2. After the ball milling is completed, the target is pressed into a mold and then sintered to obtain an alumina target.

[0040] The ball milling solution includes silane coupling agent KH550, modified chitosan agent and sodium alginate solution; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate solution is 2:5:7.

[0041] The ball milling process in this embodiment was performed at a ball milling speed of 1000 r / min and for 2 h.

[0042] The pressing pressure of this embodiment is 35 MPa and the pressing time is 2 h.

[0043] The improved sintering temperature of this embodiment is 1150° C. and the sintering time is 1 hour.

[0044] The preparation method of the modified chitosan agent of this embodiment is:

[0045] 4 parts of hydroxyapatite were immersed in 5 parts of yttrium nitrate solution, and then 1 part of sodium carboxymethyl cellulose and 1 part of stearic acid were added and mixed and ball-milled at a speed of 1500 r / min for 2 hours. After the ball milling was completed, the mixture was filtered and dried to obtain a hydroxyapatite agent;

[0046] Chitosan, water and citric acid were mixed evenly in a weight ratio of 3:7:1, and then hydroxyapatite agent accounting for 4% of the total amount of chitosan was added thereto, and the mixture was continued to be fully stirred, and then filtered and dried to obtain a modified chitosan agent.

[0047] The mass fraction of the yttrium nitrate solution in this embodiment is 2%.

[0048] The preparation method of the sodium alginate solution of this embodiment is:

[0049] Preheat the nano-silica at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is twice the total amount of the nano-silica, and then add a sodium alginate solution that is 10% of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

[0050] The mass fraction of the dopamine hydrochloride solution in this embodiment is 2%; the mass fraction of the sodium alginate solution is 4%.

[0051] The aluminum oxide target material is prepared by a method for preparing an aluminum oxide target material in this embodiment.

[0052] Example 2.

[0053] A method for preparing an aluminum oxide target material in this embodiment includes the following steps:

[0054] Alumina and ball milling liquid are ball milled in a weight ratio of 5:2. After the ball milling is completed, the target is pressed into a mold and then sintered to obtain an alumina target.

[0055] The ball milling solution includes silane coupling agent KH550, modified chitosan agent and sodium alginate solution; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate solution is 2:5:7.

[0056] The ball milling process in this embodiment was performed at a ball milling speed of 1500 r / min and for 2 h.

[0057] The pressing pressure of this embodiment is 40 MPa and the pressing time is 2 h.

[0058] The improved sintering temperature of this embodiment is 1200° C. and the sintering time is 1 hour.

[0059] The preparation method of the modified chitosan agent of this embodiment is:

[0060] 7 parts of hydroxyapatite were immersed in 8 parts of yttrium nitrate solution, and then 3 parts of sodium carboxymethyl cellulose and 2 parts of stearic acid were added and mixed and ball-milled at a speed of 1500 r / min for 2 hours. After the ball milling was completed, the mixture was filtered and dried to obtain a hydroxyapatite agent;

[0061] Chitosan, water and citric acid were mixed evenly in a weight ratio of 3:7:1, and then hydroxyapatite agent accounting for 7% of the total amount of chitosan was added thereto, and the mixture was continued to be fully stirred, and then filtered and dried to obtain a modified chitosan agent.

[0062] The mass fraction of the yttrium nitrate solution in this embodiment is 5%.

[0063] The preparation method of the sodium alginate solution of this embodiment is:

[0064] Preheat the nano-silica at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is 5 times the total amount of the nano-silica, and then add a sodium alginate solution that is 15% of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

[0065] The mass fraction of the dopamine hydrochloride solution in this embodiment is 5%; the mass fraction of the sodium alginate solution is 7%.

[0066] The aluminum oxide target material is prepared by a method for preparing an aluminum oxide target material in this embodiment.

[0067] Example 3.

[0068] A method for preparing an aluminum oxide target material in this embodiment includes the following steps:

[0069] Alumina and ball milling liquid are ball milled in a weight ratio of 5:2. After ball milling, the target is pressed into a mold and then sintered to obtain an alumina target.

[0070] The ball milling solution includes silane coupling agent KH550, modified chitosan agent and sodium alginate solution; the mass ratio of the silane coupling agent KH550, modified chitosan agent and sodium alginate solution is 2:5:7.

[0071] The ball milling process in this embodiment was performed at a ball milling speed of 1250 r / min and the ball milling was performed for 2 h.

[0072] The pressing pressure of this embodiment is 37.5 MPa, and the pressing time is 2 h.

[0073] The improved sintering temperature of this embodiment is 1175° C., and the sintering time is 1 hour.

[0074] The preparation method of the modified chitosan agent of this embodiment is:

[0075] 5.5 parts of hydroxyapatite were immersed in 6.5 parts of yttrium nitrate solution, and then 2 parts of sodium carboxymethyl cellulose and 1.5 parts of stearic acid were added and mixed and ball-milled at a speed of 1500 r / min for 2 hours. After the ball milling was completed, the mixture was filtered and dried to obtain a hydroxyapatite agent;

[0076] Chitosan, water and citric acid were mixed evenly in a weight ratio of 3:7:1, and then hydroxyapatite agent accounting for 5% of the total amount of chitosan was added thereto, and the mixture was stirred thoroughly, filtered and dried to obtain a modified chitosan agent.

[0077] The mass fraction of the yttrium nitrate solution in this embodiment is 3.5%.

[0078] The preparation method of the sodium alginate solution of this embodiment is:

[0079] Preheat the nano-silica at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is 3.5 times the total amount of the nano-silica, and then add a sodium alginate solution that is 12.5% ​​of the total amount of the dopamine hydrochloride solution, and stir thoroughly to obtain a sodium alginate solution.

[0080] The mass fraction of the dopamine hydrochloride solution in this embodiment is 3.5%; the mass fraction of the sodium alginate solution is 5.5%.

[0081] The aluminum oxide target material is prepared by a method for preparing an aluminum oxide target material in this embodiment.

[0082] Comparative Example 1.

[0083] The difference from Example 3 is that no modified chitosan agent is added.

[0084] Comparative Example 2.

[0085] The difference from Example 3 is that no hydroxyapatite agent is added to the modified chitosan agent.

[0086] Comparative Example 3.

[0087] The difference from Example 3 is that the hydroxyapatite agent is replaced by hydroxyapatite raw material.

[0088] Comparative Example 4.

[0089] The difference from Example 3 is that the sodium alginate solution is replaced by water.

[0090] Comparative Example 5.

[0091] The difference from Example 3 is that the sodium alginate solution is prepared by a different method: no preheated nano-silicon dioxide is added.

[0092] The product performance tests of Examples 1-3 and Comparative Examples 1-5 are as follows:

[0093]

[0094] It can be seen from Comparative Examples 1-5 and Examples 1-3 that the density and transparency of the products of the present invention are improved in a coordinated manner, and the acid mist resistance stability of the products is significant; when no modified chitosan agent is added to the product and water is used instead of the sodium alginate solution, the performance of the product has a significant downward trend. At the same time, when no hydroxyapatite agent is added to the modified chitosan agent, the hydroxyapatite agent is replaced by a hydroxyapatite raw material, and the sodium alginate solution is prepared by a different method, the product performance has a downward trend. Although other modification methods can improve product performance, the improvement effect is not as significant as the modification method of the present invention.

[0095] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0096] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A method for preparing an alumina target, characterized in that: The following steps are involved: Alumina and ball milling liquid are ball milled in a weight ratio of 5:

2. After the ball milling is completed, the target is pressed into a mold and then sintered to obtain an alumina target. The ball milling solution includes a silane coupling agent KH550, a modified chitosan agent, and a sodium alginate solution; wherein the mass ratio of the silane coupling agent KH550, the modified chitosan agent, and the sodium alginate solution is 2:5:7; The improved sintering temperature is 1150-1200° C. and the sintering time is 1 hour; The preparation method of the modified chitosan agent is: Immerse 4-7 parts of hydroxyapatite in 5-8 parts of yttrium nitrate solution, then add 1-3 parts of sodium carboxymethyl cellulose and 1-2 parts of stearic acid, and mix and ball-mill at a speed of 1500 r / min for 2 hours. After the ball milling is completed, filter and dry to obtain a hydroxyapatite agent; Chitosan, water and citric acid were mixed in a weight ratio of 3:7:1, and then hydroxyapatite agent of 4-7% of the total amount of chitosan was added thereto, and the mixture was stirred thoroughly, and then filtered and dried to obtain a modified chitosan agent; The preparation method of the sodium alginate solution is: Preheat the nano-silica at 60° C. for 2 h, then add it to a dopamine hydrochloride solution that is 2-5 times the total amount of the nano-silica, and then add a sodium alginate solution that is 10-15% of the total amount of the dopamine hydrochloride solution, stir thoroughly, and obtain a sodium alginate solution.

2. The method for preparing an aluminum oxide target according to claim 1, wherein: The ball milling process is performed at a speed of 1000-1500 r / min for 2 hours.

3. The method for preparing an aluminum oxide target according to claim 2, wherein: The pressing pressure is 35-40 MPa, and the pressing time is 2 h.

4. The method for preparing an aluminum oxide target according to claim 1, wherein: The mass fraction of the yttrium nitrate solution is 2-5%.

5. The method for preparing an aluminum oxide target according to claim 1, wherein: The mass fraction of the dopamine hydrochloride solution is 2-5%; the mass fraction of the sodium alginate solution is 4-7%.

6. An alumina target prepared by the method for preparing an alumina target according to any one of claims 1 to 5.

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